CN213314182U - Adsorption tower for hydrogen purification in polycrystalline silicon production process - Google Patents

Adsorption tower for hydrogen purification in polycrystalline silicon production process Download PDF

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CN213314182U
CN213314182U CN202021561147.5U CN202021561147U CN213314182U CN 213314182 U CN213314182 U CN 213314182U CN 202021561147 U CN202021561147 U CN 202021561147U CN 213314182 U CN213314182 U CN 213314182U
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adsorption tower
adsorption
main part
tower main
hydrogen purification
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杨楠
李寿琴
贾琳蔚
陈绍林
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Yunnan Tongwei High Purity Crystalline Silicon Co ltd
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Yunnan Tongwei High Purity Crystalline Silicon Co ltd
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Abstract

The utility model discloses an adsorption tower for hydrogen purification in polycrystalline silicon production technology belongs to polycrystalline silicon production technical field, including the adsorption tower main part, adsorption tower main part top is provided with first gas and imports and exports, and adsorption tower main part below is provided with second business turn over gas port, and the vertical direction of adsorption tower main part is provided with a plurality of heating pipes, and the heating pipe is the hollow tube that the lower extreme sealed, is provided with insulating heat-conducting layer and electric heating wire in the heating pipe, and the intussuseption of adsorption tower main part is filled with the active carbon. The utility model has the advantages of good regeneration performance, high heat utilization rate, high product purity, low operation cost and the like.

Description

Adsorption tower for hydrogen purification in polycrystalline silicon production process
Technical Field
The utility model relates to a polycrystalline silicon production technical field, concretely relates to adsorption tower for hydrogen purification in polycrystalline silicon production technology.
Background
The polycrystalline silicon material is an electronic material which takes silicon as a raw material and is purified to reach a certain purity through a series of physical and chemical reactions, is an extremely important intermediate product in the silicon product industry chain, is a main raw material for manufacturing silicon polished wafers, solar cells and high-purity silicon products, and is the most basic functional material in the semiconductor industry, the electronic information industry and the solar photovoltaic cell industry. The polysilicon production mostly adopts the improved Siemens technology, the improved Siemens process tail gas recovery section, H2Purifying by adopting an activated carbon adsorption tower to obtain a high-purity product H2For reducing SiHCl3And preparing polycrystalline silicon.
At present, the adsorption tower mainly has the following problems: (1) the thermal fluid is adopted for heating, so that the regeneration temperature is not high, and the regeneration is not thorough. (2) The coil pipe is in an environment with alternating cold and heat, and welding seams of the coil pipe are easy to leak. (3) The external conveying pipeline of cold and hot fluid is long, and the cold and hot loss is large. (4) The active carbon is cooled and heated mainly by means of heat conduction, the heat conduction coefficient of the active carbon is low, the coil pipes cannot be densely distributed, the heat transfer efficiency is low, and the heating and cooling time is long. (5) Due to the amplification effect, the activated carbon loading cannot be too high, resulting in a low throughput.
SUMMERY OF THE UTILITY MODEL
The utility model discloses aim at solving the problem that exists among the prior art, provide an adsorption tower for hydrogen purification among polycrystalline silicon production technology, the utility model discloses an adsorption tower main part runs through and evenly is provided with a plurality of electric heating pipe, and electric heating pipe is direct to the inside active carbon direct heating of adsorption tower main part, and regeneration temperature is higher makes regeneration effect better.
The utility model aims at realizing through the following technical scheme:
an adsorption tower for hydrogen purification in a polycrystalline silicon production process is characterized in that: including the adsorption tower main part, adsorption tower main part top is provided with first gas and imports and exports, adsorption tower main part below is provided with second business turn over gas port, the vertical direction of adsorption tower main part is provided with a plurality of heating pipes, the heating pipe is the hollow tube that the lower extreme sealed, be provided with insulating heat-conducting layer and electric heating wire in the heating pipe, the intussuseption of adsorption tower main part is filled with the active carbon.
Preferably, the electric heating wire, the insulating heat conduction layer and the heating pipe are sequentially arranged from inside to outside.
Preferably, the heating pipes are uniformly arranged in the adsorption tower main body.
Preferably, a feed inlet is arranged above the adsorption tower main body.
Preferably, the outer wall of the adsorption tower main body is provided with a cooling device, the lower end of the cooling device is provided with a cooling water inlet, and the upper end of the cooling coil is provided with a cooling water outlet.
Preferably, the insulating and heat conducting layer is made of materials such as boron nitride, aluminum oxide or magnesium oxide.
Preferably, the activated carbon is coconut shell activated carbon or coal activated carbon.
The working principle is as follows: in the using process, four adsorption towers are used together, and each tower sequentially comprises the steps of adsorption I, heating regeneration, cooling, adsorption II and the like, so that the raw material gas is subjected to adsorption twice to obtain H2The purity is higher, and the regeneration rate of the adsorption tower is higher.
A hydrogen purification device in a polysilicon production process comprises 4 adsorption towers, wherein a second gas inlet and outlet is respectively connected with a raw material inlet pipe, a first circulation pipeline, a hot hydrogen outlet pipe and a second circulation pipeline, the second gas inlet and outlet is connected with the raw material inlet pipe through a raw material branch pipe, the second gas inlet and outlet is connected with the first circulation pipeline through a first branch pipe, the second gas inlet and outlet is connected with the hot hydrogen outlet pipe through a first hot hydrogen branch pipe, the second gas inlet and outlet is connected with the second circulation pipeline through a second branch pipe, a cooler is arranged at the joint of the first circulation pipeline and the second circulation pipeline, a first gas inlet and outlet is arranged above the adsorption towers, the first gas inlet and outlet is respectively connected with the hot hydrogen inlet pipe, a product outlet pipe and a third circulation pipeline, the first gas inlet and outlet is connected with the hot hydrogen inlet pipe through a second hot hydrogen branch pipe, the first gas inlet and outlet is connected with the third circulation pipeline through a third branch pipe and a fourth branch pipe, the first gas inlet and outlet are connected with a product outlet pipe through a product branch pipe.
Preferably, be provided with the raw materials admission valve on the raw materials branch pipe, be provided with first circulation admission valve on the first branch pipe, be provided with hot hydrogen air outlet valve on the first hot hydrogen branch pipe, be provided with first circulation air outlet valve on the second branch pipe, be provided with hot hydrogen admission valve on the second hot hydrogen branch pipe, be provided with second circulation admission valve on the third branch pipe, be provided with second circulation air outlet valve on the fourth branch pipe, be provided with the product air outlet valve on the product branch pipe.
For the a adsorption column (other adsorption columns are identical in principle):
stage 1 adsorption I: as shown in FIG. 4, starting Material H2The H enters into the adsorption tower A from a second gas inlet and outlet at the bottom, the initial adsorption operation is started, and the H after the initial adsorption2The pure H is obtained from the first gas inlet and outlet of the A adsorption tower2Sending to the first gas inlet and outlet of the B adsorption tower, and purifying with pure H2And (4) discharging from a second gas inlet and outlet of the adsorption tower B to finish cooling of the adsorption tower B, and finally entering the adsorption tower C through a second gas inlet and outlet of the adsorption tower C to perform secondary adsorption. After the adsorption tower A adsorbs a period of time theta 1, the adsorption of the active carbon impurities in the adsorption tower A reaches saturation, the adsorption tower A no longer has adsorption capacity, and the raw material H2Then the adsorption tower is switched to the adsorption tower C for primary adsorption.
Stage 2 regeneration: as shown in fig. 5, the adsorption tower a starts to perform heating regeneration, and in the regeneration stage, the resistance wires in the electric heating pipes in the adsorption tower a are electrified to heat the activated carbon in the adsorption tower a. The electric heating pipes are more in arrangement and small in distance, the temperature of the electric heating pipes can reach 300 ℃ or even higher, and the heat transfer temperature difference between the electric heating pipes and the active carbon is large. At the same time, a small amount of heat H is blown back from the top2And carrying the impurities desorbed from the activated carbon out of the adsorption tower A. Heating and regenerating the adsorption tower A for a period of time theta 2, completely regenerating the activated carbon in the adsorption tower A, and starting to enter a third stage, namely cooling.
Stage 3 cooling: as shown in fig. 6, the adsorption tower a heats the regenerated activated carbon to a high temperature, and requires cooling to have adsorption capacity. The cooling mode adopts part or all of H after the initial adsorption2Reverse blowingCooling means, i.e. H initially adsorbed by the B adsorption column2Blowing part or all of the H from the top to the adsorption tower A, and discharging the H from the adsorption tower B2The temperature is low and is less than or equal to about 20 ℃, and the activated carbon in the A adsorption tower is cooled by H after a period of theta 32And (4) cooling. Cold back flushing H of A adsorption tower2Heated by active carbon, discharged from the bottom of the adsorption tower A, cooled by an external cooler and then enters an adsorption tower D for re-adsorption and purification.
Stage 4 adsorption II: as shown in FIG. 7, the adsorption column A is cooled to a predetermined temperature, and then it is cooled by the external cooler to receive the H from the adsorption column C2Secondary adsorption is carried out to obtain a product H with higher purity2. After a period of time θ 4, a cycle is completed and the initial stage I of stage 1 is repeated.
The sequential temporal and spatial representation of the four adsorption columns is given in table 2.
TABLE 2
Figure DEST_PATH_IMAGE002
The beneficial effects of this technical scheme are as follows:
(1) the built-in electric heating pipe is adopted, so that the regeneration temperature is high, and the regeneration is thorough.
(2) No liquid enters the adsorption tower, so that adverse effects caused by leakage are avoided.
(3) The built-in electric heating pipe, electric power all is used for the active carbon heating, has avoided calorific loss.
(4) The system of cold and hot fluid is cancelled, and the investment, operation and maintenance cost is greatly reduced.
(5) The regeneration and cooling time is shortened.
Drawings
Fig. 1 is a schematic structural view of the present invention;
fig. 2 is a schematic structural view of the electric heating tube of the present invention;
FIG. 3 is a schematic diagram of a hydrogen purification apparatus;
FIG. 4 is a flow diagram of stage 1 adsorption I from adsorption column A in a hydrogen purification apparatus;
FIG. 5 is a flow diagram of stage 2 regeneration of the A adsorption column in a hydrogen purification unit;
FIG. 6 is a flow diagram of stage 3 cooling of the A adsorption column in a hydrogen purification unit;
FIG. 7 is a flow diagram of stage 4 adsorption II in adsorption column A of a hydrogen purification apparatus;
wherein: 1. an adsorption tower main body; 2. a first gas inlet and outlet; 3. a second gas inlet and outlet; 5. heating a tube; 6.1, insulating and heat conducting layers; 6.2, an electric heating wire; 7. activated carbon; 9. a cooling device; 9.1, a cooling water inlet; 9.2, a cooling water outlet; 101. feeding the raw materials into a pipe; 102. a first recycle line; 103. a raw material branch pipe; 104. a first branch pipe; 105. a hot hydrogen outlet pipe; 106. a second recycle line; 107. a first hot hydrogen branch pipe; 108. a second branch pipe; 109. a cooler; 110. a hot hydrogen inlet pipe; 111. a product outlet pipe; 112. a third recycle line; 113. a second hot hydrogen branch pipe; 114. a third branch pipe; 115. a fourth branch pipe; 116. a product branch pipe; 117. a raw material air inlet valve; 118. a first-cycle intake valve; 119. a hot hydrogen outlet valve; 120. a first circulating gas outlet valve; 121. a hot hydrogen inlet valve; 122. a second-cycle intake valve; 123. a second circulation gas outlet valve; 124. and a product gas outlet valve.
Detailed Description
The present invention will be described in further detail with reference to examples, but the present invention is not limited thereto.
Example 1
As a most basic embodiment of the present invention, this embodiment discloses an adsorption tower for hydrogen purification in polycrystalline silicon production process, as shown in fig. 1 and fig. 2, including adsorption tower main part 1, 1 top of adsorption tower main part is provided with first gas and imports and exports 2, 1 below of adsorption tower main part is provided with second business turn over gas port 3, 1 vertical direction of adsorption tower main part is provided with a plurality of heating pipes 5, heating pipe 5 is the hollow tube that the lower extreme seals, be provided with electric heating pipe 6 in the heating pipe 5, electric heating pipe 6 includes insulating heat-conducting layer 6.1 and electric heating wire 6.2, electric heating wire 6.2 and insulating heat-conducting layer 6.1 set up in heating pipe 5, the intussuseption of adsorption tower main part 1 is filled with active carbon 7.
Example 2
As an optimal embodiment of the present invention, this embodiment discloses an adsorption tower for hydrogen purification in polycrystalline silicon production process, as shown in fig. 1 and fig. 2, including adsorption tower main part 1, 1 top of adsorption tower main part is provided with first gas inlet and outlet 2, 1 below of adsorption tower main part is provided with second business turn over gas port 3, 1 vertical direction of adsorption tower main part is provided with a plurality of heating pipes 5, heating pipe 5 is the hollow tube that the lower extreme seals, be provided with electric heating pipe 6 in the heating pipe 5, electric heating pipe 6 includes insulating heat-conducting layer 6.1 and electric heating wire 6.2, electric heating wire 6.2 and insulating heat-conducting layer 6.1 set up in heating pipe 5, the intussuseption of adsorption tower main part 1 is filled with active carbon 7.
Preferably, the electric heating wire 6.2, the insulating heat conduction layer 6.1 and the heating pipe 5 are arranged in sequence from inside to outside.
Preferably, the heating pipes 5 are uniformly arranged on the adsorption tower main body 1.
Preferably, a feed inlet is arranged above the adsorption tower main body 1.
Example 3
As an optimal embodiment of the present invention, this embodiment discloses an adsorption tower for hydrogen purification in polycrystalline silicon production process, as shown in fig. 1 and fig. 2, including adsorption tower main part 1, 1 top of adsorption tower main part is provided with first gas inlet and outlet 2, 1 below of adsorption tower main part is provided with second business turn over gas port 3, 1 vertical direction of adsorption tower main part is provided with a plurality of heating pipes 5, heating pipe 5 is the hollow tube that the lower extreme seals, be provided with electric heating pipe 6 in the heating pipe 5, electric heating pipe 6 includes insulating heat-conducting layer 6.1 and electric heating wire 6.2, electric heating wire 6.2 and insulating heat-conducting layer 6.1 set up in heating pipe 5, the intussuseption of adsorption tower main part 1 is filled with active carbon 7.
Preferably, the electric heating wire 6.2, the insulating heat conduction layer 6.1 and the heating pipe 5 are arranged in sequence from inside to outside.
Preferably, the heating pipes 5 are uniformly arranged on the adsorption tower main body 1.
Preferably, a feed inlet is arranged above the adsorption tower main body 1.
Preferably, the outer wall of the adsorption tower main body 1 is provided with a cooling device 9, the cooling device 9 adopts a cooling coil or a cooling jacket, the lower end of the cooling device 9 is provided with a cooling water inlet 9.1, and the upper end of the cooling device 9 is provided with a cooling water outlet 9.2.
Preferably, the insulating and heat conducting layer 6.1 is made of materials such as boron nitride, aluminum oxide or magnesium oxide.
Preferably, the activated carbon 7 is coconut shell activated carbon 7 or coal activated carbon 7.
The working principle is as follows: in the using process, four adsorption towers are used together, and each tower sequentially carries out the steps of adsorption I, heating regeneration, cooling, adsorption II and the like, so that the raw material gas is adsorbed twice, the purity of H2 obtained by adsorption is higher, and the regeneration rate of the adsorption towers is higher.
A hydrogen purification device in a polysilicon production process comprises 4 adsorption towers, wherein a second gas inlet and outlet 3 is respectively connected with a raw material inlet pipe 101, a first circulation pipeline 102, a hot hydrogen outlet pipe 105 and a second circulation pipeline 106, the second gas inlet and outlet 3 is connected with the raw material inlet pipe 101 through a raw material branch pipe 103, the second gas inlet and outlet 3 is connected with the first circulation pipeline 102 through a first branch pipe 104, the second gas inlet and outlet 3 is connected with the hot hydrogen outlet pipe 105 through a first hot hydrogen branch pipe 107, the second gas inlet and outlet 3 is connected with the second circulation pipeline 106 through a second branch pipe 108, a cooler 109 is arranged at the joint of the first circulation pipeline 102 and the second circulation pipeline 106, a first gas inlet and outlet 2 is arranged above the adsorption towers, the first gas inlet and outlet 2 are respectively connected with the hot hydrogen inlet pipe 110, a product 111 and a third circulation pipeline 112, the first gas inlet and outlet 2 is connected with the hot hydrogen inlet pipe 110 through a second hot hydrogen branch pipe 113, the first gas inlet/outlet 2 is connected to the third circulation line 112 through a third branch line 114 and a fourth branch line 115, and the first gas inlet/outlet 2 is connected to the product outlet pipe 111 through a product branch line 116.
Preferably, a raw material inlet valve 117 is arranged on the raw material branch pipe 103, a first circulation inlet valve 118 is arranged on the first branch pipe 104, a hot hydrogen outlet valve 119 is arranged on the first hot hydrogen branch pipe 107, a first circulation outlet valve 120 is arranged on the second branch pipe 108, a hot hydrogen inlet valve 121 is arranged on the second hot hydrogen branch pipe 113, a second circulation inlet valve 122 is arranged on the third branch pipe 114, a second circulation outlet valve 123 is arranged on the fourth branch pipe 115, and a product outlet valve 124 is arranged on the product branch pipe 116.
For the a adsorption column (other adsorption columns are identical in principle):
stage 1 adsorption I: as shown in FIG. 4, starting Material H2Firstly, the H enters into the adsorption tower A from a second gas inlet and outlet 3 at the bottom, the initial adsorption operation is started, and the H after the initial adsorption2Pure H is obtained from a first gas inlet and outlet 2 of the A adsorption tower2Sending to the first gas inlet and outlet 2 of the B adsorption tower, and purifying the H2And (4) discharging from a second gas inlet and outlet 3 of the B adsorption tower, cooling the B adsorption tower, and finally entering the C adsorption tower through the second gas inlet and outlet 3 of the C adsorption tower to perform secondary adsorption. After the adsorption tower A adsorbs a period of time theta 1, the impurity adsorption of the active carbon 7 in the adsorption tower A reaches saturation, the adsorption tower A no longer has adsorption capacity, and the raw material H2Then the adsorption tower is switched to the adsorption tower C for primary adsorption.
Stage 2 regeneration: as shown in fig. 5, the adsorption tower a starts to perform heating regeneration, and in the regeneration stage, the resistance wire in the electric heating tube 6 in the adsorption tower a is electrified to heat the activated carbon 7 in the adsorption tower a. The electric heating pipes 6 are more in arrangement and small in distance, the temperature of the electric heating pipes 6 can reach 300 ℃ or even higher, and the heat transfer temperature difference between the electric heating pipes and the active carbon 7 is large. At the same time, a small amount of heat H is blown back from the top2The impurities desorbed from the activated carbon 7 are carried out of the adsorption tower A. Heating and regenerating the adsorption tower A for a period of time theta 2, completely regenerating the activated carbon 7 in the adsorption tower A, and starting to enter a third stage, namely cooling.
Stage 3 cooling: as shown in fig. 6, the adsorption column a heats the regenerated activated carbon 7, which has a high temperature and requires cooling to have adsorption capacity. The cooling mode adopts part or all of H after the initial adsorption2By means of back-flushing cooling, i.e. H initially adsorbed by the B adsorption column2Blowing into the adsorption column A from the top partially or totally, due to the beginning of the discharge from the adsorption column BAdsorbed H2The temperature is low and is less than or equal to about 20 ℃, and the activated carbon 7 in the adsorption tower A is cooled by H after a period of theta 32And (4) cooling. Cold back flushing H of A adsorption tower2Heated by the activated carbon 7, discharged from the bottom of the adsorption column A, cooled by the external cooler 109, and then introduced into the adsorption column D for reabsorption purification.
Stage 4 adsorption II: as shown in FIG. 7, the adsorption column A is cooled to a predetermined temperature, and then it is cooled by the external cooler 109 to receive H from the adsorption column C2Secondary adsorption is carried out to obtain a product H with higher purity2. After a period of time θ 4, a cycle is completed and the initial stage I of stage 1 is repeated.
The sequential temporal and spatial representation of the four adsorption columns is given in table 2.
TABLE 2
Time A B C D
θ1 Adsorption I Cooling down Adsorption II Heating regeneration
θ2 Heating regeneration Adsorption II Adsorption I Cooling down
θ3 Cooling down Adsorption I Heating regeneration Adsorption II
θ4 Adsorption II Heating regeneration Cooling down Adsorption I
The beneficial effects of this technical scheme are as follows:
(1) the built-in electric heating tube 6 is adopted, so that the regeneration temperature is high, and the regeneration is thorough.
(2) No liquid enters the adsorption tower, so that adverse effects caused by leakage are avoided.
(3) An electric heating tube 6 is arranged in the heater, and electric power is completely used for heating the active carbon 7, so that heat loss is avoided.
(4) The system of cold and hot fluid is cancelled, and the investment, operation and maintenance cost is greatly reduced.
(5) The regeneration and cooling time is shortened.
The above is only the preferred embodiment of the present invention, not to the limitation of the present invention in any form, all the technical matters of the present invention all fall into the protection scope of the present invention to any simple modification and equivalent change of the above embodiments.

Claims (7)

1. An adsorption tower for hydrogen purification in a polycrystalline silicon production process is characterized in that: including adsorption tower main part (1), adsorption tower main part (1) top is provided with first gas and imports and exports (2), adsorption tower main part (1) below is provided with second business turn over gas port (3), adsorption tower main part (1) vertical direction is provided with a plurality of heating pipes (5), heating pipe (5) are the hollow tube that the lower extreme sealed, be provided with insulating heat-conducting layer (6.1) and electric heating wire (6.2) in heating pipe (5), adsorption tower main part (1) intussuseption is filled with active carbon (7).
2. The adsorption tower for hydrogen purification in the polysilicon production process according to claim 1, wherein: the electric heating wire (6.2), the insulating heat conduction layer (6.1) and the heating pipe (5) are sequentially arranged from inside to outside.
3. The adsorption tower for hydrogen purification in the polysilicon production process according to claim 1, wherein: the heating pipes (5) are uniformly arranged in the adsorption tower main body (1).
4. The adsorption tower for hydrogen purification in the polysilicon production process according to claim 1, wherein: a feed inlet is arranged above the adsorption tower main body (1).
5. The adsorption tower for hydrogen purification in the polysilicon production process according to claim 1, wherein: the adsorption tower is characterized in that a cooling device (9) is arranged on the outer wall of the adsorption tower main body (1), a cooling water inlet (9.1) is formed in the lower end of the cooling device (9), and a cooling water outlet (9.2) is formed in the upper end of the cooling device (9).
6. The adsorption tower for hydrogen purification in the polysilicon production process according to claim 1, wherein: the insulating heat conduction layer (6.1) is made of boron nitride or aluminum oxide or magnesium oxide.
7. The adsorption tower for hydrogen purification in the polysilicon production process according to claim 1, wherein: the activated carbon (7) is coconut shell activated carbon (7) or coal activated carbon (7).
CN202021561147.5U 2020-07-31 2020-07-31 Adsorption tower for hydrogen purification in polycrystalline silicon production process Active CN213314182U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115055026A (en) * 2022-05-25 2022-09-16 云南通威高纯晶硅有限公司 Method for purifying mixed gas by using tube array adsorption column

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115055026A (en) * 2022-05-25 2022-09-16 云南通威高纯晶硅有限公司 Method for purifying mixed gas by using tube array adsorption column

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