CN104312627B - A kind of crystallization process removes solvent and the method for resin in montanin wax - Google Patents
A kind of crystallization process removes solvent and the method for resin in montanin wax Download PDFInfo
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- CN104312627B CN104312627B CN201410584153.5A CN201410584153A CN104312627B CN 104312627 B CN104312627 B CN 104312627B CN 201410584153 A CN201410584153 A CN 201410584153A CN 104312627 B CN104312627 B CN 104312627B
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- montanin wax
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- filtrate
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- MKYLOMHWHWEFCT-UHFFFAOYSA-N Manthidine Natural products C1C2=CC=3OCOC=3C=C2C2C3=CC(OC)C(O)CC3N1C2 MKYLOMHWHWEFCT-UHFFFAOYSA-N 0.000 title claims abstract description 70
- SNFRINMTRPQQLE-JQWAAABSSA-N Montanin Chemical compound O[C@H]([C@@]1(CO)O[C@H]1[C@H]1[C@H]2O3)[C@]4(O)C(=O)C(C)=C[C@H]4[C@]11OC3(CCCCCCCCCCC)O[C@@]2(C(C)=C)C[C@H]1C SNFRINMTRPQQLE-JQWAAABSSA-N 0.000 title claims abstract description 70
- SNFRINMTRPQQLE-OFGNMXNXSA-N Montanin Natural products O=C1[C@@]2(O)[C@@H](O)[C@@]3(CO)O[C@H]3[C@@H]3[C@H]4[C@@]5(C(=C)C)O[C@](CCCCCCCCCCC)(O4)O[C@@]3([C@H](C)C5)[C@@H]2C=C1C SNFRINMTRPQQLE-OFGNMXNXSA-N 0.000 title claims abstract description 70
- QTZPBQMTXNEKRX-UHFFFAOYSA-N Voacristine pseudoindoxyl Natural products N1C2=CC=C(OC)C=C2C(=O)C21CCN(C1)C3C(C(C)O)CC1CC32C(=O)OC QTZPBQMTXNEKRX-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000002425 crystallisation Methods 0.000 title claims abstract description 45
- 239000002904 solvent Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 39
- 230000008025 crystallization Effects 0.000 title claims abstract description 36
- 239000011347 resin Substances 0.000 title claims abstract description 34
- 229920005989 resin Polymers 0.000 title claims abstract description 34
- 230000008569 process Effects 0.000 title claims abstract description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000002245 particle Substances 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000000706 filtrate Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 9
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000009740 moulding (composite fabrication) Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 206010013786 Dry skin Diseases 0.000 claims abstract description 3
- 230000006837 decompression Effects 0.000 claims abstract description 3
- 238000002347 injection Methods 0.000 claims abstract description 3
- 239000007924 injection Substances 0.000 claims abstract description 3
- 239000000047 product Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000002826 coolant Substances 0.000 claims description 3
- IIEWJVIFRVWJOD-UHFFFAOYSA-N ethyl cyclohexane Natural products CCC1CCCCC1 IIEWJVIFRVWJOD-UHFFFAOYSA-N 0.000 claims description 2
- 238000003828 vacuum filtration Methods 0.000 claims description 2
- 230000006378 damage Effects 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 208000027418 Wounds and injury Diseases 0.000 abstract description 2
- 208000014674 injury Diseases 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 238000004090 dissolution Methods 0.000 abstract 2
- 238000002955 isolation Methods 0.000 abstract 1
- 239000001993 wax Substances 0.000 description 68
- 238000000605 extraction Methods 0.000 description 17
- 239000003960 organic solvent Substances 0.000 description 17
- 238000005238 degreasing Methods 0.000 description 11
- 239000000243 solution Substances 0.000 description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 8
- 238000001704 evaporation Methods 0.000 description 6
- 230000008020 evaporation Effects 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000002386 leaching Methods 0.000 description 4
- 239000000284 extract Substances 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000012170 montan wax Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000006200 vaporizer Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000001172 liquid--solid extraction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 206010009866 Cold sweat Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N alpha-methyl toluene Natural products CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000002198 cosolvency Effects 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000000956 solid--liquid extraction Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
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
Landscapes
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Crystallization process removes solvent and the method for resin in montanin wax, belongs to the method for deviating from resin from montanin wax.The method step is as follows: (1) heating for dissolving: insert in crystallization kettle by montanin wax particle, injection ring hexane or ethyl acetate solvent in crystallization kettle, feed liquid mass ratio is 1:5 ~ 50, stir, steam heats crystallization kettle, control chamber pressure at 1.0 ~ 5.0MPa, until montanin wax grain dissolution; (2) crystallisation by cooling: after montanin wax grain dissolution, stops heating, water-cooled crystallization kettle, and temperature, at-10 ~ 20 DEG C, maintains low temperature crystallization 10 ~ 50min; (3) filtering drying: after crystallization terminates, filter, filter residue is separated with filtrate, and filter residue is in 40 DEG C of decompression dryings in Vacuumdrier, then press formings; (4) filtrate is reclaimed: rectifying is reclaimed, by solvent and resin isolation, and recycle.The solvent that the present invention adopts is hexanaphthene or ethyl acetate, and these two kinds of solvents are all nontoxic, little to human injury, and with or without corrosive nature, and solvent can recycle, to ecotope without harm, and environmental protection.
Description
Technical field
The present invention relates to solvent and method that a kind of method of deviating from resin from montanin wax, particularly a kind of crystallization process remove resin in montanin wax.
Background technology
Montanin wax main ingredient comprises pure wax, pitch and resin, and the composition of the montanin wax that the coal under different forming Environment extracts is different, and general pure wax component accounts for 60 ~ 70%, and resin Composition accounts for 20 ~ 30%, and asphalt component accounts for 5 ~ 20%.The montanin wax extractive technique comparative maturity of current Germany, its montanin wax resin content produced is lower, and generally about 15%, and in the montanin wax that China produces, resin content, up to 25 ~ 30%, does not reach industrial requirements far away.The too high meeting of resin content makes montanin wax be clamminess, affect the cosolvency of montanin wax and paraffin, reduce physicals and the mechanical property of montanin wax, make it be worth to have a greatly reduced quality, the montanin wax price difference that the montanin wax that China produces and Germany produce is at about 10,000 yuan per ton, and other performance index (acid number, saponification value) of the montanin wax that China produces all are better than Germany's product montanin wax, therefore reduce resin content in montanin wax and become a problem demanding prompt solution.
At present about the patent of montanin wax deresination has: the degreasing method (CN103074108A) deviating from method (CN103074109A), a kind of crude montan wax of resin object in a kind of a kind of method of crude montan wax efficient energy-saving deresination method and device (CN103897734A), continuous seepage degreasing montanin wax coproduction resin and device (CN103666561A), the efficient deresining plant of a kind of montanin wax and deresinate method (CN103614161A), montanin wax.The method of comprehensive above discovery montanin wax deresination mainly contains two classes: leaching and multi-stage counter current extraction, and the solvent usually adopted is the mixed solvent of benzene, toluene or ethyl acetate or ethyl acetate and benzene or toluene.
Leaching technology flow process is through pulverizing, after dry, screening, be separated, obtain leaching liquid and solid substance after the montanin wax particle obtained is leached 2 ~ 4h with organic solvent at normal temperatures by certain solid-to-liquid ratio by crude montan wax.Solid substance is placed in tripping device and adds the remaining organic solvent of heat extraction, obtain degreasing montanin wax; Inserted by leaching liquid in separation vessel, obtain organic solvent solution and insolubles through solid-liquid separation, organic solvent solution reclaims organic solvent through rectifying, and insolubles obtains valchovite through evaporation.
Multi-stage counter current extraction technical process be by montanin wax through pulverizing, after dry, screening, the montanin wax particle obtained is sent in multi-stage counter current extraction device and carries out liquid-solid phase extraction, extraction temperature is-20 ~ 40 DEG C, be that extraction agent carries out multi-stage counter current extraction with organic solvent, montanin wax particle is sequentially through organic solvent continuous extraction that resinous concentration reduces, with not resiniferous organic solvent extraction 60 ~ 80min after extraction 120 ~ 180min, extraction progression 3 ~ 8 grades, obtains defatted wax solid substance and resiniferous organic solvent mixed solution after extraction terminates.Heat through extracting in the defatted wax solid substance feeding vaporizer obtained, the a small amount of organic solvent contained in defatted wax solid substance is evaporated in vaporizer, reclaim after the organic solvent condensate of evaporation, defatted wax liquid is obtained after evaporation terminates, defatted wax liquid is delivered on forming machine shaping, obtains defatted wax product.The resiniferous organic solvent mixed solution obtained after extraction being terminated pumps in vaporizer, evaporation removes the organic solvent of in resinous organic solvent mixed solution 70 ~ 80%, reclaim after the organic solvent condensate of evaporation, obtain resin object after evaporation terminates, reclaim after the organic solvent condensate be evaporated.
Leach owned by France in batch operation, less investment; Multi-stage counter current extraction method is continous way operation, though the large efficiency of investment is higher, residence time of material is shorter, is applicable to fairly large degreasing.This two class methods essence is all liquid-solid extraction lock out operation, utilizes at low temperatures that resinous principle solubleness in organic solvent will much larger than the principle deresination of pure wax composition in montanin wax.But these two class methods can only remove the resin of montanin wax particle surface, the resin of particle deep layer by outer solid phase parcel cannot with solvent contacts, can not degreasing, so degreasing efficiency is not high; When utilizing benzene or toluene for solvent, in obtained finished product, can noxious solvent be remained, people's health be worked the mischief, causes stockpiling of unsold product.In addition the extraction dosage needed in multi-stage counter current extraction process is comparatively large, and energy consumption is high; Solvent recovering rate is not high, and has partial solvent in removal process and evaporate, and causes environmental pollution.
Summary of the invention
The solvent that the object of the invention is to provide a kind of crystallization process to remove resin in montanin wax and method, solve existing montanin wax deresination and all adopt solid-liquid extraction, solvent cannot enter granule interior completely, can only carry out extraction to the resin of montanin wax particle surface to remove, the resin of particle deep layer is because being wrapped the problem removing difficulty.
The object of the present invention is achieved like this: the method comprises the step that heating for dissolving, crystallisation by cooling, filtering drying and filtrate are reclaimed; Concrete steps are as follows:
(1) heating for dissolving: montanin wax particle is inserted in crystallization kettle, solvent pump is utilized to inject solvent in crystallization kettle, described solvent is cyclohexane solution or ethyl acetate, the feed liquid mass ratio of montanin wax particle and solution is 1:5 ~ 50, stir, utilize saturation steam to heat crystallization kettle, add heat and control chamber pressure at 1.0 ~ 5.0MPa, until montanin wax particle dissolves completely;
(2) crystallisation by cooling: after montanin wax particle dissolves completely, stop heating, utilize water coolant to cool crystallization kettle, make montanin wax crystallization, temperature in the kettle controls at-10 ~ 20 DEG C, maintains low temperature crystallization 10 ~ 50min;
(3) filtering drying: after crystallization terminates, utilizes vacuum filtration or centrifuging, and filter residue is separated with filtrate, by the filter residue that obtains in 40 DEG C of decompression dryings in Vacuumdrier, then press formings, obtains montanin wax finished product;
(4) filtrate is reclaimed: adopt rectification method to reclaim filtrate, be separated by solvent, to carry out recycle with resin;
Described ethyl acetate or cyclohexane solvent are all neat solvents.
Beneficial effect, owing to have employed such scheme, the method for resin in montanin wax that removes of high-efficiency environment friendly reduces the content of resin in montanin wax.The method be with hexanaphthene or ethyl acetate for solvent, utilize the method for crystallisation by cooling to remove resin in montanin wax; Montanin wax particle is dissolved in a certain amount of solvent at a higher temperature, cools after particle dissolves completely to solution, and along with the reduction of temperature, the changes in solubility of pure wax in these two kinds of solvents is comparatively large, crystallization; And the solubility with temperature change of resin is less, substantially can not crystallization, thus reach the object of separation, obtain the montanin wax that purity is higher.
Adopt the inventive method to remove resin in montanin wax and have following advantage: instant invention overcomes extraction in the past from degreasing effect and extract the drawback that montanin wax resin can only extract surface resin, resin removes more thorough, pure wax yield is higher, according to multistage crystallization operation, the montanin wax of lower resin content can also be obtained; From the operating time, heating for dissolving and crystallisation by cooling required time all short, and under low temperature, liquid-solid extraction speed is less, and the inventive method overall treatment time is compared much shorter; From environmental protection aspect, the solvent that the present invention adopts is hexanaphthene or ethyl acetate, and these two kinds of solvents are all nontoxic, little to human injury, and with or without corrosive nature, and solvent can recycle, to ecotope without harm, and environmental protection.
Accompanying drawing explanation
Fig. 1 is deresination method flow diagram of the present invention.
Embodiment
Below in conjunction with example, the present invention is further illustrated, but limit the invention never in any form, and any change done based on training centre of the present invention or improvement, all belong to improvement threshold of the present invention.
Embodiment 1: a kind of take hexanaphthene as the montanin wax deresination method of solvent, and concrete steps are:
Getting 1 ton of resin content is the montanin wax particle that 28.3% granularity is less than 10mm, montanin wax particle is inserted in jacketed type crystallization kettle, utilize solvent pump to injection ring hexane solvent in crystallization kettle, the solid-liquid ratio of montanin wax particle and cyclohexane solvent is 1:35, stir, heating (steam walks chuck), pressure control 2.0MPa, maintains heating 20min.Cut off water vapor, in crystallization kettle chuck, add water coolant the solution in crystallization kettle is cooled, make solution temperature in crystallization kettle remain on 20 DEG C, crystallisation by cooling 30min.Carry out suction filtration with vacuum pump using circulatory water, filter residue is separated with solution, the filter residue obtained is dried in 40 DEG C of product drying machines, obtains montanin wax finished product.Carry out the mensuration of degreasing rate by GB2561-81, find that the degreasing rate of montanin wax is 32.66% after measured, yield is 59.60%.
Embodiment 2: a kind of take ethyl acetate as the montanin wax deresination method of solvent, and concrete steps are:
Getting 1 ton of resin content is the montanin wax particle that 29.1% granularity is less than 10mm, montanin wax particle is inserted in crystallization kettle, solvent pump is utilized to inject ethyl acetate solvent in crystallization kettle, the solid-liquid ratio of montanin wax particle and ethyl acetate solvent is 1:30, stir, heating, pressure control 3.0MPa, maintains heating 20min.Then with water quench solution, temperature is made to remain on 20 DEG C, crystallisation by cooling 30min.Carry out suction filtration with vacuum pump using circulatory water again, the filter residue obtained is dried in 40 DEG C of product drying machines, obtains montanin wax finished product.Carry out the mensuration of degreasing rate by GB2561-81, find that the degreasing rate of montanin wax is 30.28% after measured, yield is 61.33%.
Claims (1)
1. crystallization process removes a method for resin in montanin wax, it is characterized in that: the method comprises the step that heating for dissolving, crystallisation by cooling, filtering drying and filtrate are reclaimed;
Concrete steps are as follows:
(1) heating for dissolving: montanin wax particle is inserted in crystallization kettle, utilize solvent pump to injection ring hexane or ethyl acetate solvent in crystallization kettle, the feed liquid mass ratio of montanin wax particle and solvent is 1:5 ~ 50, stir, saturation steam is utilized to heat crystallization kettle, add heat and control chamber pressure at 1.0 ~ 5.0MPa, until montanin wax particle dissolves completely;
(2) crystallisation by cooling: after montanin wax particle dissolves completely, stop heating, utilize water coolant to cool crystallization kettle, make montanin wax crystallization, temperature in the kettle controls at-10 ~ 20 DEG C, maintains low temperature crystallization 10 ~ 50min;
(3) filtering drying: after crystallization terminates, utilizes vacuum filtration or centrifuging, and filter residue is separated with filtrate, by the filter residue that obtains in 40 DEG C of decompression dryings in Vacuumdrier, then press formings, obtains montanin wax finished product;
(4) filtrate is reclaimed: adopt rectification method to reclaim filtrate, be separated by solvent, to carry out recycle with resin;
Described ethyl acetate or cyclohexane solvent are all neat solvents.
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Families Citing this family (8)
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CN105349182B (en) * | 2015-12-01 | 2017-12-29 | 中国矿业大学 | The catalysis oxidation reagent system and method for a kind of lignite wax oxidative decoloration |
CN108043324B (en) * | 2017-12-29 | 2020-01-07 | 中国矿业大学 | Method for preparing organic particles from montan wax and peat wax |
CN111154512A (en) * | 2018-11-08 | 2020-05-15 | 国家能源投资集团有限责任公司 | Method for removing resin from lignite crude wax and method for extracting lignite wax from lignite |
CN111154511A (en) * | 2018-11-08 | 2020-05-15 | 国家能源投资集团有限责任公司 | Method and system for extracting montan wax from lignite |
CN111303941B (en) * | 2018-12-12 | 2022-02-18 | 国家能源投资集团有限责任公司 | Method for extracting montan wax from lignite |
CN113403107A (en) * | 2020-03-17 | 2021-09-17 | 国家能源投资集团有限责任公司 | Method for removing resin from coarse lignite wax |
CN113403106A (en) * | 2020-03-17 | 2021-09-17 | 国家能源投资集团有限责任公司 | Method for extracting montan wax |
CN112694913B (en) * | 2020-03-18 | 2022-07-19 | 国家能源投资集团有限责任公司 | Extraction process of montan wax |
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CN101402899A (en) * | 2008-11-17 | 2009-04-08 | 昆明理工大学 | Oxidization fine purification albefaction method for montan wax |
CN101906320A (en) * | 2010-08-04 | 2010-12-08 | 李定忠 | Method for producing high purity montan wax |
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 |
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 |
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Patent Citations (4)
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CN101402899A (en) * | 2008-11-17 | 2009-04-08 | 昆明理工大学 | Oxidization fine purification albefaction method for montan wax |
CN101906320A (en) * | 2010-08-04 | 2010-12-08 | 李定忠 | Method for producing high purity montan wax |
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 |
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