阅读说明：本技术 粗褐煤蜡脱树脂的方法 (Method for removing resin from coarse lignite wax ) 是由 李晓峰 张翠清 张中华 芦海云 郭屹 苌亮 于 2020-03-17 设计创作，主要内容包括：本发明提供了一种一种粗褐煤蜡脱树脂的方法,其包括：步骤S1：将褐煤蜡颗粒融化,得到液体褐煤蜡；步骤S2：将所述液体褐煤蜡与有机溶剂混合,得到褐煤蜡溶液；步骤S3：将所述褐煤蜡溶液结晶,固液分离,得到固相和滤液；步骤S4：对步骤S3中所得的固相进行第一脱溶处理处理,得到褐煤蜡；步骤S5：对步骤S3中所得的滤液进行纳滤处理,得到纳滤后的浓缩液；步骤S6：对所述纳滤后的浓缩液进行第二脱溶处理,得到树脂。采用本发明的粗褐煤蜡脱树脂的方法得到的褐煤蜡产品不经过反复高温蒸煮,产品质量好,并且采用本发明的方法蒸汽和冷却水能耗降低,每年能节约大量的蒸汽消耗操作费用。(The invention provides a method for removing resin from coarse montan wax, which comprises the following steps: step S1: melting the montan wax particles to obtain liquid montan wax; step S2: mixing the liquid montan wax with an organic solvent to obtain a montan wax solution; step S3: crystallizing the montan wax solution, and carrying out solid-liquid separation to obtain a solid phase and a filtrate; step S4: performing first desolventizing treatment on the solid phase obtained in the step S3 to obtain montan wax; step S5: carrying out nanofiltration treatment on the filtrate obtained in the step S3 to obtain a nanofiltration concentrated solution; step S6: and carrying out second desolventizing treatment on the nanofiltration concentrated solution to obtain the resin. The lignite wax product obtained by the crude lignite wax deresination method of the invention is not subjected to repeated high-temperature cooking, the product quality is good, the energy consumption of steam and cooling water is reduced by the method of the invention, and a large amount of steam consumption operation cost can be saved every year.)

1. A method for deresination of crude montan wax, comprising:

step S1: melting the montan wax particles to obtain liquid montan wax;

step S2: mixing the liquid montan wax with an organic solvent to obtain a montan wax solution;

step S3: crystallizing the montan wax solution, and carrying out solid-liquid separation to obtain a solid phase and a filtrate;

step S4: performing first desolventizing treatment on the solid phase obtained in the step S3 to obtain montan wax;

step S5: carrying out nanofiltration treatment on the filtrate obtained in the step S3 to obtain a nanofiltration concentrated solution;

step S6: and carrying out second desolventizing treatment on the nanofiltration concentrated solution to obtain the resin.

2. The method according to claim 1, characterized in that in step S5, the nanofiltration is at a temperature of 30-80 ℃, preferably 40-60 ℃, and/or the nanofiltration is at a pressure of 2-4.5 MpaG.

3. The method as claimed in claim 1 or 2, wherein in step S5, the nanofiltration membrane has a molecular weight cut-off of 300-; and/or the concentration multiple of the concentrated solution after nanofiltration is 1-6 times, preferably 3-4 times.

4. The method according to any one of claims 1 to 3, wherein in step S1, the montan wax particles have a particle size of 6mm or less, a resin content of 20% or more, preferably 30% or more; and/or the melting temperature is 90-120 ℃, preferably 95-105 ℃.

5. The method according to any one of claims 1 to 4, wherein in step S2, the mass ratio of the liquid montan wax to the organic solvent is 1: (5-15), preferably 1: (5-10); and/or the temperature of the mixing is 60-110 ℃, preferably 60-80 ℃; and/or the organic solvent is at least one selected from C6-C20 aromatic hydrocarbons, C1-C20 aliphatic hydrocarbons, C3-C20 cycloalkanes, C1-C20 chlorinated hydrocarbons, C1-C20 alcohols and C2-C20 carboxylic acid esters; preferably, the organic solvent is selected from at least one of C6-C10 aromatic hydrocarbons, C1-C10 aliphatic hydrocarbons, C3-C10 cycloalkanes, C1-C10 chlorinated hydrocarbons, C1-C10 alcohols and C2-C10 carboxylic acid esters, more preferably, the molecular weight of the organic solvent is less than 150; further preferably, the C6-C20 aromatic hydrocarbon is selected from at least one of benzene, toluene and xylene; the C1-C20 aliphatic hydrocarbon is selected from at least one of petroleum ether, gasoline and n-hexane; the C3-C20 cycloalkane is selected from cyclohexane; the C1-C20 chlorinated hydrocarbon is selected from at least one of dichloroethylene, trichloroethylene, carbon tetrachloride and dichlorohexane; the C1-C20 alcohol is selected from at least one of methanol, ethanol, propanol, n-butanol and tert-butanol; the C2-C20 carboxylic ester is selected from at least one of ethyl acetate and butyl acetate.

6. The method according to any one of claims 1 to 5, wherein the crystallization is cooling crystallization in step S3, and preferably, the cooling crystallization is performed by cooling the montan wax solution to 35-45 ℃ with circulating water at a cooling rate of 2-3 ℃/min, and then cooling the montan wax solution to 10-18 ℃ with a low-temperature cooling medium at a cooling rate of 0.3-0.6 ℃/min, wherein, the seed crystal is added when the montan wax solution is cooled to 20-25 ℃.

7. The method according to any one of claims 1 to 6, wherein in step S4, the first desolventizing treatment removes an organic solvent by evaporation; and/or in step S6, the second desolventizing treatment removes the organic solvent by evaporation.

8. The method according to any one of claims 1 to 7, further comprising recycling the recovered organic solvent from the first desolventizing treatment, the recovered organic solvent from the second desolventizing treatment and the recovered organic solvent from the nanofiltration after being collected.

9. Montan wax obtained according to the method of any one of claims 1-8.

10. Use of a montan wax obtained according to the method of any one of claims 1 to 8 or a montan wax according to claim 9 in electric machines, precision casting, printing, paper making, textile and household chemicals.

Technical Field

The invention relates to a method for removing resin from coarse montan wax.

Background

The montan wax is a mineral wax containing wax, resin and bitumen, which is extracted from annual light coal such as lignite or peat by using an organic solvent, and has different compositions of different coal-forming plants and the montan wax extracted from coal in a coal-forming environment. The montan wax is a mixture mainly composed of resin, wax, bitumen and the like, and the content of the resin is required to be not more than 20% in the montan wax standard. In the crude wax of montan wax in China, the resin content is generally higher by 20 to 50 percent. Too high a resin content may cause stickiness of the montan wax, affect co-solubility of the montan wax with other additives, and reduce physical properties and mechanical properties of the montan wax. At present, the crude wax is obtained by extracting with an extractant, but the resin content in the crude wax is usually higher than 20%, so that the crude lignite wax needs to be subjected to resin removal to obtain a qualified lignite wax product.

The existing lignite wax resin removing method mainly comprises two types: leaching and multi-stage countercurrent extraction, and the commonly adopted solvent is organic solvent such as benzene, toluene, acetic acid, acetone and the like.

The leaching process comprises the steps of crushing the crude montan wax into particles, leaching the particles with an organic solvent for 2-4 hours at normal temperature according to a certain solid-to-liquid ratio, and separating to obtain a leaching solution and a solid matter. Heating the solid matter in a separating device to remove residual organic solvent to obtain degreased montan wax; putting the leaching solution into a separation container, adding water to separate out resin, evaporating resin-containing solid obtained by solid-liquid separation to obtain lignite resin, and rectifying and recovering the water-containing organic solvent to obtain the organic solvent for recycling.

The multistage countercurrent extraction process comprises the steps of crushing coarse montan wax into particles, feeding the particles into a multistage countercurrent extractor for liquid-solid phase extraction, carrying out multistage countercurrent extraction at the extraction temperature of-20-40 ℃, taking an organic solvent as an extractant, carrying out continuous extraction on the montan wax particles sequentially by using the organic solvent with reduced resin concentration, extracting for 120-180 min, then extracting for 60-80 min by using the organic solvent without resin, wherein the extraction stage number is 3-8, and obtaining a mixture of the solid defatted wax and the organic solvent with resin after extraction. And (3) feeding the extracted degreased wax solid into an evaporator for heating, evaporating a small amount of organic solvent contained in the degreased wax solid in the evaporator, condensing and recovering the evaporated organic solvent, obtaining degreased wax liquid after evaporation is finished, and feeding the degreased wax liquid to a forming machine for forming to obtain a degreased wax product. And (3) performing multi-effect evaporation on the resin-containing organic solvent mixed solution obtained after extraction is finished, condensing and recovering the evaporated organic solvent, obtaining a resin substance after evaporation is finished, and condensing and recovering the evaporated organic solvent.

In the existing lignite wax resin removal process, solvents are required to be recovered through rectification or multi-effect evaporation, so that the energy consumption is high; when benzene or toluene is used as a solvent, the production process is harmful to operators, and toxic solvents are remained in the prepared product to influence the product quality.

Disclosure of Invention

In view of the above situation, the present invention aims to overcome the defects of the prior art and provide a low energy consumption method for removing resin from coarse montan wax.

The invention provides a method for removing resin from coarse montan wax, which comprises the following steps:

step S1: melting the coarse lignite wax particles to obtain liquid lignite wax;

step S2: mixing the liquid montan wax with an organic solvent to obtain a montan wax solution;

step S3: crystallizing the montan wax solution, and carrying out solid-liquid separation to obtain a solid phase and a filtrate;

step S4: performing first desolventizing treatment on the solid phase obtained in the step S3 to obtain montan wax;

step S5: carrying out nanofiltration treatment on the filtrate obtained in the step S3 to obtain a nanofiltration concentrated solution;

step S6: and carrying out second desolventizing treatment on the nanofiltration concentrated solution to obtain the resin.

According to some embodiments of the invention, the nanofiltration temperature is 30 to 80 ℃ in step S5.

According to a preferred embodiment of the present invention, the nanofiltration temperature is 40 to 60 ℃ in step S5.

According to some embodiments of the invention, the pressure of the nanofiltration in step S5 is 2-4.5 MpaG.

According to some embodiments of the present invention, in step S5, the nanofiltration membrane has a molecular weight cut-off of 300-800.

According to some embodiments of the present invention, the concentration of the nanofiltration concentrate is 1 to 6 times in step S5.

According to a preferred embodiment of the present invention, the concentration ratio of the nanofiltration-treated concentrated solution is 3 to 4 times in step S5.

According to some embodiments of the present invention, in step S1, the montan wax particles have a particle size of 6mm or less.

According to some embodiments of the present invention, in step S1, the resin content of the montan wax particles is 20% or more.

According to some embodiments of the present invention, in step S1, the resin content of the montan wax particles is 30% or more.

According to some specific embodiments of the present invention, in step S1, the resin content of the montan wax particles is 45%.

According to some embodiments of the invention, the melting temperature is 90-120 ℃ in step S1.

According to a preferred embodiment of the present invention, the melting temperature is 95-105 ℃ in step S1.

According to some embodiments of the present invention, in step S2, the mass ratio of the liquid montan wax to the organic solvent is 1: (5-15).

According to a preferred embodiment of the present invention, in step S2, the mass ratio of the liquid montan wax to the organic solvent is 1: (5-10).

According to some embodiments of the invention, the temperature of the mixing is 60-110 ℃ in step S2.

According to a preferred embodiment of the present invention, the temperature of the mixing is 60 to 80 ℃ in step S2.

According to some embodiments of the invention, in step S2, the organic solvent is selected from at least one of C6-C20 aromatic hydrocarbons, C1-C20 aliphatic hydrocarbons, C3-C20 cycloalkanes, C1-C20 chlorinated hydrocarbons, C1-C20 alcohols, and C2-C20 carboxylic acid esters.

According to a preferred embodiment of the present invention, in step S2, the organic solvent is at least one selected from the group consisting of C6-C10 aromatic hydrocarbons, C1-C10 aliphatic hydrocarbons, C3-C10 cycloalkanes, C1-C10 chlorinated hydrocarbons, C1-C10 alcohols, and C2-C20 carboxylic acid esters.

According to some embodiments of the invention, in step S2, the organic solvent has a molecular weight of less than 150.

According to some embodiments of the invention, the C6-C10 aromatic hydrocarbon is selected from at least one of benzene, toluene, and xylene.

According to some embodiments of the invention, the C1-C20 aliphatic hydrocarbon is selected from at least one of petroleum ether, gasoline, and n-hexane.

According to some embodiments of the invention, the C3-C20 cycloalkane is selected from cyclohexane.

According to some embodiments of the invention, the C1-C20 chlorinated hydrocarbon is selected from at least one of dichloroethylene, trichloroethylene, carbon tetrachloride and dichlorohexane.

According to some embodiments of the invention, the C1-C20 alcohol is selected from at least one of methanol, ethanol, propanol, n-butanol and tert-butanol.

According to some embodiments of the invention, the C2-C20 carboxylic acid ester is selected from at least one of ethyl acetate and butyl acetate.

According to some embodiments of the invention, in step S3, the crystallization is a cooling crystallization.

According to a preferred embodiment of the present invention, in step S3, the cooling crystallization process is to cool the montan wax solution to 35-45 ℃ by using circulating water, the cooling rate is controlled to be 2-3 ℃/min, and then the low-temperature cooling medium is used to cool the montan wax solution to 10-18 ℃ by controlling the cooling rate to be 0.3-0.6 ℃/min, wherein, the seed crystal is added when the montan wax solution is cooled to 20-25 ℃.

According to some embodiments of the invention, in step S4, the first desolventizing treatment removes the organic solvent by evaporation.

According to some embodiments of the invention, in step S6, the second desolventizing treatment removes the organic solvent by evaporation.

According to some embodiments of the invention, the method further comprises recycling the organic solvent recovered by the first desolventizing treatment, the organic solvent recovered by the second desolventizing treatment and the organic solvent recovered by the nanofiltration treatment after being combined.

According to some embodiments of the present invention, in step S1, montan wax particles (less than or equal to 6mm) are placed in a melting kettle and heated to a temperature (95-105 ℃) to melt the montan wax particles into a liquid, and then the liquid is conveyed to a mixing kettle.

According to some embodiments of the present invention, in step S2, the solvent heated to a certain temperature is transferred to the mixing kettle to be mixed with the montan wax, and the temperature of the mixing kettle is controlled to 70-110 ℃, so that the montan wax is completely dissolved in the solvent. The adopted solvents are nontoxic or low-toxicity solvents such as ethyl acetate, butyl acetate, butanone and the like.

According to some embodiments of the present invention, in step S3, the solubility of montan wax decreases with decreasing temperature, and the resin does not crystallize out at a lower temperature, separation is performed by using the difference in solubility between montan wax and resin in the solvent, the montan wax solution in the mixing kettle is gradually cooled, the cooling rate is controlled, seed crystals are added when cooling to a temperature of 20-25 ℃ to crystallize out montan wax, and the crystallized liquid enters a filtering device to obtain a filter cake and a filtrate.

According to some embodiments of the present invention, in step S4, the filter cake from step S3 still contains a certain amount of solvent, and enters a desolventizing device to further evaporate and remove the solvent to obtain the defatted montan wax product, the solvent vapor is condensed to recover the solvent for recycling, and the resin is present in the filtrate.

According to some embodiments of the present invention, in step S5, the filtrate from step S3 enters a nanofiltration device, where substances with different molecular weights are separated by nanofiltration membranes. The molecular weight of the used organic solvent is usually less than 150, and the molecular weight of components such as montan wax, bitumen and resin in the crude montan wax is between 300-500, so that the organic solvent can permeate a nanofiltration membrane for recycling, thereby realizing the concentration of the filtrate, wherein the concentration multiple can reach 1-6 times, most of the solvent is separated in a nanofiltration device for recycling, the concentrated solution is sent to a resin desolventizing device for evaporating the solvent to obtain a resin product (step S6), and the solvent steam is condensed to recover the solvent for recycling.

According to some embodiments provided by the invention, in the step 6), the solvent recovered from the wax residue removal solution, the solvent recovered from the resin residue removal solution and the solvent separated by nanofiltration concentration are collected together for recycling, and the recycled solvent is heated to a certain temperature for completely dissolving the montan wax and then enters the mixing kettle.

According to the embodiment of the low-energy-consumption crude lignite wax deresination method provided by the invention, crude lignite grains are heated and melted, then enter a mixing kettle and are uniformly stirred and mixed with a solvent heated to a certain temperature, the lignite wax solution is cooled and crystallized by utilizing different solubilities of the resin and the lignite wax in the solvent at a low temperature, the lignite wax is separated out in a solid form, a crystallized liquid is filtered, a filter cake is desolventized to obtain a degreased lignite wax product, the solvent is recycled after being condensed and recovered, a filtrate enters a nanofiltration device for concentration, most of the solvent is separated for recycling, the concentrated liquid is evaporated to remove the solvent to obtain the resin product, and the solvent is recycled after being condensed and recovered.

In a second aspect, the present invention provides a montan wax obtained according to the method of the first aspect.

In a third aspect, the present invention provides a use of the montan wax obtained according to the method of the first aspect or the montan wax according to the second aspect in electric machines, precision casting, printing, papermaking, textile and household chemicals.

The lignite wax product obtained by the crude lignite wax deresination method of the invention is not subjected to repeated high-temperature cooking, the product quality is good, the energy consumption of steam and cooling water is reduced by the method of the invention, and a large amount of steam consumption operation cost can be saved every year.

Drawings

FIG. 1 is a schematic diagram of a process for de-resinating a crude montan wax according to one embodiment of the present invention.

Detailed Description

The present invention will be further described with reference to the following examples.

The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. The examples are intended to be illustrative of the invention and not limiting.

Example 1

Putting lignite wax particles with the particle size of less than or equal to 6mm and the resin content of 45% into a jacketed type melting kettle, arranging a stirrer in the melting kettle, introducing steam into a hollow stirrer shaft, introducing the steam into a jacket of the melting kettle and the stirrer shaft, heating the lignite wax to 95 ℃, melting the lignite wax particles into liquid, and conveying the liquid to a mixing kettle.

Conveying the ethyl acetate solvent heated to 58 ℃ to a mixing kettle, and uniformly stirring and mixing the ethyl acetate solvent and the montan wax liquid, wherein the mass ratio of the montan wax to the ethyl acetate solvent is 1:9, controlling the temperature of the mixing kettle to be 60 ℃ to completely dissolve the montan wax in the ethyl acetate solvent.

Sending the montan wax solution in the mixing kettle into a scraped wall type hollow plate cooling crystallizer for cooling to separate out montan wax crystals, wherein the cooling crystallizer selects an GLJ high-efficiency scraped wall type hollow plate cooling continuous crystallizer of Shanghai Xunchang chemical engineering equipment technical research institute, the montan wax solution is gradually cooled in the cooling crystallizer, the montan wax solution is firstly cooled by circulating water after entering the cooling crystallizer, the montan wax solution is cooled to 40 ℃ by controlling the cooling rate to be 2-3 ℃/min, then the montan wax solution is cooled by adopting a low-temperature cooling medium, the montan wax solution is cooled to 10 ℃ by controlling the cooling rate to be-0.5 ℃/min, crystal seeds discharged from the cooling crystallizer are added at the part of the cooling crystallizer, where the montan wax solution is cooled to 20 ℃, and the adding amount is 1% of the discharge amount of the cooling crystallizer.

The crystallization liquid is discharged from a cooling crystallization machine and enters a filtering device, the filtering device adopts a bag-pulling type scraper lower part discharging centrifugal machine, the centrifugal machine adopts a PLD-bag-pulling type scraper lower part discharging centrifugal machine of Jiangsu Hua centrifuge manufacturing Limited company, the lignite wax filter cake still contains a certain amount of solvent, the lignite wax filter cake enters a negative pressure desolventizing device to evaporate and remove the solvent to obtain a degreased lignite wax product, the solvent content in the lignite wax product is controlled to be 1 percent, the solvent steam is condensed to recover the solvent for recycling, the resin content in the lignite wax product is 9.4 percent and is superior to the first-level lignite wax resin content requirement specified in MT/T239 and 2006 lignite wax technical conditions, and the yield of the lignite wax is 93.9 percent.

The method comprises the following steps that filtrate discharged from a discharging centrifuge at the lower part of a bag-pulling type scraper enters a nanofiltration device, the nanofiltration membrane is Puramem Selective 8040 nanofiltration membrane of the winning company, the nanofiltration membrane can intercept substances with the molecular weight of 300-800, the main component of the filtrate is resin, in the nanofiltration device, because the nanofiltration membrane has different permeability to the substances with different molecular weights, the molecular weight of ethyl acetate can pass through the nanofiltration membrane, and the resin is intercepted by the nanofiltration membrane, so that the concentration of the filtrate is realized, the nanofiltration operation temperature is 50 ℃, and the initial operation pressure is 3.0 MPaG; when the operation pressure is more than 4.5MPaG, membrane backwashing is automatically carried out, the concentration multiple is 4, 80 percent of solvent in the nanofiltration device is directly separated out for recycling, the concentrated solution is sent to negative pressure desolventizing equipment for evaporating the solvent to obtain a resin product, the content of the solvent in the resin product is controlled to be less than 1 percent, and the solvent steam is condensed to recover the solvent for recycling.

The solvent recovered by the wax residue removal solution, the solvent recovered by the resin residue removal solution and the solvent separated by nanofiltration concentration are gathered together for recycling, and the solvent is heated to 58 ℃ and enters a mixing kettle.

The consumption and process index of the resin removing process device for treating 2000 tons of crude lignite wax are shown in the table 1.

Example 2

Putting lignite wax particles with the particle size of less than or equal to 6mm and the resin content of 45% into a jacketed type melting kettle, arranging a stirrer in the melting kettle, introducing steam into a hollow stirrer shaft, introducing the steam into a jacket of the melting kettle and the stirrer shaft, heating the lignite wax to 95 ℃, melting the lignite wax particles into liquid, and conveying the liquid to a mixing kettle.

Conveying the butyl acetate solvent heated to 79 ℃ below zero to a mixing kettle, and uniformly stirring and mixing the butyl acetate solvent and the montan wax liquid, wherein the mass ratio of the montan wax to the butyl acetate solvent is 1:10, and controlling the temperature of the mixing kettle to 80 ℃ below zero to completely dissolve the montan wax in the butyl acetate solvent.

Sending the montan wax solution in the mixing kettle into a scraped wall type hollow plate cooling crystallizer for cooling to separate out montan wax crystals, wherein the cooling crystallizer selects an GLJ high-efficiency scraped wall type hollow plate cooling continuous crystallizer of Shanghai Xunchang chemical engineering equipment technical research institute, the montan wax solution is gradually cooled in the cooling crystallizer, the montan wax solution is firstly cooled by circulating water after entering the cooling crystallizer, the montan wax solution is cooled to 40 ℃ by controlling the cooling rate to be 2-3 ℃/min, then the montan wax solution is cooled by adopting a low-temperature cooling medium, the montan wax solution is cooled to 15 ℃ by controlling the cooling rate to be-0.5 ℃/min, crystal seeds discharged from the cooling crystallizer are added at the part of the cooling crystallizer, where the montan wax solution is cooled to 25 ℃, and the adding amount is 1% of the discharge amount of the cooling crystallizer.

The crystallization liquid is discharged from a cooling crystallization machine and enters a filtering device, the filtering device adopts a bag-pulling type scraper lower part discharging centrifugal machine, the centrifugal machine adopts a PLD-bag-pulling type scraper lower part discharging centrifugal machine of Jiangsu Hua centrifuge manufacturing Limited company, the lignite wax filter cake still contains a certain amount of solvent, the lignite wax filter cake enters a negative pressure desolventizing device to evaporate and remove the solvent to obtain a degreased lignite wax product, the solvent content in the lignite wax product is controlled to be 1 percent, the solvent steam is condensed to recover the solvent for recycling, the resin content in the lignite wax product is 9.35 percent and is superior to the first-level lignite wax resin content requirement specified in MT/T239 and 2006 lignite wax technical conditions, and the yield of the lignite wax is 93.9 percent.

The method comprises the following steps that filtrate discharged from a discharging centrifuge at the lower part of a bag-pulling type scraper enters a nanofiltration device, the nanofiltration membrane is Puramem Selective 8040 nanofiltration membrane of the winning company, the nanofiltration membrane can intercept substances with the molecular weight of 300-800, the main component of the filtrate is resin, in the nanofiltration device, the molecular weight of butyl acetate can pass through the nanofiltration membrane due to different permeabilities of the nanofiltration membrane to the substances with different molecular weights, the resin is intercepted by the nanofiltration membrane, so that the concentration of the filtrate is realized, the nanofiltration operation temperature is 50 ℃, and the initial operation pressure is 3.0 MPaG; when the operation pressure is more than 4.5MPaG, membrane backwashing is automatically carried out, the concentration multiple is 4, 80 percent of solvent in the nanofiltration device is directly separated out for recycling, the concentrated solution is sent to negative pressure desolventizing equipment for evaporating the solvent to obtain a resin product, the content of the solvent in the resin product is controlled to be less than 1 percent, and the solvent steam is condensed to recover the solvent for recycling.

The solvent recovered by the wax residue removal solution, the solvent recovered by the resin residue removal solution and the solvent separated by nanofiltration concentration are gathered together for recycling, and the solvent is heated to 79 ℃ and enters a mixing kettle.

The consumption and process index of the resin removing process device for treating 2000 tons of crude lignite wax are shown in the table 1.

Example 3

Putting lignite wax particles with the particle size of less than or equal to 6mm and the resin content of 45% into a jacketed type melting kettle, arranging a stirrer in the melting kettle, introducing steam into a hollow stirrer shaft, introducing the steam into a jacket of the melting kettle and the stirrer shaft, heating the lignite wax to 95 ℃, melting the lignite wax particles into liquid, and conveying the liquid to a mixing kettle.

And conveying the butanone solvent heated to 63 ℃ to a mixing kettle, and uniformly stirring and mixing the butanone solvent and the montan wax liquid, wherein the mass ratio of the montan wax to the butanone solvent is 1:8, and the temperature of the mixing kettle is controlled to 65 ℃ so that the montan wax is completely dissolved in the butanone solvent.

Sending the montan wax solution in the mixing kettle into a scraped wall type hollow plate cooling crystallizer for cooling to separate out montan wax crystals, wherein the cooling crystallizer selects an GLJ high-efficiency scraped wall type hollow plate cooling continuous crystallizer of Shanghai Xunchang chemical engineering equipment technical research institute, the montan wax solution is gradually cooled in the cooling crystallizer, the montan wax solution is firstly cooled by circulating water after entering the cooling crystallizer, the montan wax solution is cooled to 40 ℃ by controlling the cooling rate to be 2-3 ℃/min, then the montan wax solution is cooled by adopting a low-temperature cooling medium, the montan wax solution is cooled to 15 ℃ by controlling the cooling rate to be-0.5 ℃/min, crystal seeds discharged from the cooling crystallizer are added at the part of the cooling crystallizer, where the montan wax solution is cooled to 25 ℃, and the adding amount is 1% of the discharge amount of the cooling crystallizer.

The crystallization liquid is discharged from a cooling crystallization machine and enters a filtering device, the filtering device adopts a pull-bag type scraper lower part discharge centrifuge, the centrifuge adopts a PLD-pull-bag type scraper lower part discharge centrifuge of Jiangsu Hua big centrifuge manufacturing limited company, a certain amount of solvent is still contained in the montan wax filter cake, the montan wax filter cake enters a negative pressure desolventizing device to evaporate and remove the solvent to obtain a degreased montan wax product, the solvent content in the montan wax product is controlled to be less than 1%, the solvent steam is condensed to recover the solvent for recycling, the resin content in the montan wax product is 9.4%, the requirement of the primary montan wax resin content specified in the technical conditions of MT/T239 and 2006 montan wax is better, and the yield of the montan wax is 93.9%.

The method comprises the following steps that filtrate discharged from a discharging centrifuge at the lower part of a bag-pulling type scraper enters a nanofiltration device, the nanofiltration membrane is Puramem Selective 8040 nanofiltration membrane of the winning company, the nanofiltration membrane can intercept substances with the molecular weight of 300-800, the main component of the filtrate is resin, in the nanofiltration device, as the nanofiltration membrane has different permeability to the substances with different molecular weights, the butanone molecular weight of 72 can pass through the nanofiltration membrane, and the resin is intercepted by the nanofiltration membrane, so that the concentration of the filtrate is realized, the nanofiltration operation temperature is 50 ℃, and the initial operation pressure is 3.0 MPaG; when the operation pressure is more than 4.5MPaG, membrane backwashing is automatically carried out, the concentration multiple is 4, 80 percent of solvent in the nanofiltration device is directly separated out for recycling, the concentrated solution is sent to negative pressure desolventizing equipment for evaporating the solvent to obtain a resin product, the content of the solvent in the resin product is controlled to be less than 1 percent, and the solvent steam is condensed to recover the solvent for recycling.

The solvent recovered by the wax residue removal solution, the solvent recovered by the resin residue removal solution and the solvent separated by nanofiltration concentration are gathered together for recycling, and the solvent is heated to 63 ℃ and enters a mixing kettle.

The consumption and process index of the resin removing process device for treating 2000 tons of crude lignite wax are shown in the table 1.

Example 4

The difference from the embodiment 1 is only that the filtrate discharged from the discharging centrifuge at the lower part of the bag-pulling type scraper enters a nanofiltration device, the nanofiltration membrane is Puramem Selective 8040 nanofiltration membrane of the winning company, the nanofiltration membrane can intercept substances with the molecular weight of 300-800, the main component in the filtrate is resin, in the nanofiltration device, because the nanofiltration membrane has different permeability to the substances with different molecular weights, the molecular weight of ethyl acetate is 88, and the resin can be intercepted by the nanofiltration membrane, the concentration of the filtrate is realized, the nanofiltration operation temperature is 30 ℃, and the initial operation pressure is 3.0 MPaG; when the operation pressure is more than 4.5MPaG, membrane backwashing is automatically carried out, the concentration multiple is 4, 80 percent of solvent in the nanofiltration device is directly separated out for recycling, the concentrated solution is sent to negative pressure desolventizing equipment for evaporating the solvent to obtain a resin product, the content of the solvent in the resin product is controlled to be less than 1 percent, and the solvent steam is condensed to recover the solvent for recycling.

The consumption and process index of the resin removing process device for treating 2000 tons of crude lignite wax are shown in the table 1.

Example 5

The difference from the embodiment 1 is only that the filtrate discharged from the discharging centrifuge at the lower part of the bag-pulling type scraper enters a nanofiltration device, the nanofiltration membrane is Puramem Selective 8040 nanofiltration membrane of the winning company, the nanofiltration membrane can intercept substances with the molecular weight of 300-800, the main component in the filtrate is resin, in the nanofiltration device, because the nanofiltration membrane has different permeability to the substances with different molecular weights, the molecular weight of ethyl acetate is 88, and the resin can be intercepted by the nanofiltration membrane, the concentration of the filtrate is realized, the nanofiltration operation temperature is 40 ℃, and the initial operation pressure is 3.0 MPaG; when the operation pressure is more than 4.5MPaG, membrane backwashing is automatically carried out, the concentration multiple is 4, 80 percent of solvent in the nanofiltration device is directly separated out for recycling, the concentrated solution is sent to negative pressure desolventizing equipment for evaporating the solvent to obtain a resin product, the content of the solvent in the resin product is controlled to be less than 1 percent, and the solvent steam is condensed to recover the solvent for recycling.

The consumption and process index of the resin removing process device for treating 2000 tons of crude lignite wax are shown in the table 1.

Example 6

The difference from the embodiment 1 is only that the filtrate discharged from the discharging centrifuge at the lower part of the bag-pulling type scraper enters a nanofiltration device, the nanofiltration membrane is a Puramem Selective 8040 nanofiltration membrane of the winning company, the nanofiltration membrane can intercept substances with the molecular weight of 300-800, the main component in the filtrate is resin, in the nanofiltration device, because the nanofiltration membrane has different permeability to the substances with different molecular weights, the molecular weight of ethyl acetate is 88, and the resin can be intercepted by the nanofiltration membrane, the concentration of the filtrate is realized, the nanofiltration operation temperature is 60 ℃, and the initial operation pressure is 3.0 MPaG; when the operation pressure is more than 4.5MPaG, membrane backwashing is automatically carried out, the concentration multiple is 4, 80 percent of solvent in the nanofiltration device is directly separated out for recycling, the concentrated solution is sent to negative pressure desolventizing equipment for evaporating the solvent to obtain a resin product, the content of the solvent in the resin product is controlled to be less than 1 percent, and the solvent steam is condensed to recover the solvent for recycling.

The consumption and process index of the resin removing process device for treating 2000 tons of crude lignite wax are shown in the table 1.

Example 7

The difference from the embodiment 1 is only that the filtrate discharged from the discharging centrifuge at the lower part of the bag-pulling type scraper enters a nanofiltration device, the nanofiltration membrane is a Puramem Selective 8040 nanofiltration membrane of the winning company, the nanofiltration membrane can intercept substances with the molecular weight of 300-800, the main component in the filtrate is resin, in the nanofiltration device, because the nanofiltration membrane has different permeability to the substances with different molecular weights, the molecular weight of ethyl acetate is 88, and the resin can be intercepted by the nanofiltration membrane, the concentration of the filtrate is realized, the nanofiltration operation temperature is 70 ℃, and the initial operation pressure is 3.0 MPaG; when the operation pressure is more than 4.5MPaG, membrane backwashing is automatically carried out, the concentration multiple is 4, 80 percent of solvent in the nanofiltration device is directly separated out for recycling, the concentrated solution is sent to negative pressure desolventizing equipment for evaporating the solvent to obtain a resin product, the content of the solvent in the resin product is controlled to be less than 1 percent, and the solvent steam is condensed to recover the solvent for recycling.

The consumption and process index of the resin removing process device for treating 2000 tons of crude lignite wax are shown in the table 1.

Example 8

The difference from the embodiment 1 is only that the filtrate discharged from the discharging centrifuge at the lower part of the bag-pulling type scraper enters a nanofiltration device, the nanofiltration membrane is a Puramem Selective 8040 nanofiltration membrane of the winning company, the nanofiltration membrane can intercept substances with the molecular weight of 300-800, the main component in the filtrate is resin, in the nanofiltration device, because the nanofiltration membrane has different permeability to the substances with different molecular weights, the molecular weight of ethyl acetate is 88, and the resin can be intercepted by the nanofiltration membrane, the concentration of the filtrate is realized, the nanofiltration operation temperature is 50 ℃, and the initial operation pressure is 3.0 MPaG; when the operation pressure is more than 4.5MPaG, membrane backwashing is automatically carried out, the concentration multiple is 1, 50 percent of solvent in the nanofiltration device is directly separated out for recycling, the concentrated solution is sent to negative pressure desolventizing equipment for evaporating the solvent to obtain a resin product, the content of the solvent in the resin product is controlled to be less than 1 percent, and the solvent steam is condensed to recover the solvent for recycling.

The consumption and process index of the resin removing process device for treating 2000 tons of crude lignite wax are shown in the table 1.

Example 9

The difference from the embodiment 1 is only that the filtrate discharged from the discharging centrifuge at the lower part of the bag-pulling type scraper enters a nanofiltration device, the nanofiltration membrane is a Puramem Selective 8040 nanofiltration membrane of the winning company, the nanofiltration membrane can intercept substances with the molecular weight of 300-800, the main component in the filtrate is resin, in the nanofiltration device, because the nanofiltration membrane has different permeability to the substances with different molecular weights, the molecular weight of ethyl acetate is 88, and the resin can be intercepted by the nanofiltration membrane, the concentration of the filtrate is realized, the nanofiltration operation temperature is 50 ℃, and the initial operation pressure is 3.0 MPaG; when the operation pressure is more than 4.5MPaG, membrane backwashing is automatically carried out, the concentration multiple is 2, 67 percent of solvent in the nanofiltration device is directly separated out for recycling, the concentrated solution is sent to negative pressure desolventizing equipment for evaporating the solvent to obtain a resin product, the content of the solvent in the resin product is controlled to be less than 1 percent, and the solvent steam is condensed to recover the solvent for recycling.

The consumption and process index of the resin removing process device for treating 2000 tons of crude lignite wax are shown in the table 1.

Example 10

The difference from the embodiment 1 is only that the filtrate discharged from the discharging centrifuge at the lower part of the bag-pulling type scraper enters a nanofiltration device, the nanofiltration membrane is a Puramem Selective 8040 nanofiltration membrane of the winning company, the nanofiltration membrane can intercept substances with the molecular weight of 300-800, the main component in the filtrate is resin, in the nanofiltration device, because the nanofiltration membrane has different permeability to the substances with different molecular weights, the molecular weight of ethyl acetate is 88, and the resin can be intercepted by the nanofiltration membrane, the concentration of the filtrate is realized, the nanofiltration operation temperature is 50 ℃, and the initial operation pressure is 3.0 MPaG; when the operation pressure is more than 4.5MPaG, membrane backwashing is automatically carried out, the concentration multiple is 3, 75 percent of solvent in the nanofiltration device is directly separated out for recycling, the concentrated solution is sent to negative pressure desolventizing equipment for evaporating the solvent to obtain a resin product, the content of the solvent in the resin product is controlled to be less than 1 percent, and the solvent steam is condensed to recover the solvent for recycling.

The consumption and process index of the resin removing process device for treating 2000 tons of crude lignite wax are shown in the table 1.

Example 11

The difference from the embodiment 1 is only that the filtrate discharged from the discharging centrifuge at the lower part of the bag-pulling type scraper enters a nanofiltration device, the nanofiltration membrane is a Puramem Selective 8040 nanofiltration membrane of the winning company, the nanofiltration membrane can intercept substances with the molecular weight of 300-800, the main component in the filtrate is resin, in the nanofiltration device, because the nanofiltration membrane has different permeability to the substances with different molecular weights, the molecular weight of ethyl acetate is 88, and the resin can be intercepted by the nanofiltration membrane, the concentration of the filtrate is realized, the nanofiltration operation temperature is 50 ℃, and the initial operation pressure is 3.0 MPaG; when the operation pressure is more than 4.5MPaG, membrane backwashing is automatically carried out, the concentration multiple is 5, 85 percent of solvent in the nanofiltration device is directly separated out for recycling, the concentrated solution is sent to negative pressure desolventizing equipment for evaporating the solvent to obtain a resin product, the content of the solvent in the resin product is controlled to be less than 1 percent, and the solvent steam is condensed to recover the solvent for recycling.

The consumption and process index of the resin removing process device for treating 2000 tons of crude lignite wax are shown in the table 1.

Example 12

The difference from example 1 is only that the mass ratio of montan wax to ethyl acetate solvent was 1:7, the nanofiltration operation temperature was 50 ℃, and the initial operation pressure was 3.0 MPaG; when the operation pressure is more than 4.5MPaG, membrane backwashing is automatically carried out, the concentration multiple is 4, 80 percent of solvent in the nanofiltration device is directly separated out for recycling, the concentrated solution is sent to negative pressure desolventizing equipment for evaporating the solvent to obtain a resin product, the content of the solvent in the resin product is controlled to be less than 1 percent, and the solvent steam is condensed to recover the solvent for recycling.

The consumption and process index of the resin removing process device for treating 2000 tons of crude lignite wax are shown in the table 1.

Example 13

The difference from example 1 is only that the mass ratio of montan wax to ethyl acetate solvent was 1:8, the nanofiltration operation temperature was 50 ℃, and the initial operation pressure was 3.0 MPaG; when the operation pressure is more than 4.5MPaG, membrane backwashing is automatically carried out, the concentration multiple is 4, 80 percent of solvent in the nanofiltration device is directly separated out for recycling, the concentrated solution is sent to negative pressure desolventizing equipment for evaporating the solvent to obtain a resin product, the content of the solvent in the resin product is controlled to be less than 1 percent, and the solvent steam is condensed to recover the solvent for recycling.

The consumption and process index of the resin removing process device for treating 2000 tons of crude lignite wax are shown in the table 1.

Example 14

The difference from example 1 is only that the mass ratio of montan wax to ethyl acetate solvent was 1:10, the nanofiltration operation temperature was 50 ℃, and the initial operation pressure was 3.0 MPaG; when the operation pressure is more than 4.5MPaG, membrane backwashing is automatically carried out, the concentration multiple is 4, 80 percent of solvent in the nanofiltration device is directly separated out for recycling, the concentrated solution is sent to negative pressure desolventizing equipment for evaporating the solvent to obtain a resin product, the content of the solvent in the resin product is controlled to be less than 1 percent, and the solvent steam is condensed to recover the solvent for recycling.

The consumption and process index of the resin removing process device for treating 2000 tons of crude lignite wax are shown in the table 1.

Example 15

The difference from example 1 is only that the mass ratio of montan wax to ethyl acetate solvent was 1:11, the nanofiltration operation temperature was 50 ℃, and the initial operation pressure was 3.0 MPaG; when the operation pressure is more than 4.5MPaG, membrane backwashing is automatically carried out, the concentration multiple is 4, 80 percent of solvent in the nanofiltration device is directly separated out for recycling, the concentrated solution is sent to negative pressure desolventizing equipment for evaporating the solvent to obtain a resin product, the content of the solvent in the resin product is controlled to be less than 1 percent, and the solvent steam is condensed to recover the solvent for recycling.

The consumption and process index of the resin removing process device for treating 2000 tons of crude lignite wax are shown in the table 1.

Comparative example 1:

the method comprises the steps of adopting a conventional process flow, putting lignite wax particles with the diameter less than or equal to 6mm and the resin content of 45% into a jacketed melting kettle, arranging a stirrer in the melting kettle, introducing steam into a hollow stirrer shaft, introducing the steam into a jacket of the melting kettle and the stirrer shaft, heating the lignite wax to the temperature of 95 ℃ to melt the lignite wax particles into liquid, and conveying the liquid to a mixing kettle.

Conveying the ethyl acetate solvent heated to 58 ℃ to a mixing kettle, and uniformly stirring and mixing the ethyl acetate solvent and the montan wax liquid, wherein the mass ratio of the montan wax to the ethyl acetate solvent is 1:9, controlling the temperature of the mixing kettle to be 60 ℃ to completely dissolve the montan wax in the ethyl acetate solvent.

Sending the montan wax solution in the mixing kettle into a scraped wall type hollow plate cooling crystallizer for cooling to separate out montan wax crystals, wherein the cooling crystallizer selects an GLJ high-efficiency scraped wall type hollow plate cooling continuous crystallizer of Shanghai Xunchang chemical engineering equipment technical research institute, the montan wax solution is gradually cooled in the cooling crystallizer, the montan wax solution is firstly cooled by circulating water after entering the cooling crystallizer, the montan wax solution is cooled to 40 ℃ by controlling the cooling rate to be 2-3 ℃/min, then the montan wax solution is cooled by adopting a low-temperature cooling medium, the montan wax solution is cooled to 10 ℃ by controlling the cooling rate to be-0.5 ℃/min, crystal seeds discharged from the cooling crystallizer are added at the part of the cooling crystallizer, where the montan wax solution is cooled to 20 ℃, and the adding amount is 1% of the discharge amount of the cooling crystallizer.

The crystallization liquid is discharged from a cooling crystallization machine and enters a filtering device, the filtering device adopts a pull-bag type scraper lower part discharge centrifuge, the centrifuge adopts a PLD-pull-bag type scraper lower part discharge centrifuge of Jiangsu Hua big centrifuge manufacturing limited company, a certain amount of solvent is still contained in the montan wax filter cake, the montan wax filter cake enters a negative pressure desolventizing device to evaporate and remove the solvent to obtain a degreased montan wax product, the solvent content in the montan wax product is controlled to be less than 1%, the solvent steam is condensed to recover the solvent for recycling, the resin content in the montan wax product is 11.03%, the requirement of the primary montan wax resin content specified in technical conditions of MT/T239 and 2006 montan wax is better than the requirement, and the yield of the montan wax is 91.9%.

And (3) feeding filtrate discharged from a discharge centrifuge at the lower part of the bag-pulling type scraper into an evaporation desolventizing device, wherein the filtrate mainly contains resin as a component, obtaining a resin product through multi-stage evaporation desolventizing, and condensing and recycling solvent steam for recycling, wherein the content of the solvent in the resin product is controlled to be less than 1%.

The solvent recovered by the wax residue removal solution, the solvent recovered by the resin residue removal solution and the solvent separated by evaporation concentration are gathered together for recycling, and the solvent is heated to 58 ℃ and enters a mixing kettle.

The consumption and process index of the resin removing process device for treating 2000 tons of crude lignite wax are shown in the table 1.

TABLE 1 amount of consumption and process index of lignite wax deresination process equipment

It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.