CN101497818B - Mixed solvent and method for extracting montan wax - Google Patents
Mixed solvent and method for extracting montan wax Download PDFInfo
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- CN101497818B CN101497818B CN 200910094132 CN200910094132A CN101497818B CN 101497818 B CN101497818 B CN 101497818B CN 200910094132 CN200910094132 CN 200910094132 CN 200910094132 A CN200910094132 A CN 200910094132A CN 101497818 B CN101497818 B CN 101497818B
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Abstract
The invention provides mixed solvent extracting lignite wax and an extraction method, wherein the mixed solvent comprises the following raw materials: 10-70 mass percent of octanol, 10-70 mass percent of methylbenzene and 10-70 mass percent of alcohols. Lignite is pelletized and then is extracted by the mixed solvent, and the lignite wax is obtained by dehydration, concentration, evaporation and dryness. The lignite wax is extracted in the innoxious environment, and the extracted solvent can be recovered, thereby the mixed solvent is safe and reliable, the extraction cost is low, the process condition during the whole extraction process is more common, the process is simple, the operation is convenient, the comprehensive processing cost is low, the processing ability is strong, and the product yield is higher; in addition, the extraction method can not produce emulsion phenomenon during the whole extraction process, and is an effective, low-cost, massive and innoxious extraction process.
Description
Technical field
The present invention relates to a kind of extracting method of montanin wax, especially use the mixed solvent containing octanol, extract the method for montanin wax from brown coal, belong to technical field of plant extraction.
Background technology
Brown coal are cured is the natural hard wax extracted from brown coal with organic solvent, and it has a wide range of applications in a lot of fields, is a kind of comparatively rare industrial chemicals.The montanin wax of producing is both at home and abroad at present mostly used benzene to make to extract solvent; because the toxicity of benzene is larger; not only be harmful to HUMAN HEALTH; serious environment pollution; and in the montanin wax leaching process; easily emulsification occurring and affects product yield and quality product; expensive production process has also limited outlet and the application of montanin wax simultaneously; therefore; urgently seek low toxicity or innoxious solvent and replace benzene to produce montanin wax, to reduce or decontamination, protection of the environment and operator's is healthy; reduce costs, further enlarge the application of montanin wax.
Summary of the invention
For overcoming that the toxicity that prior art faces with the benzene extraction montanin wax is large, cost is high and easily producing the difficult problem such as emulsification, the present invention aims to provide a kind of mixed solvent that extracts montanin wax.
Another object of the present invention is to provide a kind of method of extracting montanin wax with mixed solvent.
Technical scheme of the present invention is as follows:
A kind of mixed solvent that extracts montanin wax is characterized in that it is comprised of the raw material of following mass percent:
Octanol 10～70%
Described alcohols is one or more in methyl alcohol, ethanol, Virahol or the trimethyl carbinol.
Described octanol, toluene, alcohols are technical grade product.
A kind of method of extracting montanin wax is characterized in that through the following step:
A, brown coal powder is broken to granularity≤0.2mm, makes the particle that particle diameter is 2～10mm, dry to water content be 8～30% (weight ratios);
B, the brown coal particle that is 8～30% by water content: the mass ratio of mixed solvent=1: 1～3, mixed solvent is sprayed on the brown coal particulate material of steps A gained, under 20～100 ℃ of temperature condition, extract 1～8 hour, obtain extracting solution and cinder, wherein, described mixed solvent is comprised of the raw material of following mass percent:
Octanol 10～70%
C, B step gained extracting solution is dewatered and is less than 5% (weight ratio) to water content after, go out liquid wax and solvent, solvent recuperation through concentrating and separating;
D, the liquid wax of C step is further concentrated after, at 80～100 ℃ of temperature, evaporate, after separating residual solvent, at 100～120 ℃ of temperature, dry to constant weight, obtain montanin wax, isolated solvent recuperation after cooling;
E, the cinder of B step is given over to another use, isolated solvent recuperation through evaporation after precipitation.
The fragmentation of described A step and granulation all complete with conventional crusher and the nodulizer of prior art.
The extraction of described B step is to complete in extraction plant in the prior art, in the patent No., is specifically ZL2003101040690, and name is called and completes in the cylindrical extractor in the patent of invention of " a kind of method that extracts fat-soluble pigment ".
Described extraction completes like this: by mixed solvent after the material top spray is on material, from material bottom diacolation out, afterwards by diacolation solution out from the material top spray on the next stage material, after having sprayed so step by step, obtain extracting solution and cinder.
The dehydration of described C, D step, concentrated, evaporation, oven dry, solvent recuperation all complete with conventional equipment of the prior art.
The present invention compared with prior art has following advantages and effect: adopt such scheme, adopt the mixed solvent containing octanol to extract montanin wax, carry out the extraction of montanin wax fully under nontoxic envrionment conditions, and the solvent after extracting is recyclable to be used again, safety not only, reliably, and extraction cost is low, the processing condition of whole leaching process are comparatively common in addition, its technique is simple, easy to operate, the comprehensive process cost is low, working ability is strong, the product yield is higher, in another leaching process emulsion can not occur, make quality product higher, it is a kind of effective low cost, on a large scale, nontoxic, mixed solvent and processing method for harmless extraction.
The accompanying drawing explanation
Fig. 1 is cylindrical extractor external structure;
Fig. 2 is cylindrical extractor deployed configuration schematic diagram;
The sectional drawing that Fig. 3 is Fig. 1;
Fig. 4 puts material bed material lattice structure figure in cylindrical extractor.
In figure, 1 is the extractor tank body, the 2 brown coal opening for feeds that are tank body top, the 3 mixed solvent entrances that are tank body top, 4 slag notches that are tank body lower part, the 5 extracting solution spouts that are tank body lower part, 6 is rotating material barrel in tank body, the interior separate material lattice of many lattice that arrange of material barrel 6, wherein, A
1～A
12lattice are the diacolation extraction section, A
13～A
16lattice are the solvent section of draining, A
17～A
18lattice are for slagging tap and the space section, be provided with spacer screen 16 in the bottom of each lattice, so that leach extracting solution, 7 is supporting baffle, for supporting the spacer screen 16 of each material lattice bottom, 8 for being arranged on the transmission chain on material barrel 6 outer wall sprocket wheels 15, by power wheel 9, with motor 10, be connected, in order to pass through power wheel 9 under motor 10 drives, transmission chain 8, sprocket wheel 15 rotates material barrel 6, 11 for being located at the mixed solvent shower nozzle on material barrel 6 tops, described shower nozzle is by tubing 12, pump 13 is connected with the liquid outlet 14 of material barrel 6 bottoms, in order to the material extracting solution oozed out is sprayed in another material lattice, 17 for being located at the liquid bucket of material barrel bottom.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Get industrial raw material by following formula: octanol 50 grams, toluene 10 grams, methyl alcohol 40 grams, obtain mixed solvent after mixing.
Get industrial raw material by following formula: octanol 30 grams, toluene 40 grams, ethanol 30 grams, obtain mixed solvent after mixing.
Get industrial raw material by following formula: octanol 10 grams, toluene 20 grams, Virahol 70 grams, obtain mixed solvent after mixing.
Get industrial raw material by following formula: octanol 70 grams, toluene 10 grams, the trimethyl carbinol 20 grams, obtain mixed solvent after mixing.
Get industrial raw material by following formula: octanol 20 grams, toluene 60 grams, the trimethyl carbinol 20 grams, obtain mixed solvent after mixing.
With the particulate of conventional crusher brown coal powder is broken into≤0.2mm of the prior art, then become the particle of 5mm with conventional granulator granulation of the prior art, drying moisture content to water content is 20% (weight ratio), get this brown coal particle 50kg, put into the material barrel 6 of the common cylindrical shaped extractor of prior art shown in the drawings, the mixed solvent 110kg of embodiment 1 is sprayed on the brown coal granule materials, specifically: starter motor, make the speed rotation of material barrel 6 to circle in 120 minutes, material pack into the material lattice 6 of extractor charge section interior after, mixed solvent is sprayed on the material of material lattice (i.e. the first lattice) wherein through shower nozzle 11 with intermittent mode, when mixed solvent flows through this investigate things bed of material after spacer screen 16 oozes out and enters liquid bucket 17, the transudate extracted in liquid bucket 17 with pump 13 sprays to the material of the second lattice through shower nozzle 11, the transudate extracted in the second lattice bottom liquid bucket with pump 13 more afterwards, through shower nozzle 11, spray to the material of the 3rd lattice, after having sprayed so step by step, obtain brown coal extracting solution and cinder, extraction time is 4h, extracting temperature is 80 ℃, the conventional separator that extracting solution is placed in to prior art is dewatered, and after isolating moisture content, extracting solution is put into to the conventional vacuum concentrator of prior art, obtains 25L liquid wax, isolated solvent recuperation after vacuum concentration, liquid wax is proceeded in the conventional vaporizer in existing existing art, and after evaporating remaining solvent, liquid wax proceeds in Stainless steel basin, dries to constant weight in 120 ℃, after cooling montanin wax 2.84kg, productive rate 5.68%, isolated solvent recuperation, cinder is put into to the routine of prior art and blown slag ladle, give over to another use after precipitation, solvent recuperation, recovered solvent is sent basin back to after the condensation process of prior art, test by analysis and the allotment ratio after reuse again.
Get the brown coal particle 50kg identical with embodiment 6, put into the material barrel 6 of the common cylindrical shaped extractor of prior art shown in the drawings, the mixed solvent 150kg of embodiment 2 is sprayed on the brown coal granule materials, after adopting the spray step by step identical with embodiment 6 to extract, obtain brown coal extracting solution and cinder, by controlling velocity of rotation and the solvent temperature of material barrel 6, making extraction time is 2h, and extracting temperature is 100 ℃; Extracting solution is put in separator and dewatered, after isolating moisture content, extracting solution is sent in vacuum concentrator and concentrates to obtain 26L liquid wax, isolated solvent recuperation; After liquid wax is proceeded in vaporizer to the evaporation residual solvent, liquid wax proceeds in Stainless steel basin, dries to constant weight in 100 ℃, after cooling montanin wax 3.02kg, productive rate 6.04%, isolated solvent recuperation; Cinder is put into to the routine of prior art and blown slag ladle, give over to another use after precipitation, isolated solvent recuperation; Recovered solvent is sent the tank of harvesting and storing back to after the condensation process of prior art, test by analysis and the allotment ratio after reuse again.
Get the brown coal particle 50kg identical with embodiment 1, put into the material barrel 6 of the common cylindrical shaped extractor of prior art shown in the drawings, the mixed solvent 60kg of embodiment 5 is sprayed on the brown coal granule materials continuously, after adopting the spray step by step identical with embodiment 6 to extract, obtain brown coal extracting solution and cinder, by controlling velocity of rotation and the solvent temperature of material barrel 6, making extraction time is 8h, extracts 20 ℃ of temperature; Extracting solution is put in separator and dewatered, after isolating moisture content, after extracting solution is concentrated, obtain the 24L liquid wax, isolated solvent recuperation; After liquid wax is proceeded in vaporizer to the evaporation residual solvent, then proceed in Stainless steel basin, dry to constant weight in 110 ℃, after cooling montanin wax 2.91kg, productive rate 5.82%, isolated solvent recuperation; Cinder is put into to the routine of prior art and blown slag ladle, give over to another use after precipitation, isolated solvent recuperation; Recovered solvent is sent the tank of harvesting and storing back to after the condensation process of prior art, test by analysis and the allotment ratio after reuse again.
Claims (3)
1. a method of extracting montanin wax is characterized in that through the following step:
A, brown coal powder is broken to granularity≤0.2mm, makes the particle that particle diameter is 2～10mm, dry to water content be 8～30% (weight);
B, the brown coal particle that is 8～30% by water content: the mass ratio of mixed solvent=1: 1～3, mixed solvent is sprayed on steps A gained brown coal particulate material, under 20～100 ℃ of temperature condition, extract 1～8 hour, obtain extracting solution and cinder, wherein mixed solvent is comprised of the raw material of following mass percent:
Alcohols is one or more in methyl alcohol, ethanol, Virahol or the trimethyl carbinol;
C, B step gained extracting solution is dewatered and is less than 5% (weight) to water content after, concentrating and separating goes out liquid wax and solvent, reclaims solvent;
D, the liquid wax of C step is further concentrated after, at 80～100 ℃ of temperature, evaporate, after separating residual solvent, at 100～120 ℃ of temperature, dry to constant weight, obtain montanin wax, isolated solvent recuperation after cooling;
E, the cinder of B step is given over to another use, isolated solvent recuperation through evaporation after precipitation.
2. the method for extraction montanin wax according to claim 1, the extraction that it is characterized in that described B step completes like this: by mixed solvent after the material top spray is on material, from material bottom diacolation out, afterwards by diacolation solution out from the material top spray on the next stage material, after having sprayed so step by step, obtain extracting solution and cinder.
3. the method for extraction montanin wax according to claim 1, is characterized in that fragmentation, the granulation of described A step, the extraction of B step, and the dehydration of C, D step, concentrated, evaporation, oven dry, solvent recuperation all complete with conventional equipment of the prior art.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910094132 CN101497818B (en) | 2009-02-26 | 2009-02-26 | Mixed solvent and method for extracting montan wax |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910094132 CN101497818B (en) | 2009-02-26 | 2009-02-26 | Mixed solvent and method for extracting montan wax |
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| CN101497818A CN101497818A (en) | 2009-08-05 |
| CN101497818B true CN101497818B (en) | 2013-06-19 |
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| CN 200910094132 Expired - Fee Related CN101497818B (en) | 2009-02-26 | 2009-02-26 | Mixed solvent and method for extracting montan wax |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101906320B (en) * | 2010-08-04 | 2013-06-19 | 李定忠 | Method for producing high purity montan wax |
| CN102899089B (en) * | 2012-09-11 | 2014-08-20 | 国电燃料有限公司 | Production process for soft montan wax |
| CN103146446B (en) * | 2013-04-01 | 2014-10-01 | 贵州纳斯新能源技术有限公司 | High-efficiency energy-saving natural gas additive and application thereof |
| CN103881752B (en) * | 2014-04-12 | 2015-08-19 | 曲靖众一精细化工股份有限公司 | A kind of leaching method of high-quality montanin wax and device |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1056334A (en) * | 1990-05-10 | 1991-11-20 | 马拉索恩石油公司 | Recover the method for permeability of subterranean formation |
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2009
- 2009-02-26 CN CN 200910094132 patent/CN101497818B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1056334A (en) * | 1990-05-10 | 1991-11-20 | 马拉索恩石油公司 | Recover the method for permeability of subterranean formation |
Non-Patent Citations (1)
| Title |
|---|
| 叶显彬等.褐煤蜡生产工艺.《褐煤蜡化学及应用》.煤炭工业出版社,1983,参见第23页表2-1、第25页表2-2及第23页第26-30行、第33页第23行-第35页第1行. * |
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