CN108569699A - A kind of method for recovering tail gas - Google Patents
A kind of method for recovering tail gas Download PDFInfo
- Publication number
- CN108569699A CN108569699A CN201710136862.0A CN201710136862A CN108569699A CN 108569699 A CN108569699 A CN 108569699A CN 201710136862 A CN201710136862 A CN 201710136862A CN 108569699 A CN108569699 A CN 108569699A
- Authority
- CN
- China
- Prior art keywords
- adsorption tower
- tail gas
- adsorption
- adsorbent
- state
- 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.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
-
- 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
- C01B33/10784—Purification by adsorption
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Silicon Compounds (AREA)
Abstract
It is that synthesis tail gas is sent into surge tank the invention discloses a kind of method for recovering tail gas, surge tank presses 0.3~0.8Mpa.Adsorption system is made of two adsorption towers in parallel, and one is in adsorbed state, and another is in reproduced state, is respectively equipped with import and export control valve, adsorbent is activated carbon.Synthesis tail gas enters in adsorbed state adsorption tower, 0.3~0.8MPa in tower, 20~80 DEG C of temperature, a large amount of chlorosilanes are adsorbed by adsorbent, hydrogen and chlorine hydride mixed gas body are discharged to absorption bag filter, enter gas recovery surge tank after removing dust, a part is transported to hydrogen chloride synthesis system, a part is transported in the adsorption tower of reproduced state, 100~200 DEG C of temperature in tower, 0.01~0.15MPa of pressure, the chlorosilane adsorbed under high temperature parses, make adsorbent reactivation, it is filtered by regenerating in bag filter, it is recycled by synthesis tail gas pressurization condenser system after removing dust.
Description
Technical field
The invention belongs to chemical technology fields, are related specifically to a kind of method for recovering tail gas.
Background technology
Trichlorosilane consumes a large amount of chlorine and hydrogen in production, is that one kind of chlor-alkali enterprises balances chlorine simultaneously well
The product increased economic efficiency, and the important source material for producing the products such as monocrystalline silicon, polysilicon, be widely used in national defence,
National economy and the every field of daily life.
Trichlorosilane production main method be：
Si+3HCl=SiHCl3+H2, reaction temperature at 300 DEG C or so, by dedusting, pressurization condensation after, still some
On-condensible gas such as hydrogen, hydrogen chloride or a small amount of chlorosilane.Due to containing hydrogen in on-condensible gas, both make to use -35 DEG C of refrigerant depths
It is cold, but still contain 10% or so trichlorosilane and silicon tetrachloride.In tradition or at present production technology, synthesis tail gas is used
Wet-treating not only consumes lye and water, but also has new waste water and waste residue generation, pollutes the environment, and lead to list
The supplies consumptions such as chlorine, hydrogen and the silica flour of position product are high, and product cost increases.
With production-scale expansion, these problems will be protruded more, or even the skill grown as restriction enterprise development
Art bottleneck.The technique for using Dry recovery more at present, the main hydrogen chloride recycled in tail gas, and hydrogen and a small amount of chlorosilane are washed
Emptying is washed, or hydrogen and hydrogen chloride are individually recycled, wastage of material is not only caused, also increases operation difficulty and trichlorosilane
Production cost.It is increasingly heavy to the recycling of tail gas simultaneously for the requirement for reaching environmental protection, meeting national energy conservation and emission reduction
It wants.
Patent CN101279734A discloses a kind of method of technique of trichlorosilane synthetic tail gas Dry recovery, but in this method
H 2 be incorporated into washing tail gas emptying, not only cause wastage of material, also increase trichlorosilane synthesis cost.
Patent CN101125276 hydrogen membrane separators detach hydrogen, and the hydrogen separated is used as fuel or directly row
Enter air, cause wastage of material and increases trichlorosilane production cost.
Invention content
To solve the above problems, the present invention provides a kind of method for recovering tail gas, which solves trichlorine
The recycling problem of hydrogen silicon synthesis tail gas makes the hydrogen in tail gas, returns to hydrogen chloride synthesis system after hydrogen chloride mixing recycling,
Chlorosilane gas returns to the recycling of pressuring and condensing trichlorosilane synthesized product system condensing.
For achieving the above object, the present invention adopts the following technical scheme that：
A kind of method for recovering tail gas is the condensed technique of trichlorosilane synthetic tail gas feeding surge tank that will pressurize, and is kept
The pressure of surge tank is in 0.3~0.8Mpa；Adsorption system is made of two adsorption towers in parallel, wherein the suction in an adsorption tower
Attached dose is in adsorbed state, and the adsorbent in another adsorption tower is in reproduced state, and two adsorption towers are respectively equipped with respectively
Import and export control valve, adsorbent is activated carbon；The synthesis tail gas come out from surge tank passes through under adsorbed state adsorption tower
The control valve of portion's setting enters in the adsorption tower, and the pressure in adsorption tower and the pressure of surge tank are consistent and are all at this time
0.3~0.8Mpa, the temperature in adsorption tower are controlled at 20~80 DEG C, and synthesis tail gas flows from bottom to top in adsorption tower, synthesis
A large amount of chlorosilanes in tail gas are adsorbed by adsorbent, and the mixed gas of H 2 and HCl is from the gas vent control valve at the top of adsorption tower
Door is discharged in absorption bag filter and filters, and enters gas recovery surge tank, gas recovery surge tank after being filtered to remove dust
Pressure be also maintained at 0.3~0.8Mpa；The hydrogen and chlorine hydride mixed gas body of gas recovery surge tank, a part pass through control
Valve and pipeline are transported to hydrogen chloride synthesis system, and a part is transported to by control valve and pipeline in adsorption system
In carrying out regenerative adsorption in the adsorption tower of reproduced state, the adsorption tower temperature of reproduced state is controlled at 100~200 DEG C, is dropped simultaneously
The mixed gas of low tower pressure interior force to 0.01~0.15MPa, H 2 and HCl flow from above to below in adsorption tower, in high-temperature low-pressure
Under state, the chlorosilane adsorbed is promoted to be parsed from adsorbent, to make adsorbent be regenerated, the chlorine that parses
Silane and hydrogen, chlorine hydride mixed gas body out enter mistake in regeneration bag filter from regenerative adsorption tower lower part control valve
Filter is filtered to remove after dust by synthesis tail gas pressurization condenser system recycling.
A kind of method for recovering tail gas, the adsorbent state in the adsorption towers in parallel of adsorption system two can pass through
Time control program carries out periodical rotation, that is to say, that the adsorption tower in reproduced state can be with transition by cooling down and boosting
To the adsorption tower of adsorbed state, this is because the regeneration technology after the adsorbent parsing of reproduced state adsorption tower is in high temperature, low
Carried out under pressure condition, the adsorbent absorbing process of adsorbed state adsorption tower is carried out under low temperature, high pressure conditions, by cooling and
The adsorption tower of reproduced state is transitioned into the adsorption tower of adsorbed state by boosting, and the control of cooling temperature is at 20~80 DEG C, boost pressure
Control is in 0.3~0.8Mpa.
Due to using technical solution as described above, the present invention that there is following superiority：
1, the present invention recycles the hydrogen in synthesis tail gas, hydrogen chloride mixing using the characteristic of trichlorosilane synthesis material,
The step of for hydrogen chloride synthesis, and then returning to trichlorosilane synthesis system, Matter Transfer is made to utilize, reducing individually recycling and energy
Source consumes.
2, the present invention is handled using Dry recovery, not will produce waste water and waste residue, will not be caused environmental pollution, reduce three
The production cost of chlorine hydrogen silicon synthesis.It is automatically controlled by time control program, reduces manual operation, reduce operation difficulty.
Description of the drawings
Fig. 1 is the Dry recovery schematic diagram of the present invention.
Specific implementation mode
The embodiment of the present invention is illustrated in conjunction with Fig. 1.
The condensed technique of trichlorosilane synthetic tail gas of pressurizeing is sent into surge tank, keep the pressure of surge tank 0.3~
Then the gas of synthesis tail gas surge tank is sent into adsorption system the adsorption tower for being in adsorbed state, due to passing through by 0.8Mpa
Condensed technique of trichlorosilane synthetic tail gas pressure of pressurizeing is 0.3~0.8Mpa, and in adsorption system adsorbed state adsorption tower
It needs to carry out under 0.3~0.8Mpa states, so entering the absorption of adsorbed state after synthesis tail gas is stored in surge tank
Tower, it is possible to reduce decompression, boost operations step, while reducing energy consumption.
Synthesis tail gas is entered from the adsorption tower lower part of adsorbed state by control valve and pipeline, gas in adsorption tower from
Lower and upper flowing, under the conditions of 0.3~0.8Mpa of pressure, 20~80 DEG C of temperature, the chlorosilane in synthesis tail gas is inhaled by adsorbent
Attached, the mixed gas of hydrogen and hydrogen chloride out enters absorption bag filter filtering from adsorption tower top, and dust of going out is laggard
Enter gas recovery surge tank, controls gas recovery 0.3~0.8Mpa of buffer tank pressure, the hydrogen of gas recovery surge tank and chlorination
Hydrogen mixed gas, a part are transported to hydrogen chloride synthesis system by control valve and pipeline, and a part passes through control valve
It is transported in adsorption system in the adsorption tower in reproduced state with pipeline and carries out regenerative adsorption.Synthesis tail gas is by absorption work
Skill processing has recycled hydrogen and chlorine hydride mixed gas body therein and has returned to trichlorosilane synthesis system, so that Matter Transfer is utilized, subtract
The step of few individually recycling, while gas recovery 0.3~0.8Mpa of buffer tank pressure is controlled, gas recovery can be made not consume energy
Source directly returns in the adsorption tower of trichlorosilane synthesis system and reproduced state.
For the adsorption tower of adsorbed state after operation 6~12 hours, the adsorbent chlorosilane in adsorption tower reaches full
With by time control program automatically into regeneration technology.
Hydrogen in a part of gas recovery surge tank and chlorine hydride mixed gas body, from the adsorption tower top of reproduced state into
Enter, gas flows from above to below in adsorption tower, 100~200 DEG C of temperature of control, under the conditions of 0.01~0.15MPa of pressure, is inhaled
Attached chlorosilane is parsed from adsorbent, to make adsorbent be regenerated, the chlorosilane and hydrogen that parse, chlorination
Hydrogen mixed gas is out entered in regeneration bag filter from regenerative adsorption tower lower part control valve and is filtered, and is filtered to remove dust
Afterwards by synthesis tail gas pressurization condenser system recycling.By the chlorosilane in the condensing recovery synthesis tail gas that pressurizes, raw material profit is improved
With rate.
For the adsorption tower of reproduced state after operation 6~12 hours, the adsorbent chlorosilane in adsorption tower is complete
It parses, adsorbent is regenerated, and reduces adsorption tower temperature to after 20~80 DEG C, by time control program automatically into suction
Attached technique.
Absorbing process in this way Jing Guo adsorption system and regeneration technology periodic cycle, the chlorosilane in synthesis tail gas pass through
After absorption, parsing, it is sent to pressurization condenser system and is recycled, hydrogen and chlorine hydride mixed gas body are sent to chlorination after being recycled simultaneously
Hydrogen synthesis system is recycled utilization, to make technique of trichlorosilane synthetic tail gas not generate waste water and waste residue, does not cause environment dirty
It is recycled utilization in the case of dye, while being greatly reduced the production cost of trichlorosilane synthesis.
Time control program refers to 6~12 hours time intervals of setting, and the adsorption tower of adsorption system carries out absorption work automatically
The periodical rotation of skill and regeneration technology, that is to say, that the adsorption tower of adsorbed state is after 6~12 hours, and originally gas is from absorption
Tower lower part enters, and is come out from top, and gas flows from bottom to top in adsorption tower, changes into gas and enters from adsorption tower top,
Lower part comes out, and gas flows from above to below in adsorption tower, while adsorption tower temperature is increased to 100~200 DEG C, and pressure reduction is arrived
0.01~0.15MPa, to make the adsorption tower of adsorbed state automatically into reproduced state.The 6~12 of the adsorption tower of reproduced state
After hour, originally gas enters from adsorption tower top, is come out from lower part, gas flows from above to below in adsorption tower, changes into
Gas enters from adsorption tower lower part, and top comes out, and gas flows from bottom to top in adsorption tower, while reducing adsorption tower temperature and arriving
20~80 DEG C, pressure is increased to 0.3~0.8Mpa, to make the adsorption tower of reproduced state automatically into adsorbed state.In this way may be used
It is in running order always to ensure two adsorption tower continuous operation of adsorption system, improve the utilization rate of whole system.
Claims (3)
1. a kind of method for recovering tail gas, it is characterised in that：The dry method recovery is the condensed trichlorosilane synthesis that will pressurize
Tail gas is sent into surge tank, keeps the pressure of surge tank in 0.3~0.8MPa；Adsorption system is made of two adsorption towers in parallel,
Adsorbent in a wherein adsorption tower is in adsorbed state, and the adsorbent in another adsorption tower is in reproduced state, two
Adsorption tower is respectively equipped with respective import and export control valve, and adsorbent is activated carbon；The synthesis tail gas come out from surge tank
The control valve being arranged by adsorbed state adsorption tower lower part enters in the adsorption tower, at this time the pressure and buffering in adsorption tower
It is all 0.3~0.8MPa that the pressure of tank, which is consistent, and the temperature in adsorption tower is controlled at 20~80 DEG C, and synthesis tail gas is in adsorption tower
It inside flows from bottom to top, a large amount of chlorosilanes in synthesis tail gas are adsorbed by adsorbent, and the mixed gas of hydrogen and hydrogen chloride is from suction
The gas vent control valve of attached top of tower is discharged in absorption bag filter and filters, and enters recycling gas after being filtered to remove dust
The pressure of body surge tank, gas recovery surge tank is also maintained at 0.3~0.8MPa.
2. a kind of method for recovering tail gas according to claim 1, it is characterised in that：The hydrogen and chlorine of gas recovery surge tank
Change hydrogen mixed gas, a part is transported to hydrogen chloride synthesis system by control valve and pipeline, and a part passes through control valve
Door and pipeline, which are transported in adsorption system, carries out regenerative adsorption, the adsorption tower of reproduced state in the adsorption tower in reproduced state
Temperature is controlled at 100~200 DEG C, while reducing tower pressure interior force to 0.01~0.15MPa, and the mixed gas of hydrogen and hydrogen chloride exists
It is flowed from above to below in adsorption tower, under high-temperature low-pressure state, the chlorosilane adsorbed is promoted to be parsed from adsorbent, from
And adsorbent is made to be regenerated, chlorosilane and hydrogen, the chlorine hydride mixed gas body parsed is controlled from regenerative adsorption tower lower part
Valve is out entered in regeneration bag filter and is filtered, and is filtered to remove after dust by synthesis tail gas pressurization condenser system recycling.
3. a kind of method for recovering tail gas according to claim 1, it is characterised in that：In the adsorption tower in parallel of adsorption system two
Adsorbent state pass through time control program and carry out periodical rotation, that is to say, that the adsorption tower in reproduced state passes through drop
Mild boosting is transitioned into the adsorption tower of adsorbed state, this is because the regeneration technology after the adsorbent parsing of reproduced state adsorption tower
To be carried out under high temperature, low-pressure state, the adsorbent absorbing process of adsorbed state adsorption tower be under low temperature, high pressure conditions into
The adsorption tower of reproduced state, the adsorption tower of adsorbed state is transitioned by cooling down and boosting by row, cooling temperature control 20~
80 DEG C, boost pressure is controlled in 0.3~0.8MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710136862.0A CN108569699A (en) | 2017-03-09 | 2017-03-09 | A kind of method for recovering tail gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710136862.0A CN108569699A (en) | 2017-03-09 | 2017-03-09 | A kind of method for recovering tail gas |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108569699A true CN108569699A (en) | 2018-09-25 |
Family
ID=63577635
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710136862.0A Withdrawn CN108569699A (en) | 2017-03-09 | 2017-03-09 | A kind of method for recovering tail gas |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108569699A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110280098A (en) * | 2019-04-25 | 2019-09-27 | 新疆大全新能源股份有限公司 | The recovery method of chlorosilane in a kind of hydrogeneous exhaust gas |
-
2017
- 2017-03-09 CN CN201710136862.0A patent/CN108569699A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110280098A (en) * | 2019-04-25 | 2019-09-27 | 新疆大全新能源股份有限公司 | The recovery method of chlorosilane in a kind of hydrogeneous exhaust gas |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101638233B (en) | Dry method recovery technique of trichlorosilane synthetic tail gas | |
| CN101327912B (en) | Method for reclaiming hydrogen from tail gas from polysilicon production | |
| CN101357764B (en) | Polysilicon preparation method of recovering hydrogen chloride in circulating exhaust | |
| CN101357292B (en) | Method for recovering tail-gas generated during producing polycrystalline silicon using silicon tetrachloride | |
| CN103553048B (en) | The method and system that in polysilicon production process, Matter Transfer utilizes | |
| CN101377376B (en) | Method for recovering tail gas generated by polycrystalline silicon production | |
| CN101357288B (en) | Hydrogen chloride circulation recovering method from off-gas generated from the production of polycrystalline silicon | |
| CN103111157A (en) | Method for purifying and recovering discharge tail gas of regeneration process of adsorption tower in polycrystalline silicon production | |
| CN104087354B (en) | A kind of technique utilizing yellow phosphoric tail gas synthetic natural gas | |
| CN101357286B (en) | Method for recovering dichloro-dihydro silicon from off-gas generated from the production of polycrystalline silicon | |
| CN101376499B (en) | Method for preparing polysilicon | |
| CN104140106B (en) | The method processing polycrystalline silicon reduction exhaust | |
| CN101372336B (en) | Method for preparing polysilicon | |
| CN108569699A (en) | A kind of method for recovering tail gas | |
| CN203033766U (en) | Recovery system for byproducts in polycrystalline silicon production | |
| CN102584730A (en) | Equipment and process for producing melamine under low pressure | |
| CN102030312B (en) | Method for recovering hydrogen gas from trichlorosilane tail gas | |
| CN101372335B (en) | Method for preparing polysilicon | |
| CN105197959B (en) | Chemically floatation handles the method that fluorine resource is reclaimed in low product bauxite technique | |
| CN101628720A (en) | Production process for pressuring and condensing trichlorosilane synthesized product | |
| CN214456888U (en) | Hydrogen circulation system for polycrystalline silicon production | |
| CN101357287B (en) | Method for recovering hydrogen chloride from off-gas generated from the production of polycrystalline silicon | |
| CN107311108A (en) | One kind avoids absorption column regeneration delay production technology | |
| CN112758935B (en) | Hydrogen circulation system for polycrystalline silicon production | |
| CN219209451U (en) | Diethylene glycol diethyl ether process tail gas material recovery device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180925 |