阅读说明：本技术 用于粗褐煤蜡精制的装置及方法 (Device and method for refining coarse montan wax ) 是由 张中华 张翠清 芦海云 李晓峰 崔鑫 郭屹 于 2020-05-22 设计创作，主要内容包括：本发明提供了一种粗褐煤蜡精制的装置及方法。本发明提供的用于粗褐煤蜡精制的装置包括精制反应釜,所述精制反应釜的内部设置有一层或多层砂芯板,所述精制反应釜的进料口设置在底部。本发明的粗褐煤蜡精制的方法包括使粗褐煤蜡原料与臭氧接触,得到精制的褐煤蜡。该方法生产过程无毒、废水排放量大大减少,且产品精制蜡白度高。(The invention provides a device and a method for refining coarse montan wax. The device for refining the coarse montan wax comprises a refining reaction kettle, wherein one or more layers of sand core plates are arranged inside the refining reaction kettle, and a feeding hole of the refining reaction kettle is formed in the bottom of the refining reaction kettle. The method for refining the coarse montan wax comprises the step of contacting a raw material of the coarse montan wax with ozone to obtain refined montan wax. The method has the advantages of no toxicity in the production process, greatly reduced wastewater discharge amount, and high whiteness of the refined wax product.)

1. The device for refining the coarse montan wax comprises a refining reaction kettle, wherein one or more layers of sand core plates are arranged inside the refining reaction kettle, and a feeding hole of the refining reaction kettle is formed in the bottom.

2. The apparatus of claim 1, wherein the sand core plate has 1-15 layers, preferably 3-10 layers; when a plurality of layers of sand core plates are arranged in the refining reaction kettle, the distance between two adjacent layers of sand core plates is 1-20cm, preferably 3-5 cm; more preferably, the material of the sand core plate is quartz or sintered glass; the aperture of the sand core plate is 0.5-20 μm, preferably 1-10 μm; the thickness of the sand core plate is 0.1-10mm, preferably 1-5 mm; and/or the position of the discharge hole of the refining reaction kettle is higher than that of the sand core plate.

3. The apparatus according to claim 1 or 2, further comprising a montan wax raw material tank, an ozone generator, an auxiliary agent tank, a cooling tank, a filter, and a dryer, wherein the montan wax raw material tank, the ozone generator, and the auxiliary agent tank are in communication with a feed port of the refining reactor, the cooling tank is in communication with a discharge port of the refining reactor, the filter is in communication with the cooling tank, and the dryer is in communication with the filter.

4. The apparatus of any one of claims 1-3, further comprising a refined wax storage tank and a molding machine, wherein the refined wax storage tank is in communication with the dryer and the molding machine is in communication with the refined wax storage tank;

preferably, the device further comprises a condenser and a tail gas processor, wherein the condenser is communicated with the top of the refining reaction kettle and/or the top of the cooling tank, and the tail gas processor is communicated with the condenser.

5. Use of the apparatus according to any one of claims 1-4 in the refining of crude montan wax.

6. A refining method of crude montan wax comprises contacting crude montan wax raw material with ozone to obtain refined montan wax.

7. Method according to claim 6, characterized in that it is implemented in a device according to any one of claims 1-4.

8. The method of claim 7, wherein the method comprises:

step A: enabling the raw material of the coarse montan wax, the ozone and the optional auxiliary agent to enter a refining reaction kettle through a feed inlet of the refining reaction kettle to contact with each other to generate liquid montan wax;

and B: the liquid lignite wax passes through the sand core plate, flows out of a discharge hole of the refining reaction kettle, is cooled, and preferably enters a cooling tank for cooling to obtain a cooled lignite wax material flow;

preferably, the method further comprises step C: filtering the cooled montan wax material flow through a filter, returning the obtained liquid to a refining reaction kettle for recycling, and drying the obtained solid in a dryer to obtain refined montan wax;

preferably, the method further comprises step D: and the refined montan wax enters a forming machine for forming.

9. The method according to any one of claims 6 to 8,

the mass ratio of the raw material of the coarse montan wax to the ozone is 100 (0.5-20), preferably 100 (1-10); and/or

The mass ratio of the raw material of the coarse lignite wax to the auxiliary agent is 100 (0.01-2); preferably 100 (0.1-0.5); and/or

The auxiliary agent is an alcohol compound, preferably one or more selected from C2-C10 alcohol compounds, more preferably one or more selected from ethanol, propanol and butanol; and/or

The contact temperature of the raw material of the coarse montan wax and the ozone is 60-120 ℃, and the optimal contact temperature is 80-100 ℃; and/or the contact time of the raw material of the coarse montan wax and the ozone is 20 to 120min, preferably 30 to 60 min.

10. The method according to claim 8 or 9, further comprising condensing the gas in the cooling tank through a condenser, and discharging the non-condensable gas in the condenser after the non-condensable gas is treated by a tail gas treater.

Technical Field

The invention relates to a device and a method for refining coarse montan wax.

Background

Montan wax is a mineral wax extracted from wax-rich lignite by using an organic solvent, has many excellent individuality and is widely used, and no synthetic wax can replace the montan wax at present. However, the crude wax extracted directly from lignite is darker in color, which limits the application of the crude wax in more fields. Therefore, the application range of the lignite wax can be greatly widened by decoloring the lignite wax, and the value is further improved. Generally, the lighter the color of the refined wax, the wider the range of applications and the higher the price.

CN102465037A discloses an oxidation decoloration refining method of montan wax, which adopts oxydol as an oxidant and carries out two-stage refining. As the oxidant is 30 percent hydrogen peroxide, the method produces a large amount of wastewater.

CN103525462A discloses an oxidation refining method of montan wax, which adopts peroxyacetic acid and hydrogen peroxide as oxidants to carry out three-stage refining. Because the reaction of the montan wax is incomplete, the color of the product is slightly yellow.

The refined wax produced by the existing refining method is slightly yellow in color and mainly has two reasons, namely incomplete reaction caused by limited contact between the wax and an oxidant and improvement of the oxidizing capability of the oxidant.

Disclosure of Invention

Aiming at the defects of the prior art, the invention provides a device and a method for refining coarse montan wax, which are different from the traditional method, the production process of the method is nontoxic, the discharge amount of wastewater is greatly reduced, and the whiteness of the refined wax product is high.

In a first aspect, the invention provides a device for refining coarse montan wax, which comprises a refining reaction kettle, wherein one or more layers of sand core plates are arranged inside the refining reaction kettle, and a feed inlet of the refining reaction kettle is arranged at the bottom.

According to some embodiments of the present invention, the refining reactor is provided with 1-15 layers of sand core plates, for example, 1 layer, 2 layers, 3 layers, 4 layers, 5 layers, 6 layers, 7 layers, 8 layers, 9 layers, 10 layers, 11 layers, 12 layers, 13 layers, 14 layers.

According to the preferred embodiment of the invention, 3-10 layers of sand core plates are arranged inside the refining reaction kettle.

According to some embodiments of the invention, the outlet of the finishing reactor is located higher than the sand core plate. That is, the discharge port of the purification reactor is positioned at a level higher than the level of the sand core plate.

According to the preferred embodiment of the invention, when a plurality of sand core plates are arranged in the refining reaction kettle, the distance between two adjacent sand core plates is 1-20 cm.

According to a further preferred embodiment of the present invention, when a plurality of sand core plates are disposed inside the refining reactor, the distance between two adjacent sand core plates is 3-5 cm.

According to some embodiments of the invention, the material of the sand core plate is quartz or sintered glass.

According to some embodiments of the invention, the sand core plate has a pore size of 0.5 to 20 μm.

According to a preferred embodiment of the invention, the sand core plate has a pore size of 1-10 μm.

According to some embodiments of the invention, the thickness of the sand core plate is 0.1 to 10 mm.

According to a preferred embodiment of the invention, the thickness of the sand core plate is 1-5 mm.

According to some embodiments of the invention, the apparatus further comprises a montan wax feedstock tank, an ozone generator, an auxiliary agent tank, a cooling tank, a filter and a dryer, wherein the montan wax feedstock tank, the ozone generator and the auxiliary agent tank are in communication with the feed inlet of the refining reactor, the cooling tank is in communication with the discharge outlet of the refining reactor, the filter is in communication with the cooling tank, and the dryer is in communication with the filter.

According to a preferred embodiment of the present invention, the apparatus further comprises a refined wax storage tank and a molding machine, wherein the refined wax storage tank is in communication with the dryer and the molding machine is in communication with the refined wax storage tank.

According to a preferred embodiment of the present invention, the apparatus further comprises a condenser and a tail gas processor, wherein the condenser is communicated with the top of the refining reactor and/or the top of the cooling tank, and the tail gas processor is communicated with the condenser.

The feed inlet of the refining reaction kettle is arranged at the bottom of the reaction kettle, and a sand core plate is arranged in the reaction kettle. Because the density of the lignite wax is smaller than that of the mixed liquid, the lignite wax is retained on the lower surface of the sand core plate by the first sand core plate after entering the reaction kettle, and the oxidant ozone passes through from bottom to top and is fully contacted with the lignite wax. As the temperature increases and the reaction proceeds, the montan wax gradually changes from a solid to a liquid and passes through the sand core plate to become smaller particles, increasing the contact area with the oxidizing agent. In addition, the sand core plate has the effect of redistributing the oxidant more evenly. After the montan wax passes through all the sand core plates, the montan wax is collected and overflows into a cooling tank. After the refined wax is cooled, the refined wax is changed from liquid to solid, the liquid is filtered, and the mixed liquid returns to the reaction kettle for continuous use. And (4) after the refined wax passes through a dryer, forming to obtain a final product. The traditional reaction kettle has no sand core plate distribution, the oxidant can only react on the surface of the wax liquid, and the inside of the traditional reaction kettle can not participate in the reaction, so that the traditional reaction kettle is the main reason for the wax product to be always yellow.

In a second aspect, the present invention provides the use of an apparatus according to the first aspect in the refining of crude montan wax.

In a third aspect, the present invention provides a process for refining a crude montan wax, comprising contacting a crude montan wax feedstock with ozone to obtain a refined montan wax.

According to some embodiments of the invention, the method is implemented in an apparatus according to the first aspect.

According to some embodiments of the invention, the method comprises:

step A: enabling the raw material of the coarse montan wax, the ozone and the optional auxiliary agent to enter a refining reaction kettle through a feed inlet of the refining reaction kettle to contact with each other to generate liquid montan wax;

and B: and the liquid lignite wax passes through the sand core plate, flows out of a discharge hole of the refining reaction kettle, is cooled, and preferably enters a cooling tank for cooling to obtain a cooled lignite wax material flow.

According to a preferred embodiment of the invention, the method further comprises step C: and filtering the cooled lignite wax material flow through a filter, returning the obtained liquid to the refining reaction kettle for recycling, and drying the obtained solid in a dryer to obtain the refined lignite wax.

According to a preferred embodiment of the invention, the method further comprises a step D: and the refined montan wax enters a forming machine for forming.

According to a preferred embodiment of the invention, the refining of the crude montan wax comprises:

step A: enabling a crude montan wax raw material from a montan wax raw material tank, ozone from an ozone generator and an auxiliary agent from an auxiliary agent tank to enter a refining reaction kettle through a feed inlet arranged at the lower part of the refining reaction kettle to contact with each other to generate liquid montan wax;

and B: the liquid lignite wax passes through the sand core plate, flows out of a discharge hole formed in the upper part of the refining reaction kettle, is cooled, and preferably enters a cooling tank for cooling to obtain a cooled lignite wax material flow;

and C: and filtering the cooled material flow through a filter, returning the obtained liquid to the refining reaction kettle for recycling, and drying the obtained solid in a dryer to obtain the refined montan wax.

According to a preferred embodiment of the invention, the method further comprises a step D: and (4) feeding the refined montan wax into a forming machine for forming.

According to some embodiments of the invention, the temperature at which the crude montan wax feedstock is contacted with ozone is 60-120 ℃, e.g., 65 ℃, 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃, 100 ℃, 105 ℃, 110 ℃, 115 ℃.

According to a preferred embodiment of the invention, the temperature at which the raw lignite wax feed is contacted with ozone is in the range of 80 to 100 ℃.

According to some embodiments of the invention, the contact time of the raw material of the coarse montan wax with ozone is 20-120min, such as 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110 min.

According to a preferred embodiment of the invention, the contact time of the raw lignite wax feed and ozone is 30-60 min.

According to some embodiments of the invention, the coarse montan wax is flaked and/or pelletized.

According to a preferred embodiment of the invention, the coarse montan wax has a particle size of 1 to 3 mm; the whiteness was 4.2%.

The invention selects the ozone with stronger oxidation performance as the oxidant, and preferably, the oxidation temperature and time of the ozone are adjusted, so that the color developing substances in the montan wax are oxidized more thoroughly, and the white refined wax with lighter color is obtained.

According to some embodiments of the invention, the mass ratio of the raw lignite wax material to the ozone is 100 (0.5-20).

According to the preferred embodiment of the invention, the mass ratio of the raw material of the coarse montan wax and the ozone is 100 (1-10).

According to some embodiments of the invention, the mass ratio of the raw material of the coarse montan wax and the auxiliary agent is 100 (0.01-2).

According to the preferred embodiment of the invention, the mass ratio of the raw material of the coarse montan wax and the auxiliary agent is 100 (0.1-0.5)

According to some embodiments of the invention, the adjuvant is selected from alcohol compounds. In the invention, as a small amount of acidic substances are generated along with the progress of the oxidation reaction, the pH value of the system is reduced, the ozone oxidation reaction is slowed down, and the auxiliary agent mainly acts to react with the generated acidic substances, so that the pH value of the system is ensured to be in a certain range.

According to a preferred embodiment of the invention, the auxiliary agent is selected from one or more of the alcohol compounds of C2-C10.

According to a further preferred embodiment of the present invention, the adjuvant is selected from one or more of ethanol, propanol and butanol.

According to some embodiments of the invention, the method further comprises condensing the gas in the cooling tank through a condenser, and discharging the non-condensable gas in the condenser after the non-condensable gas is treated by a tail gas treater.

According to some embodiments of the invention, the montan wax feedstock is pushed from a feed tank into a finishing reactor; the ozone generator generates ozone, and the ozone enters the refining reaction kettle; the auxiliary agent in the auxiliary agent tank is supplemented according to the consumption of the auxiliary agent in the refining reaction kettle; the reaction temperature in the reaction kettle is 80-100 ℃, the montan wax is gradually decolored along with the reaction, and the montan wax passes through the sand core plate and is gathered to the top of the kettle; overflowing the gathered refined wax after the reaction into a cooling tank, and gradually solidifying the refined wax into a solid; the material flow in the cooling tank enters a filter, and the solid refined wax enters a dryer for further drying after being washed by water; the liquid mother liquor returns to the refining reactor to be continuously used as reaction mother liquor for recycling; feeding the dried solid wax into a refined wax storage tank, and then molding and packaging the solid wax by a molding machine; and (4) further condensing the non-condensable gas in the refining reaction kettle and the cooling tank in a condenser, returning the liquid to the cooling tank, and discharging the non-condensable gas after passing through a tail gas processor.

The invention has the following beneficial effects: the reaction device can increase the contact area between the oxidant and the wax, so that the color developing substances in the montan wax are oxidized more thoroughly, and white refined wax with lighter color is obtained. The refined wax prepared according to the invention has a high whiteness value, usually more than 65%, even up to 74.6%, on the premise of ensuring a high yield (usually more than 75%, even up to 90.4%), and the production process of the method is nontoxic, and the discharge amount of wastewater is greatly reduced.

Drawings

Fig. 1 is a schematic diagram of a device for refining coarse montan wax according to the invention, wherein 1, a montan wax raw material tank, 2, an ozone generator, 3, an auxiliary agent tank, 4, a refining reaction kettle, 5, a cooling tank, 6, a filter, 7, a condenser, 8, a dryer, 9, a refined wax storage tank, 10, a forming machine, 11, an exhaust gas processor, 12 and a sand core plate.

Detailed Description

The invention will be further described with reference to the following figures and examples, which are given by way of illustration only and are not intended to limit the scope of the invention.

The following examples employ a refining apparatus shown in FIG. 1, wherein 1, a montan wax raw material tank, 2, an ozone generator, 3, an auxiliary agent tank, 4, a refining reactor, 5, a cooling tank, 6, a filter, 7, a condenser, 8, a dryer, 9, a refined wax storage tank, 10, a molding machine, 11, an exhaust gas treater, 12, and a sand core plate.

The degreased wax used in all the following examples and comparative examples was obtained by degreasing lignite slack wax. Taking a certain amount of crude lignite wax, putting the crude lignite wax into ethyl acetate at room temperature for soaking, wherein the solid-to-liquid ratio (mass ratio) is 1:5, reacting for 20min, and then putting the resin into an ethyl acetate solution to change the solution into a dark color. And after filtering, continuously adding fresh ethyl acetate, repeating the same soaking and filtering processes until the ethyl acetate solution is colorless, and finishing the degreasing of the montan wax to obtain the degreased wax.

In all of the following examples and comparative examples, the whiteness was measured by the following method:

1. grinding a sample to be tested into powder with the particle size of less than 0.2mm, putting the powder into a powder testing box of a whiteness instrument (model wbs-2), and compacting the sample by using a clean round glass plate to obtain the sample with the thickness of 4-5 mm.

2. The whiteness meter adopts an LED light source, the aperture phi of the test is 30mm, and the sample is detected after preheating, zero calibration and standard calibration. The sample holder was gently lifted to the measurement port, and the indicated value was the sample whiteness, which was the blue whiteness WB ═ R457.