CN202898052U - Production device of <11>boron trifluoride electronic specific gas - Google Patents

Production device of <11>boron trifluoride electronic specific gas Download PDF

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Publication number
CN202898052U
CN202898052U CN 201220327007 CN201220327007U CN202898052U CN 202898052 U CN202898052 U CN 202898052U CN 201220327007 CN201220327007 CN 201220327007 CN 201220327007 U CN201220327007 U CN 201220327007U CN 202898052 U CN202898052 U CN 202898052U
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gas
tower
cracker
chemical exchange
synthesizer
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Expired - Fee Related
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CN 201220327007
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Chinese (zh)
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张卫江
徐姣
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Tianjin University
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Tianjin University
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Abstract

The utility model relates to a production device of <11>boron trifluoride electronic specific gas, which is formed by connecting a synthesis device 2, a chemical exchange tower 3 with a cracking device 5 in series, wherein an overhead condenser 4 is arranged on the top of a cracking tower; a heating kettle 6 is arranged at the bottom of the tower; liquid phase flowing down from the synthesis device is pumped to the top of the chemical exchange tower through a pump and then is pumped to the top of the cracking device through a pump; gas heated and cracked through the cracking device enters from the bottom of the chemical exchange tower through the condenser, carries out counter-current with the liquid phase flowing down, and carries out exchange reaction with the liquid phase, so that <11>B is enriched in a gas phase; and in addition, after anisole gas rising in the cracking device is condensed, the anisole gas is subjected to heat exchange through a heat exchanger 7, is pumped to the top of the synthesis device through a pump, and carries out synthesis reaction again. The production device of the <11>boron trifluoride electronic specific gas disclosed by the utility model has the effects that a feasible process technology and the production device are provided for industrial production of high-abundance and high-purity <11>BF3 electronic specific gas; the gas abundance of the obtained <11>BF3 product is up to 99.7%; the purity is up to 99.995%; and product requirements of <11>BF3 electronic specific gas at home and abroad currently can be satisfied.

Description

The production equipment of the special gas of boron trifluoride-11 electronics
Technical field
The present invention relates to boron trifluoride-11( 11BF 3) production equipment and the method for the special gas of electronics, technology is applicable to the industries such as electronics, medicine, and high abundance, high purity needs are provided for it 11BF 3Production technique.
Background technology
Boron trifluoride-11( 11BF 3) gas has very many-sided application on industrial production, can be used for electronic industry and optical fiber industry, can be used as the raw material of preparation fibre-optical preform, is the P type doped source of silicon and germanium extension, diffusion and ion implantation process.In semiconductor fabrication 11BF 3Be important ion implantation gas, be used for silicon ion cloth as boron dope agent simultaneously and plant the aspect, the chip of producing has high integrated, high-density characteristics, and volume is little, superior performance.Along with the develop rapidly of electronics, communications industry, 11BF 3The application of gas also has very large development prospect.
For 11BF 3Production, there are large-scale commercial production factory in developed country such as the U.S., Germany, Japan etc., wherein BASF AG of Allied-signal Inc. (US) Columbia Road and Park Avenue, Morris Township, Morris C of the U.S. and Germany produce bottled 11BF 3Higher impact is arranged in the world, and Japanese iron and steel chemical company produces 11BF 3Although higher purity is arranged, its scale less.China does not still possess at present 11BF 3The throughput of gas.
11BF 3The Technology of gas generation mainly contains two difficult points: the one, and the abundance requirement. 11BF 3The abundance of the special gas of electronics requires 〉=99.7%, and 11The B natural abundance is about 80%.The 2nd, purity requirement. 11BF 3As the special gas of electronics, quite strict to the requirement of various impurity, reach the ppm level, the total purity of product 〉=99.995%.Last century the eighties, China carries out the tackling key problem of high gas, product purity reaches more than 99.995%, has realized the production of ultrapure product, its technology is used for the fields such as aerospace, photovoltaic solar on a large scale, for the production of the special gas of electronics is laid a good foundation.Thereby real restriction 11BF 3The special gas factor of production of electronics is 99.7% abundance requirement, the present domestic successfully report that not yet has.
Summary of the invention
The technology of the present invention takes the lead in having proposed at home 11BF 3The gas generation Technology, the product abundance reaches more than 99.7%, satisfies the requirement of the special gas industry of electronics, but is the technological line of a heavy industrialization.
Technical scheme of the present invention is as follows:
A kind of boron trifluoride-11( 11BF 3) production equipment of the special gas of electronics, be in series by synthesizer (2), chemical exchange tower (3), cracker (5); The cracking cat head is provided with heating kettle (6) at the bottom of being provided with overhead condenser (4), tower; Jet flow from synthesizer and under liquid phase, beat to the chemical exchange cat head by pump, beat to the cracker cat head through pump again; The gas of opening through the cracker heating pyrolyze enters from the chemical exchange tower bottom through condenser, the liquid phase adverse current lower with spray, and the generation permutoid reaction makes 11B is enrichment in gas phase; After the methyl-phenoxide condensation of gas that rises in the cracker is got off, first by interchanger 7 heat exchange, beat to the synthesizer cat head through pump again, building-up reactions occurs again.
11BF 3Pneumatic outlet is connected with adsorption unit, and adsorption unit is comprised of one-level adsorption tower (10), secondary absorption tower (11), middle pressure rectifying tower (12) and low-pressure distillation tower (14).BF to be clean 3Gas is entered by adsorption tower (10) top, enter again adsorption tower (11) top from the bottom after out, and then bottom middle pressure rectifying tower (12), enter, therefrom press rectifying tower (12) top out by by intermediate condenser (13), by entering in the low-pressure distillation tower (14), high-purity for after purifying of low-pressure distillation tower (14) bottom 11BF 3Gas product.
Enrichment of the present invention 11BF 3Method, boron trifluoride unstripped gas enters from synthesizer (2) bottom, and methyl-phenoxide then descends from synthesizer (2) top jet flow, under 10-25 ℃ service temperature, complex reaction occurs form boron trifluoride-methyl-phenoxide complex compound; The BF that is come by cracking in the cracker 3Gas is entered by chemical exchange tower (3) bottom, and gas-liquid counter current fully contacts, and under 15-30 ℃ service temperature, chemical exchange reaction occurs; Heavier 11The B isotropic substance with gas form in the cat head enrichment, lighter 10The B isotropic substance is enrichment in liquid complexing thing at the bottom of the tower then; After the enrichment 11BF 3Gas enters into synthesizer (2) by the bottom, again with the synthetic liquid complexing thing of methyl-phenoxide; Enrichment 10The isotopic liquid complexing thing of B then enters decomposer (5), 140-170 ℃ of decomposes is 11BF 3Lean gas enters chemical exchange tower (3) again and carries out chemical exchange; So repeatedly operation, until 11BF 3Gas 11The B abundance reaches more than 99.7%, from 11BF 3Products export 8 places extraction product.
From 11BF 3The enrichment of products export extraction 11BF 3Gas, in one-level adsorption tower (10) after the foreign gas of remove portion, enter the secondary absorption tower (11) of in-built activated alumina, further remove foreign gas, last gas enters the rectifier unit that is comprised of middle pressure rectifying tower (12) and low-pressure distillation tower (14), in two rectifying tower, carry out repeatedly gas-to-liquid contact and mass transfer, finally obtain purity up to 99.995% 11BF 3Gas product obtains from rectifying tower (14) bottom.
Effect of the present invention is to be the high abundance high purity 11BF 3The suitability for industrialized production of the special gas of electronics provides a feasible Technology and production equipment, acquisition 11BF 3The gas product abundance reaches family 99.7%, and purity reaches more than 99.995%, satisfies at present both at home and abroad 11BF 3The product requirement of the special gas of electronics.
Description of drawings
Fig. 1: chemical exchange distillation enrichment 11BF 3Process flow sheet;
Fig. 2: gas purifying technique and device schema;
1.BF 3Steel cylinder; 2. synthesizer; 3. chemical exchange tower; 4. condenser; 5. cracker; 6. heating kettle; 7. interchanger; 8. 11BF 3Gas product; 9. 10BF 3The methyl-phenoxide complex compound; 10. one-level adsorption tower; 11. secondary absorption tower; 12. middle pressure rectifying tower; The reboiler 13. intermediate condenser is held concurrently; 14. low-pressure distillation tower.
Embodiment
Adopt raw material: the boron triflouride gas of natural abundance and methyl-phenoxide.
Install as shown in Figure 1, 2: be in series by synthesizer (2), chemical exchange tower (3), cracker (5); The cracking cat head is provided with heating kettle (6) composition at the bottom of being provided with overhead condenser (4), tower; Jet flow from synthesizer and under liquid phase, beat to the chemical exchange cat head by pump, beat to the cracker cat head through pump again; The gas of opening through the cracker heating pyrolyze enters from the chemical exchange tower bottom through condenser, the liquid phase adverse current lower with spray, and the generation permutoid reaction makes 11B is enrichment in gas phase; After the methyl-phenoxide condensation of gas that rises in the cracker is got off, first by interchanger 7 heat exchange, beat to the synthesizer cat head through pump again, building-up reactions occurs again.
11BF 3Pneumatic outlet is connected with adsorption unit, and adsorption unit one-level adsorption tower (10), secondary absorption tower (11), middle pressure rectifying tower (12) and low-pressure distillation tower (14) form.BF to be clean 3Gas is entered by one-level adsorption tower (10) top, enter again secondary absorption tower (11) top from the bottom after out, and then bottom middle pressure rectifying tower (12), enter, therefrom press rectifying tower (12) top out by by intermediate condenser (13), by entering in the low-pressure distillation tower (14), low-pressure distillation tower (14) bottom is the high-purity BF after purifying 3Gas product.
Example 1: unstripped gas steel cylinder 1 boron trifluoride unstripped gas enters from the synthesizer bottom, and methyl-phenoxide then descends from synthesizer top jet flow, under 10-15 ℃ service temperature, complex reaction occurs form boron trifluoride-methyl-phenoxide complex compound.The BF that cracking is come in cracker 3Gas is entered by the chemical exchange tower bottom, and gas-liquid counter current fully contacts, and under 20-25 ℃ service temperature, chemical exchange reaction occurs.Heavier 11The B isotropic substance with gas form in the cat head enrichment, lighter 10The B isotropic substance is enrichment in liquid complexing thing at the bottom of the tower then.After the enrichment 11BF 3Gas enters into synthesizer by the bottom, again with the synthetic liquid complexing thing of complexing agent.Enrichment 10The isotopic liquid complexing thing of B then enters cracker, 140-150 ℃ of decomposes is 11BF 3Lean gas enters exchange column again and carries out chemical exchange.So endless operation, until 11BF 3Gas 11The B abundance reaches more than 99.7%, the extraction product.Then enter adsorption tower and carry out removal of impurities, behind the gas feed through cooling and in one-level adsorption tower 10 the further foreign gas of remove portion, again will 11BF 3Be filled with the secondary absorption tower 11 of in-built activated alumina, further remove foreign gas, last gas enters the rectifier unit that is comprised of middle pressure rectifying tower and low-pressure distillation tower, carry out repeatedly gas-to-liquid contact and mass transfer in two rectifying tower, and finally obtaining purity can be up to 99.995% 11BF 3Gas product.
Example 2: boron trifluoride unstripped gas enters from the synthesizer bottom, and methyl-phenoxide then descends from synthesizer top jet flow, under 15-20 ℃ service temperature, complex reaction occurs form boron trifluoride-methyl-phenoxide complex compound.The BF that cracking is come in cracker 3Gas is entered by the chemical exchange tower bottom, and gas-liquid counter current fully contacts, and under 25-30 ℃ service temperature, chemical exchange reaction occurs.Heavier 11The B isotropic substance with gas form in the cat head enrichment, lighter 10The B isotropic substance is enrichment in liquid complexing thing at the bottom of the tower then.After the enrichment 11BF 3Gas enters into synthesizer by the bottom, again with the synthetic liquid complexing thing of complexing agent.Enrichment 10The isotopic liquid complexing thing of B then enters cracker, 150-160 ℃ of decomposes is 11BF 3Lean gas enters exchange column again and carries out chemical exchange.So endless operation, until 11BF 3Gas 11The B abundance reaches more than 99.7%, the extraction product.Then enter adsorption tower and carry out removal of impurities, behind the gas feed through cooling and in one-level adsorption tower 10 the further foreign gas of remove portion, again will 11BF 3Be filled with the secondary absorption tower 11 of in-built activated alumina, further remove foreign gas, last gas enters the rectifier unit that is comprised of middle pressure rectifying tower and low-pressure distillation tower, carry out repeatedly gas-to-liquid contact and mass transfer in two rectifying tower, and finally obtaining purity can be up to 99.995% 11BF 3Gas product.
Example 3: boron trifluoride unstripped gas (1) enters from the synthesizer bottom, and methyl-phenoxide then descends from synthesizer top jet flow, under 20-25 ℃ service temperature, complex reaction occurs form boron trifluoride-methyl-phenoxide complex compound.The BF that cracking is come in cracker 3Gas is entered by the chemical exchange tower bottom, and gas-liquid counter current fully contacts, and under 15-20 ℃ service temperature, chemical exchange reaction occurs.Heavier 11The B isotropic substance with gas form in the cat head enrichment, lighter 10The B isotropic substance is enrichment in liquid complexing thing at the bottom of the tower then.After the enrichment 11BF 3Gas enters into synthesizer by the bottom, again with the synthetic liquid complexing thing of complexing agent.Enrichment 10The isotopic liquid complexing thing of B then enters cracker, 160-170 ℃ of decomposes is 11BF 3Lean gas enters exchange column again and carries out chemical exchange.So endless operation, until 11BF 3Gas 11The B abundance reaches more than 99.7%, the extraction product.Then enter adsorption tower and carry out removal of impurities, behind the gas feed through cooling and in one-level adsorption tower 10 the further foreign gas of remove portion, again will 11BF 3Be filled with the secondary absorption tower 11 of in-built activated alumina, further remove foreign gas, last gas enters the rectifier unit that is comprised of middle pressure rectifying tower and low-pressure distillation tower, carry out repeatedly gas-to-liquid contact and mass transfer in two rectifying tower, and finally obtaining purity can be up to 99.995% 11BF 3Gas product.
Boron trifluoride-11(of the present invention 11BF 3) production equipment of the special gas of electronics, those skilled in the art can be by using for reference this paper content, and the links such as appropriate change processing parameter, structure design realize.System of the present invention is described by different examples of implementation, and person skilled obviously can be changed or suitably change and combination system as herein described within not breaking away from content of the present invention, spirit and scope, realizes the technology of the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are deemed to be included in spirit of the present invention, scope and the content.

Claims (2)

1. the production equipment of the special gas of boron trifluoride-11 electronics is characterized in that being in series by synthesizer (2), chemical exchange tower (3), cracker (5); The cracking cat head is provided with heating kettle (6) at the bottom of being provided with overhead condenser (4), tower; Jet flow from synthesizer and under liquid phase, beat to the chemical exchange cat head by pump, beat to the cracker cat head through pump again; The gas of opening through the cracker heating pyrolyze enters from the chemical exchange tower bottom through condenser, the liquid phase adverse current lower with spray, and the generation permutoid reaction makes 11B is enrichment in gas phase; After the methyl-phenoxide condensation of gas that rises in the cracker is got off, first by interchanger (7) heat exchange, beat to the synthesizer cat head through pump again, building-up reactions occurs again.
2. device as claimed in claim 1 is characterized in that 11BF 3Pneumatic outlet is connected with adsorption unit, and adsorption unit is comprised of one-level adsorption tower (10), secondary absorption tower (11), middle pressure rectifying tower (12) and low-pressure distillation tower (14); BF to be clean 3Gas is entered by adsorption tower (10) top, enter again adsorption tower (11) top from the bottom after out, and then bottom middle pressure rectifying tower (12), enter, therefrom press rectifying tower (12) top out by by intermediate condenser (13), by entering in the low-pressure distillation tower (14), low-pressure distillation tower (14) bottom is the high-purity BF after purifying 3Gas product.
CN 201220327007 2012-07-06 2012-07-06 Production device of <11>boron trifluoride electronic specific gas Expired - Fee Related CN202898052U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102774845A (en) * 2012-07-06 2012-11-14 天津大学 Device and method for producing boron trifluoride-11 electronic specific gas
CN105582811A (en) * 2014-11-16 2016-05-18 浙江创世雷博科技有限公司 Raw material purification method for boron isotope separation
CN113583032A (en) * 2021-07-23 2021-11-02 上海化工研究院有限公司 Cracking device and method for boron trifluoride complex

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102774845A (en) * 2012-07-06 2012-11-14 天津大学 Device and method for producing boron trifluoride-11 electronic specific gas
CN105582811A (en) * 2014-11-16 2016-05-18 浙江创世雷博科技有限公司 Raw material purification method for boron isotope separation
CN105582811B (en) * 2014-11-16 2018-04-17 浙江创世雷博科技有限公司 A kind of purification of raw materials method for Separation of Boron Isotopes
CN113583032A (en) * 2021-07-23 2021-11-02 上海化工研究院有限公司 Cracking device and method for boron trifluoride complex
CN113583032B (en) * 2021-07-23 2024-02-27 上海化工研究院有限公司 Cracking device and method for boron trifluoride complex

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Granted publication date: 20130424

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