CN101407732A

CN101407732A - Solvent and method for extracting montan wax

Info

Publication number: CN101407732A
Application number: CNA200810233651XA
Authority: CN
Inventors: 李定忠
Original assignee: Individual
Current assignee: Individual
Priority date: 2008-11-28
Filing date: 2008-11-28
Publication date: 2009-04-15

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

A kind of solvent of extracting montan wax and method

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%;

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%;

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%;

Claims

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:

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.