CN101407732A - Solvent and method for extracting montan wax - Google Patents
Solvent and method for extracting montan wax Download PDFInfo
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- CN101407732A CN101407732A CNA200810233651XA CN200810233651A CN101407732A CN 101407732 A CN101407732 A CN 101407732A CN A200810233651X A CNA200810233651X A CN A200810233651XA CN 200810233651 A CN200810233651 A CN 200810233651A CN 101407732 A CN101407732 A CN 101407732A
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- montan wax
- extraction
- extracting
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- 239000002904 solvent Substances 0.000 title claims abstract description 67
- 239000012170 montan wax Substances 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000000605 extraction Methods 0.000 claims abstract description 32
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000001993 wax Substances 0.000 claims description 27
- MKYLOMHWHWEFCT-UHFFFAOYSA-N Manthidine Natural products C1C2=CC=3OCOC=3C=C2C2C3=CC(OC)C(O)CC3N1C2 MKYLOMHWHWEFCT-UHFFFAOYSA-N 0.000 claims description 17
- 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 claims description 17
- 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 claims description 17
- 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 claims description 17
- 239000003077 lignite Substances 0.000 claims description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 239000000706 filtrate Substances 0.000 claims description 12
- 239000003245 coal Substances 0.000 claims description 10
- 238000005267 amalgamation Methods 0.000 claims description 6
- 239000002817 coal dust Substances 0.000 claims description 6
- 239000006210 lotion Substances 0.000 claims description 6
- 238000010025 steaming Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 5
- 230000008719 thickening Effects 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000011084 recovery Methods 0.000 claims description 2
- 230000007704 transition Effects 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 abstract description 27
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000036541 health Effects 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 8
- 230000008901 benefit Effects 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 239000000284 extract Substances 0.000 description 4
- 239000012046 mixed solvent Substances 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 2
- 230000001476 alcoholic effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000012184 mineral wax Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Landscapes
- Extraction Or Liquid Replacement (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention provides a solvent and a method for extracting montan wax, which is characterized in that: the solvent is prepared by 1, 2-dichloroethane and alcohol according to the volume ratio of 3:7 to 10:0; grinding, extracting, filtering, concentrating and drying are carried out to obtain the brown montan wax. Under same production conditions, the solvent and the method increase the yield of the montan wax by 2 to 3 percentage and reduce the cost of the solvent by 10 to 20 percent compared with the benzene extraction method. Moreover, with high quality, the extracted montan wax has lighter brown color. The extracting solvent used by the invention causes no pollution to the environment and does not harm the human health. Changing the solvent into the nontoxic and harmless one provided by the invention and not changing the existing production equipment or technological conditions, the solvent and the method can save energy and reduce consumption, improve the quality of the products and bring no pollution to the environment.
Description
Technical field
The present invention relates to solvent and method that a kind of extracting montan wax is used, belong to mineral extractive technique field.
Background technology
Montanin wax is a kind of high-melting-point hard wax that extracts from brown coal with organic solvent, has a wide range of applications in fields such as chemical industry, light industry, automobile, daily use chemicals, and be a kind of irreplaceable mineral wax of animals and plants wax of natural origin.
Montanin wax of the prior art, be that main solvent extracts in order to benzene mostly, because benzene has very strong toxicity, in leaching process, not only pollute the environment, even can damage the healthy of people, therefore benzene use and outlet is subjected to strict restriction, add that the price of benzene constantly soars in recent years, cause the production cost of montanin wax high.Therefore, all seeking the solvent that replaces benzene both at home and abroad,, reducing the production cost that montanin wax extracts simultaneously in the hope of reducing collection to the pollution of environment and the threat that human health is constituted.
Summary of the invention
For reducing collection to the pollution of environment and the threat that human health is constituted, reduce the production cost that montanin wax extracts simultaneously, the invention provides the solvent that a kind of extracting montan wax is used.
Another object of the present invention is to provide the described solvent of a kind of usefulness to replace the method for benzene extracting montan wax.
The present invention finishes by following technical proposal: a kind of solvent of extracting montan wax is characterized in that described solvent is formed by the preparation of raw material of following volume ratio:
1,2-ethylene dichloride: alcohol=3: 7～10: 0.
Described alcohol is one or more in methyl alcohol, ethanol, propyl carbinol or the trimethyl carbinol, and is technical grade.
Described 1, the 2-ethylene dichloride is a technical grade.
Second purpose of the present invention finished by following technical proposal: a kind of method of extracting montan wax is characterized in that through the following step:
A, be 10～50% (weight) with brown coal drying to water content, be crushed to granularity≤2mm, cross 60 mesh sieves, sieve removes coal dust, granularity is that the coal grain of 0.2～2mm is standby;
B, in steps A gained coal grain, press the coal grain: the mass/volume ratio of solvent=1: 1～1: 3 adds the solvent of technical grade concentration, extraction 30min～5h, wherein, extraction solvent adopts the solvent of following volume ratio: 1, and the 2-ethylene dichloride: alcohol=3: 7～10: 0 gets extraction liquid, get filtrate and filter residue after the filtration, filter residue with an amount of and extraction phase with solvent wash after, with washing lotion and filtrate merging, abandon filter residue;
C, step B gained amalgamation liquid is concentrated into solvent-free steaming, reclaim solvent after, with the wax liquid injection dish of remainder, under 100～130 ℃ of temperature oven dry to removing moisture content and solvent, be cooled to room temperature afterwards after, brown coal wax;
After adding an amount of neat solvent allotment in D, the solvent after recovery, recirculation is used for the extraction of montanin wax.
The mass/volume of described B step is than being kg/L, perhaps g/ml.
The extraction of described B step is the conventional extraction processes of prior art, and extraction equipment also is the conventional equipment of prior art.
The conventional filtration method that is filtered into prior art of described B step, transition also are the conventional equipment of prior art.
The conventional concentration method of the simmer down to prior art of described C step, thickening equipment also are the conventional thickening equipment of prior art.
The present invention compared with prior art has following advantage and effect, after adopting such scheme: can be under same working condition, make the montanin wax productive rate than the raising of benzene formulation 2～3 percentage points, and the solvent for use cost than the reduction of benzene formulation 10～20%, and extraction gained montanin wax color is more shallow, be brown, quality is good, the extraction solvent that the present invention uses is free from environmental pollution, does not damage the healthy of people, and technology of the present invention desolventizes uses instead outside the nontoxic solvent that the invention provides, need not to change existing production unit and processing condition, can realize saving energy and reduce the cost, improve the quality of products, purpose free from environmental pollution.
Embodiment
Embodiment 1
A, be 12% with brown coal drying to water content, be crushed to granularity≤2mm, cross 60 mesh sieves, sieve removes coal dust, granularity is that the coal grain of 0.2～2mm is standby;
B, be the above-mentioned dry brown coal 500g of 0.2～2mm with granularity, place the 3000ml round-bottomed flask, add 1000ml mixed solvent (brown coal are 1/2 with the mass/volume ratio of solvent), wherein 1,2-ethylene dichloride 900ml, concentration is 95% ethanol 100ml (promptly 1,2-ethylene dichloride and concentration are that 95% alcoholic acid volume ratio is 9: 1), reflux extraction 2h takes advantage of heat filtering in water-bath, gets filter residue and filtrate; Other get be preheating to 70 ℃ with extraction phase with mixed solvent 250ml (promptly 1,2-ethylene dichloride and concentration are that 95% alcoholic acid volume ratio is 9: 1) washing and filtering after filter residue once, with washing lotion and filtrate merging;
C, with the extraction of B step, the underpressure distillation of washing amalgamation liquid to solvent-free steaming, reclaim solvent, the wax liquid of remainder is put into Stainless Steel Disc, oven dry is to removing moisture content and solvent (about 2h) under 110 ℃ of temperature, be cooled to room temperature afterwards, get montanin wax 26.5g, productive rate 5.3%;
D, the solvent after will reclaiming are tested composition wherein by analysis, and after adding an amount of neat solvent allotment therein and reaching requirement, recirculation is used for the extraction of montanin wax.
Embodiment 2
A, be 30% with brown coal drying to water content, be crushed to granularity≤2mm, cross 60 mesh sieves, sieve removes coal dust, granularity is that the coal grain of 0.2～2mm is standby;
B, be that the above-mentioned brown coal 450g of 0.2～2mm places the 3000ml round-bottomed flask with granularity, add 1125ml mixed solvent (brown coal are 1/2.5 with the mass/volume ratio of solvent), wherein 1,2-ethylene dichloride 675ml, concentration is 95% methyl alcohol 450ml (promptly 1,2-ethylene dichloride and concentration are that the volume ratio of 95% methyl alcohol is 6: 4), reflux extraction 0.5h in the water-bath takes advantage of heat filtering to get filtrate and filter residue; Other gets the same mixture solvent 230ml that is preheated to 70 ℃ (promptly 1,2-ethylene dichloride and concentration are that the volume ratio of 95% methyl alcohol is 6: 4) washing filter residue once, with washing lotion and filtrate merging;
C, with the extraction of B step, the underpressure distillation of washing amalgamation liquid to solvent-free steaming, reclaim solvent, the wax liquid of remainder is put into Stainless Steel Disc, oven dry is to removing moisture content and solvent (about 2h) under 120 ℃ of temperature, be cooled to room temperature afterwards, get montanin wax 28.1g, productive rate 6.2%;
D, the solvent after will reclaiming are tested composition wherein by analysis, and after adding an amount of neat solvent allotment therein and reaching requirement, recirculation is used for the extraction of montanin wax.
Embodiment 3
A, be 50% with brown coal drying to water content, be crushed to granularity≤2mm, cross 60 mesh sieves, sieve removes coal dust, granularity is that the coal grain of 0.2～2mm is standby;
B, be the above-mentioned brown coal 520g of 0.2～2mm with granularity, place the 3000ml round-bottomed flask, add 520ml mixed solvent (brown coal are 1/1 with the mass/volume ratio of solvent), wherein 1,2-ethylene dichloride 156ml, concentration is 95% trimethyl carbinol 364ml (promptly 1,2-ethylene dichloride and concentration are that the volume ratio of 95% the trimethyl carbinol is 3: 7), reflux extraction 5h in the water-bath takes advantage of heat filtering to get filtrate and filter residue; Other gets the same mixture solvent 200ml that is preheated to 70 ℃ (promptly 1,2-ethylene dichloride and concentration are that the volume ratio of 95% the trimethyl carbinol is 3: 7) washing filter residue once, with washing lotion and filtrate merging;
C, with the extraction of B step, the underpressure distillation of washing amalgamation liquid to solvent-free steaming, reclaim solvent, the wax liquid of remainder is put into Stainless Steel Disc, behind the evaporating solvent,, be cooled to room temperature in oven dry (about 3h) after remove moisture content and solvent under 100 ℃ of temperature, get montanin wax 26.6g, productive rate 5.1%;
D, the solvent after will reclaiming are tested composition wherein by analysis, and after adding an amount of neat solvent allotment therein and reaching requirement, recirculation is used for the extraction of montanin wax.
Embodiment 4
A, be 10% with brown coal drying to water content, be crushed to granularity≤2mm, cross 60 mesh sieves, sieve removes coal dust, granularity is that the coal grain of 0.2～2mm is standby;
B, be the above-mentioned brown coal 600g of 0.2～2mm, place the 3000ml round-bottomed flask, add 1 granularity, 2-ethylene dichloride solvent 1800ml (brown coal are 1/3 with the mass/volume ratio of solvent), reflux extraction 1h in the water-bath takes advantage of heat filtering to get filtrate and filter residue; Other get be preheated to 70 ℃ 1,2-ethylene dichloride solvent 500ml washing filter residue once, with washing lotion and filtrate merging;
C, with the extraction of B step, the underpressure distillation of washing amalgamation liquid to solvent-free steaming, reclaim solvent, the wax liquid of remainder is put into Stainless Steel Disc, behind the evaporating solvent,, be cooled to room temperature in oven dry (about 3h) after remove moisture content and solvent under 130 ℃ of temperature, get montanin wax 39.6g, productive rate 6.6%;
D, the solvent after will reclaiming are tested composition wherein by analysis, and after adding an amount of neat solvent allotment therein and reaching requirement, recirculation is used for the extraction of montanin wax.
Claims (8)
1, a kind of solvent of extracting montan wax is characterized in that described solvent is formed by the preparation of raw material of following volume ratio:
1,2-ethylene dichloride: alcohol=3: 7～10: 0.
2, the solvent of extracting montan wax according to claim 1 is characterized in that described alcohol is one or more in methyl alcohol, ethanol, propyl carbinol or the trimethyl carbinol, and is technical grade.
3, the solvent of extracting montan wax according to claim 1 is characterized in that describedly 1, and the 2-ethylene dichloride is a technical grade.
4, a kind of method of extracting montan wax is characterized in that through the following step:
A, be 10～50% (weight) with brown coal drying to water content, be crushed to granularity≤2mm, cross 60 mesh sieves, sieve removes coal dust, granularity is that the coal grain of 0.2～2mm is standby;
B, in steps A gained coal grain, press the coal grain: the mass/volume ratio of solvent=1: 1～1: 3 adds the solvent of technical grade concentration, extraction 30min～5h, wherein, extraction solvent adopts the solvent of following volume ratio: 1, and the 2-ethylene dichloride: alcohol=3: 7～10: 0 gets extraction liquid, get filtrate and filter residue after the filtration, filter residue with an amount of and extraction phase with solvent wash after, with washing lotion and filtrate merging, abandon filter residue;
C, step B gained amalgamation liquid is concentrated into solvent-free steaming, reclaim solvent after, with the wax liquid injection dish of remainder, under 100～130 ℃ of temperature oven dry to removing moisture content and solvent, be cooled to room temperature afterwards after, brown coal wax;
After adding an amount of neat solvent allotment in D, the solvent after recovery, recirculation is used for the extraction of montanin wax.
5, the method for extracting montan wax according to claim 4, the mass/volume that it is characterized in that described B step is than being kg/L, perhaps g/ml.
6, the method for extracting montan wax according to claim 4, the extraction that it is characterized in that described B step is the conventional extraction processes of prior art, extraction equipment also is the conventional equipment of prior art.
7, the method for extracting montan wax according to claim 4 is characterized in that the conventional filtration method that is filtered into prior art of described B step, and transition also is the conventional equipment of prior art.
8, the method for extracting montan wax according to claim 4 is characterized in that the conventional concentration method of the simmer down to prior art of described C step, and thickening equipment also is the conventional thickening equipment of prior art.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810233651XA CN101407732A (en) | 2008-11-28 | 2008-11-28 | Solvent and method for extracting montan wax |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810233651XA CN101407732A (en) | 2008-11-28 | 2008-11-28 | Solvent and method for extracting montan wax |
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| Publication Number | Publication Date |
|---|---|
| CN101407732A true CN101407732A (en) | 2009-04-15 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA200810233651XA Pending CN101407732A (en) | 2008-11-28 | 2008-11-28 | Solvent and method for extracting montan wax |
Country Status (1)
| Country | Link |
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| CN (1) | CN101407732A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101906320A (en) * | 2010-08-04 | 2010-12-08 | 李定忠 | Method for producing high purity montan wax |
| CN102851076A (en) * | 2012-04-25 | 2013-01-02 | 曲靖众一精细化工股份有限公司 | Method for efficiently extracting fossilized plant wax from brown coal and device thereof |
| CN103881752A (en) * | 2014-04-12 | 2014-06-25 | 曲靖众一精细化工股份有限公司 | Method and device for leaching high-quality lignite wax |
-
2008
- 2008-11-28 CN CNA200810233651XA patent/CN101407732A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101906320A (en) * | 2010-08-04 | 2010-12-08 | 李定忠 | Method for producing high purity montan wax |
| CN101906320B (en) * | 2010-08-04 | 2013-06-19 | 李定忠 | Method for producing high purity montan wax |
| CN102851076A (en) * | 2012-04-25 | 2013-01-02 | 曲靖众一精细化工股份有限公司 | Method for efficiently extracting fossilized plant wax from brown coal and device thereof |
| CN102851076B (en) * | 2012-04-25 | 2014-08-20 | 曲靖众一精细化工股份有限公司 | Method for efficiently extracting fossilized plant wax from brown coal and device thereof |
| CN103881752A (en) * | 2014-04-12 | 2014-06-25 | 曲靖众一精细化工股份有限公司 | Method and device for leaching high-quality lignite wax |
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Open date: 20090415 |