CN110639328A - Method for removing trace carbon impurities in tail gas recovery hydrogen treatment process - Google Patents
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- CN110639328A CN110639328A CN201910869082.6A CN201910869082A CN110639328A CN 110639328 A CN110639328 A CN 110639328A CN 201910869082 A CN201910869082 A CN 201910869082A CN 110639328 A CN110639328 A CN 110639328A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2256/00—Main component in the product gas stream after treatment
- B01D2256/16—Hydrogen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
Abstract
The invention relates to a method for removing trace carbon impurities in a tail gas recovery hydrogen treatment process. A method for removing trace carbon impurities in a tail gas recovery hydrogen process, comprising: (1) the recovered hydrogen enters from the lower part of the methane adsorption tower 1, and is adsorbed and then enters a reduction unit from the upper part of the methane adsorption tower 1; (2) the adsorbent in the methane adsorption tower 1 is saturated, and a pipeline for removing the reduction unit is closed; (3) discharging gas in the methane adsorption tower 1 into the methane adsorption tower 2 until the pressure of the two towers is the same, and closing a pipeline from the methane adsorption tower 1 to the methane adsorption tower 2; repeating the operation to discharge the gas in the methane adsorption tower 1 into n methane adsorption towers; (4) and after the gas in the methane adsorption tower 1-n is pumped to the micro-positive pressure, the methane adsorption tower 1-n is in a vacuum state, and the adsorbent is integrally swept by the regenerated hydrogen to complete regeneration. The invention adopts a process method of increasing a methane adsorption tower to control the carbon content in the recovered hydrogen.
Description
Technical Field
The invention belongs to the technical field of polycrystalline silicon, and particularly relates to a method for removing trace carbon impurities in a tail gas hydrogen recovery treatment process.
Background
At present, the process for producing polycrystalline silicon specifically utilizes an improved siemens method. A series of reduction reactions of hydrogen and a deposition carrier in a reduction furnace increase the carbon content to a certain degree, quickly enrich carbon impurities, and have deposition reactions with a reduction silicon rod by virtue of the free state of the carbon and great influence on the electrical properties of a polycrystalline silicon product to a certain degree. Therefore, some means and method must be taken to control the carbon content in the recovered material.
The current common process of polysilicon manufacturers for adsorption towers is that hydrogen (containing a small amount of HCl and chlorosilane) coming out of the top of an absorption tower needs to be removed through a hydrogen adsorption tower. The device is provided with 3 hydrogen adsorption towers, one of the adsorption towers is in an adsorption process, the other adsorption tower is in a heating desorption process, the other adsorption tower is in a cooling process, and the cycle period of the operation of the three towers is about 5 hours. For a single column, the procedure is as follows: adsorption, reduced pressure heating, heating and purging, back pressure cooling, cooling and next adsorption. The process is briefly described as follows:
a. an adsorption process: the gas enters the adsorption tower in an adsorption state from the bottom of the hydrogen adsorption tower, HCL, chlorosilane and other components in the gas are adsorbed under the selective adsorption of an active carbon adsorbent, and the unadsorbed hydrogen (the purity can reach 99.9999 percent) passes through a filter from the top of the tower and then is sent to a reduction unit.
b. And (3) a reduced-pressure heating process: after the adsorption process is finished, the purging outlet valve is opened, the cold water inlet valve is closed, the hot water inlet valve and the cold water outlet valve are opened, the pressure of the gas in the adsorption tower is reduced along the adsorption direction, and the adsorbed gas is subjected to pressure reduction and analysis through hot water heating.
c. Heating and purging: after the decompression heating process is finished, closing the cold water outlet valve, opening the purging inlet valve and the hot water outlet valve, indirectly heating and flushing the adsorbent bed layer by hydrogen through hot water of the adsorption tower, and completely desorbing HCL and chlorosilane adsorbed on the adsorbent to regenerate the adsorbent.
d. And (3) a back pressure cooling process: in order to smoothly switch the adsorption tower to the next adsorption and ensure that the product purity does not fluctuate in the process, the pressure of the adsorption tower needs to be increased to the adsorption pressure so as to ensure the sufficiency of the pressure increasing process of the product and reduce the influence on the adsorption pressure fluctuation.
e. And (3) cooling: and closing the hot water outlet valve, opening the cold water outlet valve, blowing cold from top to bottom to the adsorption tower by utilizing the indirect cooling of the hydrogen through the cold water in the adsorption tower, and finishing the cooling process when the temperature in the adsorption tower is less than 50 ℃.
After the process, the adsorption tower completes a complete cycle of adsorption-regeneration and prepares for the next adsorption. The three adsorption towers alternately carry out the adsorption and regeneration operations (1 adsorption tower is always in an adsorption state), and the continuous separation and purification of hydrogen, HCL and chlorosilane can be realized.
When the adsorption of the adsorption tower reaches a saturated state, the adsorption tower needs to be purged by hydrogen so that the adsorption tower has the capacity of re-adsorption. The main component of the tail gas obtained by blowing is hydrogen, and in addition, a small amount of chlorosilane and HCL are contained. The mixed gas is sent to a regeneration system, cooled and compressed by a heat exchanger, and finally enters a cold hydrogenation unit for recycling; in the system, the pressure relief gas and part of the blowback gas of the adsorption tower are discharged outside, so that the impurity gas in the system is reduced.
However, in the actual production operation process, the adsorption separation operation is difficult to meet the design requirements, particularly, the activated carbon adsorbent cannot adsorb a large amount of nitrogen and methane impurities, and H is generated2After passing through the activated carbon adsorption tower, impurities of nitrogen and methane always appear through detection, and the quality of a polycrystalline silicon product is influenced to a certain extent.
In view of the above, the present invention provides a new method for removing trace carbon impurities in the tail gas hydrogen recovery treatment process.
Disclosure of Invention
The invention aims to provide a method for removing trace carbon impurities in a tail gas recovery hydrogen treatment process, which can effectively control the carbon content in the recovered hydrogen.
In order to realize the purpose, the adopted technical scheme is as follows:
a method for removing trace carbon impurities in a tail gas recovery hydrogen treatment process, comprising the steps of:
(1) the method comprises the following steps of (1) enabling recovered hydrogen from the top of an active carbon adsorption tower to enter from the lower part of a methane adsorption tower 1, enabling the recovered hydrogen to be discharged from an upper outlet of the methane adsorption tower 1 after being adsorbed by an adsorbent in the tower, and enabling the hydrogen to enter a reduction unit;
(2) after the methane adsorption tower 1 is adsorbed for a period of time, the adsorbent in the tower is saturated, and the pipeline of the reduction unit is closed;
(3) discharging the high-pressure gas in the methane adsorption tower 1 into the methane adsorption tower 2 by using a pipeline until the two towers obtain the same pressure, and closing a pipeline from the methane adsorption tower 1 to the methane adsorption tower 2;
repeating the operation until the pressure in the methane adsorption tower 1 is not more than 0.25 times of the pressure when the high-pressure gas in the methane adsorption tower 1 is not discharged after the high-pressure gas in the methane adsorption tower 1 is discharged into the methane adsorption tower n;
(4) and (3) extracting the gas from the methane adsorption tower 1 to the methane adsorption tower n, after the gas reaches the micro-positive pressure, utilizing a vacuum removal system to enable the methane adsorption tower 1 to the methane adsorption tower n to form a vacuum state, and blowing the whole adsorbent through regenerated hydrogen to complete regeneration.
Further, in the step (1), the recycled hydrogen is 10 ℃;
the flow rate of the gas discharged from the upper outlet of the methane adsorption column 1 is not less than 200NM3/H。
Further, in the step (2), the adsorbent is a granular resin.
Still further, the adsorbent is a 4-grade resin.
Further, in the step (3), n is not less than 3 and not more than 5.
Still further, n is 3.
Further, in the step (3), the pressure difference between the methane adsorption column 1 and the methane adsorption column n is within 60KPa, and it can be considered that the pressures of the two columns are the same.
Further, in the step (4), the pressure of the micro positive pressure is 30-50 KPa.
Compared with the prior art, the invention has the beneficial effects that:
the invention relates to a method for removing trace carbon impurities in the process of recovering hydrogen by a tail gas recovery device, which is used for recovering tail gas discharged by a reduction furnace by a Siemens improved dry method and effectively separating hydrogen and hydrogen chloride. In order to reduce the frequency of fluctuation of product quality and fulfill the aims of energy conservation and emission reduction, the hydrogen adsorbed by the activated carbon enters the methane adsorption tower, trace methane in the recovered hydrogen is adsorbed by the 4-stage resin adsorption tower, impurities in the recovered hydrogen can be successfully removed, and then the hydrogen enters the reduction furnace for polycrystalline silicon deposition reaction.
Drawings
FIG. 1 is a schematic process diagram of example 1 of the present invention.
Detailed Description
In order to further illustrate the method for removing trace carbon impurities in a tail gas hydrogen recovery processing process according to the present invention, and achieve the intended purpose, the following detailed description is provided with reference to the preferred embodiments for a method for removing trace carbon impurities in a tail gas hydrogen recovery processing process according to the present invention, and the detailed implementation modes, structures, characteristics and effects thereof are described below. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The method for removing trace carbon impurities in the tail gas recovery hydrogen treatment process of the invention will be further described in detail with reference to the following specific embodiments:
the technical scheme of the invention is as follows:
(1) the recovered hydrogen from the top of the activated carbon adsorption tower enters from the lower part of the methane adsorption tower 1, is adsorbed by the adsorbent in the tower, and then exits from the upper outlet of the methane adsorption tower 1 to a reduction unit.
(2) After the methane adsorption tower 1 is adsorbed for a period of time, the adsorbent in the tower is saturated, and the pipeline of the reduction unit is closed.
(3) And (2) discharging the high-pressure gas in the methane adsorption tower 1 into the methane adsorption tower 2 by using a pipeline until the two towers obtain the same pressure, and closing a pipeline from the methane adsorption tower 1 to the methane adsorption tower 2.
This operation is repeated until the pressure in the methane adsorption column 1 is not more than 0.25 times the pressure when the high-pressure gas in the methane adsorption column 1 is not discharged after the high-pressure gas in the methane adsorption column 1 is discharged into the methane adsorption column n.
Through this operation, the high-pressure gas in 1 the inside of reduction methane adsorption tower that can be quick, also can be fast accurate in the later stage carry out the gradient pressurization with a plurality of methane adsorption towers moreover.
(4) And (3) extracting the gas from the methane adsorption tower 1 to the methane adsorption tower n, after the gas reaches the micro-positive pressure, utilizing a vacuum removal system to enable the methane adsorption tower 1 to the methane adsorption tower n to form a vacuum state, and blowing the whole adsorbent through regenerated hydrogen to complete regeneration.
Compared with the forced exhaust in the prior art, the invention can recover more hydrogen and reduce the cost before impurities are separated out by pumping the gas (mainly hydrogen) of a plurality of methane adsorption towers to micro-positive pressure.
Preferably, in the step (1), the recovered hydrogen is 10 ℃;
the flow rate of the gas discharged from the upper outlet of the methane adsorption column 1 is not less than 200NM3/H。
Preferably, in the step (2), the adsorbent is a granular resin. Is more beneficial to adsorbing impurities such as methane and the like.
Further preferably, the adsorbent is a 4-stage resin.
Preferably, in the step (3), n is not less than 3 and not more than 5.
More preferably, n is 3. From the viewpoint of equipment cost and running cost, n is most preferably 3.
Preferably, in the step (3), the pressure difference between the methane adsorption column 1 and the methane adsorption column n is within 60KPa, and the pressures of both columns may be considered to be the same.
Preferably, in the step (4), the pressure of the micro positive pressure is 30 to 50 KPa. And the separation of impurities such as adsorbed methane, chlorosilane and hydrogen chloride is avoided while more hydrogen is recovered.
Example 1.
With reference to fig. 1, the specific operation steps are as follows:
hydrogen recovered from the top of the active carbon adsorption tower at about 10 ℃ enters from the lower part A1 of the methane adsorption tower TA, is adsorbed by the filler in the tower and then exits from the outlet A2 to a reduction unit II to be used as reaction gas for the growth of silicon rods. And the purged gas III enters a regeneration cooling compression system and is sent to a cold hydrogenation unit for repeated recycling. Finally, the residual gas is vacuumized in the adsorption tower through a vacuum system to be in a vacuum state, so that the purpose of fully desorbing the impurities is achieved.
For example, when TA is adsorbed, the valves A1 and A2 are synchronously opened to promote the regulating valve F to be opened for a long time, so that the flow meter FT is kept above 200NM 3/H. After a period of adsorption on TA, the adsorbent inside TA rapidly reaches saturation, a1 and a2 are closed, a4 is opened, and the high-pressure gas inside TA column is discharged into column TB, which is to be stamped, by means of line 4 until both columns attain the same pressure. And closing a valve of the stamping tower, repeating the processes repeatedly, and discharging the pressure in the TA tower to another adsorption tower TC to finally achieve the purpose of reducing the pressure of the TA tower. Thus, the waste of hydrogen can be effectively avoided. Closing A4, opening A6, and reducing the pressure in the tower to slight positive pressure; closing A6 and opening A7 to form a vacuum state; the A3 is started when the pressure is continuously reduced, the adsorbent is integrally swept by the regenerated hydrogen, after regeneration is completed, the A3 and the A7 are closed simultaneously, the A4 is opened, and the pressure inside the high-pressure tower is stamped by the leakage pressure of the pipeline 4, so that the pressure balance is ensured. After repeated operation, the tower pressure finally reaches the same pressure as the system pipe 2, and the adsorption state is achieved, and the operation is repeated.
Before and after the present embodiment, samples were taken from the hydrogen outlet of the methane adsorption column and analyzed for comparison, as shown in tables 1 to 2 below.
TABLE 1
TABLE 2
It can be seen from the table that the methane content in the recovered hydrogen is significantly reduced. The quality of the polysilicon product is obviously improved. After the scheme is implemented, the quality of the polycrystalline silicon product is obviously improved.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (8)
1. A method for removing trace carbon impurities in a tail gas recovery hydrogen treatment process is characterized by comprising the following steps:
(1) the method comprises the following steps of (1) enabling recovered hydrogen from the top of an active carbon adsorption tower to enter from the lower part of a methane adsorption tower 1, enabling the recovered hydrogen to be discharged from an upper outlet of the methane adsorption tower 1 after being adsorbed by an adsorbent in the tower, and enabling the hydrogen to enter a reduction unit;
(2) after the methane adsorption tower 1 is adsorbed for a period of time, the adsorbent in the tower is saturated, and the pipeline of the reduction unit is closed;
(3) discharging the high-pressure gas in the methane adsorption tower 1 into the methane adsorption tower 2 by using a pipeline until the two towers obtain the same pressure, and closing a pipeline from the methane adsorption tower 1 to the methane adsorption tower 2;
repeating the operation until the pressure in the methane adsorption tower 1 is not more than 0.25 times of the pressure when the high-pressure gas in the methane adsorption tower 1 is not discharged after the high-pressure gas in the methane adsorption tower 1 is discharged into the methane adsorption tower n;
(4) and (3) extracting the gas from the methane adsorption tower 1 to the methane adsorption tower n, after the gas reaches the micro-positive pressure, utilizing a vacuum removal system to enable the methane adsorption tower 1 to the methane adsorption tower n to form a vacuum state, and blowing the whole adsorbent through regenerated hydrogen to complete regeneration.
2. The method of claim 1,
in the step (1), the recycled hydrogen is 10 ℃;
the flow rate of the gas discharged from the upper outlet of the methane adsorption column 1 is not less than 200NM3/H。
3. The method of claim 1,
in the step (2), the adsorbent is granular resin.
4. The method of claim 3,
the adsorbent is 4-grade resin.
5. The method of claim 1,
in the step (3), n is not less than 3 and not more than 5.
6. The method of claim 5,
and n is 3.
7. The method of claim 1,
in the step (3), the pressure difference between the methane adsorption tower 1 and the methane adsorption tower n is within 60KPa, and the pressures of the two towers can be considered to be the same.
8. The method of claim 1,
in the step (4), the pressure of the micro-positive pressure is 30-50 KPa.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114146532A (en) * | 2021-12-17 | 2022-03-08 | 新疆大全新能源股份有限公司 | Operation process of active carbon adsorption tower in polycrystalline silicon tail gas recovery process |
| CN116553559A (en) * | 2023-05-31 | 2023-08-08 | 宁夏润阳硅材料科技有限公司 | Method and system for controlling content of carbon impurities in disilicon for reduction process |
| CN114146532B (en) * | 2021-12-17 | 2024-04-26 | 新疆大全新能源股份有限公司 | Operation process of active carbon adsorption tower in polycrystalline silicon tail gas recovery process |
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| CN114146532A (en) * | 2021-12-17 | 2022-03-08 | 新疆大全新能源股份有限公司 | Operation process of active carbon adsorption tower in polycrystalline silicon tail gas recovery process |
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| CN116553559A (en) * | 2023-05-31 | 2023-08-08 | 宁夏润阳硅材料科技有限公司 | Method and system for controlling content of carbon impurities in disilicon for reduction process |
| CN116553559B (en) * | 2023-05-31 | 2024-02-02 | 宁夏润阳硅材料科技有限公司 | Method and system for controlling content of carbon impurities in disilicon for reduction process |
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