CN108490113A - The assay method of chlorosilane in a kind of dichloromethane - Google Patents
The assay method of chlorosilane in a kind of dichloromethane Download PDFInfo
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Abstract
The invention belongs to a kind of assay method of chlorosilane in chemical analysis field more particularly to dichloromethane, this approach includes the following steps：A) dichloromethane sample and water are mixed, stands, takes supernatant；B) content of chlorion in the supernatant is measured, the content of chlorosilane in dichloromethane sample is calculated according to measurement result.The present invention utilizes the difference of dichloromethane and chlorosilane chemical property, the chlorion of chlorosilane in dichloromethane sample is dexterously gone out with water " extraction ", it is measured by the chloride ion content gone out to " extraction ", can accurately calculate the content of chlorosilane in dichloromethane sample.In optimal technical scheme provided by the invention, before dichloromethane sample and water hybrid reaction, modified zeolite is added into reaction system as reaction promoter, the chlorosilane in water and dichloromethane sample can be promoted fully to react, to improve " extraction " effect of water to chlorion, the accuracy of chlorosilane content measurement is further increased.
Description
Technical field
The invention belongs to a kind of assay methods of chlorosilane in chemical analysis field more particularly to dichloromethane.
Background technology
Polysilicon has semiconductor property, is particularly important defect semiconductor material, system is widely used in electronics industry
The basic material of manufacturing semiconductor radio, recorder, refrigerator, colour TV, video recorder, electronic computer etc. is production monocrystalline silicon
Direct material, be contemporary artificial intelligence, automatically control, information processing, the semiconductor devices such as opto-electronic conversion electronic information base
Plinth material.On Solar use, monocrystalline silicon and polysilicon also play huge effect, and production of polysilicon is main in the world
Traditional handicraft has：Improved Siemens, silane thermal decomposition process and fluidized bed process.The Siemens being widely adopted at present are in 1954
The method for manufacturing polycrystalline silicon (also referred to as Siemens Method) of year invention：Matched according to certain using high-purity trichlorosilane and high-purity hydrogen
Than mixing composition mixed raw material gas, it is passed through in reduction reactor, is constantly deposited on the HIGH-PURITY SILICON core of heating, make silicon
The diameter of core is gradually thicker and forms polycrystalline silicon rod.
Dichloromethane boiling point：39.8 DEG C vapour pressure：30.55kPa (10 DEG C) fusing point：-95.1℃.It is given birth in improved Siemens
It produces in polysilicon process, the refrigerant recycled in refrigeration system is dichloromethane, and dichloromethane boiling point is between trichlorosilane and four
Between silicon chloride, rectifying is difficult to remove, and cryogenic temperature can be down to -70 DEG C, since the temperature difference is big in technique, and heat exchanger is easy to occur
Leakage, makes chlorosilane penetrate into dichloromethane, causes ice maker stop jumping, entire production will be given to bring loss, by detecting dichloro
Content in silane system in methane chlorine finds heat exchanger leakage, and takes measures in time, avoids bringing loss to production being very
It is necessary to.
Dichloromethane dissolves each other with chlorosilane, and for dichloromethane boiling point between trichlorosilane and silicon tetrachloride, chlorosilane is tight
The measurement for interfering dichloromethane again, can not be detected with conventional analysis method.The peak of dichloromethane can not be with three on chromatogram
The peak of chlorine hydrogen silicon separates, and chromatograph can not detect.It is international and domestic that there is presently no measured about dichloromethane in chlorosilane
Report.
Invention content
In view of this, the purpose of the present invention is to provide a kind of assay method of chlorosilane in dichloromethane, the present invention carries
The assay method of confession can in Accurate Determining dichloromethane chlorosilane content.
The present invention provides a kind of assay methods of chlorosilane in dichloromethane, include the following steps：
A), dichloromethane sample and water are mixed, stands, takes supernatant；
B), the content of chlorion in the supernatant is measured, dichloromethane sample is calculated according to measurement result
The content of middle chlorosilane.
Preferably, the volume ratio of the dichloromethane sample and water is (5~20):40.
Preferably, the temperature of the mixing is 15~30 DEG C；The time of the mixing is 0.5~5min.
Preferably, the step a) is：Dichloromethane sample, reaction promoter and water are mixed, stands, takes supernatant；
The reaction promoter includes zeolite and the metal oxide that is supported on zeolite.
Preferably, the zeolite is ZSM-5 molecular sieve；
The metal oxide includes one kind or more in iron oxide, titanium dioxide, cerium oxide, yttrium oxide and molybdenum oxide
Kind.
Preferably, the metal oxide includes iron oxide, titanium dioxide, cerium oxide, yttrium oxide and molybdenum oxide, the oxygen
The mass ratio for changing iron, titanium dioxide, cerium oxide, yttrium oxide and molybdenum oxide is (1~2)：(1.5~3)：(0.5~1.5)：(0.1
~1)：(1~2).
Preferably, load capacity of the metal oxide on zeolite is 0.5~15wt%.
Preferably, the reaction promoter is prepared in accordance with the following methods：
It after zeolite impregnates in metal salt solution, is calcined, obtains reaction promoter.
Preferably, the amount ratio of the reaction promoter and water is (1~5) g：40ml.
Preferably, the content of chlorion in the supernatant is measured in step b) using mercurimetry.
Compared with prior art, the present invention provides a kind of assay methods of chlorosilane in dichloromethane.The present invention provides
Assay method include the following steps：A), dichloromethane sample and water are mixed, stands, takes supernatant；B), to the supernatant
The content of chlorion is measured in liquid, and the content of chlorosilane in dichloromethane sample is calculated according to measurement result.The present invention
Using the difference of dichloromethane and chlorosilane chemical property, dexterously chlorosilane in dichloromethane sample is gone out with water " extraction "
Chlorion is measured by the chloride ion content gone out to " extraction ", can accurately calculate chlorosilane in dichloromethane sample
Content.In optimal technical scheme provided by the invention, before dichloromethane sample and water hybrid reaction, thrown into reaction system
Add a certain amount of modified zeolite as reaction promoter, the chlorosilane in water and dichloromethane sample can be promoted fully to react, from
And " extraction " effect of water to chlorion is improved, further increase the accuracy of chlorosilane content measurement.The experimental results showed that adopting
When being measured to the dichloromethane of chlorine-containing silane with assay method provided by the invention, indoor relative standard deviation is
0.04%；Relative standard deviation is 1.02% between room, relative error 0.43%；Recovery of standard addition be 100.13%~
101.07%.
Specific implementation mode
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
The every other embodiment that art personnel are obtained without making creative work belongs to the model that the present invention protects
It encloses.
The present invention provides a kind of assay methods of chlorosilane in dichloromethane, include the following steps：
A), dichloromethane sample and water are mixed, stands, takes supernatant；
B), the content of chlorion in the supernatant is measured, dichloromethane sample is calculated according to measurement result
The content of middle chlorosilane.
In method provided by the invention, dichloromethane sample and water are mixed first.In the process, dichloromethane sample
Chlorosilane and water in product carry out reaction and generate hydrogen chloride and be dissolved into water phase, that is, realize to chlorion in chlorosilane
" extraction ".In the present invention, the volume ratio of the dichloromethane sample and water is preferably (5~20):40, concretely 5:40、
6:40、7:40、8:40、9:40、10:40、11:40、12:40、13:40、14:40、15:40、16:40、17:40、18:40、19:
40 or 20:40.
In the present invention, in order to promote chlorosilane and water to be reacted, reaction promoter is preferably added into reaction system,
Dichloromethane sample, reaction promoter and water are mixed.Wherein, the reaction promoter includes zeolite and is supported on zeolite
Metal oxide；The zeolite is preferably ZSM-5 molecular sieve；The metal oxide includes iron oxide, titanium dioxide, oxidation
It is one or more in cerium, yttrium oxide and molybdenum oxide.In one embodiment provided by the invention, the metal oxide includes
The mass ratio of iron oxide and molybdenum oxide, the iron oxide and molybdenum oxide is preferably (3~4)：(3~4), concretely 3.5:3.8；
In one embodiment provided by the invention, the metal oxide include iron oxide, titanium dioxide, cerium oxide, yttrium oxide and
Molybdenum oxide, the iron oxide, titanium dioxide, cerium oxide, yttrium oxide and molybdenum oxide mass ratio are preferably (1~2)：(1.5~3)：
(0.5~1.5)：(0.1~1)：(1~2), concretely 1.7:1.9:0.8:0.5:1.4.In the present invention, the metal oxygen
Load capacity of the compound on zeolite is preferably 0.5~15wt%, concretely 0.5wt%, 1wt%, 1.5wt%, 2wt%,
2.5wt%, 3wt%, 3.5wt%, 4wt%, 4.5wt%, 5wt%, 5.5wt%, 6wt%, 6.5wt%, 7wt%,
7.5wt%, 8wt%, 8.5wt%, 9wt%, 9.5wt%, 10wt%, 10.5wt%, 11wt%, 11.5wt%, 12wt%,
12.5wt%, 13wt%, 13.5wt%, 14wt%, 14.5wt% or 15wt%.In a metal oxide provided by the invention
In embodiment including iron oxide and molybdenum oxide, load capacity of the iron oxide on zeolite is preferably 3~4wt%, specifically may be used
For 3.5wt%；Load capacity of the molybdenum oxide on zeolite is preferably 3~4wt%, concretely 3.8wt%.It is carried in the present invention
The metal oxide supplied includes the oxygen in the embodiment of iron oxide, titanium dioxide, cerium oxide, yttrium oxide and molybdenum oxide
It is preferably 1~2wt% to change load capacity of the iron on zeolite, concretely 1.7wt%；Load of the titanium dioxide on zeolite
Amount is preferably 1.5~3wt%, concretely 1.9wt%；Load capacity of the cerium oxide on zeolite be preferably 0.5~
1.5wt%, concretely 0.8wt%；Load capacity of the yttrium oxide on zeolite is preferably 0.1~1wt%, concretely
0.5wt%；Load capacity of the molybdenum oxide on zeolite is preferably 1~2wt%, concretely 1.4wt%.In the present invention,
The amount ratio of the reaction promoter and water is preferably (1~5) g：40ml, concretely 1g：40ml、1.5g：40ml、2g：
40ml、2.5g：40ml、3g：40ml、3.5g：40ml、4g：40ml、4.5g：40ml or 5g：40ml.
In one embodiment provided by the invention, the reaction promoter can be prepared in accordance with the following methods：
It after zeolite impregnates in metal salt solution, is calcined, obtains reaction promoter.
In the preparation method of above-mentioned reaction promoter provided by the invention, metal salt preferably include ferric nitrate, Titanium Nitrate,
One or more in cerous nitrate, yttrium nitrate and nitric acid molybdenum, the present invention is to the concentration of the metal salt solution and the time of dipping
It is not particularly limited, those skilled in the art select suitable metal according to the metal oxide supported amount finally gone for
The concentration of salting liquid and the time of dipping.In the present invention, the temperature of the calcining is preferably 400~600 DEG C, specifically may be used
It is 400 DEG C, 430 DEG C, 450 DEG C, 470 DEG C, 500 DEG C, 520 DEG C, 550 DEG C, 580 DEG C or 600 DEG C；The time of the calcining is preferably
2~10h, concretely 2h, 2.5h, 3h, 3.5h, 4h, 4.5h, 5h, 5.5h, 6h, 6.5h, 7h, 7.5h, 8h, 8.5h, 9h,
9.5h or 10h.
In the present invention, the dichloromethane sample and water mixing or the dichloromethane sample, reaction promoter and
Water mix during, the temperature of the mixing is preferably 15~30 DEG C, concretely 15 DEG C, 18 DEG C, 20 DEG C, 22 DEG C, 25 DEG C,
27 DEG C or 30 DEG C；The time of the mixing is preferably 0.5~5min, concretely 0.5min, 1min, 1.5min, 2min,
2.5min, 3min, 3.5min, 4min, 4.5min or 5min；The mode of the mixing is preferably rocked.After mixing, it stands
For a period of time.The specific time of the standing is not particularly limited in the present invention, and water phase and organic phase can be made to be layered.It stands
After, take supernatant, i.e. water phase.
After taking supernatant, the content of chlorion in the supernatant is measured.Mode of the present invention to the measurement
It is not particularly limited, it is preferred to use mercurimetry.Chlorion in supernatant is measured using mercurimetry at one provided by the invention
In embodiment, specific continuous mode is as follows：
1) 10ml supernatants, are pipetted to triangular flask, 2 drop bromophenol blues are added dropwise, if be not in blue sodium hydroxide is added dropwise again until
Become blue, salpeter solution be then added dropwise and is adjusted to be subsequently added into 1ml diphenyl carbazone indicator after two drop of amount after yellow,
It is titrated later with mercuric nitrate standard liquid, it is terminal that aubergine, which is presented, accurately reads titration volumes.
2), Cl is calculated according to following formula-Content：
In formula (I), C is the concentration of nitric acid mercury standard solution, unit mol/L；V is the volume for consuming nitric acid mercury solution, single
Position ml.
The content of chlorosilane in dichloromethane sample is calculated according to measurement result.
The present invention utilizes the difference of dichloromethane and chlorosilane chemical property, has dexterously gone out dichloromethane with water " extraction "
The chlorion of chlorosilane in sample, is measured by the chloride ion content gone out to " extraction ", can accurately calculate dichloromethane
The content of chlorosilane in sample.In optimal technical scheme provided by the invention, before dichloromethane sample and water hybrid reaction,
A certain amount of modified zeolite is added into reaction system as reaction promoter, can promote the chlorine silicon in water and dichloromethane sample
Alkane fully reacts, and to improve " extraction " effect of water to chlorion, further increases the accuracy of chlorosilane content measurement.It is real
Test the result shows that, when being measured to the dichloromethane of chlorine-containing silane using assay method provided by the invention, indoor opposite mark
Quasi- deviation is 0.04%；Relative standard deviation is 1.02% between room, relative error 0.43%；Recovery of standard addition is 100.13%
~101.07%.
For the sake of becoming apparent from, it is described in detail below by following embodiment.
Embodiment 1
Prepare reaction promoter
ZSM-5 molecular sieve is impregnated in aqueous metal salt, wherein ferric nitrate in the metal salt solution, Titanium Nitrate,
It is one or more in cerous nitrate, yttrium nitrate and nitric acid molybdenum.
After dipping, ZSM-5 molecular sieve is moved in calciner plant and calcines 4h at 520 DEG C, obtains modified ZSM-5 point
Son sieve, i.e. reaction promoter.
In the present embodiment, it by adjusting the time of the component of aqueous metal salt, concentration and dipping, can obtain not
It is specific as follows with the reaction promoter of metal oxide supported amount：
Reaction promoter-a：Iron oxide load capacity 3.5wt%, molybdenum oxide load capacity 3.8wt%；
Reaction promoter-b：Iron oxide load capacity 1.7wt%, titanium dichloride load amount 1.9wt%, cerium oxide load capacity
0.8wt%, yttrium oxide load capacity 0.5wt%, molybdenum oxide load capacity 1.4wt%.
Embodiment 2
The measurement of chlorosilane in dichloromethane
1) 100ml samples are pipetted to be stood after shaking 2min with pure water constant volume to 500ml in colorimetric cylinder, pipette 10ml supernatants
To triangular flask.
2) 2 drop bromophenol blues are added dropwise, if not being in that sodium hydroxide is added dropwise until becoming blue in blue again, salpeter solution is added dropwise and is adjusted to yellow
After two drop of amount after color, 1ml diphenyl carbazone indicator is added, is titrated with mercuric nitrate standard liquid, aubergine, which is presented, is
For terminal, titration volumes are accurately read.
3) Cl in supernatant is calculated according to formula (I)-Content, since the chlorion in supernatant is all from chlorine
Silane, according to the Cl in supernatant-Content meter calculates the content of chlorosilane in dichloromethane sample.
4) preci-sion and accuracy is evaluated
According to step 1)~3) the dichloromethane sample that chlorosilane content is 88.29mg/L is carried out in five laboratories
Analysis calculates standard deviation by formula (a)：
S=Sqrt [(∑ (xi-xIt is average) ^2)/(N-1)] S formulas (a)
In formula (a), Sqrt is square root, and ∑ represents summation, and ^2 represents quadratic power, XIt is averageTo measure average value, N, which is represented, to be surveyed
Determine number, N=5 in experiment.
The coefficient of variation is calculated by formula (b)：
Vx=S/xIt is average100% formula (b)
In formula (b), S is standard deviation, xIt is averageTo measure average value,
It after measured and calculates, indoor relative standard deviation is 0.09%, and relative standard deviation is 1.1% between room, opposite to miss
Difference is 0.7%.
Pipette the chlorine silicon that 100mg is added in the dichloromethane sample that 100ml chlorosilane contents are 88.29mg/L in colorimetric cylinder
Alkane, according to step 1)~3) content of its chlorosilane is measured, calculate recovery of standard addition.5 groups of experiments of parallel progress, the results show that
The rate of recovery is between 98.1%~102.5%.
Embodiment 3
The measurement of chlorosilane in dichloromethane
1) 100ml samples are pipetted 20g ZSM-5 molecular sieves are added, 2min is shaken with pure water constant volume to 500ml in colorimetric cylinder
After stand, pipette 10ml supernatants to triangular flask.
2) 2 drop bromophenol blues are added dropwise, if not being in that sodium hydroxide is added dropwise until becoming blue in blue again, salpeter solution is added dropwise and is adjusted to yellow
After two drop of amount after color, 1ml diphenyl carbazone indicator is added, is titrated with mercuric nitrate standard liquid, aubergine, which is presented, is
For terminal, titration volumes are accurately read.
3) Cl in supernatant is calculated according to formula (I)-Content, since the chlorion in supernatant is all from chlorine
Silane, according to the Cl in supernatant-Content meter calculates the content of chlorosilane in dichloromethane sample.
4) preci-sion and accuracy is evaluated
The preci-sion and accuracy evaluation that the present embodiment assay method is evaluated according to the evaluation method of embodiment 2, as a result shows
Show：Indoor relative standard deviation is 0.07%, and relative standard deviation is 1.07% between room, relative error 0.64%, the rate of recovery
Between 98.5%~102.3%.
Embodiment 4
The measurement of chlorosilane in dichloromethane
1) 100ml samples are pipetted 20g reaction promoter-a are added, 2min is shaken with pure water constant volume to 500ml in colorimetric cylinder
After stand, pipette 10ml supernatants to triangular flask.
2) 2 drop bromophenol blues are added dropwise, if not being in that sodium hydroxide is added dropwise until becoming blue in blue again, salpeter solution is added dropwise and is adjusted to yellow
After two drop of amount after color, 1ml diphenyl carbazone indicator is added, is titrated with mercuric nitrate standard liquid, aubergine, which is presented, is
For terminal, titration volumes are accurately read.
3) Cl in supernatant is calculated according to formula (I)-Content, since the chlorion in supernatant is all from chlorine
Silane, according to the Cl in supernatant-Content meter calculates the content of chlorosilane in dichloromethane sample.
4) preci-sion and accuracy is evaluated
The preci-sion and accuracy evaluation that the present embodiment assay method is evaluated according to the evaluation method of embodiment 2, as a result shows
Show：Indoor relative standard deviation is 0.05%, and relative standard deviation is 1.04% between room, relative error 0.53%, the rate of recovery
Between 99.3%~101.8%.
Embodiment 5
The measurement of chlorosilane in dichloromethane
1) 100ml samples are pipetted 20g reaction promoter-b are added, 2min is shaken with pure water constant volume to 500ml in colorimetric cylinder
After stand, pipette 10ml supernatants to triangular flask.
2) 2 drop bromophenol blues are added dropwise, if not being in that sodium hydroxide is added dropwise until becoming blue in blue again, salpeter solution is added dropwise and is adjusted to yellow
After two drop of amount after color, 1ml diphenyl carbazone indicator is added, is titrated with mercuric nitrate standard liquid, aubergine, which is presented, is
For terminal, titration volumes are accurately read.
3) Cl in supernatant is calculated according to formula (I)-Content, since the chlorion in supernatant is all from chlorine
Silane, according to the Cl in supernatant-Content meter calculates the content of chlorosilane in dichloromethane sample.
4) preci-sion and accuracy is evaluated
The preci-sion and accuracy evaluation that the present embodiment assay method is evaluated according to the evaluation method of embodiment 2, as a result shows
Show：Indoor relative standard deviation is 0.04%；Relative standard deviation is 1.02% between room, relative error 0.43%；The rate of recovery
Between 100.13%~101.07%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. the assay method of chlorosilane, includes the following steps in a kind of dichloromethane：
A), dichloromethane sample and water are mixed, stands, takes supernatant；
B), the content of chlorion in the supernatant is measured, chlorine in dichloromethane sample is calculated according to measurement result
The content of silane.
2. assay method according to claim 1, which is characterized in that the volume ratio of the dichloromethane sample and water is (5
~20):40.
3. assay method according to claim 1, which is characterized in that the temperature of the mixing is 15~30 DEG C；It is described mixed
The time of conjunction is 0.5~5min.
4. assay method according to claim 1, which is characterized in that the step a) is：By dichloromethane sample, reaction
Accelerating agent and water mixing, stand, take supernatant；
The reaction promoter includes zeolite and the metal oxide that is supported on zeolite.
5. assay method according to claim 4, which is characterized in that the zeolite is ZSM-5 molecular sieve；
The metal oxide includes one or more in iron oxide, titanium dioxide, cerium oxide, yttrium oxide and molybdenum oxide.
6. assay method according to claim 5, which is characterized in that the metal oxide includes iron oxide, titanium dioxide
Titanium, cerium oxide, yttrium oxide and molybdenum oxide, the iron oxide, titanium dioxide, cerium oxide, yttrium oxide and molybdenum oxide mass ratio be
(1~2)：(1.5~3)：(0.5~1.5)：(0.1~1)：(1~2).
7. assay method according to claim 4, which is characterized in that load capacity of the metal oxide on zeolite be
0.5~15wt%.
8. assay method according to claim 4, which is characterized in that the reaction promoter is prepared into accordance with the following methods
It arrives：
It after zeolite impregnates in metal salt solution, is calcined, obtains reaction promoter.
9. assay method according to claim 4, which is characterized in that the amount ratio of the reaction promoter and water be (1~
5)g：40ml.
10. according to claim 1~9 any one of them assay method, which is characterized in that measured using mercurimetry in step b)
The content of chlorion in the supernatant.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4497942A (en) * | 1983-12-14 | 1985-02-05 | General Electric Company | Process for hydrolyzing chlorosilanes |
| CN1090580A (en) * | 1993-02-03 | 1994-08-10 | 化学工业部晨光化工研究院成都分院 | The method for hydrolysis of organic radical silicane dichloride |
| JP2000338098A (en) * | 1999-05-25 | 2000-12-08 | Shin Etsu Chem Co Ltd | Continuous determination of hydrolyzable component in hydrolyzable component-containing gas material |
| CN105510313A (en) * | 2015-11-23 | 2016-04-20 | 湖北平安电工股份有限公司 | Rapid purity detection method of industrial grade chlorosilane |
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2018
- 2018-03-28 CN CN201810263927.2A patent/CN108490113B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4497942A (en) * | 1983-12-14 | 1985-02-05 | General Electric Company | Process for hydrolyzing chlorosilanes |
| CN1090580A (en) * | 1993-02-03 | 1994-08-10 | 化学工业部晨光化工研究院成都分院 | The method for hydrolysis of organic radical silicane dichloride |
| JP2000338098A (en) * | 1999-05-25 | 2000-12-08 | Shin Etsu Chem Co Ltd | Continuous determination of hydrolyzable component in hydrolyzable component-containing gas material |
| CN105510313A (en) * | 2015-11-23 | 2016-04-20 | 湖北平安电工股份有限公司 | Rapid purity detection method of industrial grade chlorosilane |
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| Title |
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| 陈其国等: "氯硅烷水解工艺研究进展", 《化工管理》 * |
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