CN104312627A - Solvent and method for removing resin from lignite wax by virtue of crystallization process - Google Patents

Abstract

The invention discloses a solvent and method for removing resin from lignite wax by virtue of a crystallization process, belonging to methods for removing resin from lignite wax. The method comprises the following steps: (1) heating and dissolving, namely putting lignite wax particles into a crystallization kettle, injecting a cyclohexane solvent or an acetic ester solvent according to a material-liquid mass ratio of 1:(5-50), stirring, heating the crystallization kettle by using steam, and controlling the pressure of the container to be 1.0-5.0 MPa until the lignite wax particles are dissolved; (2) cooling and crystallizing, namely after the lignite wax particles are dissolved, stopping heating, performing water cooling on the crystallization kettle until the temperature is between -10 and 20 DEG C, and keeping the low temperature for crystallization for 10-50 minutes; (3) filtering and drying, namely after crystallization, filtering to separate filter residues and filtrate, performing reduced pressure drying on the filter residues at 40 DEG C in a vacuum drying machine, and then performing press forming; and (4) recovering the filtrate, namely recovering by virtue of rectification, and separating the solvent and resin for recycling. The solvent adopted in the method disclosed by the invention is cyclohexane or acetic ester, and the two solvents are nontoxic, cause small harm to human bodies, are not corrosive, can be recycled, are harmless to the ecological environment and are environment-friendly.

Description

A kind of crystallization process removes solvent and the method for resin in montanin wax

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 (CN 103074108A) deviating from method (CN 103074109A), 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 (CN 103897734A), continuous seepage degreasing montanin wax coproduction resin and device (CN 103666561A), the efficient deresining plant of a kind of montanin wax and deresinate method (CN 103614161A), 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 solvent and a method for resin in montanin wax, it is characterized in that: 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.