CN105776224A - Method for washing rectifying column reboiler - Google Patents
Method for washing rectifying column reboiler Download PDFInfo
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- CN105776224A CN105776224A CN201610151505.7A CN201610151505A CN105776224A CN 105776224 A CN105776224 A CN 105776224A CN 201610151505 A CN201610151505 A CN 201610151505A CN 105776224 A CN105776224 A CN 105776224A
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- China
- Prior art keywords
- rectifying column
- silicon chloride
- reboiler
- chloride
- silicon tetrachloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/10778—Purification
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The invention relates to a method for washing a rectifying column reboiler. The method includes the steps of (1), when the reboiler is blocked and vapor-liquid load of a rectifying column is decreased to the minimum, enabling the rectifying column to stop running; (2), discharging a mixture containing trichlorosilane, silicon tetrachloride and metal chlorides in the rectifying column to a raw material storage tank; (3), when liquid level of a column bottom decreases to 5%, stopping discharge and supplementing fresh liquid-phase silicon tetrachloride; when the liquid level of the column bottom rises to 80%, stopping supplementing the fresh liquid-phase silicon tetrachloride and starting to heat to increase temperature while turning on a condenser so as to enable the rectifying column to be in total-reflux operation; (4), when impurity content of the silicon tetrachloride in the column bottom decreases to 0.02%, stopping heating; (5), when temperature of the column bottom decreases to 80 DEG C, discharging the silicon tetrachloride and the metal chlorides dissolved in the silicon tetrachloride and pressurizing by nitrogen; when pressure of the rectifying column reaches 0.3 MPa, relieving pressure and replacing all the silicon tetrachloride by means of purging so as to start up the rectifying column normally. The method for washing the rectifying column reboiler has the advantages of high efficiency, rapidity and environmental protection.
Description
Technical field
The present invention relates to technical field of polysilicon production, particularly relate to a kind of method cleaning rectifying column reboiler.
Background technology
Production of polysilicon 90% is all use improved Siemens, and whole industry faces reduces cost and the dual-pressure of protection environment, how to realize reducing cost, reduces environmental pollution, become the basic of enterprise development.Trichlorosilane is the primary raw material of production of polysilicon, and by the method for rectification and purification, obtains the key that highly purified trichlorosilane is production of polysilicon, and the purity of trichlorosilane directly affects polysilicon product quality.Owing to using silica flour in the hydrogenated raw material of trichlorosilane, the metallic chloride impurities in silica flour is higher, and in chlorosilane production process, owing to temperature is higher, can produce a part of high chlorosilane.Rectification and purification process is a complicated physical process, rectifying column material in tower reactor in running constantly concentrates, chlorosilane and other metal chloride concentration can be gradually increased, originally it is dissolved in the parsing of the impurity in chlorosilane and becomes the solid matter that viscosity is very big, it is adsorbed on the tube wall of reboiler, affects reboiler and normally conduct heat.In order to ensure the properly functioning of tower, it is necessary to being stopped by rectifying column, open reboiler and be carried out, the cleaning for reboiler does not have good treating method so far.
Processing method conventional at present is after being stopped by rectifying column, qualified through nitrogen displacement, open reboiler end socket, it is rinsed with water, when blocking serious, must use pneumatic brill that tube bank is dredged, when using pneumatic brill, it is likely to tube bank is caused damage, shorten reboiler service life, meet air due to chlorosilane and moisture can react, produce smog, cleaning process also can produce substantial amounts of waste water and solid slag, environment is produced very big noxious waste pollution and exhaust emission, and impurity through reaction after on reboiler tube wall adhesive force can strengthen, add the difficulty of cleaning, the general cleaning reboiler time is 3 ~ 5 days.
Chinese patent 200620170299.6 discloses a kind of rectifying column and reduces the forced circulation system of reboiler polymerization, rectifying column, reboiler and tower reactor forced circulation pump, by the forced circulation of kettle material, improve material velocity of liquid assets in reboiler, reduce residence time of material, reduce the polymerization of material.In this patent, device is all more complicated, adds kettle material circulating pump, causes system running pressure high owing to system carries out supercharging, owing to chlorosilane has the characteristics such as inflammable and explosive, adds hidden danger and operating cost that system complete stability runs.
Summary of the invention
The technical problem to be solved be to provide a kind of efficiently, quickly, the method cleaning rectifying column reboiler of environmental protection.
For solving the problems referred to above, a kind of method cleaning rectifying column reboiler of the present invention, comprise the following steps:
(1) after reboiler blocks, the vapour-liquid load reduction of rectifying column, when being down to the minimum vapour-liquid load of design, stops described rectifying column；
(2) the mixture that tower is contained within trichlorosilane, Silicon chloride. and metal chloride is all expelled to raw material storage tank at 85 DEG C by tower reactor extraction pipeline, is continuing with when again driving；
(3) stop extraction when tower bottoms position is reduced to 5%, and in tower, supplement fresh liquid phase Silicon chloride. by rectifying column feeding line；When tower reactor liquid level is increased to 80%, stops supplementing fresh liquid phase Silicon chloride., and start to pass into steam to described reboiler, be heated heating up to the Silicon chloride. of described tower bottom of rectifying tower, open condenser simultaneously, make described rectifying column carry out total reflux operation；
(4) when bottom temperature is at 100 DEG C ~ 120 DEG C, Silicon chloride. circulation time 2.5 hours first, in sample analysis Silicon chloride., impurity content improves 2%, again supplements fresh liquid phase Silicon chloride., circulation time 3 hours, sample analysis, in Silicon chloride., impurity content is reduced to 4%, and third time supplements fresh liquid phase Silicon chloride., after circulating 4 hours, sample analysis, in tower reactor, Silicon chloride. impurity content is reduced to 0.02%, stops heating；
(5), when bottom temperature is down to 80 DEG C, after Silicon chloride. and the metal chloride that is dissolved in Silicon chloride. all being discharged by floss hole, use nitrogen pressurising；When described Rectification column pressure reaches 0.3MPa by described floss hole pressure release, and the Silicon chloride. in tower reactor and pipeline is all purged totally, make Silicon chloride. all replace, can normally drive to run.
Described step (3) in fresh liquid phase Silicon chloride. refer to and use reduction furnace to produce and through the Silicon chloride. that trichlorosilane content is less than 0.05%, silica flour content is less than 0.01% of separating-purifying.
Described step (1) middle reboiler refers to shell-and-tube or thermosyphon reboiler, and wherein tube side is material, and shell side is for solving thermal medium.
The present invention compared with prior art has the advantage that
1, after the present invention uses Silicon chloride. to heat up, material constantly circulates, and is softened by the solid impurity on reboiler tube wall, dissolves, and is discharged by residual liquid, reaches to clean the purpose of reboiler.
2, in the present invention trichlorosilane content of fresh liquid phase Silicon chloride. less than 0.05%, silica flour content less than 0.01%, to increase impurity dissolubility in Silicon chloride..
3, the present invention is in cleaning reboiler process, is first all discharged at a higher temperature by material significantly high for tower reactor impurity content, reduces material and resolves, to reduce the Matter Transfer time.
4, the present invention not only makes the scavenging period of rectifying column reboiler shorten, operate simpler, and reduce the risk of the device damage cleaning reboiler use impact brill and cause, extend service life of equipment, reduce production of polysilicon cost simultaneously, reduce the discharge of waste gas, waste water, reduce environmental pollution, economy, environmental benefit are notable, it is ensured that device can long-term safety, stable, run continuously.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
Fig. 1 is the structural representation of the present invention.
In figure: 1-rectifying column feeding line, 2-reboiler, 3-rectifying column, 4-condenser, 5-tower reactor extraction pipeline, 6-floss hole.
Detailed description of the invention
As it is shown in figure 1, a kind of method cleaning rectifying column reboiler, comprise the following steps:
(1) after reboiler 2 blocks, the vapour-liquid load reduction of rectifying column 3, when being down to the minimum vapour-liquid load of design, stops rectifying column 3.
Wherein: reboiler 2 refers to shell-and-tube or thermosyphon reboiler, wherein tube side is material, and shell side is for solving thermal medium.
(2) the mixture that tower is contained within trichlorosilane, Silicon chloride. and metal chloride is all expelled to raw material storage tank at 85 DEG C by tower reactor extraction pipeline 5, is continuing with when again driving.
(3) stop extraction when tower bottoms position is reduced to 5%, and in tower, supplement fresh liquid phase Silicon chloride. by rectifying column feeding line 1；When tower reactor liquid level is increased to 80%, stops supplementing fresh liquid phase Silicon chloride., and start to pass into steam to reboiler 2, be heated heating up to the Silicon chloride. of rectifying column 3 tower reactor, open condenser 4 simultaneously, make rectifying column 3 carry out total reflux operation.
Wherein: fresh liquid phase Silicon chloride. refers to and uses reduction furnace generation and the Silicon chloride. that trichlorosilane content is less than 0.05%, silica flour content is less than 0.01% through separating-purifying.
(4) when bottom temperature is at 100 DEG C ~ 120 DEG C, Silicon chloride. circulation time 2.5 hours first, in sample analysis Silicon chloride., impurity content improves 2%, again supplements fresh liquid phase Silicon chloride., circulation time 3 hours, sample analysis, in Silicon chloride., impurity content is reduced to 4%, and third time supplements fresh liquid phase Silicon chloride., after circulating 4 hours, sample analysis, in tower reactor, Silicon chloride. impurity content is reduced to 0.02%, stops heating.
(5), when bottom temperature is down to 80 DEG C, after Silicon chloride. and the metal chloride that is dissolved in Silicon chloride. all being discharged by floss hole 6, use nitrogen pressurising；When rectifying column 3 pressure reaches 0.3MPa by floss hole 6 pressure release, and the Silicon chloride. in tower reactor and pipeline is all purged totally, make Silicon chloride. all replace, can normally drive to run.
Claims (3)
1. the method cleaning rectifying column reboiler, comprises the following steps:
(1) after reboiler (2) blocks, the vapour-liquid load reduction of rectifying column (3), when being down to the minimum vapour-liquid load of design, stops described rectifying column (3)；
(2) the mixture that tower is contained within trichlorosilane, Silicon chloride. and metal chloride is all expelled to raw material storage tank at 85 DEG C by tower reactor extraction pipeline (5), is continuing with when again driving；
(3) stop extraction when tower bottoms position is reduced to 5%, and in tower, supplement fresh liquid phase Silicon chloride. by rectifying column feeding line (1)；When tower reactor liquid level is increased to 80%, stop supplementing fresh liquid phase Silicon chloride., and start to pass into steam to described reboiler (2), be heated heating up to the Silicon chloride. of described rectifying column (3) tower reactor, open condenser (4) simultaneously, make described rectifying column (3) carry out total reflux operation；
(4) when bottom temperature is at 100 DEG C ~ 120 DEG C, Silicon chloride. circulation time 2.5 hours first, in sample analysis Silicon chloride., impurity content improves 2%, again supplements fresh liquid phase Silicon chloride., circulation time 3 hours, sample analysis, in Silicon chloride., impurity content is reduced to 4%, and third time supplements fresh liquid phase Silicon chloride., after circulating 4 hours, sample analysis, in tower reactor, Silicon chloride. impurity content is reduced to 0.02%, stops heating；
(5), when bottom temperature is down to 80 DEG C, after Silicon chloride. and the metal chloride that is dissolved in Silicon chloride. all being discharged by floss hole (6), use nitrogen pressurising；When described rectifying column (3) pressure reaches 0.3MPa by described floss hole (6) pressure release, and the Silicon chloride. in tower reactor and pipeline is all purged totally, make Silicon chloride. all replace, can normally drive to run.
2. a kind of method cleaning rectifying column reboiler as claimed in claim 1, it is characterised in that: described step (3) in fresh liquid phase Silicon chloride. refer to and use reduction furnace to produce and through the Silicon chloride. that trichlorosilane content is less than 0.05%, silica flour content is less than 0.01% of separating-purifying.
3. a kind of method cleaning rectifying column reboiler as claimed in claim 1, it is characterised in that: described step (1) middle reboiler (2) refers to shell-and-tube or thermosyphon reboiler, and wherein tube side is material, and shell side is for solving thermal medium.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610151505.7A CN105776224B (en) | 2016-03-17 | 2016-03-17 | A kind of method for cleaning rectifying column reboiler |
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| CN201610151505.7A CN105776224B (en) | 2016-03-17 | 2016-03-17 | A kind of method for cleaning rectifying column reboiler |
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| CN105776224A true CN105776224A (en) | 2016-07-20 |
| CN105776224B CN105776224B (en) | 2017-11-21 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106824936A (en) * | 2017-01-03 | 2017-06-13 | 北京首钢朗泽新能源科技有限公司 | A kind of Distallation systm on-line cleaning device and method |
| CN108721933A (en) * | 2018-08-16 | 2018-11-02 | 青海黄河上游水电开发有限责任公司新能源分公司 | Cold hydrogenation low-pressure distillation processing unit, cold hydrogenation low-pressure distillation processing system and anti-blockage method |
| CN110694293A (en) * | 2019-10-30 | 2020-01-17 | 新疆东方希望新能源有限公司 | Reaction rectifying tower for recovering DCS through side line extraction |
| CN113813633A (en) * | 2021-09-29 | 2021-12-21 | 聊城鲁西氯甲烷化工有限公司 | Chloroform rectification device and rectification process |
| CN115382234A (en) * | 2022-07-15 | 2022-11-25 | 青海黄河上游水电开发有限责任公司新能源分公司 | Chlorination low pressure rectification discharge system |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN200992525Y (en) * | 2006-12-31 | 2007-12-19 | 淄博齐鲁乙烯鲁华化工有限公司 | Forced circulating system for reducing reboiler polymerization for C5 separation |
| JP2011121800A (en) * | 2009-12-09 | 2011-06-23 | Cosmo Oil Co Ltd | Cleaning method of reaction furnace for polycrystalline silicon manufacture |
| CN102602936A (en) * | 2012-03-14 | 2012-07-25 | 天津大学 | Method and device for treating residual silicon tetrachloride liquor |
-
2016
- 2016-03-17 CN CN201610151505.7A patent/CN105776224B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN200992525Y (en) * | 2006-12-31 | 2007-12-19 | 淄博齐鲁乙烯鲁华化工有限公司 | Forced circulating system for reducing reboiler polymerization for C5 separation |
| JP2011121800A (en) * | 2009-12-09 | 2011-06-23 | Cosmo Oil Co Ltd | Cleaning method of reaction furnace for polycrystalline silicon manufacture |
| CN102602936A (en) * | 2012-03-14 | 2012-07-25 | 天津大学 | Method and device for treating residual silicon tetrachloride liquor |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106824936A (en) * | 2017-01-03 | 2017-06-13 | 北京首钢朗泽新能源科技有限公司 | A kind of Distallation systm on-line cleaning device and method |
| CN106824936B (en) * | 2017-01-03 | 2020-05-08 | 北京首钢朗泽新能源科技有限公司 | Online cleaning device and method for distillation system |
| CN108721933A (en) * | 2018-08-16 | 2018-11-02 | 青海黄河上游水电开发有限责任公司新能源分公司 | Cold hydrogenation low-pressure distillation processing unit, cold hydrogenation low-pressure distillation processing system and anti-blockage method |
| CN110694293A (en) * | 2019-10-30 | 2020-01-17 | 新疆东方希望新能源有限公司 | Reaction rectifying tower for recovering DCS through side line extraction |
| CN113813633A (en) * | 2021-09-29 | 2021-12-21 | 聊城鲁西氯甲烷化工有限公司 | Chloroform rectification device and rectification process |
| CN115382234A (en) * | 2022-07-15 | 2022-11-25 | 青海黄河上游水电开发有限责任公司新能源分公司 | Chlorination low pressure rectification discharge system |
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| CN105776224B (en) | 2017-11-21 |
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Address after: 810007 No.1, Jinsi Road, Xining Economic and Technological Development Zone, Xining City, Qinghai Province Patentee after: Asia silicon (Qinghai) Co., Ltd Address before: 810007 Qinghai city of Xining Province Economic and Technological Development Zone No. 1 gold Guilu Patentee before: ASIA SILICON (QINGHAI) Co.,Ltd. |