CN202265420U - Concentrated sulfuric acid drying device for trichlorosilane - Google Patents
Concentrated sulfuric acid drying device for trichlorosilane Download PDFInfo
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- CN202265420U CN202265420U CN2011203681139U CN201120368113U CN202265420U CN 202265420 U CN202265420 U CN 202265420U CN 2011203681139 U CN2011203681139 U CN 2011203681139U CN 201120368113 U CN201120368113 U CN 201120368113U CN 202265420 U CN202265420 U CN 202265420U
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- vitriol oil
- pipeline
- graphite
- trichlorosilane
- salt solution
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Abstract
The utility model discloses a concentrated sulfuric acid drying device for trichlorosilane. A first stage 5 DEG C water graphite cooler is connected with a second stage -35 DEG C saline graphite cooler, the outlet end of the second stage -35 DEG C saline graphite cooler is connected with a third stage -35 DEG C saline graphite cooler, the outlet end of the third stage -35 DEG C saline graphite cooler is connected with a first stage entrainment separator, the outlet end of the first stage entrainment separator is connected with a second stage entrainment separator, the outlet end of the second stage entrainment separator is connected with a graphite pre-heater, and the outlet end of the graphite pre-heater is connected with a drying tower. The concentrated sulfuric acid drying device for trichlorosilane is simple in structure, safe, reliable and convenient to install and demount, reduces moisture content in hydrogen chloride gas to be below 50 ppm by using strong water absorbability of concentrated sulfuric acid, and accordingly improves conversion efficiency of trichlorosilane. Moisture in the hydrogen chloride gas is reduced so that generation of hydrolysate is completely eradicated, blockage is reduced, cleaning frequencies of follow-up condensing devices can be reduced, production efficiency is improved, and production cost is reduced.
Description
Technical field
The utility model relates to trichlorosilane and produces supplementary unit, relates in particular to a kind of vitriol oil drying plant that is used for trichlorosilane.
Background technology
Trichlorosilane is produced raw materials used hydrogen chloride gas, needs processed, the height of transformation efficiency and the quality of response situation when the height of water content is directly connected to the trichlorosilane building-up reactions in the hydrogen chloride gas before the participation reaction.At present, to the dry lyophilization method that adopts usually of hydrogen chloride gas, the principle of lyophilization was that the reduction along with temperature reduces according to the dividing potential drop of water vapor during domestic trichlorosilane was produced; And the freezing point of hydrogenchloride is-15 ℃, and therefore, the temperature of hydrogenchloride can not unconfinedly reduce during lyophilization; Generally be controlled in-14 ± 2 ℃ of scopes,, can cause the hydrogenchloride line of pipes to freeze if be lower than this temperature; Cause SR to rise, be unfavorable for producing.Receive freezing temperature limitation, when adopting the lyophilization method, the water content of hydrogenchloride can only be controlled between 500 ~ 1000ppm, can cause very big influence to the production of follow-up trichlorosilane.
The existence of moisture in the hydrogen chloride gas; Also can in building-up reactions, make reaction product generation hydrolysis, cause the trichlorosilane productive rate to reduce, the silica gel that hydrolysis generates also can blocking pipe; Make production run that difficulty take place, the hydrochloric acid that hydrolysis produces has the intensive corrosive nature to equipment.Water cut is big more in the hydrogenchloride, and the content of trichlorosilane is low more in the synthetic material.
When water-content in the hydrogenchloride 0.1% the time, trichlorosilane content is less than 80%, water-content is 0.05% o'clock in the hydrogenchloride, it is nearly 90% that trichlorosilane content rises to, the water cut that therefore reduces in the hydrogen chloride gas is crucial and is necessary.
In a word, adopt cold method to remove the moisture content in the hydrogen chloride gas, water content can only be controlled in 500 ~ 1000ppm scope, is unfavorable for the lifting of transformation efficiency in the trichlorosilane building-up reactions and avoids the generation of some hydrolyzates.
The utility model content
In view of this, the purpose of the utility model provides a kind of vitriol oil drying plant that is used for trichlorosilane, can utilize the strong absorptive of the vitriol oil, improves the transformation efficiency of trichlorosilane, and the generation of stopping hydrolyzate is simultaneously enhanced productivity, reduced production costs.
The technical scheme of the utility model realizes with following method,
A kind of vitriol oil drying plant that is used for trichlorosilane mainly comprises 5 ℃ of aquadag water coolers of one-level, secondary-35 ℃ salt solution graphite cooler, three grades of-35 ℃ of salt solution graphite coolers; One-level entrainment trap, secondary entrainment trap, graphite preheater, drying tower; Vitriol oil header tank, acid mist eliminator, plate cooler; Pipeline, spent acid jar, spent acid pump; Recycle pump, the dilute sulphuric acid storage tank is made sour pump; Vitriol oil storage tank, wherein, the exit end of 5 ℃ of aquadag water coolers of one-level is connected with the inlet end of secondary-35 ℃ salt solution graphite cooler through pipeline; The exit end of secondary-35 ℃ salt solution graphite cooler is connected with the inlet end of three grades of-35 ℃ of salt solution graphite coolers through pipeline, and the exit end of three grades of-35 ℃ of salt solution graphite coolers is connected with the inlet end of one-level entrainment trap through pipeline, and the exit end of one-level entrainment trap is connected with the inlet end of secondary entrainment trap through pipeline; The exit end of secondary entrainment trap is connected with the inlet end of graphite preheater through pipeline, and the exit end of graphite preheater passes through pipeline and is connected with the inlet end of drying tower, the exit end of drying tower pass through pipeline respectively with vitriol oil header tank; Acid mist eliminator, plate cooler connects.
5 ℃ of aquadag water coolers of one-level, secondary-35 ℃ salt solution graphite cooler, three grades of-35 ℃ of salt solution graphite coolers, one-level entrainment trap, secondary entrainment trap bottom are provided with the spent acid jar.
The spent acid jar is provided with the spent acid pump.
Drying tower is made up of bubble-cap section and packing section two portions.
Be provided with the dilute sulphuric acid storage tank through pipeline between drying tower and the plate cooler, pipeline is provided with recycle pump.
Dilute sulphuric acid storage tank bottom also is provided with sulfur waste acid pump.
Vitriol oil header tank is connected with vitriol oil storage tank through pipeline, and vitriol oil storage tank is provided with through pipeline and makes sour pump.
The positively effect of the utility model technical scheme is:
The utility model is simple in structure, do not damage equipment, safe and reliable, easy installation and removal, utilizes the strong absorptive of the vitriol oil, the water content in the hydrogen chloride gas reduced to below the 50ppm, thereby improve the transformation efficiency of trichlorosilane; The minimizing of moisture content in the hydrogen chloride gas, the generation of having stopped hydrolyzate, tamper reduces in pipeline and the equipment, can reduce the cleaning frequency of subsequent condensation equipment, enhances productivity, reduces production costs.
Description of drawings
Fig. 1 is the structural representation of the utility model.
Embodiment
Below in conjunction with accompanying drawing and embodiment the utility model is further specified.
Can find out that by Fig. 1 a kind of vitriol oil drying plant that is used for trichlorosilane mainly comprises 5 ℃ of aquadag water coolers 1 of one-level; Secondary-35 ℃ salt solution graphite cooler 2, three grades of-35 ℃ of salt solution graphite coolers 3, one entrainment traps 4, secondary entrainment trap 5, graphite preheater 6; Drying tower 7, vitriol oil header tank 8, acid mist eliminator 9; Plate cooler 10, pipeline, spent acid jar 11; Spent acid pump 12, recycle pump 13, dilute sulphuric acid storage tank 14; Make sour pump 15, vitriol oil storage tank 16, wherein; The exit end of 5 ℃ of aquadag water coolers of one-level is connected with the inlet end of secondary-35 ℃ salt solution graphite cooler through pipeline, and the exit end of secondary-35 ℃ salt solution graphite cooler is connected with the inlet end of three grades of-35 ℃ of salt solution graphite coolers through pipeline, and the exit end of three grades of-35 ℃ of salt solution graphite coolers is connected with the inlet end of one-level entrainment trap through pipeline; The exit end of one-level entrainment trap is connected with the inlet end of secondary entrainment trap through pipeline, and the exit end of secondary entrainment trap is connected with the inlet end of graphite preheater through pipeline, and the exit end of graphite preheater is connected with the inlet end of drying tower through pipeline; The exit end of drying tower through pipeline respectively with vitriol oil header tank, acid mist eliminator, plate cooler connects.
It can also be seen that by Fig. 1,5 ℃ of aquadag water coolers 1 of one-level, secondary-35 ℃ salt solution graphite cooler 2, three grades of-35 ℃ of salt solution graphite coolers 3, one-level entrainment trap 4, secondary entrainment trap 5 bottoms are provided with spent acid jar 11.
It can also be seen that by Fig. 1 spent acid jar 11 is provided with spent acid pump 12.
It can also be seen that by Fig. 1 drying tower 7 is made up of bubble-cap section and packing section two portions, the water-absorbent of the vitriol oil and concentration, temperature are relevant, and only guaranteed drying tower sulfuric acid concentration and temperature could guarantee the drying effect of hydrogen chloride gas.
It can also be seen that by Fig. 1 be provided with dilute sulphuric acid storage tank 14 through pipeline between drying tower 7 and the plate cooler 10, pipeline is provided with recycle pump 13, dilute sulphuric acid storage tank 14 bottoms also are provided with sulfur waste acid pump 17.
It can also be seen that by Fig. 1 vitriol oil header tank 8 is connected with vitriol oil storage tank 16 through pipeline, vitriol oil storage tank 16 is provided with through pipeline and makes sour pump 15.
Contain moisture hydrogen chloride gas at first get into 5 ℃ of aquadag water coolers 1 of one-level; Get into secondary-35 ℃ salt solution graphite cooler 2 and three grades of-35 ℃ of salt solution graphite coolers 3 then successively; Hydrogen chloride gas through behind the deep cooling gets into one-level entrainment trap 4, secondary entrainment trap 5 successively; Get into graphite preheater 6 then and heat, make the hydrogenchloride temperature be controlled at 10-20 ℃.Enter into the bottom of drying tower 7 through the hydrogen chloride gas after the preheating; Inner chamber from the bottom along drying tower is up; Hydrogenchloride advances behind the tower at first to contact with 78～90% dilute sulphuric acid and removes its most of moisture content, rises to the bubble-cap section then and contacts with 98% the vitriol oil and remove remaining moisture content.Through the hydrogen chloride gas after the dehydration, through acid mist eliminator 9, open the valve of drip washing, analyze hydrogenchloride purity by the analyst.Treat that hydrogenchloride purity >=90% back gets into synthesis system.
The vitriol oil adds top bubble-cap section through under meter from vitriol oil header tank 8 automatically, continuously, then step by step overflow to packing section.The liquid of packing section provides power cycle by recycle pump 13, after plate cooler 10 coolings, delivers to packing section top liquid distributor.The heat that bubble-cap section vitriol oil suction back produces is taken away by 5 ℃ of water in the Hastelloy pipe on every laminate, thereby the temperature that guarantees packing section, bubble-cap section remains 10～20 ℃.
Claims (7)
1. a vitriol oil drying plant that is used for trichlorosilane mainly comprises 5 ℃ of aquadag water coolers of one-level (1), secondary-35 ℃ salt solution graphite cooler (2), three grades of-35 ℃ of salt solution graphite coolers (3); One-level entrainment trap (4), secondary entrainment trap (5), graphite preheater (6), drying tower (7); Vitriol oil header tank (8), acid mist eliminator (9), plate cooler (10); Pipeline, spent acid jar (11), spent acid pump (12); Recycle pump (13), dilute sulphuric acid storage tank (14) is made sour pump (15); Vitriol oil storage tank (16); It is characterized in that: the exit end of 5 ℃ of aquadag water coolers of one-level (1) is connected with the inlet end of secondary-35 ℃ salt solution graphite cooler (2) through pipeline, and the exit end of secondary-35 ℃ salt solution graphite cooler (2) is connected with the inlet end of three grades of-35 ℃ of salt solution graphite coolers (3) through pipeline, and the exit end of three grades of-35 ℃ of salt solution graphite coolers (3) is connected with the inlet end of one-level entrainment trap (4) through pipeline; The exit end of one-level entrainment trap (4) is connected with the inlet end of secondary entrainment trap (5) through pipeline; The exit end of secondary entrainment trap (5) is connected with the inlet end of graphite preheater (6) through pipeline, and the exit end of graphite preheater (6) passes through pipeline and is connected with the inlet end of drying tower (7), the exit end of drying tower (7) pass through pipeline respectively with vitriol oil header tank (8); Acid mist eliminator (9), plate cooler (10) connects.
2. a kind of vitriol oil drying plant that is used for trichlorosilane according to claim 1; It is characterized in that: 5 ℃ of aquadag water coolers of one-level (1); Secondary-35 ℃ salt solution graphite cooler (2), three grades of-35 ℃ of salt solution graphite coolers (3), one-level entrainment trap (4), secondary entrainment trap (5) bottom are through pipe connection spent acid jar (11).
3. a kind of vitriol oil drying plant that is used for trichlorosilane according to claim 2, it is characterized in that: spent acid jar (11) is provided with spent acid pump (12).
4. a kind of vitriol oil drying plant that is used for trichlorosilane according to claim 1, it is characterized in that: drying tower (7) is made up of bubble-cap section and packing section two portions.
5. a kind of vitriol oil drying plant that is used for trichlorosilane according to claim 4 is characterized in that: be provided with dilute sulphuric acid storage tank (14) through pipeline between drying tower (7) and the plate cooler (10), pipeline is provided with recycle pump (13).
6. a kind of vitriol oil drying plant that is used for trichlorosilane according to claim 5 is characterized in that: dilute sulphuric acid storage tank (14) bottom also is provided with sulfur waste acid pump (17).
7. a kind of vitriol oil drying plant that is used for trichlorosilane according to claim 1 is characterized in that: vitriol oil header tank (8) is connected with vitriol oil storage tank (16) through pipeline, and vitriol oil storage tank (16) has the sour pump (15) of beating through pipe connection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011203681139U CN202265420U (en) | 2011-09-30 | 2011-09-30 | Concentrated sulfuric acid drying device for trichlorosilane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011203681139U CN202265420U (en) | 2011-09-30 | 2011-09-30 | Concentrated sulfuric acid drying device for trichlorosilane |
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| Publication Number | Publication Date |
|---|---|
| CN202265420U true CN202265420U (en) | 2012-06-06 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011203681139U Expired - Fee Related CN202265420U (en) | 2011-09-30 | 2011-09-30 | Concentrated sulfuric acid drying device for trichlorosilane |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20220093105A (en) | 2019-11-13 | 2022-07-05 | 가부시끼가이샤 도꾸야마 | How to dehumidify hydrogen chloride |
-
2011
- 2011-09-30 CN CN2011203681139U patent/CN202265420U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20220093105A (en) | 2019-11-13 | 2022-07-05 | 가부시끼가이샤 도꾸야마 | How to dehumidify hydrogen chloride |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120606 Termination date: 20150930 |
|
| EXPY | Termination of patent right or utility model |