CN203529944U - Low-temperature disilane rectification device - Google Patents

Low-temperature disilane rectification device Download PDF

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Publication number
CN203529944U
CN203529944U CN201320559665.7U CN201320559665U CN203529944U CN 203529944 U CN203529944 U CN 203529944U CN 201320559665 U CN201320559665 U CN 201320559665U CN 203529944 U CN203529944 U CN 203529944U
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cooling tower
low
tower kettle
temperature
tower reactor
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CN201320559665.7U
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郑春宁
何波
徐昕
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NANJING ARGO TECH NEW ENERGY MATERIALS Co Ltd
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NANJING ARGO TECH NEW ENERGY MATERIALS Co Ltd
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Abstract

The utility model discloses a low-temperature disilane rectification device which comprises low-temperature condensers, refrigerating machines, a first cooling tower kettle and a second rectification tower kettle, wherein the low-temperature condensers and the refrigerating machines are arranged on the first cooling tower kettle and the second rectification tower kettle; a gas inlet is formed in the low-temperature condenser connected with the first cooling tower kettle; a gas outlet is formed in the low-temperature condenser connected with the second rectification tower kettle; the first cooling tower kettle is connected with the second rectification tower kettle by virtue of a heat insulation pipeline; a grid tray and a filler layer are arranged in the first cooling tower kettle; a gas heating coiled pipe is arranged in the second rectification tower kettle. The low-temperature disilane rectification device is simple in structure and low in investment cost and is convenient to operate, so that 99 percent of disilane discharged from a reaction system is recycled and separated out; by virtue of second-stage low-temperature rectification, the purity of the disilane can meet the quality standard of 99.995 percent; a factory can conveniently produce the disilane with the high purity of 4N for high-end chips of superlarge-scale integrated circuits of lower than 20nm; the application range is large.

Description

A kind of silicoethane hypothermia distillation device
Technical field
The utility model relate to silicoethane production unit, relate in particular to a kind of silicoethane hypothermia distillation device.
Background technology
In the process of silicon magnesium legal system for silane, be attended by silicoethane generation.Its important factor is: synthetic Mg 2in Si, there is high-order silicon magnesium compound Mg 3si 2exist.Its reaction formula is as follows:
Figure 2013205596657100002DEST_PATH_IMAGE001
Silane, silicoethane and a small amount of gas mixtures such as H2 from reactive system out, in its gas phase, the boiling point of main component is: silane boiling point :-112.15 ℃ (1atm), silicoethane boiling point :-14.15 ℃ (1atm), hydrogen boiling point :-252.76 ℃ (1atm), due to silicoethane boiling point significantly high than silane, hydrogen, so adopt low temperature fractionation separating-purifying according to boiling point difference, be out a kind of economical and practical Technology.
At present on the market silicoethane purifying plant, the separating effect of monomer whose rectifying tower is poor, silicoethane can not be separated completely with foreign gas, the silicoethane of producing gas purity lower, cannot reach industrial needs.
Utility model content
For the problem of above-mentioned existence, the utility model object is to provide the silicoethane that a kind of multistage hypothermia distillation device flows out reactive system separate and purify with silane and other foreign gas, make silicoethane purity reach 99.995% quality standard.
In order to achieve the above object, the technical solution adopted in the utility model is as follows: a kind of silicoethane hypothermia distillation device, described hypothermia distillation device comprises subcooling condenser, refrigerator, the first cooling tower reactor and Second distillation column still, on the first described cooling tower reactor and Second distillation column still, be equipped with subcooling condenser and refrigerator, the subcooling condenser of the connection of the first described cooling tower reactor is provided with gas feed, the subcooling condenser that described Second distillation column still connects is provided with pneumatic outlet, the first described cooling tower reactor is connected by heat insulation pipeline with the second cooling tower reactor, in the first described cooling tower reactor, be provided with screen and packing layer, in described Second distillation column still, be provided with gas heating coil pipe.
In the first described cooling tower reactor, the head temperature of subcooler is controlled at-50 ℃, make silicoethane condensation get off to enter the first cooling tower reactor, by screen and packing layer, separated other gases, the silicoethane that condensation is got off enters Second distillation column still from heat insulation pipeline, will in the gas heating coil pipe in Second distillation column still, pass into hot N 2heat up, allow liquid phase seethe with excitement, on Second distillation column still, the head temperature of subcooler is controlled at-20 ℃, and the silane of trace in liquid phase is separated from top gaseous phase outlet, thereby obtains the silicoethane of high purity 99.995%.
As a kind of improvement of the present utility model, the outside of described the first cooling tower reactor, Second distillation column still and heat insulation pipeline is provided with low temperature thermofin, by thermofin, has guaranteed the cryogenic effect between tower reactor and connecting pipeline, reduces heat-transfer effect, stable system, separation efficiency is high.
As a kind of improvement of the present utility model, described heat insulation pipeline is provided with flow control valve, by flow control valve, according to practical situation, regulates the silicoethane liquid flow rate between the first cooling tower reactor and Second distillation column still, improves the transformation efficiency of reaction.
As a kind of improvement of the present utility model, described subcooling condenser is shell and tube heat exchanger, and described refrigerator is connected on the tube side of shell and tube heat exchanger, and the cooling system of described device and distillation system are separated into different pipelines, and rectification effect is good.
The utility model has the advantage of: the utility model is simple in structure, equipment investment cost is little; Easy to operate, make in reactive system silicoethane 99% out reclaim and separate, by secondary low temperature fractionation, make silicoethane purity reach 99.995% quality standard; The silicoethane that facilitates the high purity 4N of the high-end chip below production super large-scale integration 20 nanometers of producer, usage range is wide.
Accompanying drawing explanation
Fig. 1 is the utility model structure diagram;
Wherein, 1 first cooling tower reactor, 2 Second distillation column stills, 3 subcooling condensers, 4 coolers, 5 packing layers, 6 screens, 7 heat insulation pipelines, 8 flow control valves, 9 gas heating coil pipes.
Embodiment
Below in conjunction with accompanying drawing explanation and embodiment, the utility model is described in further detail.
embodiment 1:a kind of silicoethane hypothermia distillation device as shown in Figure 1, described hypothermia distillation device comprises subcooling condenser 3, refrigerator 4, the first cooling tower reactor 1 and Second distillation column still, on the first described cooling tower reactor 1 and Second distillation column still 2, be equipped with subcooling condenser 3 and refrigerator 4, the subcooling condenser 3 of the connection of the first described cooling tower reactor 1 is provided with gas feed, the subcooling condenser 3 that described Second distillation column still 2 connects is provided with pneumatic outlet, the first described cooling tower reactor 1 is connected by heat insulation pipeline 7 with the second cooling tower reactor 2, in the first described cooling tower reactor 1, be provided with screen 6 and packing layer 7, in described Second distillation column still 2, be provided with gas heating coil pipe 9.
embodiment 2:the working method of this device as shown in Figure 1, in the first described cooling tower reactor 1, the head temperature of subcooling condenser 3 is controlled at-50 ℃, make silicoethane condensation get off to enter the first cooling tower reactor 1, by screen 6 and packing layer 7, separated other gases, the silicoethane that condensation is got off enters Second distillation column still 2 from heat insulation pipeline 7, will in the gas heating coil pipe 9 in Second distillation column still, pass into hot N 2heat up, allow liquid phase seethe with excitement, on Second distillation column still 2, the head temperature of subcooling condenser 3 is controlled at-20 ℃, and the silane of trace in liquid phase is separated from top gaseous phase outlet, thereby obtains the silicoethane of high purity 99.995%.
embodiment 3:as shown in Figure 1, the outside of described the first cooling tower reactor 1, Second distillation column still 2 and heat insulation pipeline 7 is provided with low temperature thermofin, by thermofin, has guaranteed the cryogenic effect between tower reactor and connecting pipeline, reduces heat-transfer effect, stable system, and separation efficiency is high.
embodiment 4:as shown in Figure 1, described heat insulation pipeline 7 is provided with flow control valve 8, by flow control valve 8, according to practical situation, regulates the silicoethane liquid flow rate between the first cooling tower reactor 1 and Second distillation column still 2, improves the transformation efficiency of reaction.
embodiment 5:as shown in Figure 1, described subcooling condenser 3 is shell and tube heat exchanger, and described refrigerator 4 is connected on the tube side of shell and tube heat exchanger, and the cooling system of described device and distillation system are separated into different pipelines, and rectification effect is good.
It should be noted that, above-mentioned is only preferred embodiment of the present utility model, is not used for limiting protection domain of the present utility model, and the equivalents of having done on the basis of above-described embodiment all belongs to protection domain of the present utility model.

Claims (4)

1. a silicoethane hypothermia distillation device, described hypothermia distillation device comprises subcooling condenser, refrigerator, the first cooling tower reactor and Second distillation column still, on the first described cooling tower reactor and Second distillation column still, be equipped with subcooling condenser and refrigerator, it is characterized in that, the subcooling condenser of the connection of the first described cooling tower reactor is provided with gas feed, the subcooling condenser that described Second distillation column still connects is provided with pneumatic outlet, the first described cooling tower reactor is connected by heat insulation pipeline with the second cooling tower reactor, in the first described cooling tower reactor, be provided with screen and packing layer, in described Second distillation column still, be provided with gas heating coil pipe.
2. a kind of silicoethane hypothermia distillation device according to claim 1, is characterized in that, the outside of described the first cooling tower reactor, Second distillation column still and heat insulation pipeline is provided with low temperature thermofin.
3. a kind of silicoethane hypothermia distillation device according to claim 1 and 2, is characterized in that, described heat insulation pipeline is provided with flow control valve.
4. a kind of silicoethane hypothermia distillation device according to claim 1, is characterized in that, described subcooling condenser is shell and tube heat exchanger, and described refrigerator is connected on the tube side of shell and tube heat exchanger.
CN201320559665.7U 2013-09-10 2013-09-10 Low-temperature disilane rectification device Expired - Fee Related CN203529944U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113893567A (en) * 2021-11-01 2022-01-07 中船重工(邯郸)派瑞特种气体有限公司 Low-temperature rectifying tower for preparing monofluoromethane

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113893567A (en) * 2021-11-01 2022-01-07 中船重工(邯郸)派瑞特种气体有限公司 Low-temperature rectifying tower for preparing monofluoromethane
CN113893567B (en) * 2021-11-01 2022-09-27 中船(邯郸)派瑞特种气体股份有限公司 Low-temperature rectifying tower for preparing monofluoromethane

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