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CN102530958A - Device and method for preparing trichlorosilane - Google Patents

Device and method for preparing trichlorosilane Download PDF

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Publication number
CN102530958A
CN102530958A CN2011104326139A CN201110432613A CN102530958A CN 102530958 A CN102530958 A CN 102530958A CN 2011104326139 A CN2011104326139 A CN 2011104326139A CN 201110432613 A CN201110432613 A CN 201110432613A CN 102530958 A CN102530958 A CN 102530958A
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CN
China
Prior art keywords
silica flour
valve
high hopper
silicon powder
fly
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN2011104326139A
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Chinese (zh)
Inventor
秦永红
韩江涛
张世斌
董春青
赵建桥
王国正
马盈利
石如彦
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HENAN SHANGYU NEW ENERGY CO Ltd
Original Assignee
HENAN SHANGYU NEW ENERGY CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by HENAN SHANGYU NEW ENERGY CO Ltd filed Critical HENAN SHANGYU NEW ENERGY CO Ltd
Priority to CN2011104326139A priority Critical patent/CN102530958A/en
Publication of CN102530958A publication Critical patent/CN102530958A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a device and a method for preparing trichlorosilane. The device comprises a silicon powder delivery cabin, wherein a feed port of the silicon powder delivery cabin is connected with a silicon powder feed pipeline, a discharge port end of the silicon powder delivery cabin is provided with a discharge valve of the silicon powder delivery cabin, an outlet end of the discharge valve of the silicon powder delivery cabin is connected with a silicon powder conveying pipeline, the outlet end of the silicon powder conveying pipeline is connected with an overhead bunker, a bottom outlet of the overhead bunker is connected with a drier, the silicon powder drier is connected with a measuring tank, the measuring tank is connected with a synthetic furnace, a side outlet end of the overhead bunker is also connected with a deduster through a pipeline, and a silicon powder recovery pipeline is arranged between the deduster and the drier. The device has a simple structure, is safe and reliable, and is convenient to install and dismantle, because the conveying pipeline, the valve and the overhead bunker are reconstructed, the service lives of the conveying pipeline and the valve can be prolonged, the stopping times are reduced, the trichlorosilane production continuity is realized, meanwhile, the silicon powder waste is reduced, the environmental pollution is reduced, and the production cost is lowered.

Description

A kind of device and method of producing trichlorosilane
Technical field
The present invention relates to a kind of trichlorosilane technical field, relate in particular to a kind of device and method of producing trichlorosilane.
Background technology
The trichlorosilane products production generally generates at liquid bed formula Reaktionsofen internal reaction with industrial silica fume and hydrogen chloride gas.The conveying of primary industry silica flour adopts dense phase gas stream to carry usually.But because silica flour hardness high (Mohs' hardness is 7) is very serious to transport pipe and related valves wearing and tearing when gas delivery.If use common carbon steel pipe and plain metal seal valve, in the silica flour gas delivery, very easily be worn, a short then week in work-ing life, long only three months, cause stopping work because of pipeline or valve pipe fitting damage through regular meeting.In addition, the carbon steel piping Fe that gets off that weares and teares can get into reactive system with silica flour, and it is synthetic to influence trichlorosilane.Frequent parking maintenance makes trichlorosilane production difficulty or ease realize continuity, causes the waste of silica flour simultaneously, increases production cost.
When silica flour was carried, pressurized back got into high hopper through pipeline, and high hopper volume hour when silica flour gets into feed bin, can not get cushioning sedimentation, often causes a large amount of silica flours directly to be taken away by fly-ash separator, has increased the load of fly-ash separator.And by the silica flour that fly-ash separator absorbs, also just by the discharge of manual regular, simply pack then and reclaim, this kind working method site environment is poor, and the silica flour recovery is not thorough, causes waste.
Summary of the invention
In view of this; The purpose of this invention is to provide a kind of method of producing the device of trichlorosilane and utilizing this device to produce trichlorosilane, can prolong the work-ing life of transport pipe and valve, reduce stop frequency; Reduce the waste of silica flour; Reduce environmental pollution, realize the continuity that trichlorosilane is produced, reduce production costs.
Technical scheme of the present invention realizes with following method,
A kind of device of producing trichlorosilane comprises the silica flour sending warehouse, wherein; The opening for feed of silica flour sending warehouse is connected with the silica flour feed pipe, and the silica flour feed pipe is provided with the silica flour feed valve, and the discharge port end of silica flour sending warehouse is provided with silica flour sending warehouse bleeder valve; Silica flour sending warehouse bleeder valve exit end is connected with the silica flour transport pipe, and the pipeline intake valve is arranged on the silica flour transport pipe, and silica flour transport pipe exit end is connected with high hopper; The outlet at bottom of high hopper is provided with moisture eliminator, and moisture eliminator is connected with test tank, and test tank is connected with synthetic furnace; The side exit end of high hopper also has fly-ash separator through pipe connection; Be provided with the silica flour recovery channel between fly-ash separator and the moisture eliminator, fly-ash separator is connected with moisture eliminator through the silica flour recovery channel, and pipeline is provided with silica flour recovery channel valve; The outlet of fly-ash separator is provided with exhaust-valve, and the silica flour transport pipe adopts ceramic-lined formula composite steel tube.
Also be respectively equipped with nitrogen intake valve and aeration valve on the warehouse of silica flour sending warehouse.
The exit end of silica flour transport pipe is provided with the high hopper feed valve.
Pipeline between high hopper and the fly-ash separator is provided with vent valve.
Silica flour feed valve and silica flour sending warehouse bleeder valve all adopt the lined ceramics hard seal ball valve.
A kind of method of producing trichlorosilane, wherein, the first step, silica flour are injected silica flour in the silica flour sending warehouse by the cloth bag splendid attire;
Second step, close the silica flour feed valve, close silica flour sending warehouse bleeder valve, open the nitrogen intake valve, open aeration valve, inflated with nitrogen keeps nitrogen pressure to 0.45Mpa in the silica flour sending warehouse;
The 3rd the step, open silica flour sending warehouse bleeder valve, the pipeline intake valve, is transported to silica flour in the high hopper through silica flour transport pipe and high hopper feed valve as power with compressed nitrogen;
There is vent valve the side of the 4th step, high hopper, and vent valve links to each other with fly-ash separator, and it is negative pressure that the effect of sack cleaner makes high hopper on the one hand, is beneficial to the conveying of silica flour, is used for dedusting on the one hand, reduces environmental pollution;
Clean gas after the 5th step, the dedusting enters in the atmosphere through exhaust-valve, and the silica flour that the cloth bag filtration the gets off silica flour recovery channel valve that passes through is intermittently put into moisture eliminator with silica flour.Moisture eliminator is used for dry silica flour, and the silica flour of high hopper utilizes potential difference to flow in the moisture eliminator, and silica flour is obtained drying by the thermal source of chuck (steam or thermal conductance deep fat) heating in moisture eliminator, and drying nitrogen pressure is 5 ~ 10Kpa, and be 2-3 hour time of drying;
The 6th step, that dried silica flour utilizes potential difference to put into test tank again is subsequent use; When synthetic pressure drop in furnace diminishes, (be lower than 10-17 Kpa), open the test tank lower valve, in synthetic furnace, add silica flour; Keep the synthetic furnace normergic state; Pressure reduction is 10-17 Kpa during the synthetic furnace normal reaction, and the end or middle part temperature are 310-340 ℃, and reaction generates trichlorosilane.
The positively effect of technical scheme of the present invention is:
The present invention is simple in structure, do not damage equipment, safe and reliable, easy installation and removal, because silica flour transport pipe of the present invention adopts ceramic-lined formula composite steel tube, valve to adopt the lined ceramics hard seal ball valve, and the transformation of high hopper; Can prolong the work-ing life of transport pipe and valve; Reduce stop frequency, realize the continuity that trichlorosilane is produced, simultaneously; The silica flour that fly-ash separator absorbs is recovered in the moisture eliminator through valve; Can reduce the waste of silica flour, reduce environmental pollution, reduce production costs.
Description of drawings
Fig. 1 is a structural representation of the present invention.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is further specified.
Can find out that by Fig. 1 the device of this production trichlorosilane comprises silica flour sending warehouse 1; Wherein, the opening for feed of silica flour sending warehouse 1 is connected with the silica flour feed pipe, and the silica flour feed pipe is provided with silica flour feed valve 9; Also be respectively equipped with nitrogen intake valve 8 and aeration valve 12 on the warehouse of silica flour sending warehouse 1, the discharge port end of silica flour sending warehouse 1 is provided with silica flour sending warehouse bleeder valve 10, and silica flour sending warehouse bleeder valve 10 exit end are connected with silica flour transport pipe 2; Pipeline intake valve 11 is arranged on the silica flour transport pipe 2, and silica flour transport pipe 2 exit end are connected with high hopper 3, and the exit end of silica flour transport pipe 2 is provided with high hopper feed valve 13; The outlet at bottom of high hopper 3 is provided with moisture eliminator 5, and moisture eliminator 5 is connected with test tank 6, and test tank 6 has the synthetic furnace 7 of connection; The side exit end of high hopper 3 also has fly-ash separator 4 through pipe connection; Pipeline is provided with vent valve 14, is provided with the silica flour recovery channel between fly-ash separator 4 and the moisture eliminator 5, and fly-ash separator 4 is connected with moisture eliminator 5 through the silica flour recovery channel; Pipeline is provided with silica flour recovery channel valve 15; The outlet of fly-ash separator 4 is provided with exhaust-valve 16, and silica flour transport pipe 2 adopts ceramic-lined formula composite steel tube, and silica flour feed valve 9 all adopts the lined ceramics hard seal ball valve with silica flour sending warehouse bleeder valve 10.
The method of this production trichlorosilane; The first step, silica flour are by the cloth bag splendid attire; Each bag is one ton, and the manual operation electricblock winched to silica flour in the silica flour feeding bin directly over the silica flour sending warehouse 1 before this, utilized potential difference through valve 9 silica flour to be put into silica flour sending warehouse 1 again.Second the step, close silica flour feed valve 9, close silica flour sending warehouse bleeder valve 10, open nitrogen intake valve 8; Open aeration valve 12, to 0.45Mpa, keep nitrogen pressure toward the interior inflated with nitrogen of silica flour sending warehouse; The 3rd goes on foot, opens silica flour sending warehouse bleeder valve 10; Pipeline intake valve 11, is transported to silica flour in the high hopper 3 through silica flour transport pipe 2 and high hopper feed valve 13 as power with compressed nitrogen.There is vent valve 14 side of the 4th step, high hopper 3, and vent valve 14 links to each other with fly-ash separator 4, and it is negative pressure that the effect of sack cleaner makes high hopper on the one hand, is beneficial to the conveying of silica flour, is used for dedusting on the one hand, reduces environmental pollution.Clean gas after the 5th step, the dedusting enters in the atmosphere through exhaust-valve 16, and the silica flour that the cloth bag filtration the gets off silica flour recovery channel valve 15 that passes through is intermittently put into moisture eliminator 5 with silica flour.Moisture eliminator 5 is used for dry silica flour, and the silica flour of high hopper utilizes potential difference to flow in the moisture eliminator 5, and silica flour is heated by the thermal conductance deep fat of chuck moisture eliminator 5 in and obtains drying, and drying nitrogen pressure is 10Kpa, and be 3 hours time of drying.The 6th step, that dried silica flour utilizes potential difference to put into test tank 6 again is subsequent use, when synthetic pressure drop in furnace diminishes, (is lower than 10-17 Kpa), opens the test tank lower valve, in synthetic furnace 7, adds silica flour, keeps synthetic furnace 7 normergic states.Pressure reduction is 10-17 Kpa during synthetic furnace 7 normal reactions, and the end or middle part temperature are 310-340 ℃, and reaction generates trichlorosilane.

Claims (6)

1. a device of producing trichlorosilane comprises silica flour sending warehouse (1), it is characterized in that: the opening for feed of silica flour sending warehouse (1) is connected with the silica flour feed pipe; The silica flour feed pipe is provided with silica flour feed valve (9); The discharge port end of silica flour sending warehouse (1) is provided with silica flour sending warehouse bleeder valve (10), and silica flour sending warehouse bleeder valve (10) exit end is connected with silica flour transport pipe (2), and pipeline intake valve (11) is arranged on the silica flour transport pipe (2); Silica flour transport pipe (2) exit end is connected with high hopper (3); The outlet at bottom of high hopper (3) is provided with moisture eliminator (5), and moisture eliminator (5) is connected with test tank (6), and test tank (6) is connected with synthetic furnace (7); The side exit end of high hopper (3) also has fly-ash separator (4) through pipe connection; Be provided with the silica flour recovery channel between fly-ash separator (4) and the moisture eliminator (5), fly-ash separator (4) is connected with moisture eliminator (5) through the silica flour recovery channel, and pipeline is provided with silica flour recovery channel valve (15); The outlet of fly-ash separator (4) is provided with exhaust-valve (16), and silica flour transport pipe (2) adopts ceramic-lined formula composite steel tube.
2. a kind of device of producing trichlorosilane according to claim 1 is characterized in that: also be respectively equipped with nitrogen intake valve (8) and aeration valve (12) on the warehouse of silica flour sending warehouse (1).
3. a kind of device of producing trichlorosilane according to claim 1 is characterized in that: the exit end of silica flour transport pipe (2) is provided with high hopper feed valve (13).
4. a kind of device of producing trichlorosilane according to claim 1 is characterized in that: the pipeline between high hopper (3) and the fly-ash separator (4) is provided with vent valve (14).
5. a kind of device of producing trichlorosilane according to claim 1 is characterized in that: silica flour feed valve (9) and silica flour sending warehouse bleeder valve (10) all adopt the lined ceramics hard seal ball valve.
6. method of producing trichlorosilane, it is characterized in that: the first step, silica flour are injected silica flour in the silica flour sending warehouse (1) by the cloth bag splendid attire;
Second the step, close silica flour feed valve (9), close silica flour sending warehouse bleeder valve (10), open nitrogen intake valve (8), open aeration valve (12), toward interior the inflated with nitrogen of silica flour sending warehouse (1) to 0.45Mpa, the maintenance nitrogen pressure;
The 3rd the step, open silica flour sending warehouse bleeder valve (10), pipeline intake valve (11), is transported to silica flour in the high hopper (3) through silica flour transport pipe (2) and high hopper feed valve (13) as power with compressed nitrogen;
There is vent valve (14) side of the 4th step, high hopper (3); Vent valve (14) links to each other with fly-ash separator (4), and the effect of fly-ash separator makes high hopper (3) be negative pressure on the one hand, is beneficial to the conveying of silica flour; Be used for dedusting on the one hand, reduce environmental pollution;
Clean gas after the 5th step, the dedusting enters in the atmosphere through exhaust-valve (16); The silica flour that the cloth bag filtration the gets off silica flour recovery channel valve (15) that passes through is intermittently put into moisture eliminator (5) with silica flour; Moisture eliminator (5) is used for dry silica flour, and the silica flour of high hopper (3) utilizes potential difference to flow in the moisture eliminator (5), and silica flour is heated by the steam of chuck or thermal conductance deep fat moisture eliminator (5) in and obtains drying; Drying nitrogen pressure is 5 ~ 10Kpa, and be 2-3 hour time of drying;
The 6th step, that dried silica flour utilizes potential difference to put into test tank (6) again is subsequent use; When pressure reduction diminishes in the synthetic furnace (7), be lower than 10-17 Kpa, open the test tank lower valve, in synthetic furnace (7), add silica flour; Keep synthetic furnace (7) normergic state; Pressure reduction is 10-17 Kpa during synthetic furnace (7) normal reaction, and the end or middle part temperature are 310-340 ℃, and reaction generates trichlorosilane.
CN2011104326139A 2011-12-21 2011-12-21 Device and method for preparing trichlorosilane Pending CN102530958A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2011104326139A CN102530958A (en) 2011-12-21 2011-12-21 Device and method for preparing trichlorosilane

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2011104326139A CN102530958A (en) 2011-12-21 2011-12-21 Device and method for preparing trichlorosilane

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CN2011104326139A Pending CN102530958A (en) 2011-12-21 2011-12-21 Device and method for preparing trichlorosilane

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103408022A (en) * 2013-07-08 2013-11-27 昆明冶研新材料股份有限公司 Silicon powder conveying equipment and system with same for synthesizing trichlorosilane

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008184378A (en) * 2007-01-31 2008-08-14 Osaka Titanium Technologies Co Ltd Method for producing high-purity trichlorosilane
US20100032630A1 (en) * 2008-08-04 2010-02-11 Hariharan Alleppey V Recovery of silicon from kerf silicon waste
CN101920963A (en) * 2010-08-23 2010-12-22 湖北新蓝天新材料股份有限公司 Silica powder drying and charging method in trichlorosilane production process
CN202297152U (en) * 2011-09-30 2012-07-04 河南尚宇新能源股份有限公司 Device for reducing consumption of silica powder in trichlorosilane production process

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008184378A (en) * 2007-01-31 2008-08-14 Osaka Titanium Technologies Co Ltd Method for producing high-purity trichlorosilane
US20100032630A1 (en) * 2008-08-04 2010-02-11 Hariharan Alleppey V Recovery of silicon from kerf silicon waste
CN101920963A (en) * 2010-08-23 2010-12-22 湖北新蓝天新材料股份有限公司 Silica powder drying and charging method in trichlorosilane production process
CN202297152U (en) * 2011-09-30 2012-07-04 河南尚宇新能源股份有限公司 Device for reducing consumption of silica powder in trichlorosilane production process

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103408022A (en) * 2013-07-08 2013-11-27 昆明冶研新材料股份有限公司 Silicon powder conveying equipment and system with same for synthesizing trichlorosilane
CN103408022B (en) * 2013-07-08 2016-03-30 昆明冶研新材料股份有限公司 Silica flour transmission equipment and there is its system of synthesizing trichlorosilane

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Application publication date: 20120704