CN102923714A - Next-door thermal coupling distillation method and equipment for producing polycrystalline silicon - Google Patents
Next-door thermal coupling distillation method and equipment for producing polycrystalline silicon Download PDFInfo
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- CN102923714A CN102923714A CN2012104352195A CN201210435219A CN102923714A CN 102923714 A CN102923714 A CN 102923714A CN 2012104352195 A CN2012104352195 A CN 2012104352195A CN 201210435219 A CN201210435219 A CN 201210435219A CN 102923714 A CN102923714 A CN 102923714A
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Abstract
The invention relates to a next-door thermal coupling distillation method and equipment for producing polycrystalline silicon. The equipment comprises a low-pressure next-door rectifying tower, a medium-pressure next-door rectifying tower, a high-pressure next-door rectifying tower, a top tower condenser and a tower kettle reboiler, condensation reboilers are arranged between the two rectifying towers, rear tower top gas phase materials release heat in the condensation reboilers and are condensed into cold fluids to return to a rear tower, and front tower kettle materials absorb heat in the condensation reboilers and return to a front tower after becoming reboiling vapor. Coarse trichlorosilane materials are separated though the three next-door rectifying towers successively, low-boiling-point substances are removed at tower tops, high-boiling-point substances are removed at tower bottoms, and high-purity trichlorosilane products are extracted on the lateral line of the high-pressure tower finally. Compared with traditional distillation processes, a next-door distillation technology and a differential-pressure thermal coupling technology can decrease energy consumption and equipment investment. The next-door thermal coupling distillation method and equipment for producing polycrystalline silicon utilizes the next-door distillation technology and the differential-pressure thermal coupling technology simultaneously, the production cost and the energy consumption are decreased greatly, and distillation energy is saved by about 70%.
Description
Technical field
The present invention relates to the distillation technology field, utilize energy-efficient next door distillation technology and differential pressure heat coupling technique purify trichlorosilane, propose especially a kind of next door thermal coupling rectificating method and equipment for production of polysilicon.
Background technology
Polycrystalline silicon material is electronics and information industry and the most important base mateiral of solar energy power generating industry, and solar-grade polysilicon can be used for solar energy power generating, is the WeiLai Technology of a kind of efficient, environmental protection and cleaning, alternative existing power generation mode.And electronic-grade polycrystalline silicon can be used for making semiconductor material, is used for the manufacturing of unicircuit substrate, is widely used in space flight, artificial intelligence, the automatic field such as control and computer chip.Therefore polycrystalline silicon material has strategic importance for the development of national new forms of energy and new and high technology.
At present, the production of polysilicon technique of China's most enterprises is improved Siemens, its flow process is as follows: with chlorine and hydrogen synthesising hydrogen (or outsourcing hydrogenchloride), hydrogenchloride and industrial silica fume be synthesizing trichlorosilane at a certain temperature, then trichlorosilane is carried out rectifying separation and purify, the liquid phase trichlorosilane of the rear condensation of purifying enters in process heating vaporization and carries out CVD reaction production high purity polycrystalline silicon in the hydrogen reduction furnace.Its reduction furnace tail gas carries out dry method and reclaims, and the chlorosilane after the recovery again carries out the rectifying separation purification and obtains trichlorosilane, and its silicon tetrachloride as by-product enters the hydrogenation furnace reaction and generates trichlorosilane, thereby realizes closed cycle.Most this methods that adopt of domestic and international existing polysilicon factory are produced electronic-grade and solar-grade polysilicon.
Can be found out by the improvement Siemens process, the purity of the liquid phase trichlorosilane after the purification has directly determined the quality of polysilicon product, so the trichlorosilane purifier units is very important.Most domestic producer generally adopts large-scale rectifying tower in order to obtain highly purified trichlorosilane, and reflux ratio is also very large, so energy consumption and facility investment are large, and production cost is high.
CN 101538045A has proposed a kind of trichlorosilane differential pressure coupling rectification technology, can the decrease production cost and energy after, wherein Finestill energy-saving about 40%.CN 101538044B proposes a kind of trichlorosilane process for separating and purifying, contains light constituent chlorosilane and B, P impurity in the thick trichlorosilane, need to just can obtain highly purified trichlorosilane through repeatedly removing low-boiling-point substance and high boiling material.Although adopt the differential pressure coupling technique to reduce production energy consumption, the multitower continuous rectification, purification efficiency is low, and facility investment is large.
The next door rectifying tower is coupling in two traditional rectifying tower in the tower shell, in tower inside vertical partition plate is set, the radially mixing of liquid phase fluid has effectively been avoided in vertical next door, and no matter can both guarantee only to use a rectifying tower just can separate ternary mixture under any thermokinetics situation.The separation of tradition tertiary mixture needs two rectifying tower, so dividing wall column can effectively save a rectifying tower, a condenser and a reboiler, effectively reduces facility investment.Because the coupling of rectifying, so that energy utilization efficiency improves, for different systems, the next door distillation technology can energy-conservation 15%-50%.
The maximum characteristics of next door rectifying tower are that it extremely is good at the component of separating the boiling point that mediates, and isolated concentration of intermediate products is very high.In the production of polysilicon, contain many impurity in the trichlorosilane raw material, raw material can be divided into low-boiling-point substance, trichlorosilane and high boiling material three parts, because low-boiling-point substance and high boiling material content are few especially with respect to trichlorosilane, so the next door rectifying tower can obtain highly purified trichlorosilane.The present invention utilizes the next door distillation technology, in conjunction with differential pressure heat coupling technique purify trichlorosilane, can the decrease production energy consumption, and can save great deal of investment again, thereby reduce production costs.
Summary of the invention
The purpose of this invention is to provide a kind of next door thermal coupling rectificating method and equipment for production of polysilicon, utilize next door distillation technology and differential pressure heat coupling technique to combine, decrease production energy consumption and minimizing facility investment.
The present invention proposes a kind of next door thermal coupling rectificating method for production of polysilicon: after thick trichlorosilane raw material 8 separates through low pressure next door rectifying tower 1, top gaseous phase material 9 is divided into liquid-phase reflux material 10 and overhead extraction material 11 through behind the overhead condenser 4 according to quality reflux ratio 400 ~ 900, liquid phase material 13 is divided into two portions at the bottom of the tower, a part forms back tower steam 14 and returns low pressure next door rectifying tower 1 after 5 heating of mesolow tower condensation reboiler, another part as tower at the bottom of extraction material 15, then the highly purified trichlorosilane 12 of low pressure next door rectifying tower 1 middle part side line extraction delivers into middle pressure next door rectifying tower 2; Middle pressure next door rectifying tower 2 top gaseous phase materials 16 enter mesolow tower condensation reboiler 5, for mesolow tower condensation reboiler 5 is condensed into supercooled liquid after heat is provided, be 500 ~ 1000 to be divided into liquid-phase reflux material 17 and overhead extraction material 18 according to the quality reflux ratio, liquid phase material 20 is divided into two portions at the bottom of the tower, form back tower steam 22 after a part heats through mesohigh tower condensation reboiler 6 and return middle pressure next door rectifying tower 2, another part as tower at the bottom of extraction material 21, then rectifying tower 2 middle part side line extraction high-purity trichlorosilanes 19 in middle pressure next door deliver into high pressure next door rectifying tower 3; Rectifying tower 3 top gaseous phase materials 23 in high pressure next door enter mesohigh tower condensation reboiler 6, for mesohigh tower condensation reboiler 6 is condensed into supercooled liquid after heat is provided, be 750 ~ 1250 to be divided into liquid-phase reflux material 24 and overhead extraction material 25 according to the quality reflux ratio, liquid phase material 27 is divided into two portions at the bottom of the tower, a part forms back tower steam 29 through tower bottom reboiler 7 post-heating and returns high pressure next door rectifying tower 3, another part as tower at the bottom of extraction material 28, high pressure next door rectifying tower 3 middle part extraction trichlorosilane products 26.
Mesolow of the present invention next door rectifying tower pressure on top surface is 150kPa～400kPa, and tower top temperature is 40 ℃～50 ℃, quantity of reflux/inlet amount (L/F)=8 ~ 18; Middle pressure next door rectifying tower pressure on top surface is 300kPa～500kPa, and tower top temperature is 80 ℃ ~ 95 ℃, quantity of reflux/inlet amount (L/F)=10 ~ 20; High pressure next door rectifying tower pressure on top surface 500kPa～900kPa, tower top temperature is 100 ℃ ~ 115 ℃, quantity of reflux/inlet amount (L/F)=15 ~ 25.
The present invention can adopt the next door thermal coupling rectifying device that has now used.Also can adopt following next door thermal coupling rectifying device for production of polysilicon, comprise low pressure next door rectifying tower 1, overhead condenser 4, middle pressure next door rectifying tower 2, high pressure next door rectifying tower 3 and tower bottom reboiler 7; It is characterized in that arranging between two next door rectifying tower mesolow tower condensation reboiler 5 and mesohigh tower condensation reboiler 6.In low pressure next door rectifying tower, middle pressure next door rectifying tower and the high pressure next door rectifying tower division plate is arranged.Rectifying tower adopts column plate, random packing or structured packing.Described mesolow tower condensation reboiler 5 adds thermal low next door rectifying tower 1 materials at bottom of tower and returns low pressure next door rectifying tower 1 for the steam that boils again, and the top gaseous phase material with middle pressure next door rectifying tower 2 is cooled to supercooled liquid simultaneously; Mesohigh tower condensation reboiler 6 adds pines for pressing rectifying tower 2 materials at bottom of towers in next door to return middle pressure next door rectifying tower 2 for the steam that boils again, and the top gaseous phase material with high pressure next door rectifying tower 3 is cooled to supercooled liquid simultaneously.
The present invention has the following advantages:
(1) press the load of next door rectifying tower cat head condensation to be complementary with the load of low pressure next door rectifying tower tower bottom reboiler in, the load of high pressure next door rectifying tower cat head condensation can be complementary with the load of middle pressure next door rectifying tower tower bottom reboiler, realize thermal coupling rectifying, the coupling heat exchange reduces energy consumption.
(2) the next door distillation technology is saved 3 rectifying tower, and the differential pressure heat coupling technique is saved 2 condensers, reduces facility investment.
(3) utilize the next door thermal coupled rectifying tower can obtain the high-purity trichlorosilane product.
Description of drawings
Fig. 1 is the energy-saving technique schematic diagram that utilizes next door thermal coupled rectifying tower purify trichlorosilane;
Wherein: 1. low pressure next door rectifying tower, 2. middle pressure next door rectifying tower, 3. high pressure next door rectifying tower, 4. lower pressure column overhead condenser, 5. mesolow tower condensation reboiler, 6. mesohigh tower condensation reboiler, 7. high-pressure tower tower bottom reboiler, 8. thick trichlorosilane raw material, 9. lower pressure column top gaseous phase material, 10. lower pressure column liquid-phase reflux material, 11. lower pressure column overhead extraction material, 12. lower pressure column trichlorosilane side line extraction materials, liquid phase material at the bottom of the 13. lower pressure column towers, 14. lower pressure column returns tower steam, extraction material at the bottom of the 15. lower pressure column towers; 16. medium pressure column top gaseous phase material, 17. medium pressure column liquid-phase reflux materials, 18. medium pressure column overhead extraction materials, 19. medium pressure column trichlorosilane side line extraction materials, liquid phase material at the bottom of the 20. medium pressure column towers, extraction material at the bottom of the 21. medium pressure column towers, 22. medium pressure columns return tower steam; 23. high-pressure tower top gaseous phase material, 24. high-pressure tower liquid-phase reflux materials, 25. high-pressure tower overhead extraction materials, 26. trichlorosilane products, liquid phase material at the bottom of the 27. high-pressure tower towers, extraction material at the bottom of the 28. high-pressure tower towers, 29. high-pressure towers return tower steam.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is described in further details:
After thick trichlorosilane raw material 8 separates through low pressure next door rectifying tower 1, top gaseous phase material 9 is divided into liquid-phase reflux material 10 and overhead extraction material 11 through behind the overhead condenser 4 according to quality reflux ratio 400 ~ 900, liquid phase material 13 is divided into two portions at the bottom of the tower, a part forms back tower steam 14 and returns low pressure next door rectifying tower 1 after 5 heating of mesolow tower condensation reboiler, another part as tower at the bottom of extraction material 15, then the highly purified trichlorosilane 12 of low pressure next door rectifying tower 1 middle part side line extraction delivers into middle pressure next door rectifying tower 2; Middle pressure next door rectifying tower 2 top gaseous phase materials 16 enter mesolow tower condensation reboiler 5, for mesolow tower condensation reboiler 5 is condensed into supercooled liquid after heat is provided, be 500 ~ 1000 to be divided into liquid-phase reflux material 17 and overhead extraction material 18 according to the quality reflux ratio, liquid phase material 20 is divided into two portions at the bottom of the tower, form back tower steam 22 after a part heats through mesohigh tower condensation reboiler 6 and return middle pressure next door rectifying tower 2, another part as tower at the bottom of extraction material 21, then rectifying tower 2 middle part side line extraction high-purity trichlorosilanes 19 in middle pressure next door deliver into high pressure next door rectifying tower 3; Rectifying tower 3 top gaseous phase materials 23 in high pressure next door enter mesohigh tower condensation reboiler 6, for mesohigh tower condensation reboiler 6 is condensed into supercooled liquid after heat is provided, be 750 ~ 1250 to be divided into liquid-phase reflux material 24 and overhead extraction material 25 according to the quality reflux ratio, liquid phase material 27 is divided into two portions at the bottom of the tower, a part forms back tower steam 29 through tower bottom reboiler 7 post-heating and returns high pressure next door rectifying tower 3, another part as tower at the bottom of extraction material 28, high pressure next door rectifying tower 3 middle part extraction trichlorosilane products 26.
Low pressure next door rectifying tower pressure on top surface is 150kPa～400kPa, and tower top temperature is 40 ℃～50 ℃, quantity of reflux/inlet amount (L/F)=8 ~ 18; Middle pressure next door rectifying tower pressure on top surface is 300kPa～500kPa, and tower top temperature is 80 ℃ ~ 95 ℃, quantity of reflux/inlet amount (L/F)=10 ~ 20; High pressure next door rectifying tower pressure on top surface 500kPa～900kPa, tower top temperature is 100 ℃ ~ 115 ℃, quantity of reflux/inlet amount (L/F)=15 ~ 25.
This implementation method can adopt the next door thermal coupling rectifying device that has now used.Also can adopt following next door thermal coupling rectifying device for production of polysilicon, comprise low pressure next door rectifying tower 1, overhead condenser 4, middle pressure next door rectifying tower 2, high pressure next door rectifying tower 3 and tower bottom reboiler 7; Mesolow tower condensation reboiler 5 and mesohigh tower condensation reboiler 6 are set between two rectifying tower.In low pressure next door rectifying tower 1, middle pressure next door rectifying tower 2 and high pressure next door rectifying tower 3 towers division plate is arranged.Rectifying tower adopts column plate, random packing or structured packing.Mesolow tower condensation reboiler 5 adds thermal low next door rectifying tower 1 materials at bottom of tower and returns low pressure next door rectifying tower 1 for the steam that boils again, and the top gaseous phase material with middle pressure next door rectifying tower 2 is cooled to supercooled liquid simultaneously; Mesohigh tower condensation reboiler 6 adds pines for pressing rectifying tower 2 materials at bottom of towers in next door to return middle pressure next door rectifying tower 2 for the steam that boils again, and the top gaseous phase material with high pressure next door rectifying tower 3 is cooled to supercooled liquid simultaneously.
Embodiment 1:
The purification of 80000 ton/years of trichlorosilanes, feed composition is as follows:
Thick trichlorosilane feed composition: dichloro-dihydro silicon 0.5%; Trichlorosilane 99%; Silicon tetrachloride 0.5%.10 tons/hour of feed rates.
Low pressure next door rectifying tower pressure on top surface is 280kPa, and tower top temperature is 45 ℃, quantity of reflux/inlet amount (L/F)=13.6.
Middle pressure next door rectifying tower pressure on top surface is 480kPa, and tower top temperature is 85.4 ℃, quantity of reflux/inlet amount (L/F)=16.8.
High pressure next door rectifying tower pressure on top surface is 800kPa, and tower top temperature is 107.9 ℃, quantity of reflux/inlet amount (L/F)=20.
Each tower load is shown in following table (table one) in the trichlorosilane purification process, because rectifying adopts the differential pressure coupled method, so the cooling load of the heating load of low pressure next door rectifying tower and middle pressure next door rectifying tower is complementary, the heating load of middle pressure next door rectifying tower and the cooling load of high pressure next door rectifying tower are complementary, and data are to set up required heating or cooling load behind the condensation reboiler in the bracket:
Table one
In traditional trichlorosilane purifying technique, cooling and heating total load are 49.0148M*KCAL/HR.Adopt in the technique of next door rectifying tower, total load is 43.3103M*KCAL/HR, conserve energy 11.64%.And in the next door rectifying tower technique behind the employing differential pressure coupling technique, total load is 14.4386M*KCAL/HR only, and this energy saving technology can reach 70.54%.
Embodiment 2:
The purification of 80000 ton/years of trichlorosilanes, operational condition is with embodiment 1, and different condition is as follows:
Thick trichlorosilane feed composition: boron trichloride 0.1%; Dichloro-dihydro silicon 0.5%; Trichlorosilane 97.7%; Silicon tetrachloride 0.5%; Tri-methyl-chlorosilane 0.1%; Phosphorus trichloride 0.1%.10 tons/hour of feed rates.
Low pressure next door rectifying tower pressure on top surface is 270kPa, and tower top temperature is 45.0 ℃, quantity of reflux/inlet amount (L/F)=13.7.
Middle pressure next door rectifying tower pressure on top surface is 500kPa, and tower top temperature is 87.1 ℃, quantity of reflux/inlet amount (L/F)=16.9.
High pressure next door rectifying tower pressure on top surface is 800kPa, and tower top temperature is 107.9 ℃, quantity of reflux/inlet amount (L/F)=20.
Each tower load is shown in following table (table two) in the trichlorosilane purification process, each tower load is shown in following table (table one) in the trichlorosilane purification process, because rectifying adopts the differential pressure coupled method, so the cooling load of the heating load of low pressure next door rectifying tower and middle pressure next door rectifying tower is complementary, the heating load of middle pressure next door rectifying tower and the cooling load of high pressure next door rectifying tower are complementary, and data are to set up required heating or cooling load behind the condensation reboiler in the bracket:
Table two
In traditional trichlorosilane purifying technique, cooling and heating total load are 49.0148M*KCAL/HR.Adopt in the technique of next door rectifying tower, total load is 43.3209M*KCAL/HR, conserve energy 11.62%.And in the next door rectifying tower technique behind the employing differential pressure coupling technique, total load is 14.4295M*KCAL/HR only, and this energy saving technology can reach 70.56%.
Can illustrate by above embodiment, with respect to traditional purifying technique, the next door rectification process of employing differential pressure heat coupling technique can be energy-conservation more than 70%.
The next door rectifying tower that the present invention proposes is used for the energy-saving technique that trichlorosilane is purified, be described by embodiment, person skilled obviously can be changed or suitably change and combination system and method as herein described within not breaking away from content of the present invention, spirit and scope, realizes technology of the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are deemed to be included in spirit of the present invention, scope and the content.
Claims (5)
1. next door thermal coupling rectificating method that is used for production of polysilicon, after it is characterized in that thick trichlorosilane raw material (8) separates through low pressure next door rectifying tower (1), top gaseous phase material (9) is divided into liquid-phase reflux material (10) and overhead extraction material (11) through overhead condenser (4) is rear according to quality reflux ratio 400 ~ 900, liquid phase material at the bottom of the tower (13) is divided into two portions, a part forms back tower steam (14) and returns low pressure next door rectifying tower (1) after mesolow tower condensation reboiler (5) heating, another part as tower at the bottom of extraction material (15), low pressure next door rectifying tower (1) the middle part highly purified trichlorosilane of side line extraction (12) then delivers into middle pressure next door rectifying tower (2); Middle pressure next door rectifying tower (2) top gaseous phase material (16) enters mesolow tower condensation reboiler (5), for mesolow tower condensation reboiler (5) is condensed into supercooled liquid after heat is provided, be 500 ~ 1000 to be divided into liquid-phase reflux material (17) and overhead extraction material (18) according to the quality reflux ratio, liquid phase material at the bottom of the tower (20) is divided into two portions, form back tower steam (22) after a part heats through mesohigh tower condensation reboiler (6) and return middle pressure next door rectifying tower (2), another part as tower at the bottom of extraction material (21), middle pressure next door rectifying tower (2) middle part side line extraction high-purity trichlorosilane (19) then delivers into high pressure next door rectifying tower (3); High pressure next door rectifying tower (3) top gaseous phase material (23) enters mesohigh tower condensation reboiler (6), for mesohigh tower condensation reboiler (6) is condensed into supercooled liquid after heat is provided, be 750 ~ 1250 to be divided into liquid-phase reflux material (24) and overhead extraction material (25) according to the quality reflux ratio, liquid phase material at the bottom of the tower (27) is divided into two portions, a part forms back tower steam (29) through tower bottom reboiler (7) post-heating and returns high pressure next door rectifying tower (3), another part as tower at the bottom of extraction material (28), high pressure next door rectifying tower (3) middle part extraction trichlorosilane products (26).
2. the method for claim 1 is characterized in that low pressure next door rectifying tower pressure on top surface is 150kPa～400kPa, and tower top temperature is 40 ℃～50 ℃, quantity of reflux/inlet amount (L/F)=8 ~ 18; Middle pressure next door rectifying tower pressure on top surface is 300kPa～500kPa, and tower top temperature is 80 ℃ ~ 95 ℃, quantity of reflux/inlet amount (L/F)=10 ~ 20; High pressure next door rectifying tower pressure on top surface 500kPa～900kPa, tower top temperature is 100 ℃ ~ 115 ℃, quantity of reflux/inlet amount (L/F)=15 ~ 25.
3. a next door thermal coupling rectifying device that is used for production of polysilicon comprises low pressure next door rectifying tower (1), overhead condenser (4), middle pressure next door rectifying tower (2), high pressure next door rectifying tower (3) and tower bottom reboiler (7); It is characterized in that arranging between two next door rectifying tower mesolow tower condensation reboiler (5) and mesohigh tower condensation reboiler (6).
4. equipment as claimed in claim 3 is characterized in that in low pressure next door rectifying tower, middle pressure next door rectifying tower and the high pressure next door rectifying tower division plate being arranged; The next door rectifying tower adopts column plate, random packing or structured packing.
5. equipment as claimed in claim 3, it is characterized in that mesolow tower condensation reboiler (5) adds thermal low next door rectifying tower (1) materials at bottom of tower and returns low pressure next door rectifying tower (1) for the steam that boils again, the top gaseous phase material with middle pressure next door rectifying tower (2) is cooled to supercooled liquid simultaneously; Mesohigh tower condensation reboiler (6) adds pines for pressing next door rectifying tower (2) materials at bottom of tower to return middle pressure next door rectifying tower (2) for the steam that boils again, and the top gaseous phase material with high pressure next door rectifying tower (3) is cooled to supercooled liquid simultaneously.
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| CN103896281A (en) * | 2014-04-17 | 2014-07-02 | 天津市华瑞奕博化工科技有限公司 | Method for rectifying and purifying silicon tetrachloride by complete thermal coupling |
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| CN103950936A (en) * | 2014-03-31 | 2014-07-30 | 中国恩菲工程技术有限公司 | Method for purifying chlorosilane through non-relevant tower differential pressure thermal coupling |
| CN106276920A (en) * | 2016-08-22 | 2017-01-04 | 中国科学院过程工程研究所 | A kind of system utilizing quadruple effect coupling rectification to purify trichlorosilane and processing method thereof |
| CN107400055A (en) * | 2017-09-05 | 2017-11-28 | 天津科技大学 | A kind of LITHIUM BATTERY dimethyl carbonate rectification and purification method and equipment |
| CN107434784A (en) * | 2016-05-25 | 2017-12-05 | 天津大学 | Non-energy-consumption reclaims the method and device of caprolactam organic extractant |
| CN107434783A (en) * | 2016-05-25 | 2017-12-05 | 天津大学 | A kind of power-economizing method and device of caprolactam system |
| CN114712877A (en) * | 2022-04-15 | 2022-07-08 | 南京佳华工程技术有限公司 | Method and equipment for preparing electronic grade gas by adopting thermal coupling technology |
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| CN103950935A (en) * | 2014-03-31 | 2014-07-30 | 中国恩菲工程技术有限公司 | System for purifying chlorosilane through non-relevant tower differential pressure thermal coupling |
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| CN107434783A (en) * | 2016-05-25 | 2017-12-05 | 天津大学 | A kind of power-economizing method and device of caprolactam system |
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Application publication date: 20130213 |