CN221045497U - Heavy impurity device of fresh material recycling system - Google Patents
Heavy impurity device of fresh material recycling system Download PDFInfo
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- CN221045497U CN221045497U CN202322581048.3U CN202322581048U CN221045497U CN 221045497 U CN221045497 U CN 221045497U CN 202322581048 U CN202322581048 U CN 202322581048U CN 221045497 U CN221045497 U CN 221045497U
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- pipeline
- oxysilane
- heavy
- chlorosilane
- reflux
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- 239000012535 impurity Substances 0.000 title claims abstract description 68
- 239000000463 material Substances 0.000 title claims abstract description 25
- 238000004064 recycling Methods 0.000 title abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 35
- 238000010992 reflux Methods 0.000 claims description 41
- 238000000605 extraction Methods 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 abstract description 41
- 239000005046 Chlorosilane Substances 0.000 abstract description 40
- 238000009835 boiling Methods 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 10
- 229910021420 polycrystalline silicon Inorganic materials 0.000 abstract description 9
- 229920005591 polysilicon Polymers 0.000 abstract description 8
- 239000012071 phase Substances 0.000 abstract description 7
- 239000007791 liquid phase Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000000197 pyrolysis Methods 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 17
- PHEXXGCUKSJMBJ-UHFFFAOYSA-N [O].[SiH4] Chemical compound [O].[SiH4] PHEXXGCUKSJMBJ-UHFFFAOYSA-N 0.000 description 12
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 8
- HICCMIMHFYBSJX-UHFFFAOYSA-N [SiH4].[Cl] Chemical compound [SiH4].[Cl] HICCMIMHFYBSJX-UHFFFAOYSA-N 0.000 description 8
- 239000006227 byproduct Substances 0.000 description 6
- 238000005336 cracking Methods 0.000 description 6
- 238000007599 discharging Methods 0.000 description 6
- 230000007062 hydrolysis Effects 0.000 description 6
- 238000006460 hydrolysis reaction Methods 0.000 description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 5
- 229910052796 boron Inorganic materials 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 229910000077 silane Inorganic materials 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 3
- 239000005052 trichlorosilane Substances 0.000 description 3
- 230000000737 periodic effect Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000011874 heated mixture Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
The utility model discloses a heavy impurity recycling device for a fresh material system, and relates to the technical field of polysilicon production equipment. The main technical scheme of the utility model is as follows: a device for recycling heavy impurities in a fresh material system is characterized in that a mixture of oxysilane and chlorosilane and heavy impurities generated by the fresh material system are input into a rectifying tower, liquid-phase oxysilane and gas-phase heavy impurities form countercurrent and transfer mass and heat mutually, heavy-component oxysilane and light-component chlorosilane are separated, the heavy-component oxysilane enters a tower kettle, the light-component chlorosilane is cooled and then extracted for recycling, chlorosilane mixed in high-boiling pyrolysis residual oxysilane can be recycled, and complex compounds in the heavy impurities can be removed by using the oxysilane, so that the chlorosilane is recycled, and the technical effects of saving energy and improving the utilization rate of raw materials are achieved. The utility model is mainly used for separating chlorosilane.
Description
Technical Field
The utility model relates to the technical field of polysilicon production equipment, in particular to a heavy impurity device for a fresh material recycling system.
Background
In the process of producing polysilicon by adopting the Siemens method, byproduct oxysilane can be produced, the boiling points of the oxysilane and disilane are similar, and in the process of cracking the silane at high boiling point, the oxysilane is mixed into the process of cracking the silane at high boiling point and can not be cracked, so that the process can gradually gather, the high boiling point cracking reaction can be influenced after the process reaches a certain degree, and the requirement of the high boiling point cracking reaction is met by periodically eliminating the oxysilane.
In the process of producing polysilicon, the separation and purification of trichlorosilane are extremely critical procedures, the quality grade of the produced polysilicon is directly determined, the prior production process adopts a rectification method to separate and purify the trichlorosilane, and some adsorption impurity removing devices are added in the flow, so that some light component trace impurities which are difficult to remove by rectification are further removed, and concentrated heavy impurities are directly hydrolyzed.
In the prior art, a treatment mode of the mixture of the oxygen silane and the chlorine silane and the concentrated heavy impurities mainly adopts periodical hydrolysis, and the periodical hydrolysis can effectively treat the mixture of the oxygen silane and the chlorine silane and the complex in the concentrated heavy impurities, but the mode can cause yield loss, meanwhile, the hydrolysis also can cause waste of water resources, taking 4.5 ten thousand tons of polysilicon as an example, a fresh material system generates 1.2t heavy impurities per hour to directly hydrolyze, so that yield loss is caused, 300kg of oxygen silane is generated per hour to hydrolyze, and 300kg of chlorine silane is taken out along with the oxygen silane to participate in the reaction, so that the yield loss is caused, and further the production cost and the energy consumption of the polysilicon are improved.
Disclosure of utility model
In view of the above, the embodiment of the utility model provides a device for recycling heavy impurities in a fresh material system, and mainly aims to provide a device for recycling heavy impurities in a fresh material system, which can recycle a mixture of oxysilane and chlorosilane and a complex in concentrated heavy impurities.
In order to achieve the above purpose, the present utility model mainly provides the following technical solutions:
The embodiment of the utility model provides a device for recycling heavy impurities of a fresh material system, which comprises:
The rectification component comprises a rectification tower, a mixture pipeline and a heavy impurity pipeline, wherein the mixture pipeline is connected with an upper feed inlet of the rectification tower, and the heavy impurity pipeline is connected with a lower feed inlet of the rectification tower;
The heating component is connected to the bottom of the rectifying tower;
A cooling part connected to the top of the rectifying column;
and the extraction component is connected to the bottom of the rectifying tower.
Further, the cooling part comprises a cooler, a reflux tank and an output pipeline, one end of the cooler is connected to the top of the rectifying tower, the other end of the cooler is connected to the reflux tank, and the output pipeline is connected to the reflux tank.
Further, the reflux component comprises a reflux pump and a reflux pipeline, one end of the reflux pump is connected with the reflux tank, the other end of the reflux pump is connected with the reflux pipeline, the reflux pipeline is connected with the top of the rectifying tower, and the output pipeline is connected with the middle part of the reflux pipeline.
Further, the extraction component comprises a kettle liquid pump and an extraction pipeline, wherein one end of the kettle liquid pump is connected to the bottom of the rectifying tower, and the other end of the kettle liquid pump is connected to the extraction pipeline.
Further, the extraction component further comprises a connecting pipeline, one end of the connecting pipeline is connected to the middle part of the extraction pipeline, and the other end of the connecting pipeline is connected to the mixture pipeline.
Further, the on-off valve is arranged on the mixture pipeline, the heavy impurity pipeline and the connecting pipeline respectively.
Compared with the prior art, the utility model has the following technical effects:
According to the technical scheme provided by the embodiment of the utility model, the mixture of the oxygen silane and the chlorine silane and heavy impurities generated by a fresh material system are input into the rectifying tower, the liquid phase oxygen silane and the gas phase heavy impurities form countercurrent and transfer mass and heat mutually, the heavy component oxygen silane and the light component chlorine silane are separated, the heavy component oxygen silane enters into the tower kettle, the light component chlorine silane is cooled and then extracted and recovered, so that the chlorine silane mixed in the residual oxygen silane after high-boiling pyrolysis can be recovered, and the complex in the heavy impurities can be removed by utilizing the oxygen silane, thereby achieving the technical effects of recovering the chlorine silane, saving energy and improving the utilization rate of raw materials.
Drawings
Fig. 1 is a schematic structural diagram of a device for recycling heavy impurities in a fresh material system according to an embodiment of the present utility model.
Detailed Description
The utility model is described in further detail below with reference to the drawings and examples.
Before the specific embodiments are described, some terms in the specification need to be described, which are as follows:
heavy impurities mainly refer to impurities which are discharged from a fresh material system and are difficult to remove by rectification, and in the technical scheme, mainly refer to a mixture of chlorosilane and complex containing boron and phosphorus, wherein the complex of boron and phosphorus is converged in the chlorosilane.
The mixture of the oxysilane and the chlorosilane mainly refers to a mixture produced by mixing the oxysilane and the chlorosilane generated in the process of high-boiling pyrolysis of the silane, wherein the chlorosilane refers to a mixture of trichlorosilane and silicon tetrachloride.
As shown in fig. 1, the embodiment of the utility model further provides a device for recycling heavy impurities of a fresh material system, which comprises:
The rectification component comprises a rectification tower 11, a mixture pipeline 12 and a heavy impurity pipeline 13, wherein the mixture pipeline 12 is connected to an upper feed inlet of the rectification tower 11, and the heavy impurity pipeline 13 is connected to a lower feed inlet of the rectification tower 11;
a heating unit connected to the bottom of the rectifying column 11;
A cooling unit connected to the top of the rectifying column 11;
And a discharge unit connected to the bottom of the rectifying column 11.
In the technical scheme, the rectification component is used for separating different components and comprises a rectification tower 11, a mixture pipeline 12 and a heavy impurity pipeline 13, wherein the mixture pipeline 12 is connected with an upper feed inlet of the rectification tower 11, the heavy impurity pipeline 13 is connected with a lower feed inlet of the rectification tower 11, and the on-off valve 6 is arranged on the mixture pipeline 12 and the heavy impurity pipeline 13; the heating component is used for gasifying heavy impurities and is connected to the bottom of the rectifying tower 11; the cooling part is used for cooling the discharged chlorosilane and is connected to the top of the rectifying tower 11; the effect of the extraction part is to split the discharged oxysilane, the extraction part is connected to the bottom of the rectifying tower 11, compared with the prior art, the treatment mode of the complex in the mixture of the oxysilane and the chlorosilane and the concentrated heavy impurities mainly adopts periodic hydrolysis, the mixture of the oxysilane and the chlorosilane and the complex in the concentrated heavy impurities can be effectively treated by the periodic hydrolysis, but the mode can cause yield loss, and meanwhile, the hydrolysis can also cause waste of water resources.
Further, the cooling part includes a cooler 31, a reflux drum 32, and an output pipe 33, one end of the cooler 31 is connected to the top of the rectifying tower 11, the other end is connected to the reflux drum 32, and the output pipe 33 is connected to the reflux drum 32. In this embodiment, a cooling component is further defined, one end of the cooler 31 is connected to the top of the rectifying tower 11, the other end is connected to the reflux tank 32, chlorosilane is discharged from the top of the rectifying tower 11 and enters the cooler 31 to be cooled, and then enters the reflux tank 32, so that the technical effect of reducing the temperature of chlorosilane is achieved, optionally, a reflux component is added, the reflux component comprises a reflux pump 51 and a reflux pipeline 52, one end of the reflux pump 51 is connected to the reflux tank 32, the other end of the reflux pump is connected to the reflux pipeline 52, the reflux pipeline 52 is connected to the top of the rectifying tower 11, the output pipeline 33 is connected to the middle part of the reflux pipeline 52, part of chlorosilane returns to the rectifying tower 11 through the reflux pipeline 52 under the action of the reflux pump 51, so that the heat balance in the rectifying tower 11 is maintained, and meanwhile, the accuracy of product separation can be increased, and the rest of chlorosilane enters a fresh material system, so that the technical effects of maintaining the heat balance of the rectifying tower 11 and increasing the product separation accuracy are achieved.
Further, the extraction component comprises a tank pump 41 and an extraction pipeline 42, wherein one end of the tank pump 41 is connected to the bottom of the rectifying tower 11, and the other end is connected to the extraction pipeline 42. In this embodiment, a discharging part is further defined, the tank pump 41 provides power to convey the oxysilane into the tower kettle through the discharging pipeline 42, so as to achieve the effect of rapidly discharging the oxysilane, optionally, the discharging part further comprises a connecting pipeline 43, one end of the connecting pipeline 43 is connected to the middle part of the discharging pipeline 42, the other end of the connecting pipeline is connected to the mixture pipeline 12, the on-off valve 6 is arranged on the connecting pipeline 43, and because the oxysilane is used as a formed byproduct, the yield is lower, the situation that current interruption exists during the operation of the equipment, heavy impurities can be caused to enter the rectifying tower 11 without contacting the oxysilane, and then directly enter the top of the rectifying tower 11, so that the quality of the product is affected, and therefore, part of the oxysilane is introduced into the mixture pipeline 12 of the oxysilane and the chlorosilane, so that sufficient oxysilane enters the rectifying tower 11 from an upper feeding port and is fully contacted and reacted after heavy impurities are gasified, and the technical effect of reducing the risk is achieved.
The specific method of the technical scheme is as follows:
101. And (3) introducing the mixture of the oxysilane and the chlorosilane into an upper feed inlet of the rectifying tower.
The byproduct oxysilane can be generated in the process of producing the polycrystalline silicon by the Siemens method, and because the boiling points of the oxysilane and the chlorosilane are similar, the oxysilane can not be cracked in the process of cracking the silane at high boiling point, so that the oxysilane can not be accumulated in the chlorosilane, and when the quantity of the oxysilane reaches a certain degree, the high boiling point cracking reaction can be influenced, so that the oxysilane needs to be eliminated periodically, and the mixture mixed with the oxysilane and the chlorosilane is introduced into the upper feed inlet of the rectifying tower, so that the mixture of the oxysilane and the chlorosilane is positioned at the upper part of heavy impurities.
102. Concentrating heavy impurities generated by the fresh material system, and then introducing the heavy impurities into a lower feed inlet of the rectifying tower.
The fresh material system mainly treats fresh material, heavy impurities can be generated in the treatment process, the heavy impurities mainly comprise complex compounds of boron and phosphorus, and the heavy impurities are introduced into a feed opening of a rectifying tower after being concentrated, so that the heavy impurities are positioned at the lower part of a mixture of the oxygen silane and the chlorosilane.
103. The heavy impurities are heated by a reboiler to form gas phase heavy impurities and rise.
The heavy impurities are heated by a reboiler to raise the heavy impurities in the gas phase into the mixture of the oxysilane and the chlorosilane.
104. The liquid phase oxygen silicane and the gas phase heavy impurities form countercurrent and transfer mass and heat with each other, and the heavy component oxygen silicane and the light component chlorosilane are separated.
The heated mixture of gas phase heavy impurities and liquid phase oxygen silicane and chlorsilane transfer mass and heat mutually, heavy component oxygen silicane is discharged from the bottom of the rectifying tower, and light component chlorsilicane is discharged from the top of the rectifying tower.
105. And (3) the heavy component oxygen silane enters a tower kettle.
And discharging part of the heavy component oxysilane from the bottom of the rectifying tower, and then entering the tower kettle for subsequent working procedures.
106. Part of the heavy component oxysilane is passed into the mixture line of oxysilane and chlorosilane.
Part of heavy component oxysilane enters a mixture pipeline of the oxysilane and the chlorosilane, the effect is that because the oxysilane is used as a formed byproduct, the yield is lower, the situation that cutoff exists possibly exists during the operation of equipment, heavy impurities are directly discharged from the top of a rectifying tower without being contacted with the oxysilane after entering the rectifying tower, and then the heavy impurities directly enter a fresh material system, so that the quality of a product is influenced, and therefore, part of the oxysilane is introduced into the mixture pipeline of the oxysilane and the chlorosilane, and sufficient contact reaction is ensured after the sufficient oxysilane enters the rectifying tower from an upper feed inlet and is gasified by heavy impurities.
107. Part of the light chlorosilane enters a fresh material system, and part of the light chlorosilane flows back to the top of the rectifying tower.
Part of light chlorosilane enters a fresh material system to carry out subsequent procedures, and part of light chlorosilane flows back to the rectifying tower to maintain heat balance in the rectifying tower, and meanwhile, the product separation precision can be increased.
Taking a 4.5 ten thousand ton polysilicon device as an example, the heavy impurity produced by a fresh material system per hour is about 1.2t, the produced byproduct oxysilane is about 300kg/h, the impurity content of the top of the tower is far lower than the impurity content of the heavy impurity of the fresh material system after the heavy impurity and the byproduct oxysilane enter a rectifying tower and are mutually transferred by mass and heat, the impurity content of imported boron is about 0.05ug/ml, and the impurity content of the boron at the top of the tower is about 0.001ug/ml; according to the technical scheme provided by the embodiment of the utility model, the mixture of the oxysilane and the chlorosilane and heavy impurities generated by a fresh material system are input into a rectifying tower, the liquid-phase oxysilane and the gas-phase heavy impurities form countercurrent and transfer mass and heat mutually, the heavy-component oxysilane and the light-component chlorosilane are separated, the heavy-component oxysilane enters a tower kettle, the light-component chlorosilane is extracted and recovered after being cooled, and the chlorosilane mixed in the high-boiling pyrolysis residual oxysilane can be recovered, and complex compounds in the heavy impurities can be removed by utilizing the oxysilane, so that the chlorosilane is recovered, and the technical effects of saving energy and improving the utilization rate of raw materials are achieved.
The foregoing is merely illustrative of the present utility model, and the present utility model is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present utility model. Therefore, the protection scope of the present utility model shall be subject to the protection scope of the claims.
Claims (6)
1. An apparatus for recovering heavy impurities from a fresh material system, comprising:
The rectification component comprises a rectification tower, a mixture pipeline and a heavy impurity pipeline, wherein the mixture pipeline is connected with an upper feed inlet of the rectification tower, and the heavy impurity pipeline is connected with a lower feed inlet of the rectification tower;
The heating component is connected to the bottom of the rectifying tower;
A cooling part connected to the top of the rectifying column;
and the extraction component is connected to the bottom of the rectifying tower.
2. The apparatus of claim 1, wherein the device comprises a plurality of sensors,
The cooling part comprises a cooler, a reflux tank and an output pipeline, one end of the cooler is connected to the top of the rectifying tower, the other end of the cooler is connected to the reflux tank, and the output pipeline is connected to the reflux tank.
3. The apparatus as recited in claim 2, further comprising:
The reflux component comprises a reflux pump and a reflux pipeline, one end of the reflux pump is connected with the reflux tank, the other end of the reflux pump is connected with the reflux pipeline, the reflux pipeline is connected with the top of the rectifying tower, and the output pipeline is connected with the middle part of the reflux pipeline.
4. The apparatus of claim 1, wherein the device comprises a plurality of sensors,
The extraction component comprises a kettle liquid pump and an extraction pipeline, wherein one end of the kettle liquid pump is connected to the bottom of the rectifying tower, and the other end of the kettle liquid pump is connected to the extraction pipeline.
5. The apparatus of claim 4, wherein the device comprises a plurality of sensors,
The extraction component further comprises a connecting pipeline, one end of the connecting pipeline is connected to the middle part of the extraction pipeline, and the other end of the connecting pipeline is connected to the mixture pipeline.
6. The apparatus as recited in claim 5, further comprising:
The on-off valve is respectively arranged on the mixture pipeline, the heavy impurity pipeline and the connecting pipeline.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322581048.3U CN221045497U (en) | 2023-09-22 | 2023-09-22 | Heavy impurity device of fresh material recycling system |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322581048.3U CN221045497U (en) | 2023-09-22 | 2023-09-22 | Heavy impurity device of fresh material recycling system |
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| Publication Number | Publication Date |
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| CN221045497U true CN221045497U (en) | 2024-05-31 |
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| CN202322581048.3U Active CN221045497U (en) | 2023-09-22 | 2023-09-22 | Heavy impurity device of fresh material recycling system |
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