CN109781888A - A kind of chlorosilane pre-treating method - Google Patents
A kind of chlorosilane pre-treating method Download PDFInfo
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- CN109781888A CN109781888A CN201910098826.9A CN201910098826A CN109781888A CN 109781888 A CN109781888 A CN 109781888A CN 201910098826 A CN201910098826 A CN 201910098826A CN 109781888 A CN109781888 A CN 109781888A
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- chlorosilane
- treating method
- centrifuge
- centrifuge tube
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Abstract
The invention discloses a kind of chlorosilane pre-treating method, include the following steps: that the solution after rectifying in polysilicon production process is carried out the extraction of sample liquid by S1；Sample liquid is transferred in centrifuge tube by S2；Centrifuge tube is placed into centrifuge by S3；S4 starting centrifuge is centrifuged；S5 takes the supernatant liquor of the centrifuge tube after centrifugation；S6 takes supernatant liquor to be analyzed with chromatograph.Chlorosilane pre-treating method of the invention has reduced or remitted the spare parts consumption of gas-chromatography instrument sample introduction needle, sampling system and separation system, save the cost.Production analysis data can be effectively provided by this technology, effective Instructing manufacture has specific judgment basis to foul material component content.
Description
Technical field
The present invention relates to polysilicon process field, specially a kind of chlorosilane pre-treating method.
Background technique
The raw material trichlorosilane that current each polysilicon factory uses, during producing rectification and purification, in laboratory sampling point
The sample that analysis is got sometimes is messy a large amount of suspended matters and particulate matter, causes sample that can not analyze, the reason is that in chromatography,
Particulate matter and suspended matter in sample are easy to the damage that the analysis for a long time of blocking analysis instrument also results in chromatograph separation system
It is bad.The reason is that the dirty material chlorosilane generated in polysilicon factory production system easily blocks and Failure analysis instrument, lead to sample
It can not analyze.
Summary of the invention
In order to solve defect existing in the prior art, provide a kind of can effectively carry out sample analysis and can have the present invention
Effect extends the chlorosilane pre-treating method of gas chromatograph service life.
Present invention firstly provides a kind of chlorosilane pre-treating methods, include the following steps:
Solution after rectifying in polysilicon production process is carried out the extraction of sample liquid by S1；
Sample liquid is transferred in centrifuge tube by S2；
Centrifuge tube is placed into centrifuge by S3；
S4 starting centrifuge is centrifuged；
S5 takes the supernatant liquor of the centrifuge tube after centrifugation；
S6 takes supernatant liquor to be analyzed with chromatograph.
The present invention also provides following prioritization schemes:
Preferably, sample liquid cooling is handled after S2 step after S1 step.
Preferably, supernatant liquor is placed to room temperature before S6 step after S5 step.
Preferably, rectifying uses rectifying column rectifying.
It is furthermore preferred that the reflux ratio in rectification process is 1.5.
Preferably, the revolving speed of the centrifuge is 2000r/min.
Preferably, the sample volume in the S6 step is 5uL.
Preferably, the chromatograph in the S6 step is gas chromatograph.
It is furthermore preferred that the flow velocity of the gas chromatograph is 60mL/min.
It is furthermore preferred that the temperature of vaporization chamber of the gas chromatograph is 110-140 DEG C.
The beneficial effects of the present invention are:
1, the spare parts consumption of gas-chromatography instrument sample introduction needle, sampling system and separation system, save the cost have been reduced or remitted.
2, production analysis data can be effectively provided by this technology, effective Instructing manufacture has foul material component content
Specific judgment basis.
3, favorable reproducibility is tested, it is simple and fast, while compensating for system monitoring leakage item.
Detailed description of the invention
Fig. 1 is the flow chart of chlorosilane pre-treating method of the invention.
Specific embodiment
It is right With reference to embodiment in order to make those skilled in the art more fully understand the technical solution of invention
The present invention is described in further detail.
Chlorosilane pre-treating method of the invention, includes the following steps:
Solution after rectifying in polysilicon production process is carried out the extraction of sample liquid by S1；
Sample liquid is transferred in centrifuge tube by S2；
Centrifuge tube is placed into centrifuge by S3；
S4 starting centrifuge is centrifuged；
S5 takes the supernatant liquor of the centrifuge tube after centrifugation；
S6 takes supernatant liquor to be analyzed with chromatograph.
Preferably, sample liquid cooling is handled before S2 step after S1 step.
Preferably, supernatant liquor is placed to room temperature before S6 step after S5 step.
The rectifying is to carry out rectifying using rectifying column.
It is furthermore preferred that the reflux ratio in rectification process is 1.5.
Preferably, the revolving speed of the centrifuge is 10000r/min.The centrifuge is desk centrifuge, and revolving speed is
5000-20000r/min；Preferably 10000r/min.
Preferably, the sample volume in the S6 step is 5uL.
Preferably, the chromatograph in the S6 step is gas chromatograph.
It is furthermore preferred that the flow velocity of the gas chromatograph is 60mL/min.
It is furthermore preferred that the temperature of vaporization chamber of the gas chromatograph is 110-140 DEG C.
The present invention uses gas chromatograph, and the injection of suitable sample is furnished with to the gas chromatograph of thermal conductivity detector (TCD) (TCD)
In, the content of each ingredient is calculated by area normalization method.
Reagent and material
Hydrogen: volume fraction is not less than 99.99%, the dry, purification through silica gel and molecular sieve.
Instrument
Gas chromatograph: the gas chromatograph of any model equipped with part flow arrangement and thermal conductivity detector (TCD), machine sensitivity
Meet national standard pertinent regulations with stability.
Chromatographic work station or data processor
Desk centrifuge
Micro syringe: 10uL
Chromatographic column: 100% dimethyl polysiloxane or other can reach separation purpose capillary column
The concrete operations process of chlorosilane pre-treating method of the invention are as follows:
Solution after rectifying in polysilicon production process is first carried out to the extraction of sample liquid；Sample liquid is carried out at refrigeration
Reason cools to 0 DEG C or so, and the purpose of cooling is to reduce the volatility of low-boiling-point substance, takes 15ml chlorosilane sample liquid to plastic containers
In, using lab bench centrifuge by sample particulate matter and suspended matter pass through high speed centrifugation settle, centrifuge speed
10000 turns/min, centrifugation time 10min, the half supernatant after taking centrifuge to settle, concussion mixes, and places to room temperature, restores
After room temperature, supernatant liquor is taken to be analyzed with chromatograph；The supernatant liquor 5uL after centrifugal sedimentation is taken with micro syringe,
It is injected into gas chromatograph, the content of each ingredient is calculated by area normalization method.
The above is only the preferred embodiment of the present invention, it is noted that above-mentioned preferred embodiment is not construed as pair
Limitation of the invention, protection scope of the present invention should be defined by the scope defined by the claims..For the art
For those of ordinary skill, without departing from the spirit and scope of the present invention, several improvements and modifications can also be made, these change
It also should be regarded as protection scope of the present invention into retouching.
Claims (8)
1. a kind of chlorosilane pre-treating method, characterized by the following steps:
Solution after rectifying in polysilicon production process is carried out the extraction of sample liquid by S1；
Sample liquid is transferred in centrifuge tube by S2；
Centrifuge tube is placed into centrifuge by S3；
S4 starting centrifuge is centrifuged；
S5 takes the supernatant liquor of the centrifuge tube after centrifugation；
S6 takes supernatant liquor to be analyzed with chromatograph.
2. chlorosilane pre-treating method according to claim 1, it is characterised in that: after S1 step before S2 step, by sample
Liquid cooling processing.
3. chlorosilane pre-treating method according to claim 2, it is characterised in that: after S5 step before S6 step, by upper layer
Clear liquid is placed to room temperature.
4. chlorosilane pre-treating method according to claim 1, it is characterised in that: the revolving speed of the centrifuge is
10000r/min。
5. chlorosilane pre-treating method according to claim 1, it is characterised in that: the sample volume in the S6 step is
5uL。
6. chlorosilane pre-treating method according to claim 1, it is characterised in that: the chromatograph in the S6 step is gas
Chromatography.
7. chlorosilane pre-treating method according to claim 6, it is characterised in that: the flow velocity of the gas chromatograph is
60mL/min。
8. chlorosilane pre-treating method according to claim 7, it is characterised in that: the vaporization room temperature of the gas chromatograph
Degree is 110-140 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910098826.9A CN109781888A (en) | 2019-01-31 | 2019-01-31 | A kind of chlorosilane pre-treating method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910098826.9A CN109781888A (en) | 2019-01-31 | 2019-01-31 | A kind of chlorosilane pre-treating method |
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| Publication Number | Publication Date |
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| CN109781888A true CN109781888A (en) | 2019-05-21 |
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| CN201910098826.9A Pending CN109781888A (en) | 2019-01-31 | 2019-01-31 | A kind of chlorosilane pre-treating method |
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Citations (7)
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| JP2011220837A (en) * | 2010-04-09 | 2011-11-04 | Asahi Glass Co Ltd | Determination method of bromine element in chlorosilanes and manufacturing method of tetrachlorosilane |
| WO2012077677A1 (en) * | 2010-12-10 | 2012-06-14 | 株式会社トクヤマ | Method for detecting water leak, device for chlorosilane hydrogen reduction reaction and production method using said device |
| JP5560239B2 (en) * | 2011-07-04 | 2014-07-23 | 信越化学工業株式会社 | Gas chromatography separation method for silane / chlorosilanes and column for gas chromatography |
| CN103951693A (en) * | 2014-05-16 | 2014-07-30 | 泸州北方化学工业有限公司 | Method for monitoring cracking reaction of dimethyldichlorosilance hydrolyzates |
| CN104849366A (en) * | 2015-05-11 | 2015-08-19 | 中国恩菲工程技术有限公司 | Detection system and detection method |
| CN106770817A (en) * | 2016-11-30 | 2017-05-31 | 江西蓝星星火有机硅有限公司 | The detection method of ethyl hydrogen dichlorosilane in a kind of methylchlorosilane |
| CN108982717A (en) * | 2018-07-23 | 2018-12-11 | 湖北兴瑞硅材料有限公司 | The detection method of content of siloxane in a kind of organosilicon slag inclusion waste water |
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011220837A (en) * | 2010-04-09 | 2011-11-04 | Asahi Glass Co Ltd | Determination method of bromine element in chlorosilanes and manufacturing method of tetrachlorosilane |
| WO2012077677A1 (en) * | 2010-12-10 | 2012-06-14 | 株式会社トクヤマ | Method for detecting water leak, device for chlorosilane hydrogen reduction reaction and production method using said device |
| JP5560239B2 (en) * | 2011-07-04 | 2014-07-23 | 信越化学工業株式会社 | Gas chromatography separation method for silane / chlorosilanes and column for gas chromatography |
| CN103951693A (en) * | 2014-05-16 | 2014-07-30 | 泸州北方化学工业有限公司 | Method for monitoring cracking reaction of dimethyldichlorosilance hydrolyzates |
| CN104849366A (en) * | 2015-05-11 | 2015-08-19 | 中国恩菲工程技术有限公司 | Detection system and detection method |
| CN106770817A (en) * | 2016-11-30 | 2017-05-31 | 江西蓝星星火有机硅有限公司 | The detection method of ethyl hydrogen dichlorosilane in a kind of methylchlorosilane |
| CN108982717A (en) * | 2018-07-23 | 2018-12-11 | 湖北兴瑞硅材料有限公司 | The detection method of content of siloxane in a kind of organosilicon slag inclusion waste water |
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Application publication date: 20190521 |