CN111303941A - Method for extracting montan wax from lignite - Google Patents
Method for extracting montan wax from lignite Download PDFInfo
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- CN111303941A CN111303941A CN201811518173.7A CN201811518173A CN111303941A CN 111303941 A CN111303941 A CN 111303941A CN 201811518173 A CN201811518173 A CN 201811518173A CN 111303941 A CN111303941 A CN 111303941A
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
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Abstract
The invention relates to the field of montan wax, and discloses a method for extracting montan wax from lignite, which comprises the following steps: (1) leaching lignite particles by using an organic solvent, and performing solid-liquid separation to obtain a wax-containing liquid; (2) cooling the wax-containing liquid obtained in the step (1), adding an accelerant into the wax-containing liquid in the cooling process, and filtering and separating after crystallization to obtain a montan wax product; wherein the accelerator is polyacrylate-g-polyvinyl ester. The method of the invention extracts the high-purity montan wax by simple processes of leaching, solid-liquid separation of leaching solution, cooling, adding accelerant and crystallization, wherein the resin content can reach below 5 weight percent.
Description
Technical Field
The invention relates to a method for extracting montan wax from lignite.
Background
The main components of montan wax are pure wax, resin and asphalt. Different coal-forming plants and coal-forming environments also have different compositions of extracted montan wax from coal. Asphalt is a high-melting-point component, and after being heated, the asphalt shows the phenomena of viscosity, difficulty in flowing, difficulty in diffusion and the like, so that the viscosity is increased, and the fluidity is poor. The resin is a vegetable resin, has characteristics similar to rosin, and is sticky. 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. Particularly, when the resin is used for floor wax, shoe polish and other products, the surface of the floor or the leather shoes is not smooth, the waxing is difficult, and dust is easy to adhere to the resin. Generally, the asphalt and resin in the montan wax are harmful components, and the smaller the content, the better the quality of the montan wax. In the crude wax of the German montan wax, the resin content is generally lower than 15 percent, and the crude wax can basically and directly meet the requirements of a plurality of industrial applications; in the crude wax of montan wax in China, the resin content is generally higher and reaches 20-40%.
At present, the prior art for producing high-purity montan wax is less, and the method disclosed in CN101906320A uses a compound organic solvent, utilizes the different solubility of the organic solvent to different components, improves the quality of montan wax products, and can obtain products with resin content lower than 16% and asphalt content lower than 6%.
The resin content of the montan wax obtained by the method is still high, so that a simple method for extracting higher-purity montan wax from lignite is needed.
Disclosure of Invention
The invention aims to overcome the problems of low purity of the obtained montan wax product and the like in the prior art, and provides a method for extracting montan wax from lignite.
In order to achieve the above object, a first aspect of the present invention provides a method for extracting montan wax from lignite, the method comprising:
(1) leaching lignite particles by using an organic solvent, and performing solid-liquid separation to obtain a wax-containing liquid;
(2) cooling the wax-containing liquid obtained in the step (1), adding an accelerant into the wax-containing liquid in the cooling process, and filtering and separating after crystallization to obtain a montan wax product; wherein the accelerator is polyacrylate-g-polyvinyl ester.
The method extracts the high-purity montan wax from the lignite through simple processes of leaching, solid-liquid separation of leaching solution, cooling, addition of the accelerant and crystallization, wherein the resin content can reach below 5 weight percent, the degreasing step of the traditional method is omitted in the process, the cooling crystallization time is shortened, and the method has good application prospect.
Drawings
FIG. 1 is a schematic diagram of one embodiment of the process of the present invention;
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a method for extracting montan wax from lignite, which comprises the following steps:
(1) leaching lignite particles by using an organic solvent, and performing solid-liquid separation to obtain a wax-containing liquid;
(2) cooling the wax-containing liquid obtained in the step (1), adding an accelerant into the wax-containing liquid in the cooling process, and filtering and separating after crystallization to obtain a montan wax product; wherein the accelerator is polyacrylate-g-polyvinyl ester.
One embodiment of the method of the present invention is shown in fig. 1. In the invention, the polyacrylate-g-polyvinyl ester is a graft copolymer of acrylate and vinyl ester, wherein the polyacrylate is a main chain, and the polyvinyl ester is grafted on the main chain. The vinyl ester has the general formula R1COOCH2＝CH2Wherein R is1Is C1-C8The propylene ofThe acid ester has the formula CH2＝CH2COOR2Wherein R is2Is C1-C8Alkyl group of (1).
In the present invention, the particle size of the lignite particles is less than 15mm, preferably, the particle size of the lignite particles is less than 3 mm. Preferably, the lignite is crushed and sieved before extracting the lignite wax, for example, the lignite can be crushed by adding a crusher and then sieved by a sieve with the aperture of 3 mm. And drying the lignite particles with the particle size of less than 3mm for later use, returning the lignite particles with the particle size of more than 3mm to the previous crushing step, and crushing and sieving the lignite particles together with the raw material lignite.
In a preferred embodiment of the method according to the invention, the lignite particles are first dried to a moisture content of 15 to 30 wt.%, more preferably to a moisture content of 25 wt.%.
In the method of the present invention, the organic solvent may be a polar or non-polar solvent, and may be a single solvent or a mixture of multiple solvents, for example, one or more selected from toluene, petroleum ether, # 6 mineral spirits, n-hexane, cyclohexane, ethanol, isopropanol, n-propanol, acetone, methyl ethyl ketone, methyl formate, methyl acetate, ethyl formate, ethyl acetate, butyl acetate, propyl acetate, preferably ethanol, ethyl acetate, or acetone.
In the method of the present invention, in step (1), the leaching conditions include: the temperature is 70-100 ℃, and the time is 0.5-4 h; preferably, the temperature is 80-100 ℃ and the time is 1-3 h. And settling and carrying out solid-liquid separation on the leaching solution obtained after leaching to obtain a wax-containing solution without solid impurities and dewaxed coal. In the whole process of sedimentation and solid-liquid separation, the temperature of the leaching solution is maintained to be more than 50 ℃ to prevent wax from being separated out. Preferably, the solid-liquid separation is carried out at a temperature of from 50 ℃ to 100 ℃.
In the method of the present invention, in order to more preferably achieve crystallization of montan wax without precipitation of resin during cooling, it is necessary to control the concentration of the wax-containing liquid within a suitable range, for example, the concentration of montan wax in the wax-containing liquid is 30 to 200g/L, preferably 30 to 150 g/L. The concentration of montan wax in the wax-containing liquid is understood here to be the ratio of the mass of the product obtained after evaporation of the solvent contained in the wax-containing liquid to the volume of the wax-containing liquid.
In step (2) of the method of the present invention, the wax-containing liquid is cooled and crystallized. The cooling crystallization conditions comprise: the temperature is-10 to 30 ℃, and the duration is 10 to 90 min; preferably, the temperature is 0-25 ℃ and the duration is 10-60 min.
The inventor of the invention finds that the addition of the accelerator (polyacrylate-g-polyvinyl ester) in the process of cooling the wax-containing liquid can not only obviously shorten the cooling crystallization time, but also effectively improve the purity and yield of the montan wax. The accelerant is selected from one or more of polymethyl acrylate-g-polyvinyl acetate, polyethyl acrylate-g-polyvinyl acetate, polybutyl acrylate-g-polyvinyl acetate, polypropyl acrylate-g-polyvinyl valerate, polybutyl acrylate-g-polyvinyl propionate and polybutyl acrylate-g-polyvinyl butyrate, and preferably the accelerant is polybutyl acrylate-g-polyvinyl butyrate.
According to the invention, the addition amount of the accelerator influences the cooling crystallization time, and to a certain extent, the crystallization time is shorter as the addition amount is larger, but the quality of the obtained montan wax is influenced by an excessively large addition amount. Therefore, in a preferred embodiment of the method of the present invention, the accelerator is added in an amount of 0.1 to 5g, for example, 0.1, 0.2, 0.5, 0.6, 0.8, 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5, 5g, and any one of the ranges of any two of the above values, preferably 0.5 to 1g, based on 1L of the wax-containing liquid.
In a preferred embodiment according to the present invention, the particle size of the promoter is less than 1mm, more preferably less than 0.2 mm.
According to the invention, the accelerator can be prepared by the following method: carrying out solution polymerization on an acrylate monomer and an initiator, then adding a vinyl ester monomer into a reaction system for graft polymerization, and after the reaction is finished, carrying out spray drying to obtain the accelerator. The conditions of the solution polymerization include: the temperature is 90-110 ℃, and the time is 1-3 h; the solvent is at least one selected from No. 200 solvent oil, paraxylene, naphtha and diesel oil. The initiator used is selected from benzoyl peroxide, lauroyl peroxide, etc.
In the method, after the montan wax is crystallized and precipitated, the suspension containing montan wax particles is filtered and separated to obtain wet wax particles and a filtrate, wherein the filtrate is a degreasing solution containing resin.
The method also comprises the step of drying the wet wax particles to obtain the montan wax product. The drying conditions can be selected according to the prior art, for example according to the following: the temperature is 80-130 deg.C, preferably 90-100 deg.C. In one embodiment, the steam obtained during drying is condensed and returned to step (1) for leaching the lignite particles.
In one embodiment of the method of the present invention, the method further comprises recycling the filtrate obtained by filtering in step (2) to step (1) for leaching the lignite particles.
According to the method of the invention, after a plurality of cycles, when the filtrate, i.e. the degreasing solution, reaches saturation (wherein the resin content is more than 40% by weight), the cycle is stopped, the obtained filtrate is distilled, a resin product can be obtained at the bottom of the tower, and the tower top steam is cooled and recycled to the step (1) for leaching the lignite particles.
The method of the invention extracts the montan wax from the lignite as much as possible by utilizing the organic solvent at a higher leaching temperature, and at a lower temperature, the montan wax can be crystallized and separated out due to different solubilities of the montan wax and the resin in the organic solvent, the resin is remained in the organic solvent, and the accelerant is added in the cooling process, so that the crystallization time is obviously shortened, and the purity and the yield of the montan wax are improved. The method of the invention leads the resin content in the obtained montan wax to be lower, for example, less than 5 weight percent, even less than 2 weight percent through the processes of leaching, solid-liquid separation of leaching solution, cooling, adding accelerant and crystallization precipitation.
The present invention will be described in detail below by way of examples.
Example 1
(1) Preparing an accelerant: 500mL of No. 200 solvent oil and p-xylene are uniformly mixed according to the volume ratio of 1:1, added into a reaction kettle, continuously stirred and heated to 100 ℃. After the temperature is stable, 100mL of mixed solution of butyl acrylate and benzoyl peroxide with the volume ratio of 100:2 is added into the reaction kettle for reaction for 2 hours. Then 100mL of vinyl butyrate is added into the reaction kettle and reacted for 1 h. After the reaction is finished, spray drying is carried out to obtain the promoter of poly (butyl acrylate) -g-poly (vinyl butyrate) with the particle size of 0.1 mm.
(2) Extracting montan wax: pulverizing lignite to a particle size of less than 3mm, and leaching 50g of lignite particles (wherein the pure wax content is 3.74 wt%) with 100mL of a mixed solution of toluene and ethyl acetate (wherein the volume ratio of toluene to ethyl acetate is 1:1) at 90 ℃ for 3 h. After filtration, dewaxed coal and wax-containing liquid (the concentration of montan wax is 32g/L) are obtained. And (2) placing the obtained wax-containing liquid (the montan wax concentration is 32g/L) in a water cooling device at 5 ℃, simultaneously adding 0.07g of an accelerator (the polybutyl acrylate-g-polyvinyl butyrate obtained in the step (1)), cooling for 10min, and filtering to obtain a filtrate containing the resin and wet montan wax particles. The wet montan wax particles were dried to obtain 1.77g montan wax product. And distilling the filtrate containing the resin to obtain a resin product. The results of analyzing the contents of the montan wax products and the resin products according to GB/T2559-2005 montan wax determination method are shown in Table 1 below.
Example 2
(1) The accelerator was prepared as described in step (1) of example 1.
(2) Extracting montan wax: the lignite is crushed to the grain diameter of less than 3mm, 50g of lignite grains are taken to be leached with 200mL of cyclohexane at the temperature of 80 ℃, and the reaction time is 1 h. Filtering to obtain the dewaxed coal and the liquid containing the wax. And (3) putting the wax-containing liquid (which is concentrated to 30ml and the concentration of the montan wax is 100g/L) into a water cooling device at 15 ℃, simultaneously adding 0.015g of accelerator, cooling for 60min, and filtering to obtain a filtrate containing resin and wet montan wax particles. Drying the wet montan wax particles to obtain montan wax products. And distilling the filtrate containing the resin to obtain a resin product. The results of analyzing the contents of the montan wax products and the resin products according to GB/T2559-2005 montan wax determination method are shown in Table 1 below.
Example 3
(1) An accelerator was prepared by referring to step (1) of example 1.
(2) Extracting montan wax: the lignite is crushed to the grain diameter of less than 3mm, 50g of lignite grains are taken to be leached with 250mL of petroleum ether at the temperature of 70 ℃, and the reaction time is 2 hours. Filtering to obtain the dewaxed coal and the liquid containing the wax. And (3) putting the wax-containing liquid (which is concentrated to 20ml and the concentration of the montan wax is 146g/L) into a water cooling device at 25 ℃, simultaneously adding 0.02g of accelerator, cooling for 30min, and filtering to obtain a filtrate containing resin and wet montan wax particles. Drying the wet montan wax particles to obtain montan wax products. And distilling the filtrate containing the resin to obtain a resin product. The results of analyzing the contents of the montan wax products and the resin products according to GB/T2559-2005 montan wax determination method are shown in Table 1 below.
Example 4
Montan wax was extracted by the method described in example 1, except that the amount of the accelerator used was 0.6g, which was otherwise the same as in example 1. The content analysis of the obtained montan wax product and resin product was carried out according to GB/T2559 & 2005 montan wax determination method, and the results are shown in Table 1 below.
Example 5
Montan wax was extracted by the method described in example 1, except that the amount of the accelerator used was 0.008g, which was the same as in example 1. The content analysis of the obtained montan wax product and resin product was carried out according to GB/T2559 & 2005 montan wax determination method, and the results are shown in Table 1 below.
Example 6
Montan wax was extracted by the method described in example 1, except that the accelerator used had a particle size of 2mm, which was otherwise the same as in example 1. The content analysis of the obtained montan wax product and resin product was carried out according to GB/T2559 & 2005 montan wax determination method, and the results are shown in Table 1 below.
Example 7
Montan wax was extracted as described in example 1, except that the accelerator used was prepared by the following method: 400mL of No. 200 mineral spirits were added to the kettle, stirred continuously, and heated to 110 ℃. After the temperature is stable, 100mL of mixed solution of butyl acrylate and benzoyl peroxide with the volume ratio of 100:2 is added into the reaction kettle for reaction for 2 hours. Then 150mL of vinyl propionate is added into the reaction kettle and reacted for 1 h. After the reaction is finished, spray drying is carried out to obtain the promoter of poly (butyl acrylate) -g-poly (vinyl propionate), wherein the particle size is 0.1 mm. The rest is the same as in example 1. The content analysis of the obtained montan wax product and resin product was carried out according to GB/T2559 & 2005 montan wax determination method, and the results are shown in Table 1 below.
Example 8
Montan wax was extracted as described in example 1, except that the accelerator used was prepared by the following method: 500mL of p-xylene was added to the kettle, with constant stirring, and heated to 90 ℃. After the temperature is stable, 80mL of mixed solution of ethyl acrylate and benzoyl peroxide with the volume ratio of 100:2 is added into the reaction kettle for reaction for 2 hours. Then 100mL of vinyl acetate is added into the reaction kettle for reaction for 2 h. After the reaction is finished, the accelerant of poly (ethyl acrylate) -g-polyvinyl acetate with the grain diameter of 0.1mm is obtained by spray drying. The rest is the same as in example 1. The content analysis of the obtained montan wax product and resin product was carried out according to GB/T2559 & 2005 montan wax determination method, and the results are shown in Table 1 below.
Example 9
(1) Preparing an accelerant: 500mL of No. 200 solvent oil and naphtha are uniformly mixed according to the volume ratio of 1:1, added into a reaction kettle, continuously stirred and heated to 100 ℃. After the temperature is stabilized, 100mL of the mixed solution of propyl acrylate and benzoyl peroxide in the volume ratio of 100:1 is added into the reaction kettle and reacts for 1 h. Then 40mL of vinyl valerate is added into the reaction kettle and reacted for 2 h. After the reaction is finished, spray drying is carried out to obtain the promoter of poly propyl acrylate-g-polyvinyl valerate, and the particle size is 0.15 mm.
(2) Extracting montan wax: the lignite is crushed to the grain diameter of less than 3mm, 50g of lignite grains are taken to be leached with 200mL of ethyl acetate at the temperature of 70 ℃, and the reaction time is 4 hours. Filtering to obtain the dewaxed coal and the liquid containing the wax. And (2) putting the wax-containing liquid (which is concentrated to 104mL and has 30g/L of montan wax) into a water cooling device at the temperature of-10 ℃, simultaneously adding 0.625g of an accelerator (the polypropylene acrylate-g-polyvinyl valerate obtained in the step (1)), cooling for 80min, and filtering to obtain a filtrate containing the resin and wet montan wax particles. Drying the wet montan wax particles to obtain montan wax products. And distilling the filtrate containing the resin to obtain a resin product. The results of analyzing the contents of the montan wax products and the resin products according to GB/T2559-2005 montan wax determination method are shown in Table 1 below.
Comparative example 1
Montan wax was extracted according to example 1, except that no accelerator was added during cooling, and the procedure was the same as in example 1. The content analysis of the obtained montan wax product and resin product was carried out according to GB/T2559-2005 montan wax determination method, and the results are shown in Table 1 below.
Comparative example 2
Montan wax was extracted according to example 1, except that palm wax powder was added during cooling, which was the same as in example 1. The content analysis of the obtained montan wax product and resin product was carried out according to GB/T2559-2005 montan wax determination method, and the results are shown in Table 1 below.
Comparative example 3
Montan wax was extracted according to example 1, except that the obtained wax-containing liquid was subjected to evaporation of the solvent under reduced pressure to obtain a montan wax product. The content analysis of the obtained montan wax product was carried out according to GB/T2559-2005 montan wax determination method, and the results are shown in Table 1 below.
TABLE 1 montan wax product composition analysis
In table 1, the data of the component contents of the montan wax products are all test data, and the sum of the component contents is about 100%.
Here, the pure wax yield is calculated according to the following formula:
P％＝(Wproduct wax×ωProduct wax, wax%)/(WCoal (coal)×ωCoal, wax%)×100％
In the formula, P represents the wax yield%
WCoal (coal)Denotes the mass of lignite, g
ωCoal, waxRepresents the content of pure wax in lignite%
WProduct waxDenotes the mass of the montan wax product, g
ωProduct wax, waxIndicates the pure wax content,%, in the montan wax product.
As can be seen from the results in table 1, the montan wax product obtained in the examples of the present invention has a resin content as low as 1.12 wt%, a pure wax content of 95 wt% or more, and even as high as 98 wt% or more, and the wax yield of the process of the present invention is 80% or more, and even 90% or more. The method obtains the montan wax product with lower resin content by the processes of leaching, solid-liquid separation of leaching solution, cooling, adding the accelerant and crystallization, omits the fussy degreasing step in the prior art, and shortens the cooling crystallization time.
Claims (10)
1. A method of extracting montan wax from lignite, the method comprising:
(1) leaching lignite particles by using an organic solvent, and performing solid-liquid separation to obtain a wax-containing liquid;
(2) cooling the wax-containing liquid obtained in the step (1), adding an accelerant into the wax-containing liquid in the cooling process, and filtering and separating after crystallization to obtain a montan wax product;
wherein the accelerator is polyacrylate-g-polyvinyl ester.
2. The method according to claim 1, wherein in step (2), the accelerator is selected from one or more of polymethyl acrylate-g-polyvinyl acetate, polyethyl acrylate-g-polyvinyl acetate, polypropyl acrylate-g-polyvinyl valerate, polybutyl acrylate-g-polyvinyl acetate, polybutyl acrylate-g-polyvinyl propionate, and polybutyl acrylate-g-polyvinyl butyrate, preferably the accelerator is polybutyl acrylate-g-polyvinyl butyrate.
3. The process according to claim 1 or 2, wherein in step (2), the accelerator is added in an amount of 0.1 to 5g, preferably 0.5 to 1g, relative to 1L of the wax-containing liquid.
4. A process according to claim 1 or 2, wherein in step (2) the particle size of the promoter is less than 1mm, preferably less than 0.2 mm.
5. A process according to claim 1 or 2, wherein the accelerator is prepared by: carrying out solution polymerization on an acrylate monomer and an initiator, then adding a vinyl ester monomer into a reaction system for graft polymerization, and after the reaction is finished, carrying out spray drying to obtain the accelerator.
6. The method according to claim 1 or 2, wherein in step (1), the organic solvent is selected from one or more of toluene, petroleum ether, # 6 solvent oil, n-hexane, cyclohexane, ethanol, isopropanol, n-propanol, acetone, butanone, methyl ethyl ketone, methyl formate, methyl acetate, ethyl formate, ethyl acetate, butyl acetate, propyl acetate, preferably the organic solvent is ethanol, ethyl acetate or acetone.
7. The method according to claim 1 or 2, wherein in step (1), the leaching conditions comprise: the temperature is 70-100 ℃, and the time is 0.5-4 h; preferably, the temperature is 80-100 ℃ and the time is 1-3 h.
8. A method according to claim 1 or 2, wherein the concentration of montan wax in the wax-containing liquid is from 30 to 200g/L, preferably from 30 to 150 g/L.
9. The process according to claim 1 or 2, wherein in step (2), the cooling crystallization conditions comprise: the temperature is-10 deg.C to 30 deg.C, and the duration is 10-90min, preferably 0-25 deg.C, and the duration is 10-60 min.
10. The method according to claim 1 or 2, wherein the method further comprises recycling the filtrate obtained in step (2) to step (1) for leaching the lignite particles.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102851076A (en) * | 2012-04-25 | 2013-01-02 | 曲靖众一精细化工股份有限公司 | Method for efficiently extracting fossilized plant wax from brown coal and device thereof |
| CN104312627A (en) * | 2014-10-27 | 2015-01-28 | 中国矿业大学 | Solvent and method for removing resin from lignite wax by virtue of crystallization process |
| CN106147863A (en) * | 2016-06-21 | 2016-11-23 | 金正大生态工程集团股份有限公司 | A kind of method extracting lignite wax from brown coal |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102851076A (en) * | 2012-04-25 | 2013-01-02 | 曲靖众一精细化工股份有限公司 | Method for efficiently extracting fossilized plant wax from brown coal and device thereof |
| CN104312627A (en) * | 2014-10-27 | 2015-01-28 | 中国矿业大学 | Solvent and method for removing resin from lignite wax by virtue of crystallization process |
| CN106147863A (en) * | 2016-06-21 | 2016-11-23 | 金正大生态工程集团股份有限公司 | A kind of method extracting lignite wax from brown coal |
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