CN1202206C - Extraction separation method for supercritical water liquefied coal - Google Patents
Extraction separation method for supercritical water liquefied coal Download PDFInfo
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- CN1202206C CN1202206C CN 02135859 CN02135859A CN1202206C CN 1202206 C CN1202206 C CN 1202206C CN 02135859 CN02135859 CN 02135859 CN 02135859 A CN02135859 A CN 02135859A CN 1202206 C CN1202206 C CN 1202206C
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Abstract
The present invention relates to an extraction separation method for supercritical water liquefied coal, which relates to a preparation method for extracting a petroleum product from coal in a liquefaction mode and belongs to the technical field of the liquefaction processing of coal. The present invention has the technical scheme that the preparation method provided by the present invention has large processing capacity, short flow time and high production efficiency, and can be applied to the industrialization production. The present invention comprises the processing procedures of material preparation, feed, reaction, extraction, separation and waste exhaust. The present invention is characterized in that the feed adopts a simultaneous feed mode that supercritical water absorbs the coal powder into the water at a high speed, and then the coal powder and the water form mixed fluid which enters a reaction tank. The feed, the extraction and the separation are continuously carried out in the liquefaction reaction process so as to form a continuous processing process, and when accumulated to an allowable height, the waste is exhausted. The present invention has the characteristics of advanced science, strong processing capacity, large handling amount, high production efficiency, simple main equipment, low cost, convenient operation, etc., and can be applied to industrialization production.
Description
Technical field
The present invention relates to extract the production method of coal PetroChina Company Limited. product, particularly extract the method (hereinafter to be referred as the supercritical water liquefied coal method) of petroleum products, belong to the liquidation of coal processing technology field with supercritical water liquefied coal in the direct liquefaction mode.
Background technology
Water 〉=374.3 ℃ and 〉=temperature and pressure following time of 22.1MPa is in supercritical state, this moment, organism, rare gas element and water dissolved each other fully, organism can be dissolved at short notice.Utilize and be easy to isolating characteristic after quick flowability, high resolution and the decompression of supercritical water and come liquefaction coal, extracting of organic compounds and isolate petroleum products, be a new technology of development in recent years, relatively hydrogenation liquefaction coal and have with toluene, tetraline equal solvent liquefaction coal technology melt soon, low, the segregative advantage of solvent cost.The method of existing supercritical water liquefied coal mainly comprises charging, liquefaction reaction, extraction, steps such as trash discharge, during charging coal dust placed a screen basket, screen basket is hung in the retort by the top, cover the loam cake of retort then, in jar, inject water again and make jar in temperature and pressure rise to 400～480 ℃ and 23～28MPa respectively, coal dust and supercritical water carry out liquefaction reaction in jar, what generated after 0.5～1 hour contains the top that organic chemical combination machine thing and high temperature gas-liquid are collected to jar, at the bottom of cinder ashes the like waste accumulates in basket, extraction contains organic high temperature gas-liquid and separates, and just obtains petroleum products.
Above-mentioned existing production method has following defective:
1. feeding manner is a coal dust and water input mode respectively, the charging during each jar produced, reaction, extraction stage by stage, proceed step by step, have 0.5～1 hour interval between reaction and the extraction, the batch processed amount is little, the treatment time is long, production efficiency is low;
2. for improving processing power, often adopt the blindly measure of augmenting response tank volume, simultaneously because the structure formation that retort must adopt the top to uncap greatly, cause that the retort volume is big, complex structure, make retort be difficult for processing and fabricating, and the corresponding equipment manufacturing cost that increased;
3. the coal dust raw material concentrates in the screen basket, is unfavorable for the thorough mixing liquefaction between coal dust and the supercritical water, is unfavorable for rapid reaction;
Coal dust raw material and cinder ash the like waste by tank deck input, discharge, need by the hoisting machinery facility, during the feeding discharging material operational cost, loaded down with trivial details.
In view of this, the problem that necessary solution production method processing power of above-mentioned present stage is low, the time is long, production efficiency is low.
Summary of the invention
Technical problem to be solved by this invention provides that a kind of processing power is big, the flow process time short, the production efficiency height, and the supercritical water liquefied coal that suitability for industrialized is produced is produced the method for petroleum products.
The alleged technical problem of the present invention realizes with following technical scheme:
A kind of extraction separating method of supercritical water liquefied coal comprises following treatment step:
Get the raw materials ready: purchase coal dust, prepare the water source;
Charging: coal dust, water are delivered in the retort, and add basic catalyst NaOH in retort, addition is 2%～5% of a total feed weight.
Liquefaction reaction: make the water in the retort be in overcritical shape by increasing temperature and pressure, coal dust and supercritical water carry out liquefaction reaction in jar, and the supercritical water temperature is that 400～480 ℃, pressure are 23～28MPa;
Extraction: reaction generates in the extractive reaction jar oil, water, vapour mixture, extract is by retort outlet output;
Separate: extract is gone in the separator to separate, obtain the organic compound oil;
Wastage: with reacted cinder ashes by removing in the retort;
Its unique distinction is:
Described charging adopts hypercritical flow that coal dust is sucked in the water, together enters the synchronous feeding manner in the retort behind coal dust and the supercritical water formation mixed stream;
Described charging, extract, be separated in the liquefaction reaction process and proceed, (hereinafter to be referred as the continuous extraction method) carried out in charging, liquefaction reaction, extraction, separation synchronously;
Described wastage is carried out when waste material is accumulated to the permission height, and temporary transient interruption charging recovers charging immediately during discharging after the discharging, and it is 20%～50% of retort height that waste material allows piling height.
Obtain multiple organism for improving separating effect, the extraction separating method of above-mentioned supercritical water liquefied coal, the stage trapping mode is adopted in described separation.
The extraction separating method of above-mentioned supercritical water liquefied coal, described separation progression is two-stage, and first isolates mink cell focus, and lightweight oil is isolated in the second stage.
The extraction separating method of above-mentioned supercritical water liquefied coal, the organism that first and second grade separate formed is imported respectively in the organic solvent separator and is separated, obtains row oil, asphaltene and preceding asphaltene product.
The extract that enters when preventing discharge in the separator refluxes, the extraction separating method of above-mentioned supercritical water liquefied coal, described first and second grade separates the mink cell focus, the lightweight oil that form and is introduced into liquid storage cylinder, and accumulates within it, and then enters the organic solvent separator and separate.
Pollute for making full use of the energy and preventing, the extraction separating method of above-mentioned supercritical water liquefied coal, increase recycling in described separation back, the mixed gas of separate discharge enters interchanger, the gas-liquid separator in the recycling successively, in gas-liquid separator, add conversion catalyst, make CO and water vapor in the mixed gas be converted into CO
2And H
2Discharge.
The extraction separating method of above-mentioned supercritical water liquefied coal, described coal dust are the young brown coal of low metamorphic grade, and coal particle size is 150～300 orders.
The present invention has following characteristics:
1. aspect charging, be bold in innovation, utilize current that coal dust is brought in the water automatically and form mixed stream and import feeding manner in the retort synchronously, handle for continuous extraction and lay a good foundation with water;
2. under synchronous feeding manner prerequisite, logistics characteristic at the bottom of utilizing organism fluid light specific gravity in the liquefaction reaction process to rise to be suspended in tank deck, water and coal dust mixed solution than great slip into jar downwards, charging and extraction and liquefaction reaction process are carried out simultaneously, form continuously feeding, uninterrupted reaction, the isolating continuous treating processes of continuous extraction, increase substantially processing power, shortened treating processes;
3. when adopting the continuous extraction method, liquefaction reaction and separating treatment be free interval when operation just only, the batch processed mode that with the jar is treatment capacity relatively is in each jar time treating processes, between separation and the reaction 0.5～1 hour timed interval Duan Eryan must be arranged all, further reduce the treatment time;
4. continuous extraction method does not require that retort has enough big volume, and simultaneously, retort also need not to adopt big cover-opening structure form, so dwindled the volume of retort, simplified the retort structure, made retort be easier to processing and fabricating, corresponding facility investment and the production cost of having reduced;
5. coal water mixture and waste can be imported easily, discharge by the charging and discharging mouth on the tank body, need not to use the lifting facility, advance, the operation of discharge becomes easily simple;
6. after in reaction process, adding basic catalyst, help improving the content of organism oil in the transformation efficiency of coal dust and the resultant of reaction;
7. adopt the multi-stage separation treatment mode, and separate again, help improving the isolation of purified precision of extract, obtain comparatively meticulous multiple petroleum products by solvent separator;
8. make heat energy obtain recycling by recycling, and prevented discharge of harmful gases;
9. be easy to realize automatic control;
To sum up, the present invention has distinguishing features such as processing power is strong, treatment capacity is big, production efficiency is high, and the simple cost of major equipment is low, and is easy to operate, percentage extraction of the inventive method and oily yield can reach respectively more than 80% and 60%, can satisfy the requirement of using in suitability for industrialized production.
Description of drawings
Fig. 1 is Production Flow Chart of the present invention and device synoptic diagram.
Embodiment
In conjunction with Fig. 1 the present invention is described in further detail:
Purchase low metamorphic grade, particle diameter and be the young brown coal of 200 purposes and it is stored in the Pulverized Coal Bin 4, the weight proportion by 2%～5% is introduced water in the water tank 1 with in the catalyst n aOH enter catalyst jar 11 simultaneously; Start water pump 2, the water that contains catalyzer enters well heater 3 through water pump, heated water enters mixing tube 18, coal dust is sucked during in high speed flow through mixing tube, the formation mixed stream is entered in the retort by the opening for feed at retort 5 tops, temperature with retort, pressure is controlled at 400～480 ℃ respectively, 23～28MPa, make water be in supercritical state, coal dust and supercritical water carry out liquefaction reaction in retort, the oil that reaction generates, water, the vapour extract enters separator 6 by the outlet of retort through control valve 21 and carries out flash trapping stage, the mink cell focus that forms behind the flash trapping stage enters and is stored in the liquid storage cylinder 8, the high temperature gas-liquid that still contains organic compound of separate discharge enters separator 7 through control valve 22 and carries out the secondary separation, separating the lightweight oil that forms enters and is stored in the liquid storage cylinder 9, the high temperature gas-liquid of discharging enters interchanger 14 through control valve 23, enter gas-liquid separator 15 after in interchanger, being absorbed heat energy, gas-liquid separator 15 links to each other with conversion catalyst jar 19, in gas-liquid separator, import conversion catalyst routinely, make the CO of waste gas liquid and water vapor be converted into CO
2And H
2And draw through row's mouth 17 and 16 respectively, mink cell focus, lightweight oil in the liquid storage cylinder 8,9 enters in organic solvent separator 13 backs and separates, obtain row oil, asphaltene and preceding asphaltene petroleum products, primary separator relative response pressure tank step-down 15MPa, second-stage separator 7 relative primary separator step-down 7MPa.
Still consult Fig. 1, the present invention owing to also do not carry out reaction, does not have extract when initial launch, so extraction treatment was carried out after will lagging behind 0.5～1 hour, through behind the initial reaction, charging, reaction, extraction have just entered synchronous successive treating processes.
Still consult Fig. 1, the present invention is when initial launch, and input CO gas in retort to form oxygen reduction atmosphere, can constantly discharge CO in the normal reaction process earlier, can satisfy the reaction requirement, cuts off the input of CO after normal reaction.10 is the CO jar among the figure.
Still consult Fig. 1, in the continuous extraction process, when the piling height of dead meals such as cinder ash in the retort reach the retort height 50% the time, infrared induction device 20 on the retort sends signal, switches off the pump this moment 2 to interrupt chargings, opens the discharge valve 12 of pot bottom simultaneously, waste material just can totally emit under the effect of jar internal pressure up hill and dale, start water pump after discharging finishes immediately and recover charging, extraction does not stop during discharging, and discharge valve can adopt bottom open type baiting valve etc.
In technical process shown in the figure and the device, water pump 2, infrared rays 20, discharge valve 12 and each by-pass valve control etc. can adopt automatic control mode and control automatically by the computer realization sequencing.
Claims (7)
1. the extraction separating method of a supercritical water liquefied coal comprises following treatment step:
Get the raw materials ready: purchase coal dust, prepare the water source;
Charging: coal dust, water are delivered in the retort, and add basic catalyst NaOH in retort, addition is 2%～5% of a total feed weight.
Liquefaction reaction: make the water in the retort be in overcritical shape by increasing temperature and pressure, coal dust and supercritical water carry out liquefaction reaction in jar, and the supercritical water temperature is that 400～480 ℃, pressure are 23～28MPA;
Extraction: reaction generates in the extractive reaction jar oil, water, vapour mixture, extract is by retort outlet output;
Separate: extract is gone in the separator to separate, obtain the organic compound oil;
Wastage: with reacted cinder ashes by removing in the retort;
It is characterized in that:
Described charging adopts supercritical water that coal dust is sucked in the water at a high speed, together enters the synchronous feeding manner in the retort behind coal dust and the supercritical water formation mixed stream;
Described charging, extract, be separated in the liquefaction reaction process and proceed, charging, liquefaction reaction, extraction, separation are carried out synchronously;
Described wastage is carried out when waste material is accumulated to the permission height, and temporary transient interruption charging recovers charging immediately during discharging after the discharging, and it is 20%～50% of retort height that waste material allows piling height.
2. the extraction separating method of supercritical water liquefied coal according to claim 1 is characterized in that, the stage trapping mode is adopted in described separation.
3. the extraction separating method of supercritical water liquefied coal according to claim 2 is characterized in that, the progression of described stage trapping is two-stage.
4. the extraction separating method of supercritical water liquefied coal according to claim 3 is characterized in that, the organism of first and second grade separation formation is imported respectively in the organic solvent separator separated.
5. the extraction separating method of supercritical water liquefied coal according to claim 4, it is characterized in that, described first and second grade separates the organism that forms and is introduced into liquid storage cylinder respectively, and accumulates within it, and then enters described organic solvent separator and separate.
6. the extraction separating method of supercritical water liquefied coal according to claim 5, it is characterized in that, after separation, increase recycling, the mixed gas of separate discharge enters interchanger, the gas-liquid separator in the recycling successively, in gas-liquid separator, add conversion catalyst, make CO and water vapor in the mixed gas be converted into CO
2And H
2Discharge.
7. the extraction separating method of supercritical water liquefied coal according to claim 6 is characterized in that, described coal dust is the young brown coal of low metamorphic grade, and coal particle size is 150～300 orders.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02135859 CN1202206C (en) | 2002-12-06 | 2002-12-06 | Extraction separation method for supercritical water liquefied coal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02135859 CN1202206C (en) | 2002-12-06 | 2002-12-06 | Extraction separation method for supercritical water liquefied coal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1418932A CN1418932A (en) | 2003-05-21 |
| CN1202206C true CN1202206C (en) | 2005-05-18 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02135859 Expired - Fee Related CN1202206C (en) | 2002-12-06 | 2002-12-06 | Extraction separation method for supercritical water liquefied coal |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1292979C (en) * | 2005-01-17 | 2007-01-03 | 西安交通大学 | Coal-biomass co-overcritical water catalysis-gasification hydrogen production plant and method |
| CN101967396B (en) * | 2009-07-27 | 2013-10-16 | 新奥科技发展有限公司 | Method for extracting montan wax |
| CN102198387B (en) * | 2010-03-24 | 2014-06-11 | 淮北中润生物能源技术开发有限公司 | Continuous reaction system taking subcritical or supercritical liquid as solvent and solid as reactant |
| CN101928605A (en) * | 2010-08-17 | 2010-12-29 | 新奥科技发展有限公司 | Method for processing slurry-like residual carbon |
| CN102229810B (en) * | 2011-06-03 | 2013-11-27 | 陕西煤化工技术工程中心有限公司 | Method for extracting thermolysis coal by coal tar |
| CN102925215B (en) * | 2012-08-29 | 2014-07-16 | 新奥科技发展有限公司 | Supercritical water gasification method and apparatus |
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