CN101881719A - Test method of gel particles in polyacrylonitrile polymer solution - Google Patents
Test method of gel particles in polyacrylonitrile polymer solution Download PDFInfo
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- CN101881719A CN101881719A CN 201010210608 CN201010210608A CN101881719A CN 101881719 A CN101881719 A CN 101881719A CN 201010210608 CN201010210608 CN 201010210608 CN 201010210608 A CN201010210608 A CN 201010210608A CN 101881719 A CN101881719 A CN 101881719A
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- gel particles
- filter paper
- polyacrylonitrile polymer
- polymer fluid
- polymer solution
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Abstract
The invention relates to a test method of gel particles in polyacrylonitrile polymer solution, comprising the following steps: 1] adjusting the weight percent of the polyacrylonitrile polymer solution to be 2-8% by an organic solvent, wherein, the organic solvent is dimethyl sulfoxide, dimethylformamide or dimethyl acetylamide; 2] filtering the above solution by utilizing glass fibre filter paper, wherein, the bore diameter of the glass fibre filter paper is 0.5-2 mu m; and 3] filtering the glass fibre filter paper of the above solution under the irradiation of an ultraviolet ray fluorescent lamp, wherein if foreign matters which emit white light or bluish white light are on the filter paper, the gel particles exist in the polymerization solution; and if not, the gel particles do not exist in the polymerization solution. The invention solves the technical problems of hole blocking and broken wire or paste board caused by the gel particles of the existing polyacrylonitrile polymer solution; and the method of the invention does not need expensive detection equipment, and can rapidly and cheaply detect the existence of the gel particles in the polyacrylonitrile polymer solution.
Description
Technical field
The invention belongs to the technical field of the high molecular polymer method of inspection, relate to the method for inspection of gel particles in a kind of high molecular polymer, be used for the fast detecting polyacrylonitrile polymer and whether contain gel particles.
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.Have in the polymer fluid that impurity, polymer fluid solid content are too high, polymerization process stirs reasons such as the clean or polymer fluid of inhomogeneous, preceding polymerization afterreaction still cleaning standing time is long and can cause all that gel particles forms in the polymer fluid.If there is gel particles to exist in the polymer fluid, will cause the plug-hole phenomenon, produce fracture of wire when serious or stick with paste plate, perhaps pass spinneret orifice and form defective big in the strand because of the pressure effect, therefore, before spinning, carry out multiple times of filtration to polymer fluid, in the hope of removing various physics impurity and the big gel particles that may exist in the polymer fluid, to reduce potential defective in the precursor.Laser particle analyzer can be used for the detection of gel particles in the polymer fluid, and can provide concrete gel number and size, but equipment is comparatively expensive.
Summary of the invention
The object of the invention provides the technical matters that the method that whether has gel particles in a kind of quick and cheap detection polymer fluid can cause the plug-hole phenomenon, produce fracture of wire or stick with paste plate for the gel particles that solves existing polyacrylonitrile polymer fluid.
Technical solution of the present invention:
The method of inspection of gel particles in the polyacrylonitrile polymer fluid, its special being: may further comprise the steps:
1] with organic solvent the percentage by weight of polyacrylonitrile polymer fluid is adjusted to 2～8%; Described organic solvent is dimethyl sulfoxide, dimethyl formamide or dimethyl acetamide;
2] use glass fiber filter paper to filter above-mentioned solution, the aperture of described glass fiber filter paper is 0.5～2 μ m:
3] if the foreign matter of white sent or bluish-white light is arranged on the filter paper, then there is gel particles in the glass fiber filter paper that above-mentioned solution has been filtered in irradiation under the ultraviolet fluorescent lamp in the polymer fluid; Otherwise, do not have gel particles in the polymer fluid.
Above-mentioned steps 1] in organic solvent be 3～4% with the percentage by weight of polymer fluid adjustment.
Above-mentioned steps 2] in the aperture of glass fiber filter paper be 1 μ m.
The invention has the beneficial effects as follows: method provided by the present invention does not need expensive detection equipment, the existence of gel particles in the detection polyacrylonitrile polymer fluid that just can be quick and cheap.
Embodiment
Use and the identical solvent of solvent in the spinning solution, as dimethyl sulfoxide, dimethyl formamide, dimethyl acetamide, the polyacrylonitrile polymer concentration of spinning solution is adjusted to 2～8% weight percent content, use the glass fiber filter paper in 0.5～2 μ m aperture to filter this solution, the glass fiber filter paper that above-mentioned solution has been filtered in irradiation under the ultraviolet fluorescent lamp, have gel particles in the spinning solution if there is the foreign matter of white sent or bluish-white light promptly to illustrate on the filter paper, this spinning solution needs to handle again.
Polymer weight degree preferably 3～4%.
The pore diameter range of glass fiber filter paper is 1 μ m preferably.
Claims (3)
1. the method for inspection of gel particles in the polyacrylonitrile polymer fluid is characterized in that: may further comprise the steps:
1] with organic solvent the percentage by weight of polyacrylonitrile polymer fluid is adjusted to 2～8%; Described organic solvent is dimethyl sulfoxide, dimethyl formamide or dimethyl acetamide;
2] use glass fiber filter paper to filter above-mentioned solution, the aperture of described glass fiber filter paper is 0.5～2 μ m;
3] if the foreign matter of white sent or bluish-white light is arranged on the filter paper, then there is gel particles in the glass fiber filter paper that above-mentioned solution has been filtered in irradiation under the ultraviolet fluorescent lamp in the polymer fluid; Otherwise, do not have gel particles in the polymer fluid.
2. the method for inspection of gel particles in the polyacrylonitrile polymer fluid according to claim 1 is characterized in that: described step 1] in organic solvent be 3～4% with the percentage by weight of polymer fluid adjustment.
3. the method for inspection of gel particles in the polyacrylonitrile polymer fluid according to claim 1 and 2 is characterized in that: described step 2] in the aperture of glass fiber filter paper be 1 μ m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102106089A CN101881719B (en) | 2010-06-28 | 2010-06-28 | Test method of gel particles in polyacrylonitrile polymer solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102106089A CN101881719B (en) | 2010-06-28 | 2010-06-28 | Test method of gel particles in polyacrylonitrile polymer solution |
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| Publication Number | Publication Date |
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| CN101881719A true CN101881719A (en) | 2010-11-10 |
| CN101881719B CN101881719B (en) | 2012-01-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2010102106089A Expired - Fee Related CN101881719B (en) | 2010-06-28 | 2010-06-28 | Test method of gel particles in polyacrylonitrile polymer solution |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113804592A (en) * | 2021-09-24 | 2021-12-17 | 中国石油化工股份有限公司 | Method for detecting gel particles in PAN spinning stock solution |
Citations (5)
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| CN1475789A (en) * | 2003-07-01 | 2004-02-18 | 武汉理工大学 | Settling type laser reflection image point granularity measuring method |
| JP2006098212A (en) * | 2004-09-29 | 2006-04-13 | Shimadzu Corp | Particle size distribution measuring instrument |
| CN1865918A (en) * | 2006-05-31 | 2006-11-22 | 天津大学 | Coaxial double test-surface laser particle analyzer |
| CN101290281A (en) * | 2008-06-12 | 2008-10-22 | 丹东百特科技有限公司 | Three-light beam single lens laser particle sizer |
| CN101561403A (en) * | 2009-06-01 | 2009-10-21 | 燕山大学 | Three-dimensional orthogonality microscope image pick-up observation device and quantitative image method thereof |
-
2010
- 2010-06-28 CN CN2010102106089A patent/CN101881719B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1475789A (en) * | 2003-07-01 | 2004-02-18 | 武汉理工大学 | Settling type laser reflection image point granularity measuring method |
| JP2006098212A (en) * | 2004-09-29 | 2006-04-13 | Shimadzu Corp | Particle size distribution measuring instrument |
| CN1865918A (en) * | 2006-05-31 | 2006-11-22 | 天津大学 | Coaxial double test-surface laser particle analyzer |
| CN101290281A (en) * | 2008-06-12 | 2008-10-22 | 丹东百特科技有限公司 | Three-light beam single lens laser particle sizer |
| CN101561403A (en) * | 2009-06-01 | 2009-10-21 | 燕山大学 | Three-dimensional orthogonality microscope image pick-up observation device and quantitative image method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 《Joural of Applied Polymer Science》 19961231 P.BAJAJ ET AL 《Solution Polymerization of Acrylonitrile with Vinyl Acids in Dimethylformamide》 1539-1550 1-3 第59卷, 2 * |
| 《化工新型材料》 20091231 孟庆杰等 《纺丝液固含量对湿纺PAN初生纤维结构形态的影响》 70-72 1-3 第37卷, 第12期 2 * |
| 《合成纤维》 20081231 彭公秋等 《聚丙烯腈碳纤维原丝聚合及凝固成形的研究进展》 1-5 1-3 , 第2期 2 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113804592A (en) * | 2021-09-24 | 2021-12-17 | 中国石油化工股份有限公司 | Method for detecting gel particles in PAN spinning stock solution |
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| CN101881719B (en) | 2012-01-04 |
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