CN101865895A - Method for measuring acrylonitrile monomer content in polyacrylonitrile polymer fluid - Google Patents
Method for measuring acrylonitrile monomer content in polyacrylonitrile polymer fluid Download PDFInfo
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Abstract
The invention discloses a method for measuring the acrylonitrile monomer content in polyacrylonitrile polymer fluid, which comprises the following steps: 1) preparing polyacrylonitrile polymer fluid with standard acrylonitrile content; 2) preparing a standard acrylonitrile content curve; 3) obtaining a chromatogram map of residue acrylonitrile monomer in the polyacrylonitrile polymer fluid to be measured; and 4) measuring the residue acrylonitrile monomer in the polyacrylonitrile polymer fluid to be measured: adopting a static-state headspace method as an enrichment method of samples. The invention solves the technical problem that the existing method for measuring the acrylonitrile monomer content in polyacrylonitrile polymer fluid has larger error caused by large subjective arbitrariness, is convenient and feasible, and can quickly and accurately analyze the content of the residue acrylonitrile monomer in the polyacrylonitrile polymer fluid according to the requirements.
Description
Technical field
The invention belongs to the technical field of high molecular polymer method of testing, be specifically related to the method for testing of remaining acrylonitrile monomer content in a kind of polyacrylonitrile polymer fluid.
Background technology
Polyacrylonitrile (PAN) carbon fiber has obtained widespread use because of a series of excellent properties in every field.The high-quality precursor is the prerequisite of producing high-performance carbon fibre.The high-quality precursor should possess high-purity, high strength, high-orientation, thin dawnization and not have characteristic such as adhesion.The preparation of precursor comprises polymerization and two processing steps of spinning.Wherein, polymerization is the source that carbon fiber is produced, and also is one of committed step that improves former yarn quality.Therefore, the performance of polymer fluid directly influences the performance of precursor.And the existence of polymerization single polymerization monomer can cause following harmful effect in the polymer fluid: 1) reduced the viscosity of polymer fluid, thereby the viscosity of polymer fluid and actual viscosity measured be there are differences; 2) from solidify strand, overflow the bigger hole of formation; 3), overflow at the higher process section of boiling water drawing-off equitemperature and to become impurity because of its boiling point is lower.Therefore, the foundation of the method for testing of micro-polymerization single polymerization monomer is very important in the good polymer fluid.Adopted the method for chemistry titration to measure in the past,, and generated quantitative NaOH,, made indicator with alizarin yellow element-thymol phthalein with the titration of standard dilution heat of sulfuric acid because of vinyl cyanide and sodium sulphite remaining in the polyacrylonitrile slurries play addition reaction in aqueous solution.The advantage of the method is not need expensive testing apparatus, can finish with simple Experimental Establishment.Shortcoming is the operator is had relatively high expectations, and operator's subjectivity is bigger to result's influence, especially easily forms bigger error under the less situation of remaining acrylonitrile monomer content.
Summary of the invention
The object of the invention provides the assay method that a kind of rapid and precise mensuration remains in the polyacrylonitrile polymer fluid acrylonitrile monomer content, thereby it has solved the subjective random big bigger technical matters of error of assay method of content of monomer in the existing polyacrylonitrile polymer fluid
Technical solution of the present invention is:
The assay method of acrylonitrile monomer content in a kind of polyacrylonitrile polymer fluid, its special character is: this method may further comprise the steps:
1] polyacrylonitrile polymer fluid of preparation standard acrylonitrile content:
Get the 0.5000g vinyl cyanide and add 100ml not contain vinyl cyanide and solid content be 1% polyacrylonitrile polymer fluid, make 100ml standard solution A; Get 10ml standard solution A and add that not contain vinyl cyanide and solid content be 1% polyacrylonitrile polymer fluid, make 100ml standard solution B; Get 10ml standard solution B and add that not contain vinyl cyanide and solid content be 1% polyacrylonitrile polymer fluid, making acrylonitrile content is the polyacrylonitrile polymer fluid 100ml of 50mg/L;
2] production standard acrylonitrile content curve:
In the tool plug head space bottle of 6 25ml, add polyacrylonitrile polymer fluid 0.75ml, 1.5ml, 3.00ml, 6.00ml, 9.00ml, the 12.00ml that acrylonitrile content is 50mg/L respectively, adding respectively successively and not containing vinyl cyanide and solid content is 1% polyacrylonitrile polymer fluid 14.25ml, 13.50ml, 12.00ml, 9.00ml, 6.00ml, 3.00ml, tighten bottle cap, fully shake up; Place 75～85 ℃ of waters bath with thermostatic control respectively, heating balance 10～40min; Extracting static headspace gas 3ml inject gas chromatograph rapidly with syringe respectively, measure peak area, is horizontal ordinate with the acrylonitrile concentration, and peak area is an ordinate, drawing standard acrylonitrile content curve;
3] chromatogram of remaining acrylonitrile monemer in the acquisition polyacrylonitrile polymer fluid to be measured:
Getting the fine polymer fluid of polypropylene to be measured, is 1～5% polyacrylonitrile polymer fluid to weight percent concentration with organic solvent diluting; Polyacrylonitrile polymer fluid put into dilution in a head space bottle after requires the volume of polyacrylonitrile polymer fluid to be 0.6～0.7 times of this head space bottle volume; The head space equilibrium temperature is 75～85 ℃, and the heating equilibration time is 10～40min, makes monomer component head space enrichment in the polymer fluid; Extract static headspace gas 3ml inject gas chromatograph rapidly with syringe, obtain the chromatogram of remaining acrylonitrile monemer in the polyacrylonitrile polymer fluid to be measured;
4] mensuration of remaining acrylonitrile monemer in the polyacrylonitrile polymer fluid to be measured:
Use step 2] in the standard acrylonitrile content curve drawn, calculate the acrylonitrile monomer content of this polyacrylonitrile polymer fluid.
Utilize the chromatographic condition of selecting in the peak area process of gas chromatograph measurement vinyl cyanide to be in above-mentioned steps 2 and the step 3: to select 30m * 0.25mm, 0.5 the kapillary of μ m is as the stratographic analysis post, column temperature is 70 ℃～90 ℃, 160 ℃～180 ℃ of injector temperatures, hydrogen flowing quantity 30ml/min, air mass flow 400ml/min, high pure nitrogen flow 30ml/min, detecting device adopts hydrogen flame ionization detector, 170 ℃～180 ℃, gas sampling amount 3ml.
Above-mentioned steps 3] in the weight percent concentration of polyacrylonitrile polymer fluid be 1%;
Above-mentioned steps 3] in organic solvent be dimethyl sulfoxide, dimethyl formamide or dimethyl acetamide.
The beneficial effect that the present invention had:
1, the present invention selects for use static head space method as the sample enrichment method, and the micro-vinyl cyanide that is dissolved in the polyacrylonitrile polymer fluid is vaporized quantitatively in static headspace gas, has realized the separating of remaining acrylonitrile monemer and polyacrylonitrile polymer fluid, enrichment and quantitative measurement.
So only select static head space method for use, be because it has following remarkable advantage:
1) be applicable to can not the polymer fluid of direct boiling in the mensuration of micro-volatile constituent;
2) chromatographic column can be owing to direct injected (higher boiling, non-volatile sample) is polluted chromatographic system;
3) owing to other component concentrations of concentration ratio of volatile constituent in gas phase is big, in chromatogram, can obtain than advancing the better degree of separation of liquid-like simultaneously.
2, assay method of the present invention is convenient and easy, can analyze remaining acrylonitrile monomer content in the polyacrylonitrile polymer fluid as required fast and accurately.For the personnel that are engaged in experimental analysis, as long as according to certain training, just can very fast this assay method of grasp and then measure result accurately and reliably.
Embodiment
The present invention adopts static headspace gas chromatography as the method for measuring remaining acrylonitrile monomer content in the polyacrylonitrile polymer fluid, comprise job steps such as the mensuration of remaining acrylonitrile monomer content in the making, polyacrylonitrile polymer fluid of preparation, the standard acrylonitrile content curve of standard acrylonitrile content polyacrylonitrile polymer fluid dilution and analysis, its concrete steps are:
One, the preparation of standard acrylonitrile content polyacrylonitrile polymer fluid dilution: accurately take by weighing 0.5000g vinyl cyanide (analyzing pure) in the 100ml volumetric flask, add the solid content do not contain vinyl cyanide and be 1% polyacrylonitrile polymer fluid to scale, shake up, obtain to include the polyacrylonitrile polymer fluid of 5000mg/L standard acrylonitrile content; Accurately pipette 10ml standard acrylonitrile content polyacrylonitrile polymer fluid in the 100ml volumetric flask, add the solid content do not contain vinyl cyanide and be 1% polyacrylonitrile polymer fluid, shake up, obtain to include 500mg/L standard acrylonitrile content polyacrylonitrile polymer fluid to scale; Accurately pipette 10ml standard acrylonitrile content polyacrylonitrile polymer fluid in the 100ml volumetric flask, add the solid content do not contain vinyl cyanide and be 1% polyacrylonitrile polymer fluid, shake up, obtain to include 50mg/L standard acrylonitrile content polyacrylonitrile polymer fluid to scale;
Two, the making of standard acrylonitrile content curve: in the tool plug head space bottle of 6 25ml, add standard acrylonitrile content polyacrylonitrile polymer fluid dilution 0.75ml, 1.5ml, 3.00ml, 6.00ml, 9.00ml, 12.00ml respectively, add the solid content do not contain vinyl cyanide more successively respectively and be 1% polyacrylonitrile polymer fluid 14.25ml, 13.50ml, 12.00ml, 9.00ml, 6.00ml, 3.00ml, tighten the bottle cap that has teflon, fully shake up; Place 75 ℃～85 ℃ waters bath with thermostatic control respectively, heating balance 30 minutes, during shake head space bottle 3 times to quicken vapor-liquid equilibrium; Extracting static headspace gas 3ml inject gas chromatograph rapidly with the 3ml syringe respectively, measure peak area, is horizontal ordinate with the acetone concentration, and peak area is an ordinate, drawing standard acrylonitrile content curve.
Three, the mensuration of remaining acrylonitrile monomer content in the polyacrylonitrile polymer fluid: the solid content to be measured that pipettes 15ml is that 1% polyacrylonitrile polymer fluid is in the tool plug head space bottle of 25ml in volume, tightens the bottle cap that has teflon, fully shakes up; Place 75 ℃～85 ℃ waters bath with thermostatic control, heating balance 20-60 minute, during shake head space bottle 3 times to quicken vapor-liquid equilibrium; Extract static headspace gas 3ml inject gas chromatograph rapidly with the 3ml syringe respectively, under selected chromatographic condition, measure the peak area of vinyl cyanide, calculate remaining acrylonitrile monomer content in the polyacrylonitrile polymer fluid to be determined by external standard method then.
Selected chromatographic condition is in the above-mentioned peak area process of utilizing gas chromatograph measurement vinyl cyanide: select 30m * 0.25mm, 0.5 the kapillary of μ m is as the stratographic analysis post, column temperature is 70 ℃～90 ℃, 160 ℃～180 ℃ of injector temperatures, hydrogen flowing quantity 30ml/min, air mass flow 400ml/min, high pure nitrogen (99.999%) flow 30ml/min, detecting device adopts hydrogen flame ionization detector (FID), 170 ℃～180 ℃, gas sampling amount 3ml.
According to the actual range of remaining acrylonitrile monomer content in the polyacrylonitrile polymer fluid, select 0～50mg/l in the experiment as the typical curve concentration range.Press the method for making of typical curve, measure the peak area of variable concentrations standard vinyl cyanide, to acrylonitrile concentration C mapping, obtaining its regression equation is A=695.6C-3.123, r=0.9992 with peak area A.
Embodiment:
Pipette 6 parts in the same polyacrylonitrile polymer fluid sample of 15ml and be placed in 6 25ml head space bottles, tighten the bottle cap that has teflon, fully shake up; Place 80 ℃ of waters bath with thermostatic control respectively, heating balance 30 minutes, during shake the head space bottle 3 times, extract static headspace gas 3ml inject gas chromatograph rapidly with the 3ml syringe respectively and experimentize; At selected chromatographic condition (stratographic analysis post: 30m * 0.25mm, 0.5 the kapillary of μ m, column temperature: 80 ℃, the sample introduction temperature: 170 ℃, hydrogen flowing quantity 30ml/min, air mass flow 400ml/min, high pure nitrogen (99.999%) flow 30ml/min, detecting device: hydrogen flame ionization detector, 180 ℃, gas sampling amount 3ml) measures the peak area of vinyl cyanide under; Calculate by external standard method that acrylonitrile concentration is respectively in the polyacrylonitrile polymer fluid to be measured: 14.5mg/L, 14.3mg/L, 13.9mg/L, 14.8mg/L, 13.7mg/L, 14.2mg/L, mean value are 14.23mg/L, and result's standard deviation (SD) is 0.398.
Claims (4)
1. the assay method of acrylonitrile monomer content in the polyacrylonitrile polymer fluid, it is characterized in that: this method may further comprise the steps:
1] polyacrylonitrile polymer fluid of preparation standard acrylonitrile content:
Get the 0.5000g vinyl cyanide and add 100ml not contain vinyl cyanide and solid content be 1% polyacrylonitrile polymer fluid, make 100ml standard solution A; Get 10ml standard solution A and add that not contain vinyl cyanide and solid content be 1% polyacrylonitrile polymer fluid, make 100ml standard solution B; Get 10ml standard solution B and add that not contain vinyl cyanide and solid content be 1% polyacrylonitrile polymer fluid, making acrylonitrile content is the polyacrylonitrile polymer fluid 100ml of 50mg/L;
2] production standard acrylonitrile content curve:
In the tool plug head space bottle of 6 25ml, add polyacrylonitrile polymer fluid 0.75ml, 1.5ml, 3.00ml, 6.00ml, 9.00ml, the 12.00ml that acrylonitrile content is 50mg/L respectively, adding respectively successively and not containing vinyl cyanide and solid content is 1% polyacrylonitrile polymer fluid 14.25ml, 13.50ml, 12.00ml, 9.00ml, 6.00ml, 3.00ml, tighten bottle cap, fully shake up; Place 75～85 ℃ of waters bath with thermostatic control respectively, heating balance 10～40min; Extracting static headspace gas 3ml inject gas chromatograph rapidly with syringe respectively, measure peak area, is horizontal ordinate with the acrylonitrile concentration, and peak area is an ordinate, drawing standard acrylonitrile content curve;
3] chromatogram of remaining acrylonitrile monemer in the acquisition polyacrylonitrile polymer fluid to be measured:
Getting the fine polymer fluid of polypropylene to be measured, is 1～5% polyacrylonitrile polymer fluid to weight percent concentration with organic solvent diluting; Polyacrylonitrile polymer fluid put into dilution in a head space bottle after requires the volume of polyacrylonitrile polymer fluid to be 0.6～0.7 times of this head space bottle volume; The head space equilibrium temperature is 75～85 ℃, and the heating equilibration time is 10～40min, makes monomer component head space enrichment in the polymer fluid; Extract static headspace gas 3ml inject gas chromatograph rapidly with syringe, obtain the chromatogram of remaining acrylonitrile monemer in the polyacrylonitrile polymer fluid to be measured;
4] mensuration of remaining acrylonitrile monemer in the polyacrylonitrile polymer fluid to be measured:
Use step 2] in the standard acrylonitrile content curve drawn, calculate the acrylonitrile monomer content of this polyacrylonitrile polymer fluid.
2. the assay method of acrylonitrile monomer content in the polyacrylonitrile polymer fluid according to claim 1, it is characterized in that: utilize the chromatographic condition of selecting in the peak area process of gas chromatograph measurement vinyl cyanide to be in described step 2 and the step 3: to select 30m * 0.25mm, 0.5 the kapillary of μ m is as the stratographic analysis post, column temperature is 70 ℃～90 ℃, 160 ℃～180 ℃ of injector temperatures, hydrogen flowing quantity 30ml/min, air mass flow 400ml/min, high pure nitrogen flow 30ml/min, detecting device adopts hydrogen flame ionization detector, 170 ℃～180 ℃, gas sampling amount 3ml.
3. according to the assay method of acrylonitrile monomer content in claim 1 or 2 polyacrylonitrile polymer fluids, it is characterized in that: described step 3] in the weight percent concentration of polyacrylonitrile polymer fluid be 1%;
4. the assay method of acrylonitrile monomer content in the polyacrylonitrile polymer fluid according to claim 3 is characterized in that: described step 3] in organic solvent be dimethyl sulfoxide, dimethyl formamide or dimethyl acetamide.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102095812A (en) * | 2010-11-25 | 2011-06-15 | 中国检验检疫科学研究院 | Method for detecting acrylonitrile in cosmetics by using gas chromatograph-mass spectrography |
| CN102721765A (en) * | 2012-06-27 | 2012-10-10 | 中国科学院宁波材料技术与工程研究所 | Method for determining content of acrylonitrile monomer in polyacrylonitrile polymer liquid |
| CN102749389A (en) * | 2011-04-20 | 2012-10-24 | 中国石油化工股份有限公司 | Analytic method of acrylonitrile material |
| CN104181156A (en) * | 2014-09-10 | 2014-12-03 | 江苏恒神纤维材料有限公司 | Method for testing content of ammonia in polyacrylonitrile polymer |
| CN106353306A (en) * | 2016-08-17 | 2017-01-25 | 中简科技股份有限公司 | Method for testing residual acrylonitrile monomer content in spinning solution during carbon fiber production |
| CN107167334A (en) * | 2016-03-08 | 2017-09-15 | 莫福探测仪器有限责任公司 | The chemical vapor of the temperature influence of compound with low volatility and detection |
| CN107167335A (en) * | 2016-03-08 | 2017-09-15 | 莫福探测仪器有限责任公司 | The chemical vapor of compound with low volatility and detection |
| CN109142124A (en) * | 2018-08-30 | 2019-01-04 | 必维申优质量技术服务江苏有限公司 | A kind of improved modified acrylic fibre qualitative and quantitative analysis method |
| CN111323495A (en) * | 2018-12-14 | 2020-06-23 | 乐凯华光印刷科技有限公司 | Method for measuring residual amounts of acrylonitrile and styrene in thermoplastic nano-micron particle emulsion |
| CN113740285A (en) * | 2021-08-20 | 2021-12-03 | 北京化工大学 | Method for testing solid content of polyacrylonitrile spinning solution |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102095812B (en) * | 2010-11-25 | 2013-06-05 | 中国检验检疫科学研究院 | Method for detecting acrylonitrile in cosmetics by using gas chromatograph-mass spectrography |
| CN102095812A (en) * | 2010-11-25 | 2011-06-15 | 中国检验检疫科学研究院 | Method for detecting acrylonitrile in cosmetics by using gas chromatograph-mass spectrography |
| CN102749389A (en) * | 2011-04-20 | 2012-10-24 | 中国石油化工股份有限公司 | Analytic method of acrylonitrile material |
| CN102749389B (en) * | 2011-04-20 | 2014-07-02 | 中国石油化工股份有限公司 | Analytic method of acrylonitrile material |
| CN102721765A (en) * | 2012-06-27 | 2012-10-10 | 中国科学院宁波材料技术与工程研究所 | Method for determining content of acrylonitrile monomer in polyacrylonitrile polymer liquid |
| CN102721765B (en) * | 2012-06-27 | 2013-12-04 | 中国科学院宁波材料技术与工程研究所 | Method for determining content of acrylonitrile monomer in polyacrylonitrile polymer liquid |
| CN104181156A (en) * | 2014-09-10 | 2014-12-03 | 江苏恒神纤维材料有限公司 | Method for testing content of ammonia in polyacrylonitrile polymer |
| CN104181156B (en) * | 2014-09-10 | 2016-08-17 | 江苏恒神股份有限公司 | The method of testing of ammonia content in polyacrylonitrile polymer stock solution |
| CN107167335A (en) * | 2016-03-08 | 2017-09-15 | 莫福探测仪器有限责任公司 | The chemical vapor of compound with low volatility and detection |
| CN107167334A (en) * | 2016-03-08 | 2017-09-15 | 莫福探测仪器有限责任公司 | The chemical vapor of the temperature influence of compound with low volatility and detection |
| CN106353306A (en) * | 2016-08-17 | 2017-01-25 | 中简科技股份有限公司 | Method for testing residual acrylonitrile monomer content in spinning solution during carbon fiber production |
| CN106353306B (en) * | 2016-08-17 | 2019-10-25 | 中简科技股份有限公司 | The test method of spinning solution remaining propylene nitrile monomer content in a kind of carbon fiber production process |
| CN109142124A (en) * | 2018-08-30 | 2019-01-04 | 必维申优质量技术服务江苏有限公司 | A kind of improved modified acrylic fibre qualitative and quantitative analysis method |
| CN109142124B (en) * | 2018-08-30 | 2020-12-08 | 必维申优质量技术服务江苏有限公司 | Improved qualitative and quantitative analysis method for modified polyacrylonitrile fiber |
| CN111323495A (en) * | 2018-12-14 | 2020-06-23 | 乐凯华光印刷科技有限公司 | Method for measuring residual amounts of acrylonitrile and styrene in thermoplastic nano-micron particle emulsion |
| CN111323495B (en) * | 2018-12-14 | 2023-03-14 | 乐凯华光印刷科技有限公司 | Method for measuring residual amounts of acrylonitrile and styrene in thermoplastic nano-micron particle emulsion |
| CN113740285A (en) * | 2021-08-20 | 2021-12-03 | 北京化工大学 | Method for testing solid content of polyacrylonitrile spinning solution |
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Application publication date: 20101020 |