阅读说明：本技术 一种防粘结剂及其应用和一种组合物在制备防粘结剂中的应用 (Anti-adhesion agent, application thereof and application of composition in preparation of anti-adhesion agent ) 是由 王伟 汪恩阳 李国红 鲁佳 于 2021-10-18 设计创作，主要内容包括：本发明涉及一种防粘结剂及其应用和一种组合物在制备防粘结剂中的应用,属于石油化工技术领域。本发明的防粘结剂主要由脱蜡油和蜡下油组成；所述防粘结剂的凝点为10～40℃；所述防粘结剂在100℃时的运动粘度为6-10mm～(2)/s。本发明的防粘结剂的质量稳定,安全环保,对生态环境和人体健康无害。(The invention relates to an anti-adhesion agent, application thereof and application of a composition in preparation of the anti-adhesion agent, and belongs to the technical field of petrochemical industry. The anti-caking agent mainly comprises dewaxing oil and wax-bottom oil; the condensation point of the anti-sticking agent is 10-40 ℃; the kinematic viscosity of the anti-bonding agent at 100 ℃ is 6-10mm 2 And s. The anti-sticking agent disclosed by the invention is stable in quality, safe and environment-friendly, and harmless to the ecological environment and human health.)

1. An anti-caking agent, which is characterized in that the anti-caking agent mainly comprises dewaxing oil and wax-less oil; the condensation point of the anti-sticking agent is 10-40 ℃; the kinematic viscosity of the anti-bonding agent at 100 ℃ is 6-10mm²/s。

2. The anti-blocking agent according to claim 1, wherein the mass ratio of the dewaxed oil to the undersized oil is 40-140: 10-40.

3. The anti-blocking agent according to claim 1 or 2, wherein the dewaxing oil has a condensation point of-12 to-5 ℃; the kinematic viscosity of the dewaxed oil at 100 ℃ is 5-11mm²/s。

4. The anti-blocking agent according to claim 1 or 2, wherein the condensation point of the wax oil is 30-45 ℃; the kinematic viscosity of the wax oil at 100 ℃ is 8-11mm²/s。

5. The anti-blocking agent according to claim 1 or 2, wherein the dewaxed oil consists essentially of a reduced second dewaxing oil and a reduced third dewaxing oil; the mass ratio of the second-line reduced dewaxed oil to the third-line reduced dewaxed oil is 20-70: 20-70; the under-wax oil comprises a minus-line under-wax oil.

6. The anti-caking agent according to claim 5, wherein the reduced second-line dewaxed oil is prepared from reduced second-line distillate oil by furfural refining and ketone-benzene dewaxing; the distillation range of the reduced second-line distillate is 360-420 ℃.

7. The anti-caking agent according to claim 5, wherein the three-line-reduced dewaxed oil is prepared from three-line-reduced distillate oil by furfural refining and ketone-benzene dewaxing; the distillation range of the reduced linear distillate oil is 380-460 ℃.

8. The anti-caking agent according to claim 5, wherein the minus four-line dewaxing fluid is prepared from minus four-line distillate oil through furfural refining and ketone-benzene dewaxing; the distillation range of the minus four-line distillate oil is 420-500 ℃.

9. Use of an anti-caking agent according to any one of claims 1 to 8 as an anti-caking agent for fertilizers.

10. Use of a composition for the preparation of an anti-adhesive agent, wherein the composition consists of a dewaxed oil and a wax-less oil; the condensation point of the composition is 10-40 ℃; the kinematic viscosity of the composition at 100 ℃ is 6-10mm²/s。

Technical Field

The invention relates to an anti-adhesion agent, application thereof and application of a composition in preparation of the anti-adhesion agent, and belongs to the technical field of petrochemical industry.

Background

The compound fertilizer brings a plurality of difficulties to fertilizer users due to the problems of caking, dusting, moisture absorption, phase change, crystallization and the like. The agglomerated fertilizer must be crushed and rescreened, which adds additional cost and also results in loss of fertilizer and dust, which is a health hazard to the operator. Dust is inevitable in fertilizer production and also occurs during storage and transportation. The excessive dust amount in the production device brings harm to the environment and the health of operators, also influences the production efficiency of equipment and increases the maintenance cost of the device. Aiming at the caking of the fertilizer, various manufacturers take various measures, such as improving the production process and equipment, optimizing the raw material composition, reducing the moisture content and the outlet temperature of the product, improving the strength and the uniformity of particles and the like, and the measures relieve the caking of the fertilizer to a certain extent. The anti-caking agent is coated on the surfaces of granulated fertilizer particles, so that the problems of caking and dust of the fertilizer can be solved, and the moisture absorption degree of the fertilizer can be reduced. However, the existing anti-caking agent for compound fertilizers takes semi-asphalt and furfural extract oil as raw materials, and has dark color, large pollution and harm to the environment. The semi-asphalt and furfural extract oil contain anthracene, phenanthrene and other polycyclic aromatic hydrocarbon compounds, so that the asphalt has strong toxicity and carcinogenicity, and poses serious threats to the ecological environment and human health.

Disclosure of Invention

The invention aims to provide an anti-caking agent for solving the problems of dark color, high pollution and harm to the environment of the existing anti-caking agent for compound fertilizers.

The second purpose of the invention is to provide an anti-caking agent for fertilizer.

The third purpose of the invention is to provide the application of the composition in preparing the anti-adhesive agent.

In order to achieve the purpose, the anti-bonding agent adopts the technical scheme that:

an anti-caking agent, which mainly comprises dewaxed oil and wax-bottom oil; the condensation point of the anti-sticking agent is 10-40 ℃; the kinematic viscosity of the anti-bonding agent at 100 ℃ is 6-10mm²/s。

The anti-sticking agent disclosed by the invention is stable in quality, safe and environment-friendly, and harmless to the ecological environment and human health. The anti-bonding agent can be used for preventing bonding of fertilizer powder and also can be used for preventing bonding of explosive powder.

The pour point is obtained by measuring according to GB/T510-; the kinematic viscosity is obtained by measuring according to GB/T30515-.

Preferably, the mass fraction of the polycyclic aromatic hydrocarbon in the anti-caking agent is less than or equal to 3.0%. The mass fraction of the polycyclic aromatic hydrocarbon is measured according to IP346 'determination of polycyclic aromatic hydrocarbon-dimethyl sulfoxide enrichment and shading index method'.

Preferably, the color of the anti-blocking agent is not more than 3.5. The chromaticity is measured according to GB/T6540-.

Preferably, the anti-blocking agent has a flash point of not less than 180 ℃. The flash point is measured according to GB/T3536 & 2008 & lt & gt determination of flash point and ignition point of petroleum products & lt & gt Cleveland open cup method & gt.

Preferably, the mass ratio of the dewaxed oil to the wax-less oil is 40-140: 10-40.

Preferably, the dewaxing oil has a freezing point of-12 to-5 ℃. Preferably, the kinematic viscosity of the dewaxed oil at 100 ℃ is 5 to 11mm²/s。

Preferably, the condensation point of the wax oil is 30-45 ℃. Preferably, the kinematic viscosity of the undersea oil at 100 ℃ is from 8 to 11mm²/s。

Preferably, the dewaxed oil consists essentially of a reduced second line dewaxed oil and a reduced third line dewaxed oil. Preferably, the mass ratio of the second-line reduced dewaxing oil to the third-line reduced dewaxing oil is 20-70: 20-70.

Preferably, the condensation point of the second-line dewaxing oil is-12 to-5 ℃. Preferably, the kinematic viscosity of the second-line dewaxing oil at 100 ℃ is 5-7mm²/s。

Preferably, the condensation point of the three-line-reduced dewaxing oil is-11 to-5 ℃.Preferably, the kinematic viscosity of the three-line-reduced dewaxing oil at 100 ℃ is 8-11mm²/s。

Preferably, the under-wax oil comprises minus-line under-wax oil.

Preferably, the condensation point of the minus four-line paraffin wax bottom oil is 30-45 ℃. Preferably, the kinematic viscosity of the reduced line under-wax oil at 100 ℃ is 8-11mm²/s。

Preferably, the second-line dewaxing oil is prepared by furfural refining and ketone benzene dewaxing of second-line distillate oil.

Preferably, the distillation range of the reduced second-line distillate is 360-420 ℃.

Preferably, the three-line-reduced dewaxed oil is prepared from three-line-reduced distillate oil through furfural refining and ketone benzene dewaxing.

Preferably, the distillation range of the reduced linear distillate is 380-460 ℃.

Preferably, the minus four-line wax bottom oil is prepared by furfural refining and ketone benzene dewaxing of minus four-line distillate oil.

Preferably, the distillation range of the minus four line distillate is 420-500 ℃.

The principle of ketone-benzene dewaxing is that the binary mixed solvent of methyl ethyl ketone and toluene is used to dissolve oil and wax in raw material (minus second-line distillate oil, minus third-line distillate oil and minus fourth-line distillate oil) successively, and during the cooling process of raw material, solvent is added successively to reduce viscosity of raw material and improve its flowability, and an appropriate condition is created for wax crystallization, so that wax is formed into uniform and compact crystals, and the oil and wax can be separated conveniently by filtering method. And adding the diluted solvent again to the separated wax liquid to dissolve the oil on the surface, and filtering to realize further oil-wax separation.

The anti-caking agent of the invention is applied as a fertilizer anti-caking agent, and the adopted technical scheme is as follows:

the anti-caking agent is applied as an anti-caking agent for fertilizers.

The anti-sticking agent is coated on the surface of fertilizer granules, a layer of film is formed on the surface of the fertilizer granules, so that the water absorption on the surface of the fertilizer can be prevented, the generation of a fertilizer salt bridge is blocked, the dissolution on the surface of the fertilizer is avoided, the capillary phenomenon and the bonding among the granules are reduced, and the caking of the fertilizer can be prevented.

The technical scheme adopted by the application of the composition in preparing the anti-adhesive agent is as follows:

use of a composition consisting of a dewaxed oil and a wax-less oil for the preparation of an anti-adhesive agent; the condensation point of the composition is 10-40 ℃; the kinematic viscosity of the composition at 100 ℃ is 6-10mm²/s。

The composition of the invention is safe and environment-friendly when being used for preparing the anti-caking agent, and is harmless to the ecological environment and human health.

Detailed Description

The technical solution of the present invention will be further explained with reference to the specific embodiments. It should be noted that the purpose of this embodiment is to further illustrate the present invention, and not to limit the protection scope of the present invention.

The preparation methods of the reduced second line dewaxed oil, the reduced third line dewaxed oil and the reduced fourth line dewaxed oil in the embodiment of the invention are as follows:

(1) taking Nanyang mixed crude oil as a raw material, carrying out reduced pressure distillation in a reduced pressure distillation device with two columns connected in series under the pressure of 6kPa, and cutting reduced line distillate oil with the distillation range of 360-420 ℃, reduced line distillate oil with the distillation range of 380-460 ℃ and reduced line distillate oil with the distillation range of 420-500 ℃;

(2) the second-line-reduced distillate oil with the distillation range of 360-420 ℃ firstly enters a heat exchanger with the temperature of 110 ℃ for heating, then enters a degassing tower for decompression (the pressure is 0.01MPa) degassing, the degassed second-line-reduced distillate oil enters the lower part of an extraction tower, furfural enters from the upper part of the extraction tower, furfural is in countercurrent contact with the degassed second-line-reduced distillate oil from top to bottom, and anthracene, anthracene and the furfural in the degassed second-line-reduced distillate oil are dissolved in the furfural,The method comprises the steps of discharging waste liquid formed by polycyclic aromatic hydrocarbon compounds such as phenanthrene and the like from the bottom of a tower under self pressure, removing second-line distillate oil (namely refined oil) of the polycyclic aromatic hydrocarbon compounds and a small amount of furfural to form refined liquid, discharging the refined liquid from the top of the tower under self pressure, heating the refined liquid to 210-80 ℃ through a heating furnace after heat exchange by a refined liquid-three-effect gas (III) heat exchanger and a refined liquid-refined oil heat exchanger, entering a refined liquid flash distillation tower (with the pressure of 0.01MPa) for flash distillation, condensing the refined liquid flash distillation gas to 70-80 ℃ through a refined liquid flash distillation condenser (with the pressure of 0.02MPa and the temperature of 183 ℃), entering a furfural flash distillation tower (with the pressure of 0.02MPa) for steam stripping, introducing the refined liquid obtained from the bottom of the flash distillation tower under self pressure into a refined liquid stripping tower (with the temperature of 100-110 ℃), wherein the furfural is subjected to pressure reduction (with the pressure of 0.015-0.02 MPa), extracting from the top of the tower, extracting refined oil obtained at the bottom of a refined liquid stripping tower by a refined oil pump, cooling the refined oil in a heat exchanger for heat exchange, cooling the refined oil to 80 ℃ to obtain refined oil, adding a methyl ethyl ketone-toluene binary mixed solvent (the volume ratio of methyl ethyl ketone to toluene is 1: 2-1: 3, and the volume ratio of the binary mixed solvent to the refined oil is 1.2:1) into the refined oil successively in the cooling process, filtering to separate the wax oil to obtain oil and wax liquid, adding a methyl ethyl ketone-toluene binary mixed solvent (the volume ratio of methyl ethyl ketone to toluene is 1: 2-1: 3, and the volume ratio of the binary mixed solvent to the refined oil is 1.2:1) into the wax liquid again, filtering to separate the wax oil again to obtain oil and wax liquid, adding a methyl ethyl ketone-toluene binary mixed solvent (the volume ratio of methyl ethyl ketone to toluene is 1: 2-1: 3 into the wax liquid again, the volume ratio of the binary mixed solvent to the refined oil is 1.2:1), filtering and separating wax oil again to obtain oil and wax liquid, respectively sending the filtrate, the wax liquid and the wax oil liquid which are separated by three-stage filtering to a recovery system, removing the solvent to obtain the second-line reduced dewaxed oil, the wax and the second-line reduced wax oil in sequence, wherein the condensation point of the obtained second-line reduced dewaxed oil is-12 to-5 ℃, and the kinematic viscosity at 100 ℃ is 5-7mm²/s。

(3) The reduced-length distillate oil with the distillation range of 380-460 ℃ firstly enters a heat exchanger with the temperature of 110 ℃ for heating, then enters a degassing tower for degassing under reduced pressure (the pressure is 0.01MPa), the degassed reduced-length distillate oil enters the lower part of an extraction tower, and furfural is extracted from furfuralThe furfural enters the upper part of the tower from top to bottom and is in countercurrent contact with degassed three-way distillate oil, the furfural dissolves polycyclic aromatic hydrocarbon compounds such as anthracene, phenanthrene and the like in the degassed three-way distillate oil to form waste liquid, the waste liquid is discharged from the bottom of the tower under self pressure, the refined liquid is formed by the three-way distillate oil (namely refined oil) without polycyclic aromatic hydrocarbon compounds and a small amount of furfural, the refined liquid is discharged from the top of the tower under self pressure, the refined liquid is subjected to heat exchange through a refined liquid-three-effect gas (III) heat exchanger and a refined liquid-refined oil heat exchanger respectively, then is heated to 210 ℃ and 220 ℃ through a heating furnace, enters a refined liquid flash distillation tower (with the pressure of 0.01MPa) for flash distillation, part of the furfural obtained flash distillation is called refined liquid flash distillation gas, the refined liquid flash distillation gas is condensed to 70-80 ℃ through a refined liquid flash distillation condenser (with the pressure of 0.02MPa and the temperature of 183 ℃) and then enters a furfural flash distillation tower (with the pressure of 0.02MPa), the refined liquid obtained at the bottom enters a refined liquid stripping tower under self pressure of 100 ℃ and 110 ℃), wherein, furfural is subjected to reduced pressure (the pressure is 0.015-0.02 MPa) steam stripping, extracted from the top of the tower, refined oil obtained from the bottom of a refined liquid steam stripping tower is extracted to a heat exchanger through a refined oil pump for heat exchange and cooling, and then is cooled to 80 ℃ in a refined oil cooler to obtain refined oil, the refined oil is sequentially added with a methyl ethyl ketone-toluene binary mixed solvent (the volume ratio of the methyl ethyl ketone to the toluene is 1: 2-1: 3, the volume ratio of the binary mixed solvent to the refined oil is 1.3:1) in the cooling process to obtain oil and wax liquid, the wax oil is separated through filtration to obtain oil and wax liquid, the methyl ethyl ketone-toluene binary mixed solvent is added into the wax liquid again (the volume ratio of the methyl ethyl ketone to the toluene is 1: 2-1: 3, the volume ratio of the binary mixed solvent to the refined oil is 1.3:1), the wax oil is separated through filtration to obtain oil and wax liquid, the methyl ethyl ketone-toluene binary mixed solvent is added into the wax liquid again (the volume ratio of the methyl ethyl ketone to the toluene is 1: 2-1: 3, the volume ratio of the binary mixed solvent to the refined oil is 1.3:1), filtering and separating wax oil again to obtain oil and wax liquid, respectively sending the filtrate, the wax liquid and the wax oil liquid which are separated by three-stage filtering to a recovery system, removing the solvent to obtain three-line reduced dewaxed oil, wax and three-line reduced wax oil in sequence, wherein the condensation point of the obtained three-line reduced dewaxed oil is-11 to-5 ℃, and the kinematic viscosity at 100 ℃ is 8-11mm²/s。

(4) The crude minus four line distillate oil with the distillation range of 420-500 ℃ firstly enters a heat exchanger with the temperature of 110 DEG CHeating, degassing in a degassing tower under reduced pressure (0.01 MPa), introducing degassed four-line distillate oil into the lower part of an extraction tower, introducing furfural from the upper part of the extraction tower, contacting furfural with degassed four-line distillate oil in a countercurrent manner from top to bottom, dissolving anthracene, phenanthrene and other polycyclic aromatic compounds in the degassed four-line distillate oil by furfural to obtain waste liquid, discharging the waste liquid from the bottom of the extraction tower, removing polycyclic aromatic compounds from the four-line distillate oil (i.e. refined oil) and a small amount of furfural to obtain refined liquid, discharging the refined liquid from the top of the extraction tower under the pressure, performing heat exchange on the refined liquid by a refined liquid-three-way gas (III) heat exchanger and a refined liquid-refined oil heat exchanger respectively, heating to 210 ℃ and 220 ℃, introducing the refined liquid into a refined liquid flash distillation tower (pressure of 0.01MPa) for flash distillation, wherein part of furfural discharged flash distillation is called refined liquid flash distillation gas, performing flash distillation on the refined liquid flash distillation gas by a refined liquid flash distillation condenser (pressure of 0.02MPa, condensing at 183 ℃ to 75-85 ℃, then feeding the condensate into a furfural flash tower (the pressure is 0.02MPa), enabling the refined liquid obtained at the bottom of the flash tower to enter a refined liquid stripping tower (the temperature is 105-115 ℃) under self pressure, stripping furfural under reduced pressure (the pressure is 0.015-0.02 MPa), extracting from the tower top, pumping the refined oil obtained at the bottom of the refined liquid stripping tower to a heat exchanger for heat exchange and cooling through a refined oil pump, cooling to 80 ℃ through a refined oil cooler to obtain refined oil, adding a methyl ethyl ketone-toluene binary mixed solvent (the volume ratio of the methyl ethyl ketone to the toluene is 1: 3-1: 4 and the volume ratio of the binary mixed solvent to the refined oil is 1.4:1) in the cooling process of the refined oil, separating the wax oil through filtration to obtain oil and wax liquid, adding the methyl ethyl ketone-toluene binary mixed solvent again (the volume ratio of the methyl ethyl ketone to the toluene is 1: 3-1: 4, the volume ratio of the binary mixed solvent to the refined oil is 1.4:1), filtering and separating wax oil again to obtain oil and wax liquid, adding the methyl ethyl ketone-toluene binary mixed solvent again into the wax liquid (the volume ratio of the methyl ethyl ketone to the toluene is 1: 3-1: 4, and the volume ratio of the binary mixed solvent to the refined oil is 1.4:1), filtering and separating wax oil again to obtain oil and wax liquid, respectively sending the filtrate, the wax liquid and the wax oil liquid separated by three-stage filtering to a recovery system, removing the solvent to obtain minus-four-line dewaxed oil, wax and minus-four-line wax oil in sequence, wherein the condensation point of the minus-four-line wax oil is 30-45 ℃, and the kinematic viscosity is 100 DEG CThe degree of the alloy is 8-11mm²/s。

The concrete examples of the anti-bonding agent of the invention are as follows:

example 1

The anti-blocking agent of the embodiment comprises dewaxed oil and wax-less oil, wherein the dewaxed oil comprises reduced second line dewaxed oil and reduced third line dewaxed oil, the wax-less oil is reduced fourth line wax-less oil, and the mass ratio of the reduced second line dewaxed oil, the reduced third line dewaxed oil and the reduced fourth line wax-less oil is 20:70: 10.

Example 2

The anti-blocking agent of the embodiment comprises dewaxed oil and wax-less oil, wherein the dewaxed oil comprises reduced second line dewaxed oil and reduced third line dewaxed oil, the wax-less oil is reduced fourth line wax-less oil, and the mass ratio of the reduced second line dewaxed oil, the reduced third line dewaxed oil and the reduced fourth line wax-less oil is 70:20: 10.

Example 3

The anti-blocking agent of the embodiment comprises dewaxed oil and wax-less oil, wherein the dewaxed oil comprises reduced second line dewaxed oil and reduced third line dewaxed oil, the wax-less oil is reduced fourth line wax-less oil, and the mass ratio of the reduced second line dewaxed oil, the reduced third line dewaxed oil and the reduced fourth line wax-less oil is 30:30: 40.

Example 4

The anti-blocking agent of the embodiment comprises dewaxed oil and wax-less oil, wherein the dewaxed oil comprises reduced second line dewaxed oil and reduced third line dewaxed oil, the wax-less oil is reduced fourth line wax-less oil, and the mass ratio of the reduced second line dewaxed oil, the reduced third line dewaxed oil and the reduced fourth line wax-less oil is 35:40: 25.

The anti-caking agents of the examples 1 to 4 were tested for the mass fraction (PCA content) of the condensation point, the flash point, the chromaticity and the polycyclic aromatic hydrocarbon in the anti-caking agent according to GB/T510-.

Sample (I)	Freezing point (. degree. C.)	Flash Point (. degree.C.)	Viscosity (mm)2/s)	Color intensity	PCA content
						Example 1	12	211	9.54	3.0	1.16％
Example 2	11	196	6.68	2.0	1.12％
						Example 3	35	215	8.41	3.5	1.23％
Example 4	31	212	8.02	3.0	1.19％

As can be seen from the above table, the anti-blocking agent in examples 1 to 4 has a condensation point of 10 to 40 ℃, and can satisfy the requirements of having certain fluidity at normal temperature and having a certain wax content; the anti-blocking agents of examples 1 to 4 had flash points of not less than 180 ℃ and kinematic viscosities of 6 to 10mm at 100 ℃²The chromaticity is not more than 3.5, and the mass fraction of the polycyclic aromatic hydrocarbon is not more than 3.0 percent.

Secondly, the concrete examples of the application of the anti-caking agent of the invention as a fertilizer anti-caking agent are as follows:

the anti-caking agent of example 1, example 2, example 3 or example 4 may be used as a fertilizer anti-caking agent.

Third, the specific examples of the application of the composition of the present invention in preparing an anti-adhesive agent are as follows:

example 5

In this example, a composition comprising dewaxed oil and wax-less oil was mixed with a small amount of resin to prepare an anti-blocking agent; the dewaxed oil consists of reduced second-line dewaxed oil and reduced third-line dewaxed oil, the wax-down oil is reduced fourth-line wax-down oil, and the mass ratio of the reduced second-line dewaxed oil to the reduced third-line dewaxed oil to the reduced fourth-line wax-down oil is 20:70: 10.

Example 6

In this example, a composition consisting of dewaxed oil and wax-less oil was mixed with a small amount of synthetic wax to prepare an anti-blocking agent; the dewaxed oil consists of reduced second-line dewaxed oil and reduced third-line dewaxed oil, the wax-down oil is reduced fourth-line wax-down oil, and the mass ratio of the reduced second-line dewaxed oil to the reduced third-line dewaxed oil to the reduced fourth-line wax-down oil is 70:20: 10.

Example 7

In this example, a composition comprising dewaxed oil and wax-less oil was mixed with a small amount of resin and a small amount of synthetic wax to prepare an anti-blocking agent; the dewaxed oil consists of reduced second-line dewaxed oil and reduced third-line dewaxed oil, the wax-down oil is reduced fourth-line wax-down oil, and the mass ratio of the reduced second-line dewaxed oil to the reduced third-line dewaxed oil to the reduced fourth-line wax-down oil is 30:30: 40.