CN111154512A - Method for removing resin from lignite crude wax and method for extracting lignite wax from lignite - Google Patents
Method for removing resin from lignite crude wax and method for extracting lignite wax from lignite Download PDFInfo
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- CN111154512A CN111154512A CN201811326864.7A CN201811326864A CN111154512A CN 111154512 A CN111154512 A CN 111154512A CN 201811326864 A CN201811326864 A CN 201811326864A CN 111154512 A CN111154512 A CN 111154512A
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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
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Abstract
The invention relates to the field of purifying montan wax, and discloses a method for removing resin from montan crude wax, which comprises the following steps: (1) dissolving lignite crude wax particles by using a solvent; (2) and (2) cooling and crystallizing the solution obtained in the step (1), filtering, separating and drying to obtain the purified montan wax. The method effectively removes the resin in the lignite crude wax by a process of high-temperature dissolution, low-temperature cooling and precipitation, the resin content in the obtained finished wax is as low as less than 10 weight percent, even less than 5 weight percent, and the solvent requirement of the method is obviously lower.
Description
Technical Field
The invention relates to a method for purifying montan wax, in particular to a method for removing resin in montan crude wax and a method for extracting montan wax from lignite.
Background
Montan wax is a natural mineral wax extracted from lignite, is widely used as a substitute and a supplement of expensive natural animal wax and vegetable wax, has unique advantages in physicochemical properties compared with paraffin wax and Fischer-Tropsch wax, and is commonly used in the industries of precision casting, high-grade daily necessities and the like. The international montan wax gap is larger at present. Montan wax, also known as montan wax, contains wax, resin, and bitumen. The resin in the montan wax has a large negative influence on the performance of the montan wax, and national standards require that the resin content of the first-class montan wax is less than 20 percent and the resin content of the imported montan wax is less than 15 percent, so that the price of the domestic montan wax is 10000 yuan/ton lower than that of the imported montan wax. At present, the content of the montan wax resin in China is higher, generally between 20 and 30 percent, and can reach below 20 percent after resin removal.
CN103074109A discloses a method for removing resin substances from montan wax, which comprises the following steps: (a) crushing lignite wax: putting the montan wax extracted from lignite into a grinder for grinding, controlling the grinding temperature to be-10-30 ℃ to obtain ground montan wax, putting the ground montan wax on a screening machine for screening, and obtaining montan wax particles with the granularity of 10-100 meshes after screening; (b) multi-stage countercurrent extraction: sending the montan wax particles with the particle size of 10-100 meshes into a multistage countercurrent extractor for liquid-solid phase extraction, wherein the extraction temperature is-20-40 ℃, an organic solvent is used as an extractant for multistage countercurrent extraction, the total amount of the extractant is 4-10 times of the mass of the montan wax, the montan wax particles are sequentially subjected to continuous extraction by organic solvents with sequentially reduced resin concentration for 120-180 minutes, finally, the organic solvents without resin are used for extraction for 60-80 minutes, the extraction stages are 3-8, after the extraction is finished, a mixed solution of the solid defatted wax and the organic solvent with the resin is obtained, the content of the resin in the solid defatted wax is less than 5%, and the resin extraction rate is more than 80%; (c) evaporation forming of solid degreasing wax: 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, detecting the residual amount of the organic solvent in the degreased wax liquid, and when the residual amount of the organic solvent in the degreased wax liquid is less than 0.1%, conveying the degreased wax liquid to a forming machine for forming to obtain a degreased wax product; (d) negative pressure multi-effect evaporation: pumping the organic solvent mixed solution containing the resin substances obtained after extraction into a one-effect long-tube climbing-film evaporator, evaporating to remove 70-80% of the organic solvent in the organic solvent mixed solution containing the resin substances, condensing and recycling the organic solvent obtained after evaporation, pumping the residual solution in the one-effect long-tube climbing-film evaporator into a two-effect long-tube climbing-film evaporator, evaporating the residual organic solvent, stopping evaporation when the content of the organic solvent in the resin substances of the two-effect long-tube climbing-film evaporator is detected to be less than 0.1%, introducing the resin-containing solution into the next effect to perform multi-effect evaporation if necessary, obtaining the resin substances after evaporation, and condensing and recycling the organic solvent obtained after evaporation.
CN103897734A discloses an energy-saving and efficient resin removal method for coarse montan wax, which is characterized by comprising the steps of crushing and sieving, resin leaching, degreasing wax separation and resin separation, and specifically comprises the following steps:
A. crushing and sieving: crushing the coarse montan wax, and screening by 0.5-3mm to remove fine powder and coarse particles to obtain montan wax particles;
B. resin leaching: putting the montan wax particles and an acetone solvent into a leaching device according to a solid-liquid ratio of 1:1-1:8kg/L, leaching for 2-4h at normal temperature, and carrying out solid-liquid separation to obtain a leaching solution and montan wax solid;
C. separation of the degreased wax: putting the solid montan wax into a separation device, and removing residual acetone through heating and evaporation to obtain resin-removed montan wax and acetone;
D. resin separation: putting the leaching solution into a separation container, adding water to separate the resin from acetone, performing solid-liquid separation to obtain acetone insoluble substances and an acetone aqueous solution, rectifying the acetone aqueous solution to recover acetone, and evaporating the acetone insoluble substances to obtain lignite resin and acetone.
In the prior art, the resin is dissolved by leaching with a solvent at normal temperature to achieve the aim of removing the resin, and organic solvents such as benzene, toluene, acetone and the like are generally adopted.
The normal temperature leaching and degreasing process comprises the steps of mixing the montan wax with an organic solvent, dissolving resin and the like from the montan wax at low temperature (20-25 ℃), enabling the product wax to exist in a solid form, and separating to obtain the lignite wax without the resin. The main problems of the method are as follows:
(1) in the currently selected extracting agents (benzene, toluene and acetone), wax and resin are easy to dissolve in a solvent, so that the yield of resin removal is low, the yield is only about 60%, and wax loss is also caused;
(2) the toxicity of the solvent is high;
(3) the solvent consumption of wax per unit mass is large, and can generally reach 5L/kg wax;
(4) for crude waxes with a resin content above 50%, this method does not allow to obtain product waxes with a qualified resin content.
Therefore, a method for simply and effectively removing resin from the lignite crude wax, particularly a method suitable for high resin content lignite crude wax, is needed.
Disclosure of Invention
The invention aims to overcome the problems of high solvent consumption, low efficiency and the like in the prior art, and provides a method for removing resin from lignite crude wax and a method for extracting the lignite wax from lignite.
In order to achieve the above object, a first aspect of the present invention provides a method for removing resin from montan wax, the method comprising:
(1) dissolving lignite crude wax particles by using a solvent;
(2) and (2) cooling and crystallizing the solution obtained in the step (1), filtering, separating and drying to obtain the purified montan wax.
In a second aspect, the present invention provides a method for extracting montan wax from lignite, comprising the steps of the method according to the first aspect of the present invention.
According to the method, the resin in the lignite crude wax is effectively removed through the processes of high-temperature dissolution, low-temperature cooling and precipitation, the resin content in the obtained finished wax is as low as below 10 wt%, even as low as below 5 wt% (the resin content of the first-level lignite wax is required to be less than 20%), the solvent requirement is obviously low, the solvent amount required by each kilogram of crude wax is 3-3.5L, and the solvent amount required by each kilogram of crude wax in the traditional resin removal method is more than 5L.
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 removing resin from lignite crude wax, which comprises the following steps:
(1) dissolving lignite crude wax particles by using a solvent;
(2) and (2) cooling and crystallizing the solution obtained in the step (1), filtering, separating and drying to obtain the purified montan wax.
In the present invention, the montan crude wax is a crude product obtained when montan wax is extracted from lignite, wherein the method for extracting montan wax from lignite may be any one of the methods used in the prior art. In the present invention, the montan wax comprises 20 to 60% by weight of the resin, and 40 to 60% by weight of the montan wax pure wax component.
In the method of the invention, the particle size of the lignite crude wax particles is less than 10 mm. Preferably, the lignite slack wax is crushed and sieved. For example, the crude lignite wax can be firstly added into a crusher to be crushed, then a sieve with the aperture of 10mm is used for sieving, and the crude wax particles with the undersize part of less than 10mm are used as qualified raw materials to enter the next dissolving process. And returning the unqualified materials with the size of more than 10mm on the screen, crushing and screening until the materials are qualified.
In the method of the present invention, in the step (1), the montan wax particles are dissolved with a solvent. The solvent is an ester and/or alcohol solvent, preferably, the alcohol solvent is selected from C1-C10More preferably, the alcoholic solvent is selected from one or more of methanol, ethanol, isopropanol; preferably the ester solvent has R1COOR2In which R is1、R2Each independently selected from C1-C10Alkyl and alkenyl ofMore preferably, the ester solvent is selected from one or more of methyl acetate, ethyl acetate, propyl acetate and butyl acetate.
In one embodiment of the method of the present invention, the solvent is a mixed solvent of an ester solvent and an alcohol solvent, and may be, for example, a mixed solvent of isopropanol and ethyl acetate, a mixed solvent of isopropanol and butyl acetate, or the like.
In one embodiment of the method of the present invention, the solvent is a mixed solvent of various esters, and for example, a mixed solvent of methyl acetate and ethyl acetate, a mixed solvent of methyl acetate and propyl acetate, and a mixed solvent of butyl acetate and ethyl acetate may be used.
In the method of the present invention, in the step (1), in order to more efficiently remove the resin, the volume of the solvent is 20 to 50L, preferably 25 to 35L, and more preferably 30L per kg of the montan crude wax particles in the dissolving step. The inventors of the present application have found that when the solvent used is small, for example, 5L per kg of the crude montan wax particles, the crude montan wax forms a paste with the solvent, liquid-solid separation is difficult to achieve, and when the solvent used is large, energy consumption for solvent evaporation recovery is high. Therefore, the invention uses proper solvent to dissolve crude wax particles and reduces the energy consumption per unit refined wax production by means of solvent circulation, and the volume of the solvent required after circulation is 2-10L, preferably 3-5L per kg of crude lignite wax particles.
In the method of the present invention, in step (1), the dissolving conditions include: the temperature is 40-70 deg.C, and the time is 10-90 min; preferably, the temperature is 40-60 ℃, and the time is 20-70 min; more preferably, the temperature is 45-55 ℃ and the time is 30-60min, more preferably, the temperature is 50 ℃ and the time is 45 min. In a preferred embodiment, the dissolution is accompanied by stirring. In the present invention, the temperature during dissolution is achieved by means known in the art, for example by heating in a water bath.
In the present invention, the dissolution process is intended to result in a clear solution. In a preferred mode, complete dissolution of the montan wax can be achieved by technical means such as ultrasound. In yet another embodiment, a clear solution may be obtained by filtration or the like before the cooling crystallization step is performed.
In the method of the present invention, in order to remove the resin from the crude montan wax in the cooling crystallization step and to achieve further purification of the crude montan wax, it is necessary to control the concentration of the above solution within a suitable range, for example, the concentration of the crude montan wax in the solution is 20 to 50g/L, preferably 20 to 35 g/L; the resin concentration is 5-200g/L, preferably 5-150 g/L. In the present invention, the concentration of montan wax in a solution is defined as the ratio of the mass of montan wax at the cooling temperature to the volume of the solution; the concentration of resin in the solution is defined as the ratio of the mass of resin at the cooling temperature to the volume of the solution.
In the method of the present invention, in the step (2), the solution obtained in the step (1) is subjected to cooling crystallization, wherein the cooling crystallization conditions comprise: the temperature is 5-30 deg.C, and the duration is 60-120 min; preferably, the temperature is 5-15 ℃ for a duration of 70-110min, more preferably, the temperature is 5 ℃ for a duration of 90 min.
In the process according to the invention, the technical means for achieving cooling can be chosen according to the prior art, for example by using cooling circulation water. And cooling the solution for a certain time, and after the montan wax particles are crystallized, filtering and separating the suspension containing the montan wax particles to obtain wet wax particles and degreasing liquid containing resin.
In the method of the present invention, in the step (2), the wet wax particles are dried to obtain refined wax particles. The drying conditions include: the temperature is 105-130 ℃, preferably 120-130 ℃. In one embodiment, the steam obtained during the drying process is condensed and passed into the solvent for dissolving the montan wax particles.
According to the invention, the method further comprises: and (3) recycling the filtrate (namely the degreasing fluid containing the resin) obtained in the step (2) to the step (1) for dissolving the lignite crude wax particles. This is repeated several times, and the cycle is stopped until the content of resin in the filtrate obtained reaches saturation (for example, the content is more than 29% by weight).
According to the invention, the method further comprises: the saturated filtrate is distilled to obtain resin at the bottom of the tower, and the steam at the top of the tower is cooled and returned to the step (1) for dissolving the lignite crude wax particles.
According to the invention, the dried montan wax is shaped to obtain a purified montan wax product. The shaping step can be selected according to the prior art
The method of the invention uses a solvent to dissolve the lignite slack wax particles at a higher temperature and cools the solution, during which the wax crystallizes out, while the resin remains in the solution, which is separated by filtration. The method effectively removes the resin in the montan wax through the processes of high-temperature dissolution, low-temperature cooling and precipitation, and obtains the montan wax with less resin content, for example, the resin content can be as low as less than 10 weight percent, even less than 5 weight percent (the resin content of the primary montan wax is required to be less than 20 percent). In addition, in the method, the required amount of the solvent is obviously lower, and the required amount of the solvent per kilogram of the crude wax is only 3-3.5L.
In a second aspect, the present invention provides a method for extracting montan wax from lignite, comprising the steps of the method according to the first aspect of the present invention.
The method for extracting the montan wax from the lignite provided by the second aspect of the invention at least comprises two steps: (1) separating the lignite slack wax from the lignite using any operable method; (2) the process according to the first aspect of the invention removes resin from the montan wax.
According to the method of the second aspect of the present invention, the method used in step (1) includes extraction using various organic solvents.
The present invention will be described in detail below by way of examples.
Example 1
Crushing and sieving the crude montan wax (the resin content is 57 percent) to prepare the crude montan wax particles with the particle size of less than 10 mm. 10g of lignite crude wax particles and 300mL of ethyl acetate are mixed in a dissolving tank, sealed and placed in a water bath at 50 ℃, and the temperature is kept for 45 min. The concentration of montan wax in the obtained solution was 33g/L, and the resin content was 18.98 g/L. And (3) placing the dissolving tank in cooling water of 5 ℃, and keeping the temperature for 90min to separate out wax particles by crystallization. After crystallization, the wax particles were separated from the filtrate (i.e., the degreasing fluid) by vacuum filtration. Adding brown coal crude wax (resin content 57%) into the filtrate, repeating the above process for 9 times, concentrating and evaporating saturated circulating filtrate to obtain resin, and condensing overhead vapor for dissolving brown coal crude wax. Mixing the wet wax particles obtained by ten times, drying in a drying oven at 105 ℃, and forming to obtain the purified montan wax product.
According to the above procedure, 3L of degreasing solvent was required per kg of crude wax. Meanwhile, the composition analysis of the obtained resin and montan wax was carried out in accordance with GB/T2559-2005 montan wax determination method, and the results are shown in tables 1 and 2.
The acid value of the obtained purified wax is 38, the saponification value is 112, and the product requirements of the first-grade wax are met.
Example 2
Referring to the method of example 1, except that 300mL of ethyl acetate was replaced with 500mL of a mixed solution of butyl acetate and isopropyl alcohol, the mixed solution was mixed with montan wax particles, sealed, and then placed in a water bath at 40 ℃ and maintained at a constant temperature for 70 min. The concentration of montan wax in the obtained solution was 20g/L, and the resin content was 18.98 g/L. The rest is the same as in example 1.
The degreasing solvent required per kg of crude wax was 2.8L according to the above procedure. Meanwhile, the composition analysis of the obtained resin and montan wax was carried out in accordance with GB/T2559-2005 montan wax determination method, and the results are shown in tables 1 and 2.
The acid value of the obtained purified wax is 45, the saponification value is 132, and the product requirements of the first-grade wax are met.
Example 3
Referring to the method described in example 1, except that the dissolving tank was placed in cooling water at 25 ℃ and kept at a constant temperature for 110min, wax particles were crystallized out. The rest is the same as in example 1.
According to the above procedure, 3L of degreasing solvent was required per kg of crude wax. Meanwhile, the composition analysis of the obtained resin and montan wax was carried out in accordance with GB/T2559-2005 montan wax determination method, and the results are shown in tables 1 and 2.
The acid value of the obtained purified wax is 34, the saponification value is 135, and the product requirements of the first-grade wax are met.
Example 4
Referring to the method described in example 1, except that 10g of montan wax particles and 1000mL of ethyl acetate were mixed in a dissolution tank. The concentration of montan wax in the finally obtained solution was 10 g/L. The rest is the same as in example 1.
According to the above procedure, 10L of degreasing solvent was required per kg of crude wax. Meanwhile, the composition analysis of the obtained resin and montan wax was carried out in accordance with GB/T2559-2005 montan wax determination method, and the results are shown in tables 1 and 2.
The acid value of the obtained purified wax is 45, the saponification value is 105, and the product requirement of the first-grade wax is met.
Example 5
Referring to the method described in example 1, except that the dissolving tank was placed in a cooling liquid at 0 ℃ and kept at a constant temperature for 90min, wax particles were crystallized out. The rest is the same as in example 1.
According to the above procedure, 3L of degreasing solvent was required per kg of crude wax. Meanwhile, the composition analysis of the obtained resin and montan wax was carried out in accordance with GB/T2559-2005 montan wax determination method, and the results are shown in tables 1 and 2.
The acid value of the obtained purified wax is 48, the saponification value is 124, and the product requirements of the first-grade wax are met.
Example 6
Referring to the method described in example 1, except that the dissolving tank was placed in cooling water at 35 ℃ and kept at a constant temperature for 90min, wax particles were crystallized out. The rest is the same as in example 1.
According to the above procedure, 3L of degreasing solvent was required per kg of crude wax. Meanwhile, the composition analysis of the obtained resin and montan wax was carried out in accordance with GB/T2559-2005 montan wax determination method, and the results are shown in tables 1 and 2.
The acid value of the obtained purified wax is 41, the saponification value is 119, and the product requirements of the first-grade wax are met.
Example 7
Crushing and sieving the lignite crude wax (the resin content is 54 percent) to prepare crude wax particles with the particle size of less than 10 mm. Mixing 45g of lignite crude wax particles and 200mL of 95% ethanol in a dissolving tank, sealing, placing in a water bath at 55 ℃, and keeping the temperature for 30 min. The concentration of montan wax in the resulting solution was 22.5 g/L. And (3) placing the dissolving tank in cooling water of 15 ℃, and keeping the temperature for 60min to separate out wax particles by crystallization. After crystallization, the wax particles were separated from the filtrate (i.e., the degreasing fluid) by vacuum filtration. Adding coarse wax particles with the resin content of 54% into the filtrate again, repeating the process for 5 times, concentrating and evaporating the circulating filtrate to obtain resin, and condensing the tower top steam for recycling to dissolve the lignite coarse wax. And mixing the wet wax particles obtained in 6 times, drying in a drying oven at 105 ℃, and forming to obtain a purified wax product.
The solvent required per kg of crude wax was 3.33L according to the above procedure. Meanwhile, the composition analysis of the obtained resin and montan wax was carried out in accordance with GB/T2559-2005 montan wax determination method, and the results are shown in tables 1 and 2.
The acid value of the obtained purified wax is 35, the saponification value is 120, and the product requirements of the first-grade wax are met.
Comparative example 1
Crushing and sieving the lignite crude wax (the resin content is 51 percent) to prepare crude wax particles smaller than 10 mm. 30g of crude montan wax particles are soaked in 300mL of ethyl acetate, sealed and stirred at room temperature for 180min, and the wax is separated by vacuum filtration. Concentrating and evaporating the filtrate obtained by filtering to obtain resin, drying the solid wax obtained by filtering in a drying oven at 105 ℃, and forming to obtain a purified wax product.
The solvent required per kg of crude wax was 10L according to the above procedure. Meanwhile, the composition analysis of the obtained resin and montan wax was carried out in accordance with GB/T2559-2005 montan wax determination method, and the results are shown in tables 1 and 2.
The acid value of the obtained purified wax was 28 and the saponification value was 115, and the yield was high, but the product requirement of the secondary wax was not satisfied.
TABLE 1
The product component content data in table 1 and the following table are all test data, and the sum of the component contents is about 100%.
The yield in table 1 can be calculated according to the following formula:
calculating the yield of the wax: p% ═ WPurified wax×ωPurifying wax, wax％/(WCrude wax×ωCrude wax, wax％)×100％
P represents the yield of wax,%
WPurified waxDenotes the mass of purified wax, kg
ωPurifying wax, waxThe content of wax in the purified wax is shown as% by weight
WCrude waxDenotes the mass of the crude wax, kg
ωCrude wax, waxRepresents the wax content in the crude wax, wt%
TABLE 2
As can be seen from the results in Table 1, examples 1 to 7 of the present invention have significantly better effects in removing resin from the montan wax, and can reduce the resin content to less than 20% by weight, even to 2.54%, and the obtained montan wax satisfies the product requirements of the first-class wax, and the yield is more than 75%. Even the resin content of the montan wax obtained by the method described in example 5 approaches the product requirements for a secondary wax, whereas the resin content of the montan wax obtained by the method described in comparative example 1 is greater than 30% by weight. In addition, in the embodiments 1 to 7 of the present invention, the amount of the solvent required per kg of the crude wax is significantly small, so that the production cost can be significantly reduced, the efficiency can be improved, and the operation can be more convenient.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A method for removing resin from lignite slack wax, comprising:
(1) dissolving lignite crude wax particles by using a solvent;
(2) and (2) cooling and crystallizing the solution obtained in the step (1), filtering, separating and drying to obtain the purified montan wax.
2. The method according to claim 1, wherein, in step (2), the cooling crystallization conditions comprise: the temperature is 5-30 deg.C, and the duration is 60-120 min; preferably, the temperature is 5-15 ℃ and the duration is 70-110 min.
3. The process according to claim 1 or 2, wherein in step (1) the solvent is an ester and/or alcohol solvent, preferably the alcohol solvent is selected from C1-C10More preferably, the alcoholic solvent is selected from one or more of methanol, ethanol, isopropanol; preferably the ester solvent has R1COOR2In which R is1、R2Are each selected from C1-C10More preferably, the ester solvent is selected from one or more of methyl acetate, ethyl acetate, butyl acetate and propyl acetate.
4. The method of claim 1 or 2, wherein in step (1), the conditions of dissolution comprise: the temperature is 40-70 deg.C, and the time is 10-90 min; preferably, the temperature is 40-60 ℃, and the time is 20-70 min; more preferably, the temperature is 45-55 deg.C and the time is 30-60 min.
5. The method of claim 1 or 2, wherein in step (2), the drying conditions comprise: the temperature was 105 ℃ and 130 ℃.
6. The method according to claim 1 or 2, wherein the method further comprises:
and (3) recycling the filtrate obtained in the step (2) to the step (1) for dissolving the lignite crude wax particles.
7. The method according to claim 1 or 2, wherein the concentration of the montan wax in the solution obtained in step (1) is from 20 to 50g/L, and the resin concentration is from 5 to 200 g/L; preferably, the concentration of the montan wax is 20-35g/L, and the resin concentration is 5-150 g/L.
8. The method according to claim 1 or 2, wherein the solvent is used in an amount of 2 to 10L, preferably 3 to 5L, with respect to 1 kg of the montan crude wax particles.
9. The method according to claim 1 or 2, wherein the resin content of the montan wax is 20 to 60 wt.%.
10. A method of extracting montan wax from lignite comprising the steps of the method of any one of claims 1-9.
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| CN114570223A (en) * | 2020-11-30 | 2022-06-03 | 台湾聚合化学品股份有限公司 | Method for recycling and regenerating derivative oligomer in process |
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| CN103074108A (en) * | 2012-12-07 | 2013-05-01 | 云天化集团有限责任公司 | Degreasing method of crude montan wax |
| 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 |
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| CN114570223A (en) * | 2020-11-30 | 2022-06-03 | 台湾聚合化学品股份有限公司 | Method for recycling and regenerating derivative oligomer in process |
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