CN101314716A - Dehydration and alcohol depolymerization process for low-disintegration coal in mild condition - Google Patents
Dehydration and alcohol depolymerization process for low-disintegration coal in mild condition Download PDFInfo
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Abstract
A dehydration and alcohol depolymerization process for low-rank coal under mild condition comprises the following steps: mixing acetone and butanone at equal volume ratio to obtain an organic dehydration solvent, adding brown coal powder in a reaction kettle to obtain dehydrated brown coal powder and organic dehydration mixture solution, and separating the organic dehydration solvent for recycling; adding the dehydrated brown coal powder and methanol into a reaction kettle to obtain residual coal and alcoholysis products, and press-filtering the alcoholysis products to an extractor through a filter plate under stirring and the pressure in the kettle; adding the alcoholysis products into the extractor, spraying eluant into the extractor to obtain a soluble material, adding the soluble material into a distilling still to obtain fine organic components rich in low-carbon hydrocarbon, low-carbon alkoxyl organic materials, phenols, esters, heavy organic components, etc.; and recrystallizing the methanol solvent by heating and cooling to obtain pure organic chemicals with high value added such as alkyl naphthalene, alkyl anthracene and chemical containing polyatomic rings with N and S heteroatoms.
Description
Technical field
The present invention relates to a kind of brown coal or lower-grade metamorphic bituminous dehydration and the method for pure depolymerization, low-disintegration coal dehydration and alcohol depolymerization process under particularly a kind of mild conditions.
Background technology
Brown coal are typical low-rank coal, the macromolecular structure of oxygen enrichment in having kept the coal-forming plant to a greater extent.Organic oxygen part in the brown coal exists with the substituent form of aromatic ring, and part connects two or more aromatic rings as bridged bond and constitutes macromolecular system.Intensive hydrogen bond action between organic oxygen and water molecules in the brown coal micropore, therefore dehydration difficulty from brown coal also is to cause the low and high important factor of moisture of brown coal calorific value.
China's lignite resource is abundant, and reserves account for 77% of national brown coal reserves.Because most of brown coal exist in the problems, particularly transportation such as high ash content, high-moisture, low heat value, low ash smelting point, poor heat stability and easy-weathering spontaneous combustion and take a large amount of transport power and consume a large amount of transportation energy, thereby are regarded as inferior fuel.
At present, the organic oxygen in water in the brown coal and the coal is by hydrogen bonded, and a kind of drying means of physical evaporation dewaters to brown coal, and the power consumption when this method is dewatered to brown coal is big, and the brown coal after the dehydration are difficult to preserve; A kind of hydrothermal treatment consists method: this method is that the temperature of rising hydrothermal treatment consists is to increase dehydration rate, more organic matter becomes the waste water leachable in the brown coal but also make, so the high-temperature water heat treating process is not realized the high value added utilization of brown coal when paying the greater energy consumption cost; A kind of brown coal solvent extraction dehydration treatment method is with 2, and the 2-Propanal dimethyl acetal carries out processed as solvent to brown coal, and preliminary fundamental research shows, uses boiling point and all higher solvent of price to be difficult to recycle; " HyperCoal " is one of clean coal technology of developing energetically in recent years in the world, but often has problems such as stopping up filter plate in the heat filtering process.
In sum, traditional method energy consumption height, the dehydration rate of brown coal dehydration are low; Conventional coal trans-utilization generally be high temperature, high pressure or and catalyzer in the presence of carry out, require the quality of coal higher, related hydrogenation and cracked energy consumption and hydrogen consumption are bigger, the material of reactor are required harsh, added value is low.
Summary of the invention
The objective of the invention is to provide low-disintegration coal dehydration and alcohol depolymerization process under the mild conditions of the little and product high added value of a kind of gentleness, technological process cleaning, energy consumption material consumption of operational condition.
The object of the present invention is achieved like this: technological process is as follows:
The condition of the processed of brown coal powder: select the acetone of equal-volume ratio and butanone to mix as organic dehydrated solvent, 100 orders-200 purpose brown coal powder and organic dehydrated solvent are put into to the reactor that screen plate is arranged, the weight ratio of organic dehydrated solvent and brown coal powder is controlled to be 2: 1-5: 1, controlled temperature is at 50 ℃-90 ℃, fully stirred and be incubated 2 hours-5 hours, use pneumatic pump in reactor, to pressurize, and control pressure is not more than 0.5MPa, the brown coal powder that obtains dewatering and organic dehydration mixing solutions, organic dehydration mixing solutions is put into still kettle, temperature is controlled at 100 ℃-130 ℃, obtains organic dehydrated solvent, and organic dehydrated solvent recycles;
With the brown coal powder and the methyl alcohol adding bottom of dehydration is in the withstand voltage reactor of stainless steel micropore filter plate, and methanol reagent is 1 with the mixed weight ratio of the brown coal powder of dehydration: 1-5: 1, and methyl alcohol is pure reagent; Be controlled at 250 ℃-300 ℃ in temperature, operating pressure is at 10MPa-15MPa, with 200 rev/mins of-350 rev/mins of stirrings, kept 2 hours-5 hours, brown coal powder to dehydration carries out overcritical alcoholysis reaction, obtain residual cinder and alcoholysis product, alcoholysis product stir and still under self the pressure effect, by the screen plate press filtration in extractor;
Alcoholysis product is placed extractor, temperature is controlled at 20 ℃-60 ℃, in extractor, drench eluent then, the flow velocity that adds is 20ml/min-50ml/min, eluent is successively according to the order drip washing of methyl alcohol, butanone, ethyl acetate and tetrahydrofuran (THF) neat solvent 1-2 hour, utilizing gas-chromatography to follow the tracks of detects, the solvend that obtains is put into to still kettle, 100 ℃-130 ℃ of controlled temperature obtain respectively that enrichment lower carbon number hydrocarbons, low-carbon alkoxy organism, phenols, ester class and heavy organic composition etc. are meticulous unit family part; Through the heating refrigerative recrystallization process that carries out with 5 times of methanol solvates, meticulous group of family's part can obtain a series of as alkylnaphthalene, alkyl anthracene and contain the pure organic chemicals that polynary ring includes N, the heteroatomic high additive value of S.
Beneficial effect: owing to adopted such scheme, with lower boiling and the water miscible oxygen organic solvent of ketone that contains as dewatering agent, by dissolving-filtration-distillatory method dewatering agent is thoroughly separated with the brown coal that are removed moisture, the method by organic ketone dewatering agent cycling extraction can remove the most moisture in the brown coal; Make brown coal and organic low-carbon alcohol carry out alcoholysis reaction under mild conditions, less energy consumption is also low to the material requirement of reactor, and raw material does not use fat coal and hydrogen; Heat filtering employing pressurized heat under magnetic agitation of alcoholysis thermosol thing filters and carries out, and can effectively prevent the obstruction of micropore filter plate; Overcritical alcoholysis and solvent extraction method are to carry out in closed system, and solvent for use is the solvent that boiling point is lower than 100 ℃, reclaim and recycle than being easier to; The separation method that adopts ultrafiltration, extraction, distillation and recrystallization to combine adapts to the requirement of product diversification and high added valueization; The gentleness of operational condition, technological process cleaning, the energy consumption material consumption is little and the product high added value, has reached purpose of the present invention.
Advantage: the present invention directly or extend organic chemicals or important chemical material as a series of high additive values: the overcritical alcoholysis reaction by brown coal can obtain enrichment lower carbon number hydrocarbons, low-carbon alkoxy organism, phenols, ester class respectively and be used to prepare the raw material of high-performance carbon fiber or can be used as ultralow grey solid fuel, gained oxygen-bearing liquid constituent class can be used as the fuel of diesel motor and the raw material of synthetic senior tensio-active agent like biofuel; The phenols chemical can be used for novolak resin, oxidation inhibitor, sterilant, sterilant, tensio-active agent, softening agent, spices and dyestuff etc.; Utilize the meticulous family part that obtains behind the organic solvent extraction can obtain pure organic chemicals through recrystallization, because the residual cinder of being retained in the extractor has porousness, can be used as carbon absorbents such as cheap sorbing material is used to dispose of sewage, slow-release fertilizer agent and use.Operational condition gentleness, technological process cleaning, little, the rich choice of products of energy consumption material consumption have realized the optimization and the high value added utilization of organic matter in the coal.
Along with fast development of national economy with to the raising of environmental quality requirement, the clean fuel situation that supply falls short of demand will be increasingly sharpened.Under the situation that oil, Sweet natural gas and renewable energy source temporarily can't satisfy the demands, the low cost development low grade coal is converted into effective technology of utilizing such as clean fuel, high additive value organic chemicals and is of great significance.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Embodiment 1:
The recovery of effective dehydration of the solvent extraction of first brown coal and dehydrated solvent:
The 100 purpose brown coal powders that the acetone of adding 400ml equal proportion amount and butanone mixed solvent and 400g grind in advance in the reactor of 1L, the temperature of dehydration is at 70 ℃ in the control still, fully stir and be incubated 2 hours, afterwards by the pneumatic pump pressing mode, by the screen plate in the reaction enclosure still dehydration brown coal are thoroughly separated with dehydrating solution, the organic dehydrated solvent in 120 ℃ of employing distillatory methods acquisition dehydrating solutions also recycles.
The heat filtering of the overcritical alcoholysis of second brown coal and alcoholysis thermosol thing:
Is in the withstand voltage reactor of stainless steel micropore filter plate with the methyl alcohol of 3: 1 proportionals with dehydration brown coal adding bottom, under magnetic agitation, temperature is controlled at 250 ℃, operating pressure is carried out the overcritical alcoholysis reaction of 4 hours brown coal at 12MPa, the pressure that in magnetic agitation, utilizes in the still self afterwards with thermosol alcoholysis reaction mixture by the screen plate press filtration in extractor.
The fine separation of the mix products that the 3rd alcoholysis reaction obtains:
At 45 ℃, use the drip washing 1 and a half hours successively of methyl alcohol, butanone, ethyl acetate and tetrahydrofuran (THF) eluent respectively with the flow velocity of 40ml/min-50ml/min, the mix products 1 and a half hours of dewatered coal alcoholysis reaction in the extractor is till the solvend in the mix products that utilizes the complete wash-out dewatered coal of single solvent alcoholysis reaction.Adopt the distillatory methods to concentrate different cuts successively and remove eluent at 120 ℃, can obtain respectively that enrichment lower carbon number hydrocarbons, low-carbon alkoxy organism, phenols, ester class and heavy organic composition etc. are meticulous unit family part.Can obtain the pure organic chemicals of a series of high additive values through meticulous group of family's part of recrystallization.
Principle of work: utilize the organic dehydrated solvent of selecting that can be recycled to remove the interior external moisture of brown coal effectively; Utilize the pressure filtration method to make easily that the dissolved organism that goes out separates with system with mixed solvent in the brown coal, utilize the distillatory method to make moisture, organism and the separated from solvent in the solvent simultaneously and organic dehydrated solvent is recycled; Under super critical condition, adopt methyl alcohol or ethanol that dewatered coal is carried out thermal depolymerization, and the solvend of depolymerization is carried out the Rapid Thermal filtration, to prevent the obstruction of filter plate effectively; Relend the method and the technology of the selective dissolution, column chromatography for separation and the recrystallization that help the opposed polarity organic solvent, can carry out fine separation to family's component of the thermosol thing of overcritical alcoholysis, make it to obtain family's component of high added value chemical and can be used as the utilization of oxygen-bearing liquid fuel composition, be easy to prepare the pitch composition of high-performance carbon material and can be used as ultralow grey solid fuel, because the loose porous sorbing material that can be used as again of residual coal uses.
Brown coal are typical low-rank coal, the macromolecular structure of oxygen enrichment in having kept the coal-forming plant to a greater extent.Organic oxygen part in the brown coal exists with the substituent form of aromatic ring, and part connects two or more aromatic rings as bridged bond and constitutes macromolecular system.The intensive hydrogen bond action is to adopt dewater from the brown coal basic reason of difficulty of traditional method between organic oxygen and water molecules in the brown coal micropore, also is to cause the low and high important factor of moisture of brown coal calorific value.Under relatively mild condition, utilize small molecules, lower boiling and water miscible organic solvent to infiltrate in the brown coal micropore, and then destroy the hydrogen bond between oxygen organic macromolecule and water molecules of containing in the brown coal, can remove the moisture in the brown coal so effectively.The organic oxygen level that exists with forms such as hydroxyl, carboxyl, carbonyl and ehter bonds in the brown coal is higher in addition, catalyzed alcoholysis can destroy these that connect macro-radical and contain the oxygen key, make brown coal carry out depolymerization effectively, and can the transform portion hydroxyl, carboxyl is respectively methoxyl group and methoxycarbonyl, increased the solubility in selected organic solvent, utilize the alcoholysis reaction of organic alcohol under the super critical condition can further cut off in the dehydration brown coal and contain the oxo bridge key in the organic macromole, realize the directed depolymerization and the follow-up high value added utilization of brown coal.
Embodiment 2:
(1) recovery of effective dehydration of the solvent extraction of brown coal and dehydrated solvent:
The organic dehydrated solvent and the about 1000g 200 purpose brown coal powders that in the reactor of 5L, add the 2L proportional, temperature is set in 90 ℃ of insulations 2 hours and fully stirring, at 130 ℃ of organic dehydrated solvents that adopt the distillatory methods from the solvent extraction mixing solutions, to steam the organic extract of water, coal successively and can be recycled;
(2) heat filtering of the overcritical alcoholysis of brown coal and alcoholysis thermosol thing;
The methyl alcohol of 1: 1 proportional and dehydration brown coal are added in the withstand voltage reactor that the bottom is stainless steel micropore (aperture≤0.8 a micron) filter plate, under magnetic agitation, temperature is set at 300 ℃, operating pressure is 15MPa, open the valve that the filter plate bottom connects extractor after between 2 hours reaction times, the pressure that under magnetic agitation, utilizes in the still self with the thermosol thing by the filter plate press filtration in extractor;
(3) fine separation of alcoholysis reaction mixture;
At 20 ℃, flow velocity with 80ml/min-100ml/min is used methyl alcohol respectively, butanone, the drip washing 1 hour successively of ethyl acetate and tetrahydrofuran (THF) eluent, utilizing gas-chromatography to follow the tracks of detects, the solvend that obtains is put into to still kettle, 130 ℃ of controlled temperature, dewatered coal alcoholysis product in the extractor, can obtain the enrichment lower carbon number hydrocarbons respectively, the low-carbon alkoxy organism, phenols, ester class and be used to prepare the raw material of high-performance carbon fiber or can be used as ultralow grey solid fuel, utilize the thick group of family's part process recrystallization that obtains behind the organic solvent extraction can obtain the organic chemicals of a series of high additive values, the residual cinder of being retained in the extractor can be used as carbon absorbent.
Embodiment 3:
1) recovery of effective dehydration of the solvent extraction of brown coal and dehydrated solvent:
The organic dehydrated solvent and the 5000g 150 purpose brown coal powders that in the 10L reactor, add the 4000ml proportional, temperature is set in 50 ℃ of insulations 5 hours and fully stirring, at 100 ℃ of organic dehydrated solvents that adopt the distillatory methods from the solvent extraction mixing solutions, to steam the organic extract of water, coal successively and can be recycled;
2) heat filtering of the overcritical alcoholysis of brown coal and alcoholysis thermosol thing;
The methyl alcohol of 5: 1 proportionals and dehydration brown coal are added in the withstand voltage reactor that the bottom is stainless steel micropore (aperture≤0.8 a micron) filter plate, under magnetic agitation, temperature is set in 270 ℃ of scopes, operating pressure is 10MPa, open the valve that the filter plate bottom connects extractor after between 5 hours reaction times, the pressure that under magnetic agitation, utilizes in the still self with the thermosol thing by the filter plate press filtration in extractor;
3) fine separation of alcoholysis reaction mixture;
In 60 ℃ of temperature ranges, use methyl alcohol respectively, butanone, the drip washing 2 hours successively of the ethyl acetate or the mixtures of eluents of pressing different ratios, utilizing gas-chromatography to follow the tracks of detects, the solvend that obtains is put into to still kettle, 100 ℃ of controlled temperature, dewatered coal alcoholysis product in the extractor, can obtain the enrichment lower carbon number hydrocarbons respectively, the low-carbon alkoxy organism, phenols, ester class and be used to prepare the raw material of high-performance carbon fiber or can be used as ultralow grey solid fuel, utilize the thick group of family's part process recrystallization that obtains behind the organic solvent extraction can obtain the organic chemicals of a series of high additive values, the residual cinder of being retained in the extractor can be used as carbon absorbent.
Claims (1)
1, dehydration of the low-disintegration coal under a kind of mild conditions and alcohol depolymerization process, it is characterized in that: technological process is as follows:
The condition of the processed of brown coal powder: select the acetone of equal-volume ratio and butanone to mix as organic dehydrated solvent, 100 orders-200 purpose brown coal powder and organic dehydrated solvent are put into to the reactor that screen plate is arranged, the weight ratio of organic dehydrated solvent and brown coal powder is controlled to be 2: 1-5: 1, controlled temperature is at 50 ℃-90 ℃, fully stirred and be incubated 2 hours-5 hours, use pneumatic pump in reactor, to pressurize, and control pressure is not more than 0.5MPa, the brown coal powder that obtains dewatering and organic dehydration mixing solutions, organic dehydration mixing solutions is put into still kettle, temperature is controlled at 100 ℃-130 ℃, obtains organic dehydrated solvent, and organic dehydrated solvent recycles;
With the brown coal powder and the methyl alcohol adding bottom of dehydration is in the withstand voltage reactor of stainless steel micropore filter plate, and methanol reagent is 1 with the mixed weight ratio of the brown coal powder of dehydration: 1-5: 1, and methyl alcohol is pure reagent; Be controlled at 250 ℃-300 ℃ in temperature, operating pressure is at 10MPa-15MPa, with 200 rev/mins of-350 rev/mins of stirrings, kept 2 hours-5 hours, brown coal powder to dehydration carries out overcritical alcoholysis reaction, obtain residual cinder and alcoholysis product, alcoholysis product stir and still under self the pressure effect, by the screen plate press filtration in extractor;
Alcoholysis product is placed extractor, temperature is controlled at 20 ℃-60 ℃, in extractor, drench eluent then, the flow velocity that adds is 20ml/min-50ml/min, eluent is successively according to the order drip washing of methyl alcohol, butanone, ethyl acetate and tetrahydrofuran (THF) neat solvent 1-2 hour, utilizing gas-chromatography to follow the tracks of detects, the solvend that obtains is put into to still kettle, 100 ℃-130 ℃ of controlled temperature obtain respectively that enrichment lower carbon number hydrocarbons, low-carbon alkoxy organism, phenols, ester class and heavy organic composition etc. are meticulous unit family part; Through the heating refrigerative recrystallization process that carries out with 5 times of methanol solvates, meticulous group of family's part can obtain-and series is as alkylnaphthalene, alkyl anthracene and contain the pure organic chemicals that polynary ring includes N, the heteroatomic high additive value of S.
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