CN106348302A - Method of purifying silicane according to adsorption method - Google Patents
Method of purifying silicane according to adsorption method Download PDFInfo
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- CN106348302A CN106348302A CN201510413573.1A CN201510413573A CN106348302A CN 106348302 A CN106348302 A CN 106348302A CN 201510413573 A CN201510413573 A CN 201510413573A CN 106348302 A CN106348302 A CN 106348302A
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- silane
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- silicane
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Abstract
The invention relates to a method of purifying silicane according to an adsorption method. Adsorbing columns are filled with an adsorbent, and after coarse silicane is added through an inlet of the adsorbing columns and adsorbed by the adsorbent, high-purity silicane is extracted from an extraction opening. The number of the adsorbing column is one, or the multiple adsorbing columns are connected in series. For the adsorbing columns connected in series, a silicane inlet and an outlet are connected with the adsorbing columns via pipelines. The adsorbing temperature of the adsorbing columns is controlled at -200 DEG C to 200 DEG C. The adsorbent is substance which adsorbs impurities in the silicane and does not the silicane. The adsorbent is a molecular sieve, active carbon, silica gel, activated aluminum oxide, a similar adsorbent and the like preferably. The single adsorbent or the mixed adsorbent is filled in each adsorbing column, the operation technology of purifying the silicane by adsorbing and separation is simple, the equipment investment is low, and the obtained silicane is high in purity. The purity of the purified silicane reaches 6N or above. The adsorbent in the adsorbing purification is easy to regenerate, the cost is low, the silicane is flammable and explosive, and the method is mild in silicane purification condition and high in safety.
Description
Technical field
The present invention relates to absorption method purify silane method, high purity silane will be become using the thick silane purification that the methods such as little Song method, discrimination method, new silane thermal decomposition process are produced, using absorption method of purification separating-purifying, the silane purity after purification reach 6n and more than.Simple using the method purification silane process, obtain silane purity height, energy saving.
Technical background
Polycrystalline silicon material is electronics and information industry and the most important basic material of solar energy power generating industry, and solar-grade polysilicon can be used for solar energy power generating, is the WeiLai Technology of a kind of efficient, environmental protection and cleaning, alternative existing power generation mode.And electronic-grade polycrystalline silicon can be used for manufacturing semi-conducting material, for the manufacture of IC substrate, it is widely used in space flight, artificial intelligence, automatically controls and the fields such as computer chip.Therefore polycrystalline silicon material has strategic importance for the development of national new forms of energy and new and high technology.
Production of polysilicon main method includes at present: improved Siemens, silane decomposition method, zinc reduction, reducing silica method etc., wherein silane thermal decomposition process produce polysilicon have the advantages that following: 1) silane and impurity hydride nature difference are easy to greatly purify, 2) thermal decomposition product non-corrosiveness, reduces to equipment corrosion, 3) thermolytic mechanism is poor, decomposition temperature is low, consume electricity low, energy saving, 4) flow process is simple, reducing agent need not be used, it is to avoid reducing agent pollutes.Due to silane thermal decomposition process produce polysilicon have the advantages that above, silane thermal decomposition process increasingly becomes the main method producing polysilicon, prepare silane requirement in polysilicon using silane decomposition method high-purity, and do not reach requirement using the silane purity that the methods such as little Song method, discrimination method, new silane thermal decomposition process are produced, need the silane of further purifying and preparing high-purity, silane purity does not reach requirement and directly affects product quality, so how the silane of purifying and preparing high-purity is a urgent problem.Using absorption method separating-purifying, the silane purity after purification reach 6n and more than.Simple using the method purification silane process, obtain silane purity height, energy saving.
In recent years, it was increasingly becoming the strategic industry first developed of country with polysilicon, solved the problems, such as silane purification in silane thermal decomposition process production polysilicon, promoted that polysilicon industry reaches energy-conservation, consumption reduction, safe and environment-friendly target seem increasingly important and urgent further.
Content of the invention
Do not reach requirement using the thick silane purity that the methods such as little Song method, discrimination method, new silane thermal decomposition process are produced, need the silane of further purifying and preparing high-purity, silane purity do not reach requirement especially in silane boron impurity content will directly affect the quality of product polysilicon, so how the silane of purifying and preparing high-purity is a urgent problem.It is an object of the invention to purification silane, produce highly purified silane.The principle of absorption method purification is: adsorbent is a kind of porous mass, and unwanted impurity can be selected to separate in the way of adsorbing from silane by it.
For achieving the above object, the method that absorption method of the present invention purifies silane.
A kind of method that absorption method purifies silane；Equipped with adsorbent in adsorption column, by adsorbing column inlet addition, after adsorbent absorption, high purity silane is through extraction mouth extraction for thick silane.
Adsorption column is one or more series connection.Multiple series connection adsorption columns are to be connected with adsorption column by pipeline with outlet by silane inlet.
The adsorption temp of adsorption column controls at -200～200 DEG C.
Adsorbent is to adsorb the impurity of silane and does not adsorb the material of silane.Adsorbent is preferably molecular sieve, activated carbon, silica gel, activated alumina and similar adsorbent etc., and wherein molecular sieve includes 3a, 4a, 5a, 13x and various modified molecular sieve.
Single adsorbent can be loaded it is also possible to load the adsorbent of mixing in any proportion, such as 3a, 4a mixed adsorbent, 3a, 4a, 5a and active carbon mixed adsorbent in each adsorption column；
Uniformly filling can also be layered by mixed packing when wherein loading mixed adsorbent；
Same adsorbent or different adsorbent is loaded in several adsorption columns of series connection.
The apparatus and method that absorption method of the present invention purifies silane have the advantage that
[1] present invention absorption purification silane separating-purifying silane operating procedure is simple, and equipment investment is few, and the silane purity obtaining is high.Silane purity after purification reach 6n and more than.
[2] adsorbent regenerating easily in absorption purification, low cost, silane is inflammable and explosive, and the method purifies silane mild condition, safe.
[3] creativeness and novelty, absorption purification silane is proposition simultaneously creative first at home and abroad, creative and novelty.
Brief description
Fig. 1: absorption method purifies an adsorption column flow chart of silane.
Fig. 2: absorption method purifies two adsorption column flow charts of silane.
Wherein: thick silane inlet -1, adsorption column -2, adsorbent -3, high purity silane extraction mouth -4, silane inlet -5 after preliminary purification.
Specific embodiment
Below by example with reference, invention is described further.
Absorption method purification silane includes in single adsorption column or the adsorption column of several series connection, single absorption column device mainly includes thick silane inlet (1), adsorption column (2), adsorbent (3), high purity silane extraction mouth (4), equipped with adsorbent wherein in adsorption column, silane inlet is connected with adsorption column by pipeline with outlet；The adsorption column of several series connection, (as Fig. 2) taking two series connection adsorption columns as a example, including silane inlet (5) after: thick silane inlet (1), adsorption column (2), adsorbent (3), high purity silane extraction mouth (4), preliminary purification, wherein equipped with adsorbent in adsorption column, connected by pipeline between two adsorption columns, be connected with adsorption column by pipeline between the entrance of silane and outlet.
Thick silane is passed through the adsorption column (2) of two series connection from silane inlet 1, and silane impurity is adsorbed in adsorption column and removes, and high purity silane is from silane extraction mouth (4) extraction.
Actual conditions is exemplified below:
Embodiment 1:
The present embodiment is carried out in adsorption-type silane knot screen, will be filled in 4a molecular sieve in single suction attached column, and at 30～40 DEG C, before purification, silane purity is 99.9% to adsorption column temperature control, and after purification, the purity from overhead extraction silane reaches 99.9999%.
Embodiment 2:
Adsorption-type silane knot screen is carried out, will be filled in 4a molecular sieve in single suction attached column, at -200～-180 DEG C, before purification, silane purity is 99.9% to adsorption column temperature control, and after purification, the purity from overhead extraction silane reaches 99.9999%.
Embodiment 3:
Adsorption-type silane knot screen is carried out, will be filled in 4a molecular sieve in single suction attached column, at 180～200 DEG C, before purification, silane purity is 99.9% to adsorption column temperature control, and after purification, the purity from overhead extraction silane reaches 99.9999%.
Embodiment 4:
The present embodiment is carried out in adsorption-type silane knot screen, the 1:1 mixing in molar ratio of 4a and 3a molecular sieve is filled in single suction attached column, at 30～40 DEG C, before purification, silane purity is 99.9% to adsorption column temperature control, and after purification, the purity from overhead extraction silane reaches 99.9999%.
Embodiment 5:
The present embodiment is carried out in adsorption-type silane knot screen, the 1:1000 mixing in molar ratio of 4a and 3a molecular sieve is filled in single suction attached column, at 30～40 DEG C, before purification, silane purity is 99.9% to adsorption column temperature control, and after purification, the purity from overhead extraction silane reaches 99.9999%.
Embodiment 6:
The present embodiment is carried out in adsorption-type silane knot screen, the 1000:1 mixing in molar ratio of 4a and 3a molecular sieve is filled in single suction attached column, at 30～40 DEG C, before purification, silane purity is 99.9% to adsorption column temperature control, and after purification, the purity from overhead extraction silane reaches 99.9999%.
Embodiment 7:
The present embodiment is carried out in adsorption-type silane knot screen, 4a, 3a molecular sieve is filled in two series connection first of adsorption columns and second adsorption column respectively, two adsorption column temperature controls are at 30～40 DEG C, before purification, silane purity is 99.9%, and after purification, the purity from overhead extraction silane reaches 99.9999%.
Embodiment 8:
The present embodiment is carried out in adsorption-type silane knot screen, uniform for 4a, 3a molecular sieve mixing is filled in two series connection first of adsorption columns and second adsorption column respectively, two adsorption column temperature controls are at 30～40 DEG C, before purification, silane purity is 99.9%, and after purification, the purity from overhead extraction silane reaches 99.9999%.
Claims (10)
1. a kind of method that absorption method purifies silane；It is characterized in that equipped with adsorbent in adsorption column, thick silane leads to
Cross absorption column inlet add, impurity be adsorbed post absorption after, high purity silane through extraction mouth extraction.
2. the method for claim 1, is characterized in that adsorption column is one or more series connection.
3. method as claimed in claim 2, is characterized in that multiple series connection adsorption columns are by silane inlet and outlet
It is connected with adsorption column by pipeline.
4. the method for claim 1, is characterized in that adsorption temp controls at -200～200 DEG C.
5. the method for claim 1, is characterized in that adsorbent is to adsorb the impurity of silane and does not inhale
The material of attached silane.
6. the method for claim 1, its feature adsorbent is molecular sieve, activated carbon, silica gel, work
Property aluminium oxide.
7. method as claimed in claim 6, its feature adsorbent wherein molecular sieve includes 3a, 4a, 5a,
13x molecular sieve.
8. the method for claim 1, it is characterized in that loading in each adsorption column single adsorbent or
The adsorbent of filling mixing.
9. method as claimed in claim 8, is characterized in that loading during mixed adsorbent according to uniform mixing dress
Fill out or be layered filling.
10. method as claimed in claim 2, is characterized in that loading same suction in the several adsorption columns connected
Attached dose or different adsorbent.
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| CN201510413573.1A CN106348302A (en) | 2015-07-14 | 2015-07-14 | Method of purifying silicane according to adsorption method |
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| CN201510413573.1A CN106348302A (en) | 2015-07-14 | 2015-07-14 | Method of purifying silicane according to adsorption method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109336919A (en) * | 2018-11-02 | 2019-02-15 | 辽宁新邦新材料有限公司 | The purification process and device of the precursor material of organosilicon material |
| CN109467570A (en) * | 2018-11-02 | 2019-03-15 | 辽宁新邦新材料有限公司 | Precursor material, organosilicon material, organosilicon macromolecule material, composition and the product of organosilicon material |
| CN111829918A (en) * | 2019-04-22 | 2020-10-27 | 新特能源股份有限公司 | Test device for adsorbing chlorosilane and test method for adsorbing chlorosilane |
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| KR100635960B1 (en) * | 2003-12-08 | 2006-10-19 | 에어 프로덕츠 앤드 케미칼스, 인코오포레이티드 | A purification material for purifying impure hydride gases, a method of making the same, a method for purifying the hydride gases and purified hydride gases produced by the purification method |
| CN105712351A (en) * | 2016-04-18 | 2016-06-29 | 张玲 | Method for adsorption purification of silicane |
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2015
- 2015-07-14 CN CN201510413573.1A patent/CN106348302A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100635960B1 (en) * | 2003-12-08 | 2006-10-19 | 에어 프로덕츠 앤드 케미칼스, 인코오포레이티드 | A purification material for purifying impure hydride gases, a method of making the same, a method for purifying the hydride gases and purified hydride gases produced by the purification method |
| CN105712351A (en) * | 2016-04-18 | 2016-06-29 | 张玲 | Method for adsorption purification of silicane |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109336919A (en) * | 2018-11-02 | 2019-02-15 | 辽宁新邦新材料有限公司 | The purification process and device of the precursor material of organosilicon material |
| CN109467570A (en) * | 2018-11-02 | 2019-03-15 | 辽宁新邦新材料有限公司 | Precursor material, organosilicon material, organosilicon macromolecule material, composition and the product of organosilicon material |
| CN111829918A (en) * | 2019-04-22 | 2020-10-27 | 新特能源股份有限公司 | Test device for adsorbing chlorosilane and test method for adsorbing chlorosilane |
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