CN102580617A - High-temperature high-pressure autoclave and using method thereof - Google Patents
High-temperature high-pressure autoclave and using method thereof Download PDFInfo
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Abstract
The invention relates to a high-temperature high-pressure autoclave and a using method thereof, which are used for a reaction process when gas phase, liquid phase and solid phase exist simultaneously, especially for a process of requiring filtering solid particles after reaction. The reaction autoclave can be operated and used under high-temperature high-pressure conditions, achieves direct feeding, hot filtering and discharging solid matter on the premise of not opening an autoclave body, cleans a filter element through nitrogen blowback and ensures continuous equipment operation. The reaction autoclave has the advantages of being high in equipment integration degree and easy to operate and is especially suitable for a hot extraction process under high-temperature high-pressure conditions.
Description
Technical field
The invention belongs to chemical industry equipment and technical field, be specifically related to a kind of high temperature and high pressure kettle and method for using thereof.High temperature and high pressure kettle of the present invention can be used for gas, the simultaneous course of reaction of liquid or solid three-phase, is specially adapted to relating to the extraction heat technology that solid residue separates under the HTHP.
Background technology
At present, the solvent extraction of coal is one of main contents of coal chemistry research, and its research not only has important significance for theories, has actual using value simultaneously.As far back as 20 beginnings of the century, people just adopt solvent extraction to attempt from coking coal, to isolate the caking property component in succession.Number of research projects turns to through the research solvent extract and illustrates the structure of coal subsequently, from molecular level research coal, discloses organic molecule structure in the coal.For the solvent thermal extraction research of coal under HTHP, two kinds of modes are adopted in the laboratory usually: one is to use a kind of extractor of flow model, and two are to use autoclave reactor.(Miura K, Shimada M, Mae K such as Miura; Huan H.Fuel; 2001,80 (11): 1573) invented and a kind ofly from coal, produce the method for clean fuel through solvent thermal extraction, this method is used a kind of extractor of flow model; The extraction yield of bituminous coal can reach 65%～80% when in the time of 350 ℃, using naphthane as solvent, when the carbolic oil that uses polarity during as solvent the extraction yield of brown coal and ub-bituminous coal can reach 80%.(Sang Woo Park, Cheol Hyeon Jang.Bioresource Technology, 2001 such as Sang; The high-temperature high-pressure reaction kettle that 102:8205) uses a kind of 316 stainless steels to make; Open a discharge gate in the bottom of kettle, treat through discharge gate material to be discharged after the extraction heat completion of coal; Be transferred to the independent separation receiving system in high-temperature high-pressure reaction kettle bottom, carry out the Separation of Solid and Liquid operation.
The research of domestic solvent thermal extraction about coal is considerably less.China Coal Research Institute (Shi Zhijie, Zhang Shengzhen, Xing Lingyan etc. coal conversion, 2009,32 (1): 34-39) utilize the extraction heat solvent of coal liquefaction derived oils, on the extraction heat device, studied the extraction heat performance of low-order coal such as Datang triumph brown coal as coal.This extraction heat device also is to utilize common autoclave to transform; Promptly open a discharge gate at autoclave body bottom; Treat after the extraction heat completion of coal; Open the discharge gate valve and rapidly material is discharged, be transferred to the independent separation receiving system in autoclave bottom, carry out the Separation of Solid and Liquid operation.
Employed high temperature and high pressure kettle in the solvent thermal abstraction technique of existing coal; All be to be employed in autoclave body bottom to open a discharge gate; And reacted material is transferred to a mode of separating receiving system separately; So just can't guarantee the feed separation under the extraction heat operating temperature, thereby cause the purpose product yield to descend.
Summary of the invention
The present invention provides a kind of high temperature and high pressure kettle and method for using thereof for solving the problem in the present technology.High temperature and high pressure kettle of the present invention can be used for gas, the simultaneous course of reaction of liquid or solid three-phase, is specially adapted to relating to the extraction heat technology that solid residue separates under the HTHP.
The present invention adopts following technical scheme to be achieved:
A kind of high temperature and high pressure kettle of the present invention, it comprises kettle and kettle cover, connects with bolt between said kettle and the kettle cover; Said autoclave body bottom is provided with material filtering discharger, solid residue emptying device and nitrogen back-blowing device.
Said kettle cover is provided with former charging aperture, gas feed, gas vent, pressure taps (Pressure gauge) and temperature tube (thermocouple).
Said material filtering discharger is connected with kettle through flange in the center of autoclave body bottom, and the upper end of said material filtering discharger, autoclave body bottom are built-in with the stainless steel sintered filter core.
Said nitrogen back-blowing device is installed on the material filtering discharger, and below the outside of the bottom of stainless steel sintered filter core and kettle.
Said solid residue emptying device is to have the ball valve of high pressure resistant and high temperature or the stainless steel tube of gate valve, and it is welded on kettle is built-in with the stainless steel sintered filter core near bottom centre position.
Described high temperature and high pressure kettle, the quantity of said stainless steel sintered filter core 11 are 1-5, and specification is 0.5 μ m, 1 μ m, 2 μ m, 5 μ m or 10 μ m.
Described high temperature and high pressure kettle, the material of said kettle and kettle cover are stainless steel.
A kind of method of using above-mentioned high temperature and high pressure kettle, it comprises the steps:
A, coal dust is broken to granularity≤200 μ m, under 100～150 ℃ of conditions dry 12～96 hours subsequent use.
B, step a gained coal grain and solvent are fully mixed the back add in the high temperature and high pressure kettle, said coal grain and solvent are 1: 2～12 (g/ml) by quality and volume ratio; Said solvent is to contain aromatic ring structure, boiling point greater than 200 ℃ organic solvent.
C, with nitrogen replacement high temperature and high pressure kettle air and inflated with nitrogen wherein to 5MPa; Keep the still internal pressure constant in 30min; Bleed off nitrogen then; Inflated with nitrogen to 0～5MPa be to be rapidly heated to 300～450 ℃ under 100～600 commentaries on classics/min stir at rotating speed, and constant temperature was accomplished extraction process in 0.5～4 hour again.
D, open valve on the material filtering discharger of high temperature and high pressure kettle bottom fast, utilize pressure reduction to carry out heat filtering, filter and finish the back valve-off.
After e, the temperature of treating high temperature and high pressure kettle are reduced to room temperature, open the valve on the solid residue emptying device of autoclave body bottom, inflated with nitrogen to pressure is 0.1～0.3MPa in high temperature and high pressure kettle simultaneously, and the time keeps 10～50min, with thorough discharge residue.
F, treat that the e step is accomplished after, open the nitrogen back blow port on the autoclave body bottom material filtering discharger, inflated with nitrogen in high temperature and high pressure kettle, the time keeps 10～50min, with cleaning stainless steel sintered filter core.The residue that blowback goes out is discharged through solid residue emptying device.
High temperature and high pressure kettle of the present invention is particularly suitable under HTHP, handling or reacting, and need be under HTHP with liquid phase material in solid particle carry out separating process, be particularly suitable for the extraction heat process of coal.
The present invention compared with prior art has following significant advantage:
(1) in a reactor, realize coal solvent thermal extraction and two processes of feed separation under HTHP simultaneously, equipment is simple, technological process is short, small investment.
(2) feed separation under the extraction heat operating temperature makes the extraction yield improve, and the extraction heat purpose solid product yield of coal is greater than 70%, and ash content is less than 0.1%.
(3) the built-in stainless steel sintered filter core of autoclave body bottom is to be threaded with flange, and the stainless steel sintered filter core is loaded and unloaded from flange easily.
(4) autoclave body bottom is connected with the flange of having fixed the stainless steel sintered filter core is whole, and the flange integral body of having fixed the stainless steel sintered filter core is loaded and unloaded from kettle easily.
(5) the nitrogen back blow port that is provided with on the material filtering discharger of autoclave body bottom can clean filter core, has guaranteed the unobstructed of filter core.
(6) the solid residue emptying device that material inlet that is provided with on the kettle cover and autoclave body bottom are provided with has solved the turnover problem of raw material with reaction back solid material under the prerequisite of not opening kettle cover.
In a word, but the present invention has that continued operation, purpose product yield height, good product quality, technological process are short, smooth operation and the characteristics of control easily.Utilize coal extraction heat rate that this high temperature and high pressure kettle can make coal greater than 80%, coal extraction heat purpose solid product yield is greater than 70%, and ash content is less than 0.1%.
Description of drawings
Fig. 1 is the general structure sketch map of a kind of high temperature and high pressure kettle of the present invention.
Fig. 2 is the vertical view of a kind of high temperature and high pressure kettle of the present invention.
Each part description among the figure:
The 1-heating furnace body; The 2-kettle cover; 3-temperature tube (thermocouple); The 4-gas feed; 5-magnetic agitation motor; The former charging aperture of 6-; The 7-gas vent; The 8-pressure taps; The 9-kettle; The 10-paddle; 11-stainless steel sintered filter core; 12-solid residue emptying device; The 13-flange; The 14-discharging opening; 15-nitrogen back-blowing device; 16-material filtering discharger.
The specific embodiment
Below in conjunction with accompanying drawing the present invention is done further detailed description.
Referring to Fig. 1, Fig. 2.
A kind of high temperature and high pressure kettle mainly comprises kettle 9 and kettle cover 2, leans on bolt to connect between kettle and the kettle cover, and material is a stainless steel; Said autoclave body bottom is provided with material filtering discharger 16, solid residue emptying device 12 and nitrogen back-blowing device 15; Said kettle cover 2 is provided with material inlet 6, gas feed 4, gas vent 7, pressure taps 8 (Pressure gauge) and the temperature tube 3 (thermocouple) of liquid, solid powder.
Described material filtering discharger 16 is connected with kettle 9 through flange 13 in the center of kettle 9 bottoms, and is built-in with stainless steel sintered filter core 11.
Said nitrogen back-blowing device 15 is installed on the material filtering discharger 16, and below the outside of the bottom of stainless steel sintered filter core 11 and kettle 9.
Described solid residue emptying device 12 is to have the ball valve of high pressure resistant and high temperature or the stainless steel tube of gate valve, and it directly is welded on kettle is built-in with stainless steel sintered filter core 11 near bottom centre position.
The quantity of described stainless steel sintered filter core 11 is 1-5, and specification is 0.5 μ m, 1 μ m, 2 μ m, 5 μ m, 10 μ m.
The method of above-mentioned high temperature and high pressure kettle, described method for using be specially adapted to need be under HTHP with liquid phase material in solid particle carry out separating process, be particularly suitable for the extraction heat process of coal.
A kind of method for using of using above-mentioned high temperature and high pressure kettle, the specific embodiment is:
A, coal dust is broken to granularity≤200 μ m, under 100～150 ℃ of conditions dry 12～96 hours subsequent use.
B, step a gained coal grain and solvent are fully mixed the back add in the high temperature and high pressure kettles through former charging aperture 6, said coal grain and solvent are 1: 2～12 (g/ml) by quality and volume ratio; Said solvent is to contain aromatic ring structure, boiling point greater than 200 ℃ organic solvent.
C, extraction process; Feed nitrogen from gas feed 4, to 5MPa, maintenance still internal pressure is constant in 30min with nitrogen replacement high temperature and high pressure kettle air and inflated with nitrogen wherein; Bleed off nitrogen from gas vent 7 then; Inflated with nitrogen to 0～5MPa again is that the magnetic agitation of 100～600 commentaries on classics/min is rapidly heated to 300～450 ℃ for 5,10 times at rotating speed, and constant temperature 0.5～4 hour.
After d, extraction are accomplished, open the discharging valve on the material filtering discharger 16 fast, utilize the pressure reduction between receiving system that high temperature and high pressure kettle is inner with its outside is connected to carry out heat filtering, filter and finish the back valve-off.
After e, the temperature of treating high temperature and high pressure kettle are reduced to room temperature; Open the valve on the autoclave body bottom solid residue emptying device 12; Be 0.1～0.3MPa through gas feed 4 places inflated with nitrogen to pressure in high temperature and high pressure kettle simultaneously; Time keeps 10～50min, with thorough discharge residue, closes gas feed 4 place's valves after the end.
F, treat that the e step is accomplished after; Open the nitrogen back blow port 15 on the material filtering discharger 16; Inflated with nitrogen in high temperature and high pressure kettle, the time keeps 10～50min, with thorough cleaning stainless steel sintered filter core; The residue that blowback goes out is discharged through solid residue emptying device 12, close the valve of opening after the end.
The method of above-mentioned high temperature and high pressure kettle, be specially adapted to need be under HTHP with liquid phase material in solid particle carry out separating process, be particularly suitable for the extraction heat process of coal.
Use this high temperature and high pressure kettle, coal is carried out extraction heat.With granularity≤200 μ m, the moisture-free coal grain 300g after under 100 ℃ dry 96 hours is by quality and volume ratio; Coal grain and solvent are 1: 2, add N-methyl pyrrolidone 600ml, after it is fully mixed; Material inlet 6 from kettle cover 2 is added in the high temperature and high pressure kettle, to 5MPa, keeps the still internal pressure constant in 30min with nitrogen replacement autoclave air and inflated with nitrogen wherein; Bleed off nitrogen then; Inflated with nitrogen is to 5MPa again, is to be rapidly heated to 450 ℃ under 600 commentaries on classics/min stir at rotating speed, and constant temperature 4 hours.Extraction is opened the valve on the material filtering discharger 16 after finishing fast, utilizes the pressure reduction between receiving system that high temperature and high pressure kettle is inner with its outside is connected to carry out heat filtering, filters and finishes the back valve-off.After the temperature of treating high temperature and high pressure kettle is reduced to room temperature; Opening the valve on the solid residue emptying device 12, is 0.1MPa through gas feed 4 places inflated with nitrogen to pressure in high temperature and high pressure kettle simultaneously, and the time keeps 50min; With thorough discharge residue, close gas feed place valve after the end.Open the nitrogen back blow port on the material filtering discharger 16 then; Inflated with nitrogen in high temperature and high pressure kettle, the time keeps 50min, with thorough cleaning stainless steel sintered filter core; The residue that blowback goes out is discharged through the solid residue emptying device 12 of autoclave body bottom, close the valve of opening after the end.The extraction heat rate of reaction back coal is 83.2%, and coal extraction heat purpose solid product yield is 73.8%, and ash content is less than 0.1%.
Use this high temperature and high pressure kettle, coal is carried out extraction heat.With granularity≤200 μ m, the moisture-free coal grain 50g after under 150 ℃ of conditions dry 12 hours is by quality and volume ratio; Coal grain and solvent are 1: 12, add 1-methyl naphthalene 600ml, after it is fully mixed; Material inlet 6 from kettle cover 2 is added in the high temperature and high pressure kettle, to 5MPa, keeps the still internal pressure constant in 30min with nitrogen replacement autoclave air and inflated with nitrogen wherein; Bleed off nitrogen then; Inflated with nitrogen is to 0MPa again, is to be rapidly heated to 300 ℃ under 100 commentaries on classics/min stir at rotating speed, and constant temperature 0.5 hour.Extraction is opened the valve on the material filtering discharger 16 after finishing fast, utilizes the pressure reduction between receiving system that high temperature and high pressure kettle is inner with its outside is connected to carry out heat filtering, filters and finishes the back valve-off.After the temperature of treating high temperature and high pressure kettle is reduced to room temperature; Opening the valve on the solid residue emptying device 12, is 0.3MPa through gas feed 4 places inflated with nitrogen to pressure in high temperature and high pressure kettle simultaneously, and the time keeps 10min; With thorough discharge residue, close gas feed place valve after the end.Open the nitrogen back blow port on the material filtering discharger 16 then; Inflated with nitrogen in high temperature and high pressure kettle, the time keeps 10min, with thorough cleaning stainless steel sintered filter core; The residue that blowback goes out is discharged through the solid residue emptying device 12 of autoclave body bottom, close the valve of opening after the end.The extraction heat rate of reaction back coal is 86.5%, and coal extraction heat purpose solid product yield is 74.7%, and ash content is less than 0.1%.
Use this high temperature and high pressure kettle, coal is carried out extraction heat.With granularity≤200 μ m, the moisture-free coal grain 100g after under 120 ℃ of conditions dry 48 hours is by quality and volume ratio; Coal grain and solvent are 1: 7, add technical grade GB washing oil 700ml, after it is fully mixed; Material inlet 6 from kettle cover 2 is added in the high temperature and high pressure kettle, to 5MPa, keeps the still internal pressure constant in 30min with nitrogen replacement autoclave air and inflated with nitrogen wherein; Bleed off nitrogen then; Inflated with nitrogen is to 1MPa again, is to be rapidly heated to 380 ℃ under 400 commentaries on classics/min stir at rotating speed, and constant temperature 1 hour.Extraction is opened the valve on the material filtering discharger 16 after finishing fast, utilizes the pressure reduction between receiving system that high temperature and high pressure kettle is inner with its outside is connected to carry out heat filtering, filters and finishes the back valve-off.After the temperature of treating high temperature and high pressure kettle is reduced to room temperature; Open the valve on the solid residue emptying device 12 of autoclave body bottom; Be 0.2MPa through gas feed 4 places inflated with nitrogen to pressure in high temperature and high pressure kettle simultaneously; Time keeps 30min, with thorough discharge residue, closes gas feed place valve after the end.Open the nitrogen back blow port on the material filtering discharger 16 then; Inflated with nitrogen in high temperature and high pressure kettle, the time keeps 30min, with thorough cleaning stainless steel sintered filter core; The residue that blowback goes out is discharged through the solid residue emptying device 12 of autoclave body bottom, close the valve of opening after the end.The extraction heat rate of reaction back coal is 85.5%, and coal extraction heat purpose solid product yield is 80.8%, and ash content is less than 0.1%.
Use this high temperature and high pressure kettle, coal is carried out extraction heat.With granularity≤200 μ m, the moisture-free coal grain 200g after under 130 ℃ of conditions dry 36 hours is by quality and volume ratio; Coal grain and solvent are 1: 4, add 2-methyl naphthalene 800ml, after it is fully mixed; Material inlet 6 from kettle cover 2 is added in the high temperature and high pressure kettle, to 5MPa, keeps the still internal pressure constant in 30min with nitrogen replacement autoclave air and inflated with nitrogen wherein; Bleed off nitrogen then; Inflated with nitrogen is to 3MPa again, is to be rapidly heated to 340 ℃ under 200 commentaries on classics/min stir at rotating speed, and constant temperature 3 hours.Extraction is opened the valve on the material filtering discharger 16 after finishing fast, utilizes the pressure reduction between receiving system that high temperature and high pressure kettle is inner with its outside is connected to carry out heat filtering, filters and finishes the back valve-off.After the temperature of treating high temperature and high pressure kettle is reduced to room temperature; Open the valve on the solid residue emptying device 12 of autoclave body bottom; Be 0.15MPa through gas feed 4 places inflated with nitrogen to pressure in high temperature and high pressure kettle simultaneously; Time keeps 40min, with thorough discharge residue, closes gas feed place valve after the end.Open on the material filtering discharger 16 nitrogen back blow port then; Inflated with nitrogen in high temperature and high pressure kettle, the time keeps 40min, with thorough cleaning stainless steel sintered filter core; The residue that blowback goes out is discharged through the solid residue emptying device 12 of autoclave body bottom, close the valve of opening after the end.The extraction heat rate of reaction back coal is 81.6%, and coal extraction heat purpose solid product yield is 74.3%, and ash content is less than 0.1%.
Claims (4)
1. a high temperature and high pressure kettle is characterized in that, it comprises kettle (9) and kettle cover (2), connects with bolt between said kettle and the kettle cover; Said autoclave body bottom is provided with material filtering discharger (16), solid residue emptying device (12) and nitrogen back-blowing device (15);
Said kettle cover (2) is provided with former charging aperture (6), gas feed (4), gas vent (7), pressure taps (8) and temperature tube (3);
Said material filtering discharger (16) is connected with kettle through flange (13) in the center of kettle (9) bottom, and is built-in with stainless steel sintered filter core (11) bottom the upper end of said material filtering discharger (16), kettle (9);
Said nitrogen back-blowing device (15) is installed on the material filtering discharger (16), and in the bottom of stainless steel sintered filter core (11) and the outside below of kettle (9);
Said solid residue emptying device (12) is to have the ball valve of high pressure resistant and high temperature or the stainless steel tube of gate valve, and it is welded on kettle is built-in with stainless steel sintered filter core (11) near bottom centre position.
2. high temperature and high pressure kettle as claimed in claim 1 is characterized in that,
The quantity of said stainless steel sintered filter core (11) is 1-5, and specification is 0.5 μ m, 1 μ m, 2 μ m, 5 μ m or 10 μ m.
3. high temperature and high pressure kettle as claimed in claim 1 is characterized in that,
The material of said kettle and kettle cover is a stainless steel.
4. a method of using above-mentioned high temperature and high pressure kettle is characterized in that it comprises the steps:
A, coal dust is broken to granularity≤200 μ m, under 100～150 ℃ of conditions dry 12～96 hours subsequent use;
B, step a gained coal grain and solvent are fully mixed the back add in the high temperature and high pressure kettle, said coal grain and solvent are 1: 2～12 (g/ml) by quality and volume ratio; Said solvent is to contain aromatic ring structure, boiling point greater than 200 ℃ organic solvent;
C, with nitrogen replacement high temperature and high pressure kettle air and inflated with nitrogen wherein to 5MPa; Keep the still internal pressure constant in 30min; Bleed off nitrogen then; Inflated with nitrogen to 0～5MPa be to be rapidly heated to 300～450 ℃ under 100～600 commentaries on classics/min stir at rotating speed, and constant temperature was accomplished extraction process in 0.5～4 hour again;
D, open valve on the material filtering discharger of high temperature and high pressure kettle bottom fast, utilize pressure reduction to carry out heat filtering, filter and finish the back valve-off;
After e, the temperature of treating high temperature and high pressure kettle are reduced to room temperature, open the valve on the solid residue emptying device of autoclave body bottom, inflated with nitrogen to pressure is 0.1～0.3MPa in high temperature and high pressure kettle simultaneously, and the time keeps 10～50min, with thorough discharge residue;
F, treat that the e step is accomplished after, open the nitrogen back blow port on the autoclave body bottom material filtering discharger, inflated with nitrogen in high temperature and high pressure kettle, the time keeps 10～50min, with cleaning stainless steel sintered filter core.The residue that blowback goes out is discharged through solid residue emptying device.
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| CN105733618A (en) * | 2016-04-19 | 2016-07-06 | 河南城建学院 | Heavy organic matter pyrolyzing reaction kettle and pyrolyzing device |
| CN106076205A (en) * | 2016-08-18 | 2016-11-09 | 精晶药业股份有限公司 | Simple high-voltage reactor is used in a kind of test |
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| CN105733618A (en) * | 2016-04-19 | 2016-07-06 | 河南城建学院 | Heavy organic matter pyrolyzing reaction kettle and pyrolyzing device |
| CN105733618B (en) * | 2016-04-19 | 2019-04-12 | 河南城建学院 | A kind of heavy organic matter pyrolytic reaction kettle and pyrolysis installation |
| CN106076205A (en) * | 2016-08-18 | 2016-11-09 | 精晶药业股份有限公司 | Simple high-voltage reactor is used in a kind of test |
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| CN102580617B (en) | 2014-07-02 |
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