CN109913268B - Method for co-producing resin and montan wax from lignite - Google Patents
Method for co-producing resin and montan wax from lignite Download PDFInfo
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- 239000011347 resin Substances 0.000 title claims abstract description 100
- 229920005989 resin Polymers 0.000 title claims abstract description 100
- 239000012170 montan wax Substances 0.000 title claims abstract description 89
- 238000000034 method Methods 0.000 title claims abstract description 73
- 239000003077 lignite Substances 0.000 title claims abstract description 70
- 239000002904 solvent Substances 0.000 claims abstract description 65
- 238000000605 extraction Methods 0.000 claims abstract description 48
- 238000011282 treatment Methods 0.000 claims abstract description 37
- 239000001993 wax Substances 0.000 claims abstract description 27
- 239000002245 particle Substances 0.000 claims abstract description 26
- 239000007790 solid phase Substances 0.000 claims abstract description 25
- 239000007791 liquid phase Substances 0.000 claims abstract description 23
- 238000001704 evaporation Methods 0.000 claims abstract description 12
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 48
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 38
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 9
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 9
- 239000010426 asphalt Substances 0.000 claims description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 8
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 7
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 5
- 239000003208 petroleum Substances 0.000 claims description 5
- SYBYTAAJFKOIEJ-UHFFFAOYSA-N 3-Methylbutan-2-one Chemical compound CC(C)C(C)=O SYBYTAAJFKOIEJ-UHFFFAOYSA-N 0.000 claims description 4
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000008096 xylene Substances 0.000 claims description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 3
- 150000002576 ketones Chemical class 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 2
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims description 2
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N alpha-methyl toluene Natural products CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 claims description 2
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 claims description 2
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- 238000010992 reflux Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 3
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- 239000000126 substance Substances 0.000 description 3
- 239000003245 coal Substances 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 239000013557 residual solvent Substances 0.000 description 2
- DSEKYWAQQVUQTP-XEWMWGOFSA-N (2r,4r,4as,6as,6as,6br,8ar,12ar,14as,14bs)-2-hydroxy-4,4a,6a,6b,8a,11,11,14a-octamethyl-2,4,5,6,6a,7,8,9,10,12,12a,13,14,14b-tetradecahydro-1h-picen-3-one Chemical compound C([C@H]1[C@]2(C)CC[C@@]34C)C(C)(C)CC[C@]1(C)CC[C@]2(C)[C@H]4CC[C@@]1(C)[C@H]3C[C@@H](O)C(=O)[C@@H]1C DSEKYWAQQVUQTP-XEWMWGOFSA-N 0.000 description 1
- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
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- 235000021355 Stearic acid Nutrition 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
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- 239000012166 beeswax Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
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- 239000003759 ester based solvent Substances 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- XMHIUKTWLZUKEX-UHFFFAOYSA-N hexacosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCC(O)=O XMHIUKTWLZUKEX-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000005453 ketone based solvent Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000012184 mineral wax Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 235000019809 paraffin wax Nutrition 0.000 description 1
- 235000019271 petrolatum Nutrition 0.000 description 1
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- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 150000003097 polyterpenes Chemical class 0.000 description 1
- 239000010117 shenhua Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the field of lignite wax preparation, in particular to a method for co-producing resin and lignite wax from lignite. The method comprises the following steps: (1) carrying out first extraction treatment on lignite particles and a first solvent to extract fat, and then carrying out solid-liquid separation to obtain a first solid phase and a first liquid phase; (2) evaporating the first liquid phase to separate resin and first solvent; (3) and carrying out second extraction treatment on the first solid phase and a second solvent to extract wax, then carrying out solid-liquid separation to obtain a second liquid phase and a second solid phase, and removing the solvent of the second liquid phase to obtain the montan wax. The method for coproducing resin and montan wax from lignite can directly prepare high-purity resin products and low-resin montan wax from lignite, and is high in coproduction yield, simple to operate and suitable for industrial application.
Description
Technical Field
The invention relates to the field of lignite wax preparation, in particular to a method for co-producing resin and lignite wax from lignite.
Background
The montan wax is a mineral wax containing wax, resin and bitumen, which is extracted from lignite by using an organic solvent, and the composition of the montan wax extracted from coal in different coal-forming plants and coal-forming environments is different. The montan wax has complex chemical composition, good physicochemical properties and no carcinogenic effect. The montan wax is characterized by high melting point, hard and brittle quality, good moisture resistance, good chemical stability, high mechanical strength, bright surface like a mirror, low conductivity and the like. And can be melted into uniform cerate together with other waxes, such as paraffin wax, beeswax, stearic acid and ceresin, and some synthetic materials, such as polyethylene and polypropylene. Therefore, it has wide applications in various fields.
The montan wax resin mainly comprises terpene, polyterpene, resin acid, etc., and can darken the color of the wax. In the crude wax of the montan wax in China, the resin content is generally higher by 20-40%, and if the resin content in the montan wax is too high, the montan wax is sticky, the co-solubility of the montan wax and other additives is influenced, and the physical properties and the mechanical properties of the montan wax are reduced. In order to reach a higher product quality standard, a crude wax degreasing process is required to remove resin, and resin byproducts obtained by the existing production process have poor quality and are often accumulated as wastes, so that the method becomes an important problem troubling enterprises and also seriously influences the product economy. In fact, the high-quality resin has better insulating property, bioactivity and the like, and can be widely applied to the industries of electric appliances, paints and medicines. In addition, in the existing lignite wax extraction process, the lignite crude wax is extracted firstly, and then the lignite crude wax is degreased, so that the wax loss is high, and the resin purity in a degreased product is low, so that the lignite wax cannot be used as a product.
Disclosure of Invention
The present invention is directed to overcoming the above-mentioned disadvantages of the prior art and providing a method for co-producing resin and montan wax from lignite by directly producing a high purity resin product and a low resin montan wax from lignite.
In order to achieve the above object, an aspect of the present invention provides a method for co-producing resin and montan wax from lignite, the method comprising:
(1) carrying out first extraction treatment on lignite particles and a first solvent to extract fat, and then carrying out solid-liquid separation to obtain a first solid phase and a first liquid phase;
(2) evaporating the first liquid phase to separate a resin product and a first solvent;
(3) carrying out second extraction treatment on the first solid phase and a second solvent to extract wax, then carrying out solid-liquid separation to obtain a second liquid phase and a second solid phase, and removing the solvent of the second liquid phase to prepare montan wax;
the first solvent is one or more of an ester solvent, an aromatic hydrocarbon solvent and a ketone solvent, and the second solvent is one or more of an alkane solvent, an ester solvent, an aromatic hydrocarbon solvent and petroleum ether;
the temperature of the first extraction treatment is-10 ℃ to 30 ℃, and the temperature of the second extraction treatment is 60 ℃ to 100 ℃.
In a second aspect, the invention provides montan wax or resin made by the above-described method.
The method for coproducing resin and montan wax from lignite can directly prepare high-purity resin products and low-resin montan wax from lignite, and is high in coproduction yield, simple to operate and suitable for industrial application.
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.
In one aspect, the present invention provides a method for co-producing resin and montan wax from lignite, the method comprising:
(1) carrying out first extraction treatment on lignite particles and a first solvent to extract fat, and then carrying out solid-liquid separation to obtain a first solid phase and a first liquid phase;
(2) evaporating the first liquid phase to separate a resin product and a first solvent;
(3) carrying out second extraction treatment on the first solid phase and a second solvent to extract wax, then carrying out solid-liquid separation to obtain a second liquid phase and a second solid phase, and removing the solvent of the second liquid phase to prepare montan wax;
the first solvent is one or more of an ester solvent, an aromatic hydrocarbon solvent and a ketone solvent, and the second solvent is one or more of an alkane solvent, an ester solvent, an aromatic hydrocarbon solvent and petroleum ether;
the temperature of the first extraction treatment is-10 ℃ to 30 ℃, and the temperature of the second extraction treatment is 60 ℃ to 100 ℃.
According to the present invention, the method for co-producing resin and montan wax from lignite according to the present invention can extract wax-rich lignite that is conventional in the art, particularly dehydrated lignite, and for this purpose, the water content of the lignite particles is preferably 25 wt% or less, preferably 15 wt% or less, for example, 1 to 15 wt%, 10 to 15 wt%, etc. Among them, in order to make the contact between the lignite particles and the solvent more excellent, the particle size of the lignite particles may be 10mm or less, preferably 6mm or less, preferably 5mm or less, and particularly 3mm or less.
According to the present invention, in the step (1), the resin in the lignite particles can be extracted by the first solvent through contact mixing of the lignite particles and the first solvent, wherein the first solvent is one or more selected from ester solvents, aromatic hydrocarbon solvents and ketone solvents, preferably one or more selected from methyl acetate, ethyl acetate, acetone, methyl butanone, methyl isobutyl ketone, benzene, toluene and xylene, and more preferably one or more selected from acetone, methyl butanone, methyl acetate and ethyl acetate. Of course, it should be understood that the first solvent may contain other impurities, is not necessarily completely pure, and may be of industrial grade.
According to the invention, in step (1), the amount of the first solvent may vary within wide limits, preferably the weight ratio of the amounts of the lignite particles and the first solvent is 1: 1-8, preferably 1: 2-6, e.g. 1: 3-5.
According to the present invention, the temperature of the first extraction treatment does not need to be too high as long as-10 ℃ to 30 ℃ is maintained, and in order to improve the extraction efficiency, it is preferable that the temperature of the first extraction is 0 to 30 ℃, preferably 10 to 25 ℃.
According to the invention, the first extraction treatment is preferably carried out for a period of time ranging from 0.5 to 10 hours, preferably from 1 to 6 hours, more preferably from 1 to 3 hours.
According to the invention, the first extracted material is subjected to solid-liquid separation, for example by means of centrifugation, which results in substantially defatted lignite particles, i.e. the first solid phase, and a first liquid phase mixed with a mixture of resin and first solvent. In step (2), the first liquid phase is treated to separate a resin product and a first solvent.
According to the invention, in step (2), the evaporation treatment will generally result in a vapour of the first solvent, which vapour is then condensed back to yield the first solvent. The evaporation treatment is a conventional operation in the art, and the present invention is not particularly limited thereto. The obtained resin has high resin content, such as more than 97 wt%, preferably more than 99 wt%, such as 98-99.8 wt%; the content of other components in the resin obtained is still low, for example, the asphalt content is 1 wt% or less, preferably 0.3 wt% or less, for example, 0.01 to 0.2 wt%; the wax content is 3% by weight or less, preferably 2% by weight or less, for example, 0.1 to 1.2% by weight.
According to the present invention, the first solvent obtained by the evaporation treatment in step (2) may also be reused in the first extraction treatment, and for this reason, the method preferably further comprises reusing the first solvent separated by the evaporation treatment in step (2) in step (1) to perform the first extraction treatment.
According to the present invention, step (3) may be carried out by subjecting the first solid phase to a heat treatment to remove the adhering solvent, prior to the second extraction treatment, the heat treatment preferably including: the temperature is 40-80 deg.C, and the time is 30-200 min.
According to the present invention, the montan wax in the lignite particles is allowed to be extracted into the second solvent by the second extraction process in step (3). Preferably, the second solvent is one or more of n-pentane, n-hexane, cyclopentane, cyclohexane, methyl acetate, ethyl acetate, benzene, toluene, xylene, and petroleum ether, preferably one or more of methyl acetate, ethyl acetate, benzene, and toluene.
Wherein the amount of the second solvent can vary within wide limits, preferably the weight ratio of the amount of the first solid phase to the amount of the second solvent is 1: 1-8, preferably 1: 1-6, e.g. 1: 2-5.
According to the present invention, the second extraction process needs to be performed at a relatively high temperature, and in order to improve extraction efficiency, it is preferable that the temperature of the second extraction process is 70 to 90 ℃. Preferably, the time of the second extraction treatment is 1 to 8 hours, preferably 1.5 to 5 hours.
According to the present invention, the second extraction process is performed such that the montan wax component is incorporated into the second solvent, and the remaining second solid phase is defatted and dewaxed montan, whereby montan wax can be produced by removing (e.g., evaporating) the second solvent from the second liquid phase, and the separated second solvent can be reused in the second extraction process of step (3).
Wherein, the montan wax with low resin content and high wax content is prepared by the method of the invention, preferably, the wax content in the montan wax is more than 80 weight percent, preferably more than 90 weight percent, such as 88 to 95 weight percent, preferably 91 to 95 weight percent; the content of bitumen is 5 wt% or less, preferably 3 wt% or less, for example 1-3 wt%; the content of the resin is 20% by weight or less, preferably 10% by weight or less, for example, 2 to 9% by weight, preferably 3 to 6% by weight.
In a second aspect, the invention provides montan wax or resin made by the above-described method.
The method for coproducing resin and montan wax from lignite can directly prepare high-purity resin products and low-resin montan wax from lignite, and is high in coproduction yield, simple to operate and suitable for industrial application.
The present invention will be described in detail below by way of examples.
In the following examples, the lignite was purchased from Shenhua Baoqing coal electric chemical company, and was dehydrated before treatment to obtain a water content of 10 to 15 wt%. And the lignite is pulverized into lignite particles having a particle size of less than 6mm for the following use.
Resin yield refers to the weight percent of the weight of the resin product obtained versus the weight of lignite (dry basis).
Montan wax yield refers to the weight percent ratio of the weight of the resulting montan wax product to the weight of the lignite (dry basis).
The resin and asphalt contents were measured according to GB/T2559-2005 montan wax measurement method.
Example 1
This example serves to illustrate the process of the invention for the co-production of resin and montan wax from lignite.
(1) Taking 50g of lignite particles and 200g of ethyl acetate, stirring and mixing for 3 hours at 15 ℃ and 100r/min to carry out first extraction treatment, and then carrying out centrifugal separation to obtain a liquid phase and a solid phase;
(2) evaporating the obtained liquid phase to obtain a resin product, and condensing and refluxing the steam to obtain ethyl acetate;
(3) heating the solid phase obtained in the step (1) at 60 ℃ for 1h to evaporate the residual solvent, stirring and mixing the solid phase with 200g of methylbenzene at 80 ℃ for 1h at 100r/min to perform second extraction treatment, filtering, evaporating the filtrate to obtain a montan wax product, and condensing and refluxing steam to obtain methylbenzene; and drying the filter cake to obtain the degreased and dewaxed lignite product.
Wherein, the contents of the relevant components of the resin product and the montan wax product are shown in Table 1, and the resin yield and the montan wax yield are shown in Table 2.
Example 2
This example serves to illustrate the process of the invention for the co-production of resin and montan wax from lignite.
(1) Taking 50g of lignite particles and 150g of methyl acetate, stirring and mixing for 2 hours at 20 ℃ and 100r/min to carry out first extraction treatment, and then carrying out centrifugal separation to obtain a liquid phase and a solid phase;
(2) carrying out rotary evaporation on the obtained liquid phase to obtain a resin product, and condensing and refluxing the vapor to obtain methyl acetate;
(3) heating the solid phase obtained in the step (1) at 50 ℃ for 1.5h to evaporate the residual solvent, stirring and mixing the solid phase with 180g of methylbenzene at 90 ℃ and 100r/min for 1.5h to perform second extraction treatment, then filtering, performing rotary evaporation on the filtrate to obtain a montan wax product, and condensing and refluxing steam to obtain methylbenzene; and drying the filter cake to obtain the degreased and dewaxed lignite product.
Wherein, the contents of the relevant components of the resin product and the montan wax product are shown in Table 1, and the resin yield and the montan wax yield are shown in Table 2.
Example 3
This example serves to illustrate the process of the invention for the co-production of resin and montan wax from lignite.
The method according to embodiment 1, wherein the duration of the first extraction process in step (1) is 6 h.
The resin products and montan wax products were finally obtained, and the contents of the relevant components are shown in Table 1, and the resin yields and montan wax yields are shown in Table 2.
Example 4
This example serves to illustrate the process of the invention for the co-production of resin and montan wax from lignite.
The method of embodiment 1, wherein the duration of the first extraction process in step (1) is 0.5 h.
The resin products and montan wax products were finally obtained, and the contents of the relevant components are shown in Table 1, and the resin yields and montan wax yields are shown in Table 2.
Example 5
This example serves to illustrate the process of the invention for the co-production of resin and montan wax from lignite.
The method according to embodiment 1, wherein the duration of the second extraction process in step (3) is 6 h.
The resin products and montan wax products were finally obtained, and the contents of the relevant components are shown in Table 1, and the resin yields and montan wax yields are shown in Table 2.
Example 6
This example serves to illustrate the process of the invention for the co-production of resin and montan wax from lignite.
The method of embodiment 1, wherein the duration of the second extraction process in step (3) is 0.5 h.
The resin products and montan wax products were finally obtained, and the contents of the relevant components are shown in Table 1, and the resin yields and montan wax yields are shown in Table 2.
Example 7
This example serves to illustrate the process of the invention for the co-production of resin and montan wax from lignite.
The process of example 1, wherein in step (1) an equal part by weight of toluene is used instead of ethyl acetate.
The resin products and montan wax products were finally obtained, and the contents of the relevant components are shown in Table 1, and the resin yields and montan wax yields are shown in Table 2.
Example 8
This example serves to illustrate the process of the invention for the co-production of resin and montan wax from lignite.
The process of example 1, wherein in step (1) an equal part by weight of methyl butanone is used instead of ethyl acetate.
The resin products and montan wax products were finally obtained, and the contents of the relevant components are shown in Table 1, and the resin yields and montan wax yields are shown in Table 2.
Example 9
This example serves to illustrate the process of the invention for the co-production of resin and montan wax from lignite.
The process of example 1, wherein in step (1) an equal part by weight of acetone is used instead of ethyl acetate.
The resin products and montan wax products were finally obtained, and the contents of the relevant components are shown in Table 1, and the resin yields and montan wax yields are shown in Table 2.
Example 10
This example serves to illustrate the process of the invention for the co-production of resin and montan wax from lignite.
The process of example 1, wherein in step (3) an equal weight portion of n-hexane is used instead of toluene.
The resin products and montan wax products were finally obtained, and the contents of the relevant components are shown in Table 1, and the resin yields and montan wax yields are shown in Table 2.
Example 11
This example serves to illustrate the process of the invention for the co-production of resin and montan wax from lignite.
The process of example 1, wherein in step (3) an equal part by weight of ethyl acetate is used instead of toluene.
The resin products and montan wax products were finally obtained, and the contents of the relevant components are shown in Table 1, and the resin yields and montan wax yields are shown in Table 2.
Example 12
This example serves to illustrate the process of the invention for the co-production of resin and montan wax from lignite.
The process of example 1, wherein 75g of ethyl acetate are used in step (1).
The resin products and montan wax products were finally obtained, and the contents of the relevant components are shown in Table 1, and the resin yields and montan wax yields are shown in Table 2.
Comparative example 1
50g of lignite particles and 200g of toluene are stirred and mixed for 2 hours at 80 ℃ and 100r/min to dewax and degrease, then the mixture is filtered, and the filtrate is evaporated to obtain a crude lignite wax product; drying the filter cake to obtain a degreased and dewaxed lignite product;
stirring and mixing 10g of crude montan wax product and 40g of ethyl acetate at 20 ℃ and 100r/min for 1h for degreasing, then filtering, and carrying out rotary evaporation on the filtrate to obtain a resin product; drying the filter cake to obtain the montan wax product.
Wherein, the contents of the relevant components of the resin product and the montan wax product are shown in Table 1, and the resin yield and the montan wax yield are shown in Table 2.
Comparative example 2
The method of example 1 except that in step (1) the temperature of the first extraction process is 40 ℃ and in step (2) the temperature of the second extraction process is 105 ℃;
the resin products and montan wax products were finally obtained, and the contents of the relevant components are shown in Table 1, and the resin yields and montan wax yields are shown in Table 2.
Comparative example 3
The process of example 1 was followed except that in step (1), ethyl acetate was replaced with an equal part by weight of n-hexane.
The resin products and montan wax products were finally obtained, and the contents of the relevant components are shown in Table 1, and the resin yields and montan wax yields are shown in Table 2.
TABLE 1
TABLE 2
| Yield of resin% | Yield of montan wax% | |
| Example 1 | 4.2 | 6.9 |
| Example 2 | 4.6 | 7.0 |
| Example 3 | 4.4 | 6.9 |
| Example 4 | 3.2 | 7.3 |
| Example 5 | 4.2 | 7.1 |
| Example 6 | 4.2 | 5.8 |
| Example 7 | 3.3 | 7.8 |
| Example 8 | 4.0 | 6.9 |
| Example 9 | 4.5 | 6.8 |
| Example 10 | 4.2 | 5.8 |
| Example 11 | 4.2 | 7.2 |
| Example 12 | 3.2 | 7.9 |
| Comparative example 1 | 2.8 | 5.3 |
| Comparative example 2 | 5.6 | 6.2 |
| Comparative example 3 | 1.1 | 9.9 |
As can be seen from the data in tables 1-2, the process of the present invention enables the production of high purity resin products and low resin montan wax directly from lignite, with high co-production yields.
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 (26)
1. A method for co-producing resin and montan wax from lignite, the method comprising:
(1) carrying out first extraction treatment on lignite particles and a first solvent to extract fat, and then carrying out solid-liquid separation to obtain a first solid phase and a first liquid phase;
(2) evaporating the first liquid phase to separate a resin product and a first solvent;
(3) carrying out second extraction treatment on the first solid phase and a second solvent to extract wax, then carrying out solid-liquid separation to obtain a second liquid phase and a second solid phase, and removing the solvent of the second liquid phase to prepare montan wax;
the first solvent is one or more of an ester solvent, an aromatic hydrocarbon solvent and a ketone solvent, and the second solvent is one or more of an alkane solvent, an ester solvent, an aromatic hydrocarbon solvent and petroleum ether;
the temperature of the first extraction treatment is-10 ℃ to 30 ℃, and the temperature of the second extraction treatment is 60 ℃ to 100 ℃.
2. The method according to claim 1, wherein the lignite particles have a particle size of 10mm or less.
3. The method according to claim 1, wherein the lignite particles have a particle size of 6mm or less.
4. The method of claim 1, wherein the lignite particles have a water content of 25 wt.% or less.
5. The method of claim 1, wherein the water content of the lignite particles is 15 wt% or less.
6. The method of claim 1, wherein the first solvent is one or more of methyl acetate, ethyl acetate, acetone, methyl butanone, methyl isobutyl ketone, benzene, toluene, and xylene.
7. The method according to claim 1, wherein the lignite particles and the first solvent are used in a weight ratio of 1: 1-8.
8. The method according to claim 1, wherein the lignite particles and the first solvent are used in a weight ratio of 1: 2-6.
9. The method of any one of claims 1-8, wherein the temperature of the first extraction is 0-30 ℃.
10. The method of any one of claims 1-8, wherein the temperature of the first extraction is 10-25 ℃.
11. The method according to any one of claims 1 to 8, wherein the time of the first extraction treatment is 0.5 to 10 h.
12. The method according to any one of claims 1 to 8, wherein the time of the first extraction treatment is 1 to 6 h.
13. The method according to any one of claims 1 to 8, wherein the method further comprises recycling the first solvent separated by the evaporation treatment of step (2) to step (1) for the first extraction treatment.
14. The method of any one of claims 1-8, wherein the second solvent is one or more of n-pentane, n-hexane, cyclopentane, cyclohexane, methyl acetate, ethyl acetate, benzene, toluene, xylene, and petroleum ether.
15. The process of any one of claims 1-8, wherein the second solvent is one or more of methyl acetate, ethyl acetate, benzene, and toluene.
16. The method according to any one of claims 1 to 8, wherein the weight ratio of the amount of the first solid phase to the second solvent is 1: 1-8.
17. The method according to any one of claims 1 to 8, wherein the weight ratio of the amount of the first solid phase to the second solvent is 1: 1-6.
18. The method according to any one of claims 1 to 8, wherein the first solid phase is subjected to a heat treatment to remove the adhering solvent before the second extraction treatment, the heat treatment being performed under conditions comprising: the temperature is 40-80 deg.C, and the time is 30-200 min.
19. The method according to any one of claims 1 to 8, wherein the temperature of the second extraction treatment is 70-90 ℃.
20. The method according to any one of claims 1 to 8, wherein the time of the second extraction treatment is 1 to 8 h.
21. The method according to any one of claims 1 to 8, wherein the time of the second extraction treatment is 1.5 to 5 h.
22. The method of any of claims 1-8, wherein the resin content in the resin product is 97 wt% or more; the content of the asphalt is less than 1 weight percent; the wax content is 3 wt% or less.
23. The method of any of claims 1-8, wherein the resin product has a resin content of 99 wt% or more; the content of the asphalt is less than 0.3 weight percent; the wax content is 2 wt% or less.
24. The method according to any one of claims 1 to 8, wherein the wax content of the montan wax is 80 wt.% or more; the content of the bitumen is less than 5 wt%; the content of the resin is 20 wt% or less.
25. The method according to any one of claims 1 to 8, wherein the wax content in the montan wax is 90 wt% or more; the content of the bitumen is less than 3 wt%; the content of the resin is 10 wt% or less.
26. Montan wax or resin produced by the method of any one of claims 1-25.
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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 |
| CN103666561A (en) * | 2013-12-04 | 2014-03-26 | 曲靖众一精细化工股份有限公司 | A method of continuously producing resin-removed lignite wax and resin and a device thereof |
| CN103897734A (en) * | 2014-04-12 | 2014-07-02 | 曲靖众一精细化工股份有限公司 | Energy-saving efficient resin-removing method and device for coarse lignite wax |
| 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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| 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 |
| CN103666561A (en) * | 2013-12-04 | 2014-03-26 | 曲靖众一精细化工股份有限公司 | A method of continuously producing resin-removed lignite wax and resin and a device thereof |
| CN103897734A (en) * | 2014-04-12 | 2014-07-02 | 曲靖众一精细化工股份有限公司 | Energy-saving efficient resin-removing method and device for coarse lignite wax |
| 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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