CN101766942B - Trichlorosilane de-dusting device and de-dusting process - Google Patents
Trichlorosilane de-dusting device and de-dusting process Download PDFInfo
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- CN101766942B CN101766942B CN2010100113016A CN201010011301A CN101766942B CN 101766942 B CN101766942 B CN 101766942B CN 2010100113016 A CN2010100113016 A CN 2010100113016A CN 201010011301 A CN201010011301 A CN 201010011301A CN 101766942 B CN101766942 B CN 101766942B
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Abstract
The invention discloses a trichlorosilane de-dusting device and a de-dusting process. The de-dusting device comprises a scrubbing tower, wherein the lower part of the scrubbing tower is provided with a synthetic gas feeding pipe, and the upper part thereof is provided with a synthetic gas discharge pipe; the scrubbing tower is connected with a silicon tetrachloride addition device; the synthetic gas flowing out of a synthetic furnace is de-dusted by a cloth bag and then is de-dusted by adopting the wet method; during the wet-method de-dusting, the spraying process is adopted, and silicon tetrachloride that is the by-product in the trichlorosilane process is adopted as a detergent, therefore, the silicon tetrachloride that is the by-product generated by the trichlorosilane can be recycled, so that the silicon tetrachloride can be well utilized, so as to meet the environmental requirement; and the problems that the pipeline is blocked by aluminium choride and ferric trichloride can be also solved. The invention can reduce the blocking degree of the device and the pipeline caused by the subsequent material in the condensation process of a main condensator to the utmost limit and can prolong the period of stable operation, thereby greatly improving the safety and the continuity of the production of a system.
Description
Technical field
The present invention relates to a kind of trichlorosilane cleaner, can in trichlorosilane is produced, remove impurity such as in silica flour, containing aluminium, iron, the invention still further relates to the production technology of this cleaner, belong to chemical technology field.
Background technology
In trichlorosilane is produced owing in silica flour, contain impurity such as aluminium, iron, with the HCL reaction engineering in, generate alchlor, ferric trichloride is very easy to stop up the follow-up system pipeline, cause the instability, discontinuous of whole production system.Trichlorosilane manufacturer is provided with 2-4 platform forecooler at present, and the cooling of the chloride of aluminium, iron in forecooler, is cleared up a forecooler weekly and solved the system pipeline blocking problem.The periodic cleaning forecooler, dangerous height, equipment operating cost increase, and consumption manpower consumption material resources are unfavorable for the continous-stable operation of producing.
Summary of the invention
The problem to be solved in the present invention provides a kind of security of can resolution system stopping up, improving whole trichlorosilane technology greatly, can make and produce the trichlorosilane cleaner that continous-stable carries out, and the present invention also provides the dust collecting process of this cleaner.
For addressing the above problem, the present invention institute by the following technical solutions:
A kind of trichlorosilane cleaner comprises the tower of giving a dinner of welcome, and the bottom of the tower of giving a dinner of welcome is provided with the forming gas inlet pipe, and top is provided with forming gas and goes out pipe, and it is characterized in that: the described tower of giving a dinner of welcome is connected with the silicon tetrachloride adding set.
Below be further improvement of these options of the present invention:
The silicon tetrachloride adding set comprises the first circulation flow container that is connected with the tower of giving a dinner of welcome by pipeline, the first circulation flow container is provided with first circulation fluid and goes out pipe, this first circulation fluid goes out pipe and is connected with first circulating pump, first circulating pump is provided with first circulation and pumps pipe, and this first circulation is pumped pipe and is communicated with the top of the tower of giving a dinner of welcome.
As further improvement:
Described forming gas goes out the forming gas cooling device is installed on the pipe, and this cooling device comprises overhead condenser, is provided with chilled brine outlet pipe, chilled brine water inlet pipe, gas phase extraction pipeline and condensed water and goes out pipe on overhead condenser.
Further improve:
Described condensed water goes out pipe and is provided with condensed water circulation device, and this EGR comprises and is connected with second circulating tank, is provided with second circulation fluid and goes out pipe on second circulating tank, and this second circulation fluid goes out pipe and is communicated with by the top of second circulating pump with the tower of giving a dinner of welcome.
The liquid that condensation has been descended enters second circulating tank, to replenish the silicon tetrachloride of the loss that is in the suds.
Further improve:
Described first circulation is pumped and is connected with the gaseous phase materials vaporising device on the pipe, this vaporising device comprises agitator tank, be provided with agitating device in the agitator tank, be provided with heating steam inlet pipe and gaseous phase materials recurrent canal on agitator tank top, described gaseous phase materials recurrent canal is communicated with the bottom of the tower of giving a dinner of welcome, and is provided with in the agitator tank bottom that steam condensate (SC) goes out pipe and material goes out to manage.
Described material goes out to be connected with the material hydrolysis device on the pipe, and material hydrolysis device and material go out to be provided with device for transporting objects between the pipe.
Device for transporting objects comprises with material going out to manage the feed bin that is communicated with, and is provided with screw feeder below feed bin, and the outlet of screw feeder is connected with the material hydrolysis device.
The material hydrolysis device comprises the hydrolytic decomposition pot that is communicated with the outlet of screw feeder by pipeline, and the top of hydrolytic decomposition pot is provided with the alkali lye inlet pipe, tail gas goes out pipe and recirculated water goes out pipe, is provided with recirculated water inlet pipe and slag charge in the bottom of hydrolytic decomposition pot and goes out pipe.
A kind of dust collecting process of trichlorosilane cleaner, this technology may further comprise the steps:
A, at first add the silicon tetrachloride material in the first circulation flow container, the second circulation flow container, liquid level is 30-70%, and opens first circulating pump and second circulating pump, liquid idle loop in the beginning tower;
B, the chilled brine water inlet pipe of opening overhead condenser and chilled brine outlet pipe make the work of chilled brine normal circulation;
C, open the forming gas inlet pipe, forming gas is entered give a dinner of welcome tower and flow from bottom to top, the silicon tetrachloride that enters the tower of giving a dinner of welcome from first circulating pump and second circulating pump sprays downwards from the top of the tower of giving a dinner of welcome, and finishes the dedusting to forming gas.
This technology is further comprising the steps of:
D, the partial material that flows out from first circulating pump enter agitator tank, treat a jar interior liquid level reach-during %, slowly put into heating steam by the heating steam inlet pipe material evaporated, the gaseous phase materials that evaporates returns the tower bottom of giving a dinner of welcome by the gaseous phase materials recurrent canal;
Material in E, the agitator tank goes out pipe through material and enters feed bin, enter into hydrolytic decomposition pot through screw feeder, open the alkali lye inlet pipe then, put into 20-30% sodium hydroxide lye, make material obtain hydrolysis, the qualified material after the hydrolysis goes out tube drainage to the silica flour slag bath by slag charge.
The synthesis gas that comes out in the synthetic furnace, entering wet dedusting again through behind the bag-type dust, tower spray technology is adopted in wet dedusting, adopt the silicon tetrachloride as by-product in the trichlorosilane technology to make washing agent, so both can be recycling the silicon tetrachloride as by-product produced of trichlorosilane, silicon tetrachloride can well be utilized, meet environmental protection requirement, can solve the difficult problem of alchlor, ferric trichloride blocking pipe again.The present invention removes the more tiny solid dust of part of failing to remove in the forming gas in operations such as preceding road whirlwind, sedimentation, bag filtering dust collecting by the method for spray, reduce the equipment that follow-up material causes and the chocking-up degree of pipeline to greatest extent in the main condenser condensation process, prolong the stable operation cycle, improved security, continuity that system produces greatly.
The invention will be further described below in conjunction with drawings and Examples:
Description of drawings
Accompanying drawing is the process chart of the embodiment of the invention.
Among the figure: the 1-overhead condenser; 2-chilled brine outlet pipe; 3-gas phase extraction pipeline; 4-chilled brine water inlet pipe; The 5-tower of giving a dinner of welcome; 6-second circulating tank; 7-second circulating pump; The 8-agitator tank; 9-heating steam inlet pipe; The 10-steam condensate (SC) goes out pipe; The 11-feed bin; The 12-screw feeder; The 13-hydrolytic decomposition pot; 14-alkali lye inlet pipe; 15-tail gas goes out pipe; 16-recirculated water goes out pipe; 17-recirculated water inlet pipe; The 18-slag charge goes out pipe; 19-first circulating pump; The 20-first circulation flow container; 21-forming gas inlet pipe; The 22-forming gas goes out pipe; The 23-condensed water goes out pipe; Pipe is pumped in 24-first circulation; 25-gaseous phase materials recurrent canal; 26-first circulation fluid goes out pipe; 27-second circulation fluid goes out pipe; The 28-material goes out pipe.
The specific embodiment
Embodiment, as shown in the figure, a kind of trichlorosilane cleaner, comprise the tower 5 of giving a dinner of welcome, the give a dinner of welcome bottom of tower 5 is provided with forming gas inlet pipe 21, top is provided with forming gas and goes out pipe 22, the described tower 5 of giving a dinner of welcome is connected with the silicon tetrachloride adding set, the silicon tetrachloride adding set comprises the first circulation flow container 20 that is connected with the tower 5 of giving a dinner of welcome by pipeline, the first circulation flow container 20 is provided with first circulation fluid and goes out pipe 26, this first circulation fluid goes out pipe 26 and is connected with first circulating pump 19, first circulating pump 19 is provided with first circulation and pumps pipe 24, this first circulation is pumped pipe 24 and is communicated with the top of the tower 5 of giving a dinner of welcome, described forming gas goes out on the pipe 22 the forming gas cooling device is installed, this cooling device comprises overhead condenser 1, on overhead condenser 1, be provided with chilled brine outlet pipe 2, chilled brine water inlet pipe 4, gas phase extraction pipeline 3 and condensed water go out pipe 23, described condensed water goes out pipe 23 and is provided with condensed water circulation device, this EGR comprises and is connected with second circulating tank 6, be provided with second circulation fluid and go out pipe 27 on second circulating tank 6, this second circulation fluid goes out pipe 27 and is communicated with by the top of second circulating pump 7 with the tower 5 of giving a dinner of welcome.The liquid that condensation is got off enters second circulating tank, to replenish the silicon tetrachloride of the loss that is in the suds.
Described first circulation is pumped on the pipe 24 and is connected with the gaseous phase materials vaporising device, this vaporising device comprises agitator tank 8, be provided with agitating device in the agitator tank 8, be provided with heating steam inlet pipe 9 and gaseous phase materials recurrent canal 25 on agitator tank 8 tops, described gaseous phase materials recurrent canal 25 is communicated with the bottom of the tower 5 of giving a dinner of welcome, be provided with in agitator tank 8 bottoms that steam condensate (SC) goes out pipe 10 and material goes out pipe 28, described material goes out on the pipe 28 to be connected with the material hydrolysis device, and material hydrolysis device and material go out between the pipe 28 to be provided with device for transporting objects.
Device for transporting objects comprises with material going out to manage 28 feed bins that are communicated with 11, is provided with screw feeder 12 below feed bin 11, and the outlet of screw feeder 12 is connected with the material hydrolysis device.
The material hydrolysis device comprises the hydrolytic decomposition pot 13 that is communicated with the outlet of screw feeder 12 by pipeline, and the top of hydrolytic decomposition pot 13 is provided with alkali lye inlet pipe 14, tail gas goes out pipe 15 and recirculated water goes out pipe 16, is provided with recirculated water inlet pipe 17 and slag charge in the bottom of hydrolytic decomposition pot 13 and goes out pipe 18.
The dust collecting process of above-mentioned dust arrester may further comprise the steps: at first add silicon tetrachloride or mix the trichlorosilane material in the first circulation flow container 20, the second circulation flow container 6, liquid level is 30-70%, and open first circulating pump 19 and second circulating pump 7, begin liquid idle loop in the tower; Open the chilled brine water inlet pipe 4 and the chilled brine outlet pipe 2 of overhead condenser 1, make the work of chilled brine normal circulation; Adjusting is installed in the valve opening on the chilled brine outlet pipe 2, make the overhead condensation amount reach a desired value, under normal operation, the temperature and pressure of each point is answered kept stable on the tower, note the overhead reflux quantitative changeization simultaneously, whether look handleless cup observation cat head condensate liquid from cat head often limpid transparent, whether solid suspension is arranged, if liquid is not when clarifying, can suitably strengthen overhead condensation liquid capacity of returns, strengthen the effect of giving a dinner of welcome and open forming gas inlet pipe 21, forming gas is entered give a dinner of welcome tower 5 and flow from bottom to top, the temperature and pressure of noting each point simultaneously changes, the silicon tetrachloride that enters the tower 5 of giving a dinner of welcome from first circulating pump 19 and second circulating pump 7 sprays downwards from the top of the tower 5 of giving a dinner of welcome, and finishes the dedusting to forming gas.
The partial material that flows out from first circulating pump 19 enters agitator tank 8, when treating that a jar interior liquid level reaches 30-50%, slowly put into heating steam by heating steam inlet pipe 9 material is evaporated, the gaseous phase materials that evaporates returns the tower bottom of giving a dinner of welcome by gaseous phase materials recurrent canal 25; Gaseous phase materials in the agitator tank returns the front and back in the tower of giving a dinner of welcome, and notices that each point temperature in the tower, pressure change, and adjusts overhead reflux amount size at any time, keeps system stability.
Material in the agitator tank 8 goes out pipe 28 through material and enters feed bin 11, enter into hydrolytic decomposition pot 13 through screw feeder 12, open alkali lye inlet pipe 14 then, the sodium hydroxide lye of putting into 20-30% makes material obtain hydrolysis, alkali lye can be prepared in hydrolytic decomposition pot 13 in advance, also can directly use the finished product liquid caustic soda as hydrolyzate, material after the hydrolysis measure pH value for ~ 8-10 is qualified, the qualified material after the hydrolysis goes out to manage 18 by slag charge and is discharged into the silica flour slag bath.
When the tower of giving a dinner of welcome stops, require to stop gas-phase feed earlier, close chilled brine again after stablizing 1～2h.
Claims (7)
1. a trichlorosilane cleaner comprises the tower of giving a dinner of welcome (5), and the bottom of the tower of giving a dinner of welcome (5) is provided with forming gas inlet pipe (21), and top is provided with forming gas and goes out pipe (22), and it is characterized in that: the described tower of giving a dinner of welcome (5) is connected with the silicon tetrachloride adding set;
The silicon tetrachloride adding set comprises the first circulation flow container (20) that is connected with the tower of giving a dinner of welcome (5) by pipeline, the first circulation flow container (20) is provided with first circulation fluid and goes out pipe (26), this first circulation fluid goes out pipe (26) and is connected with first circulating pump (19), first circulating pump (19) is provided with first circulation and pumps pipe (24), and this first circulation is pumped pipe (24) and is communicated with the top of the tower of giving a dinner of welcome (5);
Described forming gas goes out on the pipe (22) the forming gas cooling device is installed, this cooling device comprises overhead condenser (1), is provided with chilled brine outlet pipe (2), chilled brine water inlet pipe (4), gas phase extraction pipeline (3) and condensed water and goes out pipe (23) on overhead condenser (1);
It is characterized in that: described condensed water goes out pipe (23) and is provided with condensed water circulation device, this EGR comprises second circulating tank (6), be provided with second circulation fluid and go out pipe (27) on second circulating tank (6), this second circulation fluid goes out pipe (27) and is communicated with by the top of second circulating pump (7) with the tower of giving a dinner of welcome (5).
2. a kind of trichlorosilane cleaner according to claim 1, it is characterized in that: described first circulation is pumped on the pipe (24) and is connected with the gaseous phase materials vaporising device, this gaseous phase materials vaporising device comprises agitator tank (8), agitator tank is provided with agitating device in (8), be provided with heating steam inlet pipe (9) and gaseous phase materials recurrent canal (25) on agitator tank (8) top, described gaseous phase materials recurrent canal (25) is communicated with the bottom of the tower of giving a dinner of welcome (5), is provided with in agitator tank (8) bottom that steam condensate (SC) goes out pipe (10) and material goes out to manage (28).
3. a kind of trichlorosilane cleaner according to claim 2 is characterized in that: described material goes out on the pipe (28) to be connected with the material hydrolysis device, and material hydrolysis device and material go out between the pipe (28) to be provided with device for transporting objects.
4. a kind of trichlorosilane cleaner according to claim 3, it is characterized in that: device for transporting objects comprises with material and goes out the feed bin (11) that pipe (28) is communicated with, be provided with screw feeder (12) in the below of feed bin (11), the outlet of screw feeder (12) is connected with the material hydrolysis device.
5. a kind of trichlorosilane cleaner according to claim 4, it is characterized in that: the material hydrolysis device comprises the hydrolytic decomposition pot (13) that is communicated with the outlet of screw feeder (12) by pipeline, the top of hydrolytic decomposition pot (13) is provided with alkali lye inlet pipe (14), tail gas goes out pipe (15) and recirculated water goes out pipe (16), is provided with recirculated water inlet pipe (17) and slag charge in the bottom of hydrolytic decomposition pot (13) and goes out pipe (18).
6. the dust collecting process of a trichlorosilane cleaner, it is characterized in that: this technology may further comprise the steps:
A, at first add the silicon tetrachloride material in the first circulation flow container (20), the second circulation flow container (6), liquid level is 30-70%, and opens first circulating pump (19) and second circulating pump (7), the interior liquid idle loop of beginning tower;
B, the chilled brine water inlet pipe (4) of opening overhead condenser (1) and chilled brine outlet pipe (2) make the work of chilled brine normal circulation;
C, open forming gas inlet pipe (21), forming gas is entered give a dinner of welcome tower (5) and flow from bottom to top, the silicon tetrachloride that enters the tower of giving a dinner of welcome (5) from first circulating pump (19) and second circulating pump (7) sprays downwards from the top of the tower of giving a dinner of welcome (5), finishes the dedusting to forming gas.
7. the dust collecting process of a kind of trichlorosilane cleaner according to claim 6 is characterized in that: this technology is further comprising the steps of:
D, the partial material that flows out from first circulating pump (19) enter agitator tank (8), when treating that a jar interior liquid level reaches 30-50%, slowly put into heating steam by heating steam inlet pipe (9) material is evaporated, the gaseous phase materials that evaporates returns the tower bottom of giving a dinner of welcome by gaseous phase materials recurrent canal (25);
Material in E, the agitator tank (8) goes out pipe (28) through material and enters feed bin (11), enter into hydrolytic decomposition pot (13) through screw feeder (12), open alkali lye inlet pipe (14) then, put into 20-30% sodium hydroxide lye, make material obtain hydrolysis, the qualified material after the hydrolysis goes out pipe (18) by slag charge and is discharged into the silica flour slag bath.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010100113016A CN101766942B (en) | 2010-01-04 | 2010-01-04 | Trichlorosilane de-dusting device and de-dusting process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010100113016A CN101766942B (en) | 2010-01-04 | 2010-01-04 | Trichlorosilane de-dusting device and de-dusting process |
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| Publication Number | Publication Date |
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| CN101766942A CN101766942A (en) | 2010-07-07 |
| CN101766942B true CN101766942B (en) | 2011-09-14 |
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| CN2010100113016A Active CN101766942B (en) | 2010-01-04 | 2010-01-04 | Trichlorosilane de-dusting device and de-dusting process |
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| CN103170206A (en) * | 2011-12-20 | 2013-06-26 | 西安航天远征流体控制股份有限公司 | Method for removing silicon powder in reaction gas in hydrogenation process by venturi scrubber |
| CN102794070B (en) * | 2012-07-25 | 2014-12-10 | 新疆大全新能源有限公司 | Processing method for trichlorosilane gas |
| CN103693649B (en) * | 2013-11-25 | 2016-02-17 | 新特能源股份有限公司 | The removal of impurities of synthetic gas production technique and useless chlorosilane liquid produced recovery method |
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Owner name: SHANDONG XINLONG TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: SHANDONG XINLONG SILICAS INDUSTRY SCIENCE AND TECHNOLOGY CO., LTD. Effective date: 20140212 |
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Free format text: CORRECT: ADDRESS; FROM: 262700 WEIFANG, SHANDONG PROVINCE TO: 262709 WEIFANG, SHANDONG PROVINCE |
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Effective date of registration: 20140212 Address after: 262709 New Dragon Industrial Zone, Shouguang City, Shandong Patentee after: Shandong Xinlong Technology Co., Ltd. Address before: 262700 New Dragon Industrial Zone, Shouguang City, Shandong Patentee before: Shandong Xinlong Silicas Industry Science and Technology Co., Ltd. |