Production device for improving purity of silane

Abstract

The utility model discloses a production device for improving the purity of silane, which comprises a first heat exchanger which is sequentially connected with a primary purification component and a secondary purification component through a pipeline, the primary purification assembly comprises a first resin column used for carrying out liquid phase adsorption on liquid silane and a first rectifying tower used for carrying out rectification separation on the silane, and the secondary purification assembly comprises a second resin column used for carrying out gas phase adsorption on silane gas and a second rectifying tower used for carrying out rectification separation on the silane. According to the utility model, two purification operations of resin complexing adsorption and rectification are combined for the first time, and the permutation and combination of rectification and complexing adsorption are optimized again, so that the purpose of removing impurities is achieved. According to the process, the removal and rectification load of trace impurities by single rectification operation is greatly reduced, and the rectification pressure and energy consumption can be effectively reduced.

Description

TECHNICAL FIELD

[0001] The utility model relates to the technical field of silane purification equipment, specifically relates to a production device of improving silane purity. BACKGROUND

[0002] Electronic grade silane gas is mainly applied to the fields of semiconductor manufacturing, solar cell, display panel and the like, is often applied to chemical vapor deposition, chemical mechanical polishing and the other key processes in integrated circuit, and the tiny gas purity difference will lead to the reduction of the whole product performance even scrap. Electronic gas purity often requires 5N above grade, and the purity of silane gas reaches 6N (99.9999%) and above. At present, the nonmetallic impurities such as hydrogen, nitrogen, arsenic, boron, phosphorus and the like in silane are removed by rectification mode mostly in domestic, but the rectification purification time is long, the efficiency is low, and the impurity removal effect is poor. UTILITARY MODEL

[0003] The utility model aims at providing a production device of improving silane purity to solve the above insufficient in prior art.

[0004] In order to realize the above-mentioned purpose, the utility model provides the following technical scheme: a production device of improving silane purity, comprising: first heat exchanger, the first heat exchanger is connected with primary purification assembly and secondary purification assembly in proper order through pipeline, the primary purification assembly includes the first resin column for carrying out liquid phase adsorption to liquid silane and the first rectifying column for rectifying separation to silane, the secondary purification assembly includes the second resin column for carrying out gas phase adsorption to silane gas and the second rectifying column for rectifying separation to silane.

[0005] Further, the second heat exchanger for heat exchange is arranged between the first rectifying column and the second resin column.

[0006] Further, the discharge pipeline of the second rectifying column is bifurcated and is communicated with the third heat exchanger for heat exchange and the feed pipe of the second resin column.

[0007] Further, the feed pipe of the first heat exchanger is sequentially provided with the regulating valve and the first cut-off valve.

[0008] Further, the second cut-off valve is arranged on the pipeline connected between the discharge end of the second rectifying column and the feed end of the second resin column.

[0009] Further, the sampling analysis port is arranged on the top discharge pipe of the third heat exchanger.

[0010] In the above technical scheme, the production device of improving silane purity provided by the utility model has the beneficial effects that:

[0011] The utility model discloses first use resin complexation adsorption and rectification two kinds of purification operation combination, reoptimization rectification and complexation adsorption permutation and combination to reach the purpose of removing impurities. The process greatly reduces the removal rectification load of trace impurities of single rectification operation, can effectively reduce rectification pressure and energy consumption.

[0012] It should be understood that the foregoing general description and the following detailed description are only exemplary and explanatory in nature and are not intended to limit the present disclosure.

[0013] This application file provides the summary of various implementations or examples of the technology described in the present disclosure, and is not the full disclosure of the entire scope or all features of the disclosed technology. BRIEF DESCRIPTION OF DRAWINGS

[0014] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the drawings needed in the embodiments will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments described in the utility model, and other drawings can also be obtained by those skilled in the art according to these drawings.

[0015] Figure 1 The structural schematic diagram provided by the utility model embodiment.

[0016] Explanation of reference signs:

[0017] 1, first heat exchanger; 2, first resin column; 3, first rectification tower; 4, second heat exchanger; 5, second resin column; 6, second rectification tower; 7, third heat exchanger; 8, regulating valve; 9, first cut-off valve; 10, second cut-off valve. DETAILED DESCRIPTION

[0018] In order to make the purpose, technical scheme and advantages of the embodiments of the present disclosure clearer, the technical scheme of the embodiments of the present disclosure will be described clearly and completely below in conjunction with the drawings of the embodiments of the present disclosure. Obviously, the described embodiments are part of the embodiments of the present disclosure, not all the embodiments. Based on the described embodiments of the present disclosure, all other embodiments obtained by those skilled in the art without creative labor belong to the scope of protection of the present disclosure.

[0019] Please refer to Figure 1The utility model provides a kind of production device for improving the purity of silane, comprising: first heat exchanger 1, first heat exchanger 1 is sequentially connected with primary purification assembly and secondary purification assembly by pipeline, silane crude gas is preliminary heat exchanged by first heat exchanger 1, reduce the temperature of silane crude gas, facilitate entering primary purification assembly and being purified, primary purification assembly includes the first resin column 2 for liquid phase adsorption to liquid silane and the first rectifying column 3 for rectification separation to silane, the pressure of first resin column 2 is controlled as micro negative pressure, temperature is negative temperature, silane gasifies under low temperature, carries out liquid phase adsorption in first resin column 2, after adsorption, silane enters first rectifying column 3 and is rectified and purified, secondary purification assembly includes the second resin column 5 for gas phase adsorption to silane gas and the second rectifying column 6 for rectification separation to silane, gaseous silane formed after rectification in first rectifying column 3 carries out gas phase adsorption in second resin column 5, the pressure in second resin column 5 is controlled as micro positive pressure, temperature is positive temperature, after adsorption in second resin column 5, silane gas enters second rectifying column 6 and is rectified secondly, and further purified silane is obtained, first rectifying column 3 and second resin column 5 are provided with second heat exchanger 4 for heat exchange, the discharge pipeline of second rectifying column 6 is bifurcated and is communicated with third heat exchanger 7 for heat exchange and the feed pipe of second resin column 5, the feed pipe of first heat exchanger 1 is sequentially provided with regulating valve 8 and first cut-off valve 9, the pipeline that the discharge end of second rectifying column 6 is connected with the feed end of second resin column 5 is provided with second cut-off valve 10, the top discharge pipe of third heat exchanger 7 is provided with sampling analysis port, second heat exchanger 4 is the preparation for preliminary adjustment of silane temperature before secondary purification, and third heat exchanger 7 liquefies silane gas for storage, whether the qualified silane gas is analyzed by sampling at the top of third heat exchanger 7, if not, second cut-off valve 10 will be opened, and the exported silane gas is reintroduced into secondary purification assembly and is purified again.

[0020] In the utility model, reference Figure 1 , the implementation steps of silane crude gas purification are as follows:

[0021] Step one: open regulating valve 8 and first cut-off valve 9, after preliminary heat exchange and cooling of silane crude gas through first heat exchanger 1, enter first resin column 2. The outer coil of first resin column 2 is cooled by liquid nitrogen, and the temperature is controlled at-120 to-140 DEG C, and the pressure is micro negative pressure. Silane is subjected to liquid phase adsorption in first resin column 2.

[0022] Step two: after liquid phase adsorption, silane is pressed to first rectifying column 3 by liquid phase pressure pipeline, and the rectifying column is heated, and the temperature and pressure of first rectifying column 3 are controlled. Heavy components are removed at the bottom, and light components are removed. Silane gas from the top enters second resin column 5.

[0023] Step three: control the pressure of the second resin column 5 to be slightly positive, the temperature is 0-20℃, the silane gas in the second resin column 5 carries out gas phase adsorption.

[0024] Step four: the silane gas from the second resin column 5 enters the second rectifying tower 6, carries out rectification and removes light components, then the analysis pipeline carries out sampling analysis, if the analysis is qualified, the liquid phase is taken out to the silane product tank, if the analysis is unqualified, re-enters the second resin column 5 to carry out secondary adsorption.

[0025] In the utility model, reference Figure 1 , the silane crude gas produced by the synthetic reaction is controlled by the valve opening degree of the regulating valve 8, the silane crude gas first carries out heat exchange through the first heat exchanger 1, reduces the temperature of the silane gas, enters the first resin column 2, controls the pressure of the first resin column 2 to be slightly negative and the temperature to be negative, the silane gas is liquefied under low temperature, carries out liquid phase adsorption in the first resin column 2, the adsorbed silane is pressed to the first rectifying tower 3 through the liquid phase pipeline and carries out rectification.Subsequently, the silane gas carries out gas phase adsorption through the second resin column 5, controls the pressure of the second resin column 5 to be slightly positive and the temperature to be positive, again enters the second rectifying tower 6 to carry out rectification.The silane gas after rectification carries out sampling analysis, if the analysis is qualified, is punched into the silane product tank, if the analysis is unqualified, is transferred to the second resin column 5 and the second rectifying tower 6, carries out adsorption and rectification again.

[0026] The above only describes some exemplary embodiments of the utility model in a descriptive way, undoubtedly, for ordinary skilled person in the art, the described embodiments can be modified in various different ways without departing from the spirit and scope of the utility model. Therefore, the above drawings and description are illustrative in nature and should not be understood as limiting the scope of protection of the utility model claims.

Claims

1. A production apparatus for improving the purity of silane, comprising: The first heat exchanger (1) is characterized in that the first heat exchanger (1) is connected with a primary purification assembly and a secondary purification assembly in sequence through pipelines, the primary purification assembly comprises a first resin column (2) for liquid-phase adsorption of liquid silane and a first rectifying tower (3) for rectifying separation of the silane, and the secondary purification assembly comprises a second resin column (5) for gas-phase adsorption of silane gas and a second rectifying tower (6) for rectifying separation of the silane.

2. The apparatus for producing silane with improved purity according to claim 1, wherein A second heat exchanger (4) for heat exchange is arranged between the first rectifying tower (3) and the second resin column (5).

3. The apparatus for producing silane with improved purity according to claim 2, wherein The discharge pipeline of the second rectifying tower (6) is bifurcated and connected with a third heat exchanger (7) for heat exchange and a feed pipe of the second resin column (5).

4. The apparatus for producing silane with improved purity according to claim 3, wherein An adjusting valve (8) and a first cut-off valve (9) are arranged on the feed pipe of the first heat exchanger (1) in sequence.

5. The apparatus for producing silane with improved purity according to claim 4, wherein A second cut-off valve (10) is arranged on the pipeline connecting the discharge end of the second rectifying tower (6) with the feed end of the second resin column (5).

6. The apparatus for producing silane with improved purity according to claim 5, wherein A sampling analysis port is formed in the top discharge pipe of the third heat exchanger (7).

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