CN114517111A - Purification method and system of montan wax crude extract - Google Patents
Purification method and system of montan wax crude extract Download PDFInfo
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- 239000012170 montan wax Substances 0.000 title claims abstract description 120
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000000287 crude extract Substances 0.000 title claims abstract description 25
- 238000000746 purification Methods 0.000 title claims description 22
- 239000002904 solvent Substances 0.000 claims abstract description 207
- 239000000284 extract Substances 0.000 claims abstract description 110
- 239000002994 raw material Substances 0.000 claims abstract description 55
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 22
- 238000000605 extraction Methods 0.000 claims description 109
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 35
- 238000000926 separation method Methods 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- 239000001294 propane Substances 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 2
- 239000001273 butane Substances 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims description 2
- 239000011347 resin Substances 0.000 abstract description 88
- 229920005989 resin Polymers 0.000 abstract description 88
- 239000003077 lignite Substances 0.000 abstract description 60
- 239000001993 wax Substances 0.000 abstract description 47
- 238000005406 washing Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000010426 asphalt Substances 0.000 description 47
- 239000000047 product Substances 0.000 description 31
- 238000004458 analytical method Methods 0.000 description 13
- 238000002156 mixing Methods 0.000 description 11
- 239000007787 solid Substances 0.000 description 10
- 229910002092 carbon dioxide Inorganic materials 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 238000001704 evaporation Methods 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000000194 supercritical-fluid extraction Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000002817 coal dust Substances 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Images
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0403—Solvent extraction of solutions which are liquid with a supercritical fluid
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09F—NATURAL RESINS; FRENCH POLISH; DRYING-OILS; DRIERS (SICCATIVES); TURPENTINE
- C09F1/00—Obtaining purification, or chemical modification of natural resins, e.g. oleo-resins
- C09F1/02—Purification
Abstract
The invention aims to provide a method for purifying a montan wax crude extract, which comprises the following steps of S2: extracting the raw material of the montan wax crude extract by using an extracting agent to obtain an extract and an extract residue; wherein the extractant comprises a supercritical solvent and optionally an entrainer. Compared with the traditional solvent washing method, the method for purifying the products by the lignite wax crude extract has the advantages of low energy consumption, higher quality of the obtained wax products, high purity of the obtained lignite wax products, low solvent residue and higher economic value, and meanwhile, the lignite resin has higher purity and the economic value is greatly increased.
Description
Technical Field
The invention relates to the field of lignite wax purification, in particular to a purification method and a purification system for a lignite crude wax extract.
Background
The main components of the montan wax are pure wax, resin and asphalt, and the composition of different coal-forming plants is different from that of the montan wax extracted from coal under coal-forming environment. In the crude wax of the German montan wax, the resin content is lower and is generally 10-30%, and the requirements of various industrial applications can be basically and directly met; in the crude wax of montan wax in China, the resin content is usually higher by 20-50%. Too high a resin content can cause the montan wax to be sticky. The viscosity, the chromaticity and the utilization approach of the bitumen in the montan wax are influenced, the cosolubility of the montan wax and other additives is influenced, the physical and chemical properties and the mechanical properties of the montan wax are poor, and the subsequent refining process of the montan wax is also influenced.
The traditional extraction process of the montan wax usually adopts organic solvent extraction, and the crude montan wax extract is obtained by evaporating and separating the extraction liquid from the solvent. And according to the product quality requirement, particularly the lignite wax extract with high resin content in some Chinese countries, the crude wax extract is subjected to resin and asphalt removal to obtain the crude wax. The resin is removed by separating the wax and the resin by cold solvent washing or crystallization by utilizing the difference of the solubility of the wax and the resin in solvents under different conditions. The two modes need to be subjected to evaporation concentration, cooling crystallization and re-evaporation concentration, and need to be switched back and forth at the boiling point of the solvent and normal temperature, so that the process is not easy to control accurately, the difficulty of the solid-liquid separation process in the process is high, and a certain amount of coal powder is difficult to avoid remaining in the crude extract, so that the ash content of the product is high, and the influence on the quality is large; on the other hand, the solvent residue and the general condition of the crude montan wax product are still high, which can bring certain influence on the refining and application of the product.
Disclosure of Invention
The invention provides a purification method of a montan wax crude extract, which aims to solve the technical problems in the existing montan wax purification field. The invention utilizes the dissolution characteristics and high selectivity of the supercritical solvent to extract the lignite crude extract, selects proper supercritical process operating conditions to separate out asphalt, lignite resin and lignite wax products, can obviously reduce the solvent residue in the products and improve the quality of the lignite wax products.
In a first aspect, the present invention provides a method for purifying a crude montan wax extract, comprising the steps of S2: crushing the raw material of the crude extract of the montan wax; extracting the crushed raw materials by using an extracting agent in a supercritical state to obtain an extract and an extraction residue; wherein the extractant comprises a supercritical solvent and optionally an entrainer.
Supercritical fluid extraction technology has been developed and applied rapidly in recent years. The supercritical fluid has the advantages of strong diffusivity, low surface tension, high density, high viscosity which is higher than that of gas but far lower than that of liquid, and the like, has strong extraction capability, and is widely applied to the industries of medicine, food, chemical industry and the like; and the solubility of the supercritical fluid changes with the change of the supercritical conditions, and by utilizing the characteristic, the extraction products with different components and molecular weights can be obtained by changing the supercritical extraction conditions.
In some embodiments, the crude montan wax extract material can also be extracted after being dissolved in a solvent.
In some embodiments, the supercritical solvent is obtained after the solvent is subjected to pressurization and heating treatment to reach a critical state before extraction.
In some embodiments, the solvent comprises CO2Propane, butane, pentane and n-hexane.
In some embodiments, the solvent is CO2And/or propane.
In some embodiments, the entrainer comprises one or more of ethanol, ethyl acetate, butyl acetate, acetone, isopropanol, preferably ethanol and/or acetone.
In some specific embodiments, the molar ratio of the entrainer to the solvent is (0-0.2):1 is, for example, 0.02:1, 0.03:1, 0.04:1, 0.05:1, 0.06:1, 0.07:1, 0.08:1, 0.1:1, 0.15:1, 0.18:1 and any value therebetween, preferably (0.04-0.09): 1.
in some preferred embodiments, the purity of the entrainer is 96% or greater.
In some embodiments, the extraction temperature is not less than the critical temperature of the solvent.
In some embodiments, the extraction temperature is above 10 ℃ critical temperature, preferably 30-40 ℃.
In some embodiments, the extraction pressure is not less than the critical pressure of the solvent.
In some specific embodiments, the extraction pressure is above the critical pressure, preferably 10-30MPa above the critical pressure, e.g., in the range of 10MPa, 20MPa, 30MPa, and any combination thereof.
In some embodiments, the extraction time is 0.1 to 3 hours, such as 0.5 hours, 0.8 hours, 1 hour, 1.5 hours, 2 hours, and any value therebetween, preferably 0.5 to 2 hours.
In some embodiments, the feed-to-liquid ratio of the crude montan wax feedstock to the extractant is from 1:5 to 1:20(g/mL), i.e., 5 to 20mL of extractant is added for 1g of the crude montan wax feedstock. It is preferably 1:8 to 1:10(g/mL) from the viewpoint of extraction efficiency and economy.
In some embodiments, the purification method further comprises step S1: crushing the raw material of the montan wax crude extract to 10-50 meshes.
In some embodiments, further comprising a pressure reduction and flashing step.
Preferably, the supercritical solvent carrying the extracted product should be filtered through a filtration device before carrying out said depressurization and flash steps; such as a porous metal or ceramic filter.
In some embodiments, the purification method further comprises the steps of:
s3 first-stage separation: after extraction is finished, the extractor is slowly depressurized, and raffinate at the lower layer of the extraction tank enters a flash tower I to be separated from a solvent, so that coal dust impurities and asphalt are separated out. The extract enters a separator I;
s4 secondary separation: the extraction liquid entering the separator I is further depressurized, and the bottom raffinate enters a flash tower II to be further separated from the solvent, so that the montan wax is separated out. The extract enters a separator II;
s5 three-stage separation: the extraction liquid entering the separator II is further depressurized, and the bottom extraction residue enters a flash tower III to be separated from the extracting agent, so that the lignite resin is separated out.
In some embodiments, the extraction is slowly heated or depressurized in step S3 to separate the extraction solution, and the montan wax, the montan resin, and the extractant are separated sequentially.
In some embodiments, continuous dynamic extraction and separation of the montan wax crude extract feedstock can also be performed.
In some preferred embodiments, the temperature rise speed is 5-10 ℃/h, and the pressure reduction speed is 0.3-1 MPa/min.
In some preferred embodiments, step S3 includes:
separating the extract to separate out montan wax;
optionally, carrying out flash evaporation treatment on the separated montan wax to further remove the solvent in the montan wax;
separating the extract from which the montan wax is separated to obtain montan resin and an extractant;
optionally, carrying out flash evaporation treatment on the separated lignite resin to further remove the solvent in the lignite resin; .
In some embodiments, the purification method further comprises step S6: the entrainer and the solvent obtained by separation are recycled to the step S2 to continuously participate in the extraction.
According to the method of the invention, the pure wax content of the obtained montan wax product is more than 85 percent.
In a second aspect, the present invention provides a supercritical purification system for crude montan wax extract, comprising:
a solvent tank for storing a solvent;
the supercritical unit is used for receiving the solvent from the solvent tank and carrying out pressurization and temperature rise treatment on the solvent to obtain a supercritical solvent;
an optional entrainer tank for storing optional entrainer;
and the extraction unit is connected with the supercritical unit and the optional entrainer tank and is used for receiving the supercritical solvent and the optional entrainer and extracting the raw material of the crude montan wax extract to obtain an extract and a raffinate.
In some embodiments, further comprising: and the separation unit is connected with the extraction unit and is used for receiving the extract and the extractant and separating the extract and the extractant.
In some embodiments, the purification system further comprises:
a mixing unit for mixing the supercritical solvent and the entrainer.
In some embodiments, the extraction unit is an extraction tank.
The separation unit can simplify the process flow according to different raw materials and product quality requirements.
In some embodiments, the separation unit comprises:
a first separation unit for receiving and separating the extract to separate out the montan wax, the montan resin and the extractant;
and the second separation unit is used for receiving and separating the raffinate to separate the asphalt and the solvent.
In some embodiments, the first separation unit comprises:
a separator I for receiving the extract and separating the extract to separate out the montan wax;
a separator II for receiving the extract from the separator I and separating the extract to obtain lignite resin and an extractant;
and the rectifying tower is used for receiving the extracting agent from the separator II and separating the extracting agent to obtain the solvent and the entrainer.
In some embodiments, the outlet of the separator I is connected to a flash tower I for performing a flash treatment on the separated montan wax to further remove the solvent therein. In some embodiments, the outlet of the separator II is connected to a flash tower II for performing flash evaporation treatment on the separated lignite resin to further remove the solvent therein.
In some embodiments, the distillation column is connected to a solvent tank and an entrainer tank respectively, and the solvent and the entrainer separated from the distillation column are recycled to the solvent tank and the entrainer tank.
In some embodiments, the flash column I and flash column II are connected to a solvent tank, and the resulting solvent is recycled back to the solvent tank.
In some embodiments, the second separation unit is a flash column.
Compared with the traditional solvent washing method, the method for purifying the crude extract of the montan wax has the advantages that the obtained montan wax product has higher quality, the purity of the obtained montan wax product is high, the solvent residue is low, the ash content is reduced, meanwhile, the purity of the montan resin is higher, the economic value is greatly increased, and the industrial production prospect is considerable.
Drawings
FIG. 1 is a schematic diagram of a method and system for purifying crude montan wax extracts according to one embodiment of the present invention;
FIG. 2 is a schematic view of a method and system for purifying crude montan wax extracts according to another embodiment of the present invention.
Description of reference numerals: 1-a solvent tank; 2-entrainer tank; 3-a solvent pump; 4-a mixer; 5-a preheater; 6-an extraction tank; 7-separator I; 8-separator II; 9-a rectifying tower; 10-a flash column; 11-flash column I; 12-flash column II; a-bitumen, B-montan wax; c-lignite resin; d-solvent; e-entrainer.
Detailed Description
The present invention will be further illustrated by the following examples, but is not limited to these examples.
Fig. 1 shows a montan wax crude extract purification system according to an embodiment of the present invention, including: the device comprises a solvent tank (1), a solvent pump (3-1), a preheater (5), an extraction tank (6), a separator I (7), a separator II (8), a flash tower (10), a flash tower I (11) and a flash tower II (12). Wherein the solvent tank is connected with the preheater through a solvent pump, and the preheater is connected with the extraction tank; the extraction tank comprises an extractant outlet and a raffinate outlet, the extractant outlet is connected with the separator I, and the raffinate outlet is connected with the flash tower; the separator I comprises a solvent outlet and a solid outlet, the solid outlet is connected with the flash tower I, and the solvent outlet is connected with the separator II; the separator II comprises a solvent outlet and a solid outlet, the solid outlet is connected with the flash tower II, and the solvent outlet is connected to a solvent tank through a cooling pump; the flash tower I, the flash tower II and the flash tower comprise a solvent outlet and a solid outlet, and the solvent outlet is connected to a solvent tank through a cooling pump.
The extraction process flow of the crude montan wax extract by using the system is as follows: adding the raw material of the crude extract of the montan wax into an extraction tank, pressurizing a solvent in a solvent tank to a supercritical state by a solvent pump, preheating the solvent to an extraction temperature by a preheater, and introducing the preheated solvent into the extraction tank to extract the raw material; after extracting for a certain time, the lower raffinate enters a flash tower to be separated from the solvent, and the separated asphalt-enriched component is separated out; the upper layer solvent and the extract enter a separator I after slowly reducing the pressure or raising the temperature; the extract at the lower layer of the separator I enters a flash tower I to be further separated from the solvent, the lignite wax enrichment component is separated out, and the solvent and the extract at the upper layer of the separator I enter a separator II after being slowly depressurized or heated; and (3) the extract at the lower layer of the separator II enters a flash tower II to be further separated from the solvent, and the lignite resin enrichment component is separated out.
Fig. 2 shows a system for purifying a crude montan wax extract according to another embodiment of the invention, which includes: the device comprises a solvent tank (1), an entrainer tank (2), a solvent pump (3-1), a solvent pump (3-2), a mixer (4), a preheater (5), an extraction tank (6), a separator I (7), a separator II (8), a rectifying tower (9), a flash tower (10), a flash tower I (11) and a flash tower II (12). Wherein the solvent tank and the entrainer tank are respectively connected with a mixer through a solvent pump, and the mixer is connected with the extraction tank through a preheater; the extraction tank comprises an extractant outlet and a raffinate outlet, the extractant outlet is connected with the separator I, and the raffinate outlet is connected with the flash tower; the separator I comprises a solvent outlet and a solid outlet, the solid outlet is connected with the flash tower I, and the solvent outlet is connected with the separator II; the separator II comprises a solvent outlet and a solid outlet, the solid outlet is connected with the flash tower II, and the solvent outlet is connected with the rectifying tower; the flash tower I, the flash tower II and the flash tower comprise a solvent outlet and a solid outlet, and the solvent outlet is connected to a solvent tank through a cooling pump; the rectifying tower comprises a solvent outlet and an entrainer outlet, the solvent outlet is connected to the solvent tank through a cooling pump, and the entrainer outlet is connected to the entrainer tank.
The extraction process flow of the crude extract of the montan wax by using the system is as follows: adding the raw material of the crude extract of the montan wax into an extraction tank, pressurizing a solvent in the solvent tank to a supercritical state by a solvent pump, mixing the solvent and an entrainer in a mixer according to a certain proportion to obtain an extractant, preheating the extractant by a preheater to an extraction temperature, and introducing the preheated extractant into the extraction tank to extract the raw material; after extracting for a certain time, the lower raffinate enters a flash tower to be separated from the solvent, and the separated asphalt-enriched component is separated out; the upper layer solvent and the extract enter a separator I after slowly reducing the pressure or raising the temperature; the extract at the lower layer of the separator I enters a flash tower I to be further separated from the solvent, and the lignite wax enrichment component is separated out; the solvent and the extract on the upper layer of the separator I enter a separator II after slowly reducing the pressure or raising the temperature; and (3) the extract at the lower layer of the separator II enters a flash tower II to be further separated from the solvent, and the lignite resin enrichment component is separated out. And (3) feeding the extractant on the upper layer of the separator into a rectifying tower, separating out entrainer and solvent, cooling the entrainer to return to an entrainer tank, and cooling the solvent and the solvent collected by each flash tower to return to a solvent tank.
The embodiment of the invention takes the crude montan wax extract obtained by extracting the brown coal in a certain place by using toluene as a solvent as a raw material to carry out subsequent purification operation, and the analysis of the raw material components of the crude montan wax extract is shown in the following table 1:
TABLE 1
| Content of resin% | Content of bitumen is% | Pure wax content,% of | |
| Crude extract of montan wax | 42.1 | 5.4 | 52.5 |
The raw materials, the resins obtained in the following examples and comparative examples, and montan wax were subjected to composition analysis, and the resin and asphalt contents were measured according to GB/T2559-2005 montan wax determination method.
Example 1
Purifying raw material of crude extract of montan wax by using the system of fig. 1, crushing 50g of raw material of crude extract of montan wax to 20-50 meshes, putting the crushed raw material into an extraction tank, and adding CO in a solvent tank2Pressurizing to 30MPa by a solvent pump, preheating to 35 ℃ by a preheater, introducing 400mL of the solution into an extraction tank; the temperature in the extraction tank is controlled at 35 ℃ and the pressure is controlled at 30 MPa. After reacting for 2 hours, the lower raffinate of the extraction tank enters a flash tower to be separated from the solvent, bitumen is separated out, and the upper solvent and the extract of the extraction tank enter a separator I after slowly heating to 40 ℃; allowing the lignite wax on the lower layer of the separator I to enter a flash tower I for further separation from the solvent to separate out lignite wax, slowly heating the solvent and the extract on the upper layer of the separator I to 45 ℃, and then allowing the solvent and the extract to enter a separator II; the lignite resin at the lower layer of the separator II enters a flash tower II to be further separated from the solvent, the lignite resin is separated out, and the obtained lignite wax and resin product component analysis is shown in a table 2.
TABLE 2
| Extract/g | Content of resin/%) | Ground asphalt/%) | Pure wax/% | |
| Bitumen component | 7.4 | 8.4 | 80.9 | 10.7 |
| Montan wax component | 22.2 | 16.9 | 4.2 | 78.9 |
| Resin component | 18.1 | 81.8 | 2.7 | 15.5 |
Example 2
Purifying the raw material of the crude extract of montan wax by using the system of fig. 2, crushing 50g of the raw material of the crude extract of montan wax to 20-50 meshes, putting the crushed raw material into an extraction tank, and adding CO in a solvent tank2Pressurizing the ethanol in the entrainer tank to 30MPa by a solvent pump respectively, and mixing in a mixer to obtain an extracting agent, CO2The mol ratio of the extracting agent to the ethanol is 1:0.04, the extracting agent is preheated to 35 ℃ by a preheater, and then 400mL of extracting agent is introduced into an extraction tank; the temperature in the extraction tank is controlled at 35 ℃ and the pressure is controlled at 30 MPa. After reacting for 2 hours, separating the lower-layer raffinate in the extraction tank in a flash tower to separate out asphalt, slowly heating the upper-layer solvent and the extract in the extraction tank to 40 ℃, and then feeding the solvent and the extract in a separator I; allowing the lignite wax on the lower layer of the separator I to enter a flash tower I for further separation from the solvent to separate out lignite wax, slowly heating the solvent and the extract on the upper layer of the separator I to 45 ℃, and then allowing the solvent and the extract to enter a separator II; is divided intoThe lignite resin at the lower layer of the separator II enters a flash tower II to be further separated from the solvent, the lignite resin is separated out, and the obtained lignite wax and resin product composition analysis is shown in a table 3.
TABLE 3
| Extract/g | Content of resin/%) | Ground asphalt/%) | Pure wax/% | |
| Bitumen component | 5.2 | 2.1 | 87.2 | 10.7 |
| Montan wax component | 24.3 | 13.8 | 0.9 | 85.3 |
| Resin component | 18.2 | 90.8 | 2.1 | 7.1 |
Example 3
Purifying the raw material of the crude extract of montan wax by using the system of fig. 2, crushing 50g of the raw material of the crude extract of montan wax to 20-50 meshes, putting the crushed raw material into an extraction tank, and adding CO in a solvent tank2Pressurizing the ethanol in the entrainer tank to 30MPa by a solvent pump respectively, and mixing in a mixer to obtain an extracting agent, CO2The mol ratio of the extractant to the ethanol is 1:0.04, the extractant is preheated to 40 ℃ by a preheater, and then 400mL of the extractant is introduced into an extraction tank; the temperature in the extraction tank is controlled at 40 ℃ and the pressure at 30 MPa. After reacting for 4 hours, separating the lower-layer raffinate in the extraction tank in a flash tower to separate out asphalt, slowly heating the upper-layer solvent and the extract in the extraction tank to 40 ℃, and then feeding the solvent and the extract in a separator I; allowing the montan wax on the lower layer of the separator I to enter a flash tower I for further separation from the solvent to separate out montan wax, slowly heating the solvent and the extract on the upper layer of the separator I to 50 ℃, and then allowing the solvent and the extract to enter a separator II; the lignite resin at the lower layer of the separator II enters a flash tower II to be further separated from the solvent, the lignite resin is separated out, and the obtained lignite wax and resin product component analysis is shown in Table 4.
TABLE 4
| Extract/g | Content of resin/%) | Di% by mol | Pure wax/% | |
| Bitumen component | 5.6 | 2.4 | 90.1 | 7.5 |
| Montan wax component | 25.9 | 12.1 | 1.2 | 87.7 |
| Resin component | 17.2 | 91.7 | 1.3 | 7.0 |
Example 4
Purifying the raw material of the crude montan wax extract by using the system shown in FIG. 2, crushing 50g of the raw material of the crude montan wax extract to 20-50 meshes, putting the crushed raw material into an extraction tank, and adding CO into a solvent tank2And acetone in the entrainer tank are respectively pressurized to 30MPa by a solvent pump and then enter a mixer to be mixed to obtain an extracting agent, CO2The mol ratio of the extracting agent to acetone is 1:0.04, the extracting agent is preheated to 40 ℃ by a preheater, and then 400mL of extracting agent is introduced into an extraction tank; the temperature in the extraction tank is controlled at 40 ℃ and the pressure is controlled at 30 MPa. After reacting for 4 hours, separating the lower-layer raffinate in the extraction tank in a flash tower to separate out asphalt, slowly heating the upper-layer solvent and the extract in the extraction tank to 40 ℃, and then feeding the solvent and the extract in a separator I; allowing the montan wax on the lower layer of the separator I to enter a flash tower I for further separation from the solvent to separate out montan wax, slowly heating the solvent and the extract on the upper layer of the separator I to 50 ℃, and then allowing the solvent and the extract to enter a separator II; the lignite resin at the lower layer of the separator II enters a flash tower II to be further separated from the solvent, the lignite resin is separated out, and the obtained lignite wax and resin product component analysis is shown in Table 5.
TABLE 5
| Extract/g | Content of resin/%) | Ground asphalt/%) | Pure wax/% | |
| Bitumen component | 4.9 | 5.4 | 92.3 | 2.3 |
| Montan wax component | 26.4 | 10.1 | 1.5 | 88.4 |
| Resin component | 17.6 | 90.3 | 1.4 | 8.3 |
Example 5
Purifying raw materials of the crude montan wax extract by using the system shown in figure 2, crushing 50g of raw materials of the crude montan wax extract to 20-50 meshes, putting the crushed raw materials into an extraction tank, and adding CO in the solvent tank2Pressurizing the ethanol in the entrainer tank to 30MPa by a solvent pump respectively, and mixing in a mixer to obtain an extracting agent, CO2The mol ratio of the extractant to the ethanol is 1:0.1, the extractant is preheated to 35 ℃ by a preheater, and then 400mL of the extractant is introduced into an extraction tank; the temperature in the extraction tank is controlled at 35 ℃ and the pressure is controlled at 30 MPa. After reacting for 2 hours, the lower raffinate of the extraction tank enters a flash tower to be separated from the solvent, bitumen is separated out, and the upper solvent and the extract of the extraction tank enter a separator I after slowly heating to 40 ℃; allowing the lignite wax on the lower layer of the separator I to enter a flash tower I for further separation from the solvent to separate out lignite wax, slowly heating the solvent and the extract on the upper layer of the separator I to 45 ℃, and then allowing the solvent and the extract to enter a separator II; the lignite resin at the lower layer of the separator II enters a flash tower II to be further separated from the solvent, the lignite resin is separated out, and the obtained lignite wax and resin product component analysis is shown in Table 6.
TABLE 6
| Extract/g | Content of resin/%) | Ground asphalt/%) | Pure wax/% | |
| Bitumen component | 4.9 | 8.8 | 77.9 | 13.3 |
| Montan wax component | 25.1 | 17.1 | 9.4 | 73.5 |
| Resin component | 18.3 | 82.3 | 7.0 | 10.7 |
Example 6
Purifying the raw material of the crude montan wax extract by using the system shown in FIG. 2, crushing 50g of the raw material of the crude montan wax extract to 20-50 meshes, putting the crushed raw material into an extraction tank, and adding CO in a solvent tank2Pressurizing the ethanol in the entrainer tank to 40MPa by a solvent pump respectively, and mixing in a mixer to obtain an extracting agent, CO2The mol ratio of the extracting agent to the ethanol is 1:0.04, the extracting agent is preheated to 40 ℃ by a preheater, and 400mL of extracting agent is introduced into an extraction tank; the temperature in the extraction tank is controlled at 40 ℃ and the pressure is controlled at 40 MPa. After reacting for 4 hours, the lower raffinate of the extraction tank enters a flash tower to be separated from the solvent, bitumen is separated out, and the upper solvent and the extract of the extraction tank enter a separator I after slowly heating to 45 ℃; allowing the montan wax on the lower layer of the separator I to enter a flash tower I for further separation from the solvent to separate out montan wax, slowly heating the solvent and the extract on the upper layer of the separator I to 50 ℃, and then allowing the solvent and the extract to enter a separator II; the lignite resin at the lower layer of the separator II enters a flash tower II to be further separated from the solvent, the lignite resin is separated out, and the obtained lignite wax and resin product component analysis is shown in Table 7.
TABLE 7
| Extract/g | Content of resin/%) | Ground asphalt/%) | Pure wax/% | |
| Bitumen component | 5.1 | 4.4 | 85.4 | 10.2 |
| Montan wax component | 26.7 | 13.7 | 5.1 | 81.2 |
| Resin component | 19.2 | 83.1 | 6.2 | 10.7 |
Example 7
Purifying raw materials of a crude montan wax extract by using the system of fig. 1, crushing 50g of raw materials of the crude montan wax extract to 20-50 meshes, putting the crushed raw materials into an extraction tank, pressurizing propane in a solvent tank to 30MPa by using a solvent pump, then feeding the pressurized propane into a preheater, preheating the preheated propane to 120 ℃ by using the preheater, and introducing 400mL of an extracting agent into the extraction tank; controlling the temperature in the extraction tank to be 120 ℃ and the pressure to be 30MPa, after reacting for 2 hours, feeding the lower-layer raffinate in the extraction tank into a flash tower to be separated from the solvent, separating out asphalt, slowly heating the upper-layer solvent and the extract in the extraction tank to 125 ℃, and feeding the solvent and the extract into a separator I; allowing the montan wax on the lower layer of the separator I to enter a flash tower I for further separation from the solvent to separate out montan wax, slowly heating the solvent and the extract on the upper layer of the separator I to 130 ℃, and then allowing the solvent and the extract to enter a separator II; the lignite resin at the lower layer of the separator II enters a flash tower II to be further separated from the solvent, the lignite resin is separated out, and the obtained lignite wax and resin product component analysis is shown in Table 8.
TABLE 8
| Extract/g | Content of resin/%) | Ground asphalt/%) | Pure wax/% | |
| Bitumen component | 6.4 | 8.9 | 74.6 | 16.5 |
| Montan wax component | 23.2 | 11.2 | 8.5 | 80.3 |
| Resin component | 18.8 | 83.6 | 6.7 | 9.7 |
Example 8
Purifying raw materials of a crude montan wax extract by using the system shown in FIG. 2, crushing 50g of raw materials of the crude montan wax extract to 20-50 meshes, putting the crushed raw materials into an extraction tank, pressurizing propane in a solvent tank and ethanol in an entrainer tank to 30MPa respectively by using a solvent pump, then mixing the pressurized raw materials in a mixer to obtain an extractant, wherein the molar ratio of the propane to the ethanol is 1:0.04, preheating the extractant to 120 ℃ by using a preheater, and then introducing the preheated extractant into the extraction tank; the temperature in the extraction tank is controlled at 120 ℃ and the pressure is controlled at 30 MPa. After reacting for 2 hours, the lower raffinate of the extraction tank enters a flash tower to be separated from the solvent, bitumen is separated out, and the upper solvent and the extract of the extraction tank slowly rise to 125 ℃ and then enter a separator I; allowing the montan wax on the lower layer of the separator I to enter a flash tower I for further separation from the solvent to separate out montan wax, slowly heating the solvent and the extract on the upper layer of the separator I to 130 ℃, and then allowing the solvent and the extract to enter a separator II; the lignite resin at the lower layer of the separator II enters a flash tower II to be further separated from the solvent, the lignite resin is separated out, and the obtained lignite wax and resin product component analysis is shown in Table 9.
TABLE 9
| Extract/g | Content of resin/%) | Ground asphalt/%) | Pure wax/% | |
| Bitumen component | 3.4 | 1.9 | 88.9 | 9.2 |
| Montan wax component | 26.6 | 9.8 | 1.5 | 88.7 |
| Resin component | 18.9 | 90.2 | 2.0 | 7.8 |
Example 9
Purifying raw materials of a crude montan wax extract by using the system shown in FIG. 2, crushing 50g of raw materials of the crude montan wax extract to 20-50 meshes, putting the crushed raw materials into an extraction tank, pressurizing propane in a solvent tank and ethanol in an entrainer tank to 30MPa respectively by using a solvent pump, then mixing the pressurized raw materials in a mixer to obtain an extractant, wherein the molar ratio of the propane to the ethanol is 1:0.04, preheating the extractant to 120 ℃ by using a preheater, and then introducing the preheated extractant into the extraction tank; the temperature in the extraction tank is controlled at 120 ℃ and the pressure is controlled at 30 MPa. After reacting for 4 hours, the lower raffinate of the extraction tank enters a flash tower to be separated from the solvent, bitumen is separated out, and the upper solvent and the extract of the extraction tank slowly rise to 125 ℃ and then enter a separator I; allowing the montan wax on the lower layer of the separator I to enter a flash tower I for further separation from the solvent to separate out montan wax, slowly heating the solvent and the extract on the upper layer of the separator I to 130 ℃, and then allowing the solvent and the extract to enter a separator II; the lignite resin at the lower layer of the separator II enters a flash tower II to be further separated from the solvent, the lignite resin is separated out, and the obtained lignite wax and resin product component analysis is shown in a table 10.
| Extract/g | Content of resin/%) | Ground asphalt/%) | Pure wax/% | |
| Bitumen component | 3.2 | 2.7 | 89.5 | 7.8 |
| Montan wax component | 26.1 | 8.7 | 1.6 | 90.7 |
| Resin component | 19.2 | 89.1 | 1.2 | 9.7 |
Example 10
Purifying raw materials of a crude montan wax extract by using the system of FIG. 2, crushing 50g of raw materials of the crude montan wax extract to 20-50 meshes, putting the crushed raw materials into an extraction tank, pressurizing propane in a solvent tank and acetone in an entrainer tank to 30MPa by using a solvent pump respectively, then mixing the pressurized raw materials in a mixer to obtain an extractant, wherein the molar ratio of the propane to the acetone is 1:0.04, preheating the extractant to 120 ℃ by using a preheater, and then introducing the preheated extractant into the extraction tank; the temperature in the extraction tank is controlled at 120 ℃ and the pressure is controlled at 30 MPa. After reacting for 4 hours, the lower raffinate of the extraction tank enters a flash tower to be separated from the solvent, bitumen is separated out, and the upper solvent and the extract of the extraction tank slowly rise to 125 ℃ and then enter a separator I; allowing the montan wax on the lower layer of the separator I to enter a flash tower I for further separation from the solvent to separate out montan wax, slowly heating the solvent and the extract on the upper layer of the separator I to 130 ℃, and then allowing the solvent and the extract to enter a separator II; the lignite resin at the lower layer of the separator II enters a flash tower II to be further separated from the solvent, the lignite resin is separated out, and the obtained lignite wax and resin product component analysis is shown in Table 11.
TABLE 11
Example 11
The method comprises the steps of purifying raw materials of the crude montan wax extract by using the system of fig. 2, crushing 50g of raw materials of the crude montan wax extract to 20-50 meshes, putting the crushed raw materials into an extraction tank, pressurizing propane in a solvent tank and ethanol in an entrainer tank to 30MPa respectively by a solvent pump, then mixing the pressurized raw materials in a mixer to obtain an extractant, wherein the molar ratio of the propane to the ethanol is 1:0.04, the extractant is preheated to 140 ℃ by a preheater, continuously introducing the preheated extractant into the extraction tank at the flow rate of 100mL/min, and controlling the temperature and the pressure in the extraction tank to be 30 MPa. After reacting for 2 hours, the lower raffinate of the extraction tank enters a flash tower to be separated from the solvent, bitumen is separated out, and the upper solvent and the extract of the extraction tank slowly rise to 145 ℃ and then enter a separator I; allowing the montan wax on the lower layer of the separator I to enter a flash tower I for further separation from the solvent to separate out montan wax, slowly heating the solvent and the extract on the upper layer of the separator I to 150 ℃, and then allowing the solvent and the extract to enter a separator II; the lignite resin at the lower layer of the separator II enters a flash tower II to be further separated from the solvent, the lignite resin is separated out, and the obtained lignite wax and resin product component analysis is shown in Table 12.
TABLE 12
| Extract/g | Content of resin/%) | Ground asphalt/%) | Pure wax/% | |
| Bitumen component | 2.9 | 1.6 | 89.5 | 9.9 |
| Montan wax component | 26.3 | 8.6 | 1.8 | 90.6 |
| Resin component | 19.6 | 90.9 | 1.6 | 7.5 |
Comparative example 1
And (2) comparing a normal-temperature cold solvent elution method, crushing the montan wax until the particle size is smaller than 50 meshes, dissolving 50g of the crushed montan wax and 250mL of a toluene solvent at normal temperature to carry out degreasing reaction, controlling the stirring speed to be 100r/min, fully reacting for 2 hours, and filtering to obtain filtrate and filter residues. Repeating the above elution steps to elute the filter residue until the filtrate is colorless, and obtaining filter residue which is montan wax (containing asphalt); all the collected filtrates were subjected to heating rotary evaporation to recover the solvent and obtain a resin, and the obtained montan wax and resin product were analyzed for composition, see Table 13.
Watch 13
| Content of resin/%) | Ground asphalt/%) | Pure wax/% | |
| Montan wax products | 23.6 | 5.9 | 70.5 |
| Resin product | 60.8 | 0.6 | 38.6 |
As is clear from the data of examples 1 to 11, the method and system of the present invention can effectively separate montan wax from foreign resins and asphaltum in crude montan wax extract with high yield and high purity of the separated product. Comparative example 1 no bitumen could be separated and the product obtained from the separation was of lower purity.
Examples 1-6 and 7-11 are conditions using different solvents for carbon dioxide and propane, and overall the overall extraction yield is higher with propane, especially the extraction yield of the sum of montan wax and resin fractions, but the energy consumption of propane is relatively high.
From example 1 versus examples 2-6 and example 7 versus examples 8-11, it is seen that the examples were with and without entrainer under different extraction solvent conditions, respectively, and that the entrainer gave better extraction of resin and montan wax, and the purity of the extracted product was higher.
As can be seen from the comparison of examples 3 and 4, 9 and 10, the type of entrainer affects the extraction yield and purification efficiency, ethanol is used as the entrainer to facilitate the production of higher purity bitumen, and acetone is used as the entrainer to facilitate the production of higher total and purity montan wax and resin.
As can be seen from examples 2, 3 and 6 and 8, 9 and 11, the extraction temperature and time affect the purification effect, and the higher temperature and the longer extraction time are favorable for bringing better purification effect, and the purity of the extracted bitumen, montan wax and resin products is higher.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.
Claims (10)
1. A method for purifying a crude montan wax extract, which is characterized by comprising a step S2: crushing the raw material of the crude extract of the montan wax; and extracting the crushed raw material by using an extracting agent in a supercritical state to obtain an extract and a raffinate, wherein the extracting agent comprises a supercritical solvent and an optional entrainer.
2. The purification method according to claim 1, wherein the supercritical solvent is obtained by pressurizing and heating a solvent to a critical state; preferably the solvent comprises CO2One or more of propane, butane, pentane and n-hexane, and more preferably CO2And/or propane.
3. The purification method according to claim 1 or 2, wherein the entrainer comprises one or more of ethanol, ethyl acetate, butyl acetate, acetone, isopropanol, preferably ethanol and/or acetone.
4. The purification process according to any one of claims 1 to 3, wherein the molar ratio of entrainer to solvent is (0-0.2):1, preferably (0.04-0.09): 1.
5. A purification method according to any one of claims 1 to 4, wherein in the extraction step, the extraction temperature is 10 ℃ above the supercritical temperature of the selected solvent, preferably 30 to 40 ℃ above; and/or the extraction pressure is above the critical pressure, preferably above the critical pressure by 10-30 MPa; and/or the extraction time is 0.1-3h, preferably 0.5-2 h.
6. The purification method according to any one of claims 1 to 5, wherein the feed-to-liquid ratio of the raw material of the crude montan wax extract to the extractant is from 1:5 to 1:20(g/mL), preferably from 1:8 to 1:10 (g/mL).
7. The purification method according to any one of claims 1 to 6, further comprising step S1: crushing the raw material of the montan wax crude extract to 10-50 meshes.
8. The extraction process of claim 1, further comprising the steps of depressurizing and flashing; preferably, the supercritical solvent carrying the extracted product should be filtered through a filtration device before carrying out said depressurization and flash steps; preferably, the filter device is a porous metal or ceramic filter.
9. A system for purifying a crude montan wax extract, comprising:
a solvent tank for storing a solvent;
the solvent treatment unit is used for receiving the solvent from the solvent tank and carrying out pressurization and temperature rise treatment on the solvent to obtain a supercritical solvent;
an optional entrainer tank for storing optional entrainer;
and the extraction unit is connected with the supercritical unit and the optional entrainer tank and is used for receiving the supercritical solvent and the optional entrainer and extracting the raw material of the crude montan wax extract to obtain an extract and a raffinate.
10. The system for purifying a crude montan wax extract according to claim 9, further comprising: and the separation unit is connected with the extraction unit and is used for receiving the extract and the raffinate and separating the extract and the raffinate.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5011594A (en) * | 1987-12-18 | 1991-04-30 | Fried. Krupp Gmbh | Process for the continuous extraction of mixtures of organic substances with supercritical solvents |
| CN101029255A (en) * | 2007-02-01 | 2007-09-05 | 中国矿业大学 | Brown-coal green extractive solvent and its production |
| WO2011011972A1 (en) * | 2009-07-27 | 2011-02-03 | 新奥科技发展有限公司 | Method for extracting lignite wax |
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2020
- 2020-11-20 CN CN202011315105.8A patent/CN114517111A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5011594A (en) * | 1987-12-18 | 1991-04-30 | Fried. Krupp Gmbh | Process for the continuous extraction of mixtures of organic substances with supercritical solvents |
| CN101029255A (en) * | 2007-02-01 | 2007-09-05 | 中国矿业大学 | Brown-coal green extractive solvent and its production |
| WO2011011972A1 (en) * | 2009-07-27 | 2011-02-03 | 新奥科技发展有限公司 | Method for extracting lignite wax |
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