CN112678829A - High-purity disilane continuous production system and preparation process - Google Patents
High-purity disilane continuous production system and preparation process Download PDFInfo
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- CN112678829A CN112678829A CN202110105858.4A CN202110105858A CN112678829A CN 112678829 A CN112678829 A CN 112678829A CN 202110105858 A CN202110105858 A CN 202110105858A CN 112678829 A CN112678829 A CN 112678829A
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- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000010924 continuous production Methods 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 52
- 229910000077 silane Inorganic materials 0.000 claims description 52
- 238000000197 pyrolysis Methods 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000009835 boiling Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 8
- 238000000354 decomposition reaction Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000011863 silicon-based powder Substances 0.000 claims description 6
- 238000000746 purification Methods 0.000 claims description 5
- 239000002699 waste material Substances 0.000 claims description 5
- 239000007795 chemical reaction product Substances 0.000 claims description 4
- 238000000926 separation method Methods 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 12
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- VEDJZFSRVVQBIL-UHFFFAOYSA-N trisilane Chemical compound [SiH3][SiH2][SiH3] VEDJZFSRVVQBIL-UHFFFAOYSA-N 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000012856 packing Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910001868 water Inorganic materials 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000005234 chemical deposition Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 229910021338 magnesium silicide Inorganic materials 0.000 description 2
- YTHCQFKNFVSQBC-UHFFFAOYSA-N magnesium silicide Chemical compound [Mg]=[Si]=[Mg] YTHCQFKNFVSQBC-UHFFFAOYSA-N 0.000 description 2
- 229920000548 poly(silane) polymer Polymers 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- FXMNVBZEWMANSQ-UHFFFAOYSA-N chloro(silyl)silane Chemical compound [SiH3][SiH2]Cl FXMNVBZEWMANSQ-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
The invention discloses a high-purity disilane continuous production system and a preparation process, and belongs to the technical field of chemical reaction separation. The one end of feed line and pre-heater is connected, the other end of pre-heater passes through the pipeline and is connected with the feed end of reactor, the discharge end of reactor passes through the pipeline and is connected with the one end of filter, the other end of filter passes through the pipeline and is connected with rectifying column I, I top of the tower of rectifying column is connected with the reactor feed end through the pipeline, I bottom of the tower of rectifying column is connected with rectifying column II through the pipeline, II tops of the tower of rectifying column are connected with the retort through the pipeline, II bottoms of the tower of rectifying column are connected with the collector through the pipeline. The system can realize continuous production of high-purity disilane products, and the purity of the disilane produced by the system reaches more than 99.999 percent.
Description
Technical Field
The invention relates to a high-purity disilane continuous production system and a preparation process, and belongs to the technical field of chemical reaction separation.
Background
The high-purity disilane is an important raw material in the processes of solar cells, amorphous silicon films, chemical deposition and the like, mainly applied to the growth of silicon nitride films and silicon oxide films by a semiconductor technology, and has the characteristics of high deposition speed and low deposition temperature compared with silane in the chemical deposition process. Can prevent the generation of spherical protrusions in amorphous silicon and improve the uniformity of deposition, and is mainly used for manufacturing high-end chips below 20 nanometers. In ion implantation, the disilane beam current is strong, and the effect is better than other ion sources. In semiconductor technology, which is used for epitaxy and diffusion process, disilane is used, and cheap glass can be used to replace expensive quartz glass as the substrate of LCD.
The preparation method of disilane mainly comprises the following steps: silane is heated and transformed into disilane, a chloro disilane reduction method, magnesium silicide is reacted with ammonium chloride for synthesis, magnesium silicide is reacted with inorganic acid, a direct synthesis method of silicon and hydrogen, and the like. In comparison, the disilane is prepared by adopting the silane as the raw material, and the method has the advantages of single raw material, easy purification and continuous production.
Disilane can be obtained by pyrolysis of silane. However, at the high temperatures of pyrolysis, more silane is converted to elemental silicon, with the formation of worthless by-products such as polysilane. Therefore, an efficient method for producing disilane, which is suitable for mass production, is sought.
The pyrolysis production of disilane also produces other silanes. Chip manufacturing requires a high purity of disilane. The removal of a large amount of other side-reaction impurities results in loss of the target product and the purification cost is high. Therefore, a production method and apparatus with less generation of impurities by side reactions are required.
Disclosure of Invention
The invention provides a continuous production system and a process method of high-purity disilane, which can realize continuous production of high-purity disilane products by adopting a continuous rectification method, and the purity of the disilane produced by the system reaches more than 99.999 percent.
The invention provides a high-purity disilane continuous production system, wherein a feeding pipeline is connected with one end of a preheater, the other end of the preheater is connected with the feeding end of a reactor through a pipeline, the discharging end of the reactor is connected with one end of a filter through a pipeline, the other end of the filter is connected with a rectifying tower I through a pipeline, the top of the rectifying tower I is connected with the feeding end of the reactor through a pipeline, the bottom of the rectifying tower I is connected with a rectifying tower II through a pipeline, the top of the rectifying tower II is connected with a collector through a pipeline, and the bottom of the rectifying tower II is connected with a mixing tank through a pipeline.
Further, in the above technical solution, the temperature of the preheater is set to 380-400 ℃.
Further, in the above technical solution, the temperature of the reactor is set to 430-.
Further, in the technical scheme, the raw silane enters the preheater through the feeding pipeline, the feeding pressure of the raw silane is more than or equal to 0.2MPa, and the feeding speed is 3-5 kg/h.
A continuous production preparation process of high-purity disilane comprises the following steps:
1) starting a preheater, preheating to 380-400 ℃, starting a reactor, and preheating to 430-480 ℃;
2) introducing raw silane into the preheater through a feed pipe, wherein the feeding pressure of the raw silane is more than or equal to 0.2MPa, and the feeding speed is 3-5 kg/h;
3) preheating silane to 380-400 ℃ in a preheater, and then introducing the silane into a reactor to carry out pyrolysis reaction at 430-480 ℃ to produce disilane;
4) the reaction product enters a filter for filtration, and silicon powder generated by decomposition is removed;
5) further purifying in a rectifying tower I, feeding silane obtained at the top of the rectifying tower I at the top temperature into a feed inlet of a reactor for further pyrolysis reaction, and feeding the bottom material flow of the rectifying tower I into a rectifying tower II for further purification;
6) disilane obtained from the top of the rectifying tower II enters a collector, and high boiling point substances at the bottom of the rectifying tower II enter a mixing tank for waste treatment.
The new device is used for manufacturing high-purity disilane, and provides a method for producing disilane from silane. The preheating temperature of the silane is controlled to be 380-. The introducing pressure of the raw material silane is kept above 0.2 MPa.
Advantageous effects of the invention
The system of the invention is designed and used with a preheater to avoid overheating of the process stream and to minimize the residence time of the material in the reaction system to minimize the formation of undesirable silane impurities and to minimize the decomposition of reactants and products into elemental silicon. And recovering unreacted silane and returning the silane to the reaction system. The mixture after pyrolysis reaction in the reactor contains target product disilane, and simultaneously contains hydrogen, silane, silicon powder, trisilane, siloxane and the like, and in order to obtain high-purity disilane, a double-stage rectification process is adopted to realize the separation of the products. The mixture has relatively large boiling point difference and is suitable for purification by a rectification method, and the reaction mixture passes through a rectification tower to remove high-boiling-point polysilane, low-boiling-point silane, hydrogen and the like. The system can realize continuous production of high-purity disilane products, and the purity of the disilane produced by the system reaches more than 99.999 percent.
Drawings
FIG. 1 is a schematic view of a continuous production system for high purity disilane.
In the figure, 1, a preheater; 2. a reactor; 3. a filter; 4. a rectifying tower I; 5. a rectifying tower II; 6. a mixing tank; 7. a collector.
Detailed Description
The following non-limiting examples will allow one of ordinary skill in the art to more fully understand the present invention, but are not intended to limit the invention in any way.
Example 1
The utility model provides a high-purity disilane continuous production system, feed line is connected with pre-heater 1's one end, pre-heater 1's the other end passes through the pipeline and is connected with the feed end of reactor 2, reactor 2's discharge end passes through the pipeline and is connected with the one end of filter 3, the other end of filter 3 passes through the pipeline and is connected with rectifying column I4, rectifying column I4 top of the tower is connected with 2 feed ends of reactor through the pipeline, rectifying column I4 bottom of the tower is connected with rectifying column II 5 through the pipeline, rectifying column II 5 top of the tower is connected with collector 7 through the pipeline, rectifying column II 5 bottom of the tower is connected with blending tank 6 through the pipeline.
The temperature of the preheater 1 was set to 380-400 ℃. The temperature of the reactor 2 was set to 430-. Raw silane enters the preheater 1 through a feeding pipeline, the feeding pressure of the raw silane is more than or equal to 0.2MPa, and the feeding speed is 3-5 kg/h.
Example 2
A continuous production preparation process of high-purity disilane comprises the following steps:
1) starting a preheater, preheating to 400 ℃, starting a reactor, and preheating to 450 ℃; the preheater is a 316L stainless steel pipe with the length of about 900mm and the diameter of 60 mm; the volume of the reactor is 12L, and the length is 600 mm;
2) introducing raw silane into the preheater through a feed pipeline, wherein the feed pressure of the raw silane is 0.55MPa, and the feed rate is 3 kg/h;
3) preheating silane to 400 ℃ in a preheater, and then feeding the silane into a reactor to carry out pyrolysis reaction at 450 ℃ to produce disilane; the composition of the obtained material is 97.6 wt% of silane and 2.1 wt% of disilane;
4) the product enters a filter for filtration, and silicon powder generated by decomposition is removed;
5) feeding the intermediate material, purifying the intermediate material in a rectifying tower I (the diameter is 100mm, the theta ring packing and the effective packing height are 8000mm), feeding silane obtained at the top of a tower top temperature rectifying tower I into a reactor, continuously carrying out pyrolysis reaction, emptying hydrogen obtained at the top of the tower top temperature rectifying tower I, and purifying the bottom material flow of the rectifying tower I, which comprises high boiling point substances such as disilane, trisilane and siloxane, in a rectifying tower II (the diameter is 300mm, the theta ring packing and the effective packing height are 1000 mm);
6) disilane obtained from the top of the rectifying tower II enters a collector, and high boiling point substances obtained from the bottom of the rectifying tower II enter a mixing tank for waste treatment.
The mixture is separated by a rectifying tower I, the byproduct silane and hydrogen are removed as light component materials (hydrogen is exhausted), the polysilanesiloxane and the like are removed as heavy components by a rectifying tower II, high-purity disilane is collected for detection, and the content of impurities such as oxygen, nitrogen, carbon dioxide, water, silane, trisilane, siloxane and the like is less than 10 ppm.
Example 3
1) Starting a preheater, preheating to 380 ℃, starting a reactor, and preheating to 430 ℃;
2) introducing raw silane into the preheater through a feed pipeline, wherein the feeding pressure of the raw silane is more than or equal to 0.2MPa, and the feeding rate is 5 kg/h;
3) preheating silane to 380 ℃ in a preheater, and then feeding the silane into a reactor to carry out pyrolysis reaction at 480 ℃ to produce disilane;
4) the reaction product enters a filter for filtration, and silicon powder generated by decomposition is removed;
5) the silane obtained at the top of the tower top temperature rectifying tower I enters a feed inlet of a reactor to be subjected to pyrolysis reaction continuously, hydrogen obtained at the top of the tower top temperature rectifying tower I is exhausted, and the bottom material flow of the rectifying tower I comprises high boiling point substances such as disilane, trisilane, siloxane and the like and enters a rectifying tower II to be purified;
6) disilane obtained from the top of the rectifying tower II enters a collector, and high boiling point substances at the bottom of the rectifying tower II enter a mixing tank for waste treatment.
Example 4
1) Starting a preheater, preheating to 400 ℃, starting a reactor, and preheating to 480 ℃;
2) introducing raw silane into the preheater through a feed pipeline, wherein the feeding pressure of the raw silane is more than or equal to 0.2MPa, and the feeding rate is 5 kg/h;
3) preheating silane to 380 ℃ in a preheater, and then feeding the silane into a reactor to carry out pyrolysis reaction at 430 ℃ to produce disilane;
4) the reaction product enters a filter for filtration, and silicon powder generated by decomposition is removed;
5) the silane obtained at the top of the tower top temperature rectifying tower I enters a feed inlet of a reactor to be subjected to pyrolysis reaction continuously, hydrogen obtained at the top of the tower top temperature rectifying tower I is exhausted, and the bottom material flow of the rectifying tower I comprises high boiling point substances such as disilane, trisilane, siloxane and the like and enters a rectifying tower II to be purified;
6) disilane obtained from the top of the rectifying tower II enters a collector, and high boiling point substances at the bottom of the rectifying tower II enter a mixing tank for waste treatment.
Example 5
The procedure was as in example 2, except that the feed rate of the starting silane was 5 kg/hr and the reactor temperature was 440 ℃.
And 3) performing pyrolysis reaction on the reactor in the step 3), wherein the obtained material composition is 98.1% of silane and 1.3% of disilane, separating a mixture which enters a rectifying tower through a filter, collecting disilane for detection, and the content of impurities such as oxygen, nitrogen, carbon dioxide, water, silane, trisilane and siloxane is less than 10 ppm.
Example 6
The procedure is the same as in example 2, except that: preheating silane to 380 deg.c in preheater, and pyrolyzing at 480 deg.c in reactor to produce disilane. After pyrolysis reaction, filtering and rectifying the obtained material twice, collecting disilane for detection, and detecting, wherein the content of impurities such as oxygen, nitrogen, carbon dioxide, water, silane, trisilane, siloxane and the like is less than 10 ppm.
Claims (5)
1. The utility model provides a high-purity disilane continuous production system, a serial communication port, the one end of feed line and pre-heater (1) is connected, the other end of pre-heater (1) passes through the pipeline and is connected with the feed end of reactor (2), the discharge end of reactor (2) passes through the pipeline and is connected with the one end of filter (3), the other end of filter (3) passes through the pipeline and is connected with rectifying column I (4), rectifying column I (4) top of the tower passes through the pipeline and is connected with reactor (2) feed end, rectifying column I (4) bottom of the tower passes through the pipeline and is connected with rectifying column II (5), rectifying column II (5) top of the tower passes through the pipeline and is connected with collector (7), rectifying column II (5) bottom of the tower passes through the pipeline and is connected with blending tank (6).
2. The continuous production system of high purity disilane according to claim 1, wherein the temperature of the preheater (1) is set at 380-400 ℃.
3. The continuous production system for high purity disilane according to claim 1, wherein the temperature of the reactor (2) is set at 430-480 ℃.
4. The continuous production system of high-purity disilane according to claim 1, wherein the raw silane enters the preheater (1) through a feeding pipeline, the feeding pressure of the raw silane is more than or equal to 0.2MPa, and the feeding rate is 3-5 kg/h.
5. A continuous production preparation process of high-purity disilane is characterized by comprising the following steps:
1) starting a preheater, preheating to 380-400 ℃, starting a reactor, and preheating to 430-480 ℃;
2) introducing raw silane into the preheater through a feed pipe, wherein the feeding pressure of the raw silane is more than or equal to 0.2MPa, and the feeding speed is 3-5 kg/h;
3) preheating silane to 380-400 ℃ in a preheater, and then introducing the silane into a reactor to carry out pyrolysis reaction at 430-480 ℃ to produce disilane;
4) the reaction product enters a filter for filtration, and silicon powder generated by decomposition is removed;
5) further purifying in a rectifying tower I, feeding silane obtained at the top of the rectifying tower I at the top temperature into a feed inlet of a reactor for further pyrolysis reaction, and feeding the bottom material flow of the rectifying tower I into a rectifying tower II for further purification;
6) disilane obtained from the top of the rectifying tower II enters a collector, and high boiling point substances at the bottom of the rectifying tower II enter a mixing tank for waste treatment.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114314596A (en) * | 2021-12-01 | 2022-04-12 | 全椒亚格泰电子新材料科技有限公司 | Method and system for continuously synthesizing high-order silane by utilizing microwave heating fixed bed |
| CN114436264A (en) * | 2021-12-29 | 2022-05-06 | 浙江中宁硅业有限公司 | Production process and production system of silane |
| CN115403048A (en) * | 2022-10-13 | 2022-11-29 | 中船(邯郸)派瑞特种气体股份有限公司 | Method for purifying disilane |
| CN115591272A (en) * | 2022-10-27 | 2023-01-13 | 大连科利德光电子材料有限公司（Cn） | Method and system for purifying silicon-based precursor |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10647582B1 (en) * | 2019-09-11 | 2020-05-12 | Taiwan Speciality Chemicals Corporation | High efficiency synthesis and purification recycling system of higher silane |
-
2021
- 2021-01-26 CN CN202110105858.4A patent/CN112678829A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10647582B1 (en) * | 2019-09-11 | 2020-05-12 | Taiwan Speciality Chemicals Corporation | High efficiency synthesis and purification recycling system of higher silane |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114314596A (en) * | 2021-12-01 | 2022-04-12 | 全椒亚格泰电子新材料科技有限公司 | Method and system for continuously synthesizing high-order silane by utilizing microwave heating fixed bed |
| CN114314596B (en) * | 2021-12-01 | 2024-01-19 | 全椒亚格泰电子新材料科技有限公司 | Method and system for continuously synthesizing higher-order silane by utilizing microwave heating fixed bed |
| CN114436264A (en) * | 2021-12-29 | 2022-05-06 | 浙江中宁硅业有限公司 | Production process and production system of silane |
| CN115403048A (en) * | 2022-10-13 | 2022-11-29 | 中船(邯郸)派瑞特种气体股份有限公司 | Method for purifying disilane |
| CN115403048B (en) * | 2022-10-13 | 2023-11-07 | 中船(邯郸)派瑞特种气体股份有限公司 | Disilane purification method |
| CN115591272A (en) * | 2022-10-27 | 2023-01-13 | 大连科利德光电子材料有限公司（Cn） | Method and system for purifying silicon-based precursor |
| CN115591272B (en) * | 2022-10-27 | 2023-04-07 | 大连科利德光电子材料有限公司 | Method and system for purifying silicon-based precursor |
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Application publication date: 20210420 |