CN104181156A - Method for testing content of ammonia in polyacrylonitrile polymer - Google Patents
Method for testing content of ammonia in polyacrylonitrile polymer Download PDFInfo
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- CN104181156A CN104181156A CN201410459759.6A CN201410459759A CN104181156A CN 104181156 A CN104181156 A CN 104181156A CN 201410459759 A CN201410459759 A CN 201410459759A CN 104181156 A CN104181156 A CN 104181156A
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Abstract
The invention provides a method for testing content of ammonia in a polyacrylonitrile polymer. The method sequentially comprises the following steps: weighing a to-be-tested sample to a central position of a glass sheet, extruding and performing film-drawing on the sample by adopting the same glass sheet, washing for three times by adopting pure water, and titrating the washing liquid by using a standard solution of hydrochloric acid, so as to calculate the content of ammonia in the sample. The testing method is a method capable of simply and accurately testing the content of ammonia in polyacrylonitrile, and the problem that the addition amount and residual quantity of ammonia cannot be accurately controlled because the content of ammonia in the polyacrylonitrile polymer cannot be accurately tested in the ammonia modification process at present is solved.
Description
Technical field
The present invention relates to the method for testing of ammonia content in a kind of polyacrylonitrile polymer.
Background technology
High temperature resistant, corrosion-resistant, the feature such as thermal expansivity is little, good stability of the dimension, high specific strength, high ratio modulus that carbon fiber has, be a kind of desirable functional material and structured material, be widely used in the fields such as Aero-Space, the energy, traffic, electronics, civil engineering work and Leisure Sport.The carbon fiber overwhelming majority of production and selling is all polyacrylonitrile (PAN) base carbon fibre in the world at present.
PAN-based carbon fiber is that vinyl cyanide (AN) carries out free radical polymerization with comonomer, and then spinning, pre-oxidation carbonization are prepared from, and it is the effective ways that improve final carbon fiber performance that polyacrylonitrile is carried out to ammonia modification.There are document and patent report both at home and abroad to the performance that passes into a certain amount of ammonia in the polyacrylonitrile spinning solution after polymerization and can improve precursor and carbon fiber, pass into ammonia and can neutralize remaining itaconic acid, make the pH of spinning liquid reach (U.S.Pat.No.4603041) (U.S.Pat.No.6221492 B1) of 8 left and right (U.S.Pat.No.4336022) simultaneously.But how the amount that passes into ammonia is controlled, and in stoste, the method for testing of residual ammonia content does not have relevant report at present.
Summary of the invention
The object of this invention is to provide a kind of method that can simply, accurately test ammonia content in polyacrylonitrile, realize polyacrylonitrile is carried out to the accurate quantification control that ammonia modification is.
Technical solution of the present invention is:
The method of testing of ammonia content in a kind of polyacrylonitrile polymer, take testing sample to glass sheet center, adopt the extruding of same glass sheet and by sample membrane, adopt after pure water rinsing 3 times, flushing liquid is carried out to titration with hydrochloric acid standard solution, carry out the ammonia content in calculation sample.
Further, be specially:
Step 1: polyacrylonitrile polymer to be measured is poured in measuring cup, by decrement method ten thousand/ analytical balance on take testing sample 1.0-2.0g in circular glass sheet in the heart, be accurate to 0.0001g, be designated as M;
Step 2: being pressed in to drip with an identical glass sheet again has on the glass sheet of sample, and 2 blocks of glass sheet overlap, and with pointing the slurries that push gently in glass sheet, are squeezed into a circle, and circular one side and one side of glass sheet overlap, and the slurries that are pressed into are thin;
Step 3: rotate a glass sheet 180 and spend, 2 blocks of glass sheet point-blank, outwards draw 2 blocks of glass sheet gently, until 2 blocks of glass sheet separate;
Step 4: with the slurries on pure water rinsing glass sheet, be flushed in the beaker of a 500ml, attention can not spill, slurries are met after water, the film forming of can condensing, the one side of clamping film with tweezers, take off gently film, film is put into the beaker of wash-down water, soaked one minute, then wash-down water is poured in conical flask;
Step 5: pure water is poured in beaker, soaked film one minute, then water is poured in the conical flask of step 4 into 3 times so repeatedly;
Step 6: drip 2 methyl red-methylene blue indicator in conical flask, with the solution in Hydrochloric Standard Titration titration conical flask, being titrated to solution colour purpling look is terminal, writes down volume V;
Step 7: according to formula
calculate the ammonia content wt% in polyacrylonitrile polymer;
In formula: wt% is the ammonia content in polyacrylonitrile polymer to be measured, V is that titration consumes the volume of hydrochloric acid standard solution, the concentration that C is Hydrochloric Standard Titration, and M is the quality of the polyacrylonitrile polymer to be measured that takes, 17.03---the molal weight of ammonia.
Further, circular glass sheet diameter is 9cm.
The invention has the beneficial effects as follows: this method of testing, it is a kind of method that can simply, accurately test ammonia content in polyacrylonitrile, solve current polyacrylonitrile in ammonia modifying process, in polyacrylonitrile polymer, the content of ammonia cannot accurately be tested, thereby makes the addition of ammonia and the problem that residual volume cannot accurately be controlled.
Embodiment
Describe the preferred embodiments of the present invention below in detail.
Embodiment mono-
The present embodiment is the method for testing of ammonia content in a kind of polyacrylonitrile polymer, and its detailed process is:
Step 1, adopts decrement method to take 1.4967g polymkeric substance to be measured to glass sheet center.
Step 2, being pressed in to drip with the identical vial of another piece has on the vial of sample, and 2 blocks of glass sheet overlap, and with pointing the slurries that push gently in glass sheet, are squeezed into a circle, and circular one side and one side of glass sheet overlap, and the slurries that are pressed into are thin.
Step 3, rotates a glass sheet 180 and spends, 2 blocks of glass sheet point-blank, 2 glass
Glass sheet outwards draws gently, until 2 blocks of glass sheet separate.
Step 4, with the slurries on pure water rinsing glass sheet, is flushed in the beaker of a 500ml, and attention can not spill.Slurries are met after water, the film forming of can condensing, and the one side of clamping film with tweezers, takes off film gently.Film is put into the beaker of wash-down water, soaked one minute.Then wash-down water is poured in conical flask.
Step 5, pours pure water in beaker into, soaks film one minute, then water is poured in the conical flask of step 4 into 3 times so repeatedly;
Step 6, in conical flask, drip 2 methyl red-methylene blue indicator, with the solution in Hydrochloric Standard Titration (concentration is C=0.005159mol/l) titration conical flask, being titrated to solution colour purpling look is terminal, writes down volume V=0.44ml;
Step 7, adopts formula
calculating ammonia content wt% in polyacrylonitrile polymer is 0.00258%.
Embodiment bis-
The present embodiment is the method for testing of ammonia content in a kind of polyacrylonitrile polymer, and its detailed process is:
Step 1, adopts decrement method to take 1.7009g polymkeric substance to be measured to glass sheet center.
Step 2, being pressed in to drip with the identical vial of another piece has on the vial of sample, and 2 blocks of glass sheet overlap, and with pointing the slurries that push gently in glass sheet, are squeezed into a circle, and circular one side and one side of glass sheet overlap, and the slurries that are pressed into are thin.
Step 3, rotates a glass sheet 180 and spends, 2 blocks of glass sheet point-blank, 2 glass
Glass sheet outwards draws gently, until 2 blocks of glass sheet separate.
Step 4, with the slurries on pure water rinsing glass sheet, is flushed in the beaker of a 500ml, and attention can not spill.Slurries are met after water, the film forming of can condensing, and the one side of clamping film with tweezers, takes off film gently.Film is put into the beaker of wash-down water, soaked one minute.Then wash-down water is poured in conical flask.
Step 5, pours pure water in beaker into, soaks film one minute, then water is poured in the conical flask of step 4 into 3 times so repeatedly;
Step 6, in conical flask, drip 2 methyl red-methylene blue indicator, with the solution in Hydrochloric Standard Titration (concentration is C=0.005159mol/l) titration conical flask, being titrated to solution colour purpling look is terminal, writes down volume V=0.50ml;
Step 7, adopts formula
calculating ammonia content wt% in polyacrylonitrile polymer is 0.00258%.
Embodiment tri-
The present embodiment is the method for testing of ammonia content in a kind of polyacrylonitrile polymer, and its detailed process is:
Step 1, adopts decrement method to take 1.9616g polymkeric substance to be measured to glass sheet center.
Step 2, being pressed in to drip with the identical vial of another piece has on the vial of sample, and 2 blocks of glass sheet overlap, and with pointing the slurries that push gently in glass sheet, are squeezed into a circle, and circular one side and one side of glass sheet overlap, and the slurries that are pressed into are thin.
Step 3, rotates a glass sheet 180 and spends, 2 blocks of glass sheet point-blank, 2 glass
Glass sheet outwards draws gently, until 2 blocks of glass sheet separate.
Step 4, with the slurries on pure water rinsing glass sheet, is flushed in the beaker of a 500ml, and attention can not spill.Slurries are met after water, the film forming of can condensing, and the one side of clamping film with tweezers, takes off film gently.Film is put into the beaker of wash-down water, soaked one minute.Then wash-down water is poured in conical flask.
Step 5, pours pure water in beaker into, soaks film one minute, then water is poured in the conical flask of step 4 into 3 times so repeatedly;
Step 6, in conical flask, drip 2 methyl red-methylene blue indicator, with the solution in Hydrochloric Standard Titration (concentration is C=0.005159mol/l) titration conical flask, being titrated to solution colour purpling look is terminal, writes down volume V=0.58ml;
Step 7, adopts formula
calculating ammonia content wt% in polyacrylonitrile polymer is 0.00260%.
The experimental result of embodiment is as following table:
Claims (3)
1. the method for testing of ammonia content in a polyacrylonitrile polymer, it is characterized in that, take testing sample to glass sheet center, adopt the extruding of same glass sheet and by sample membrane, after employing pure water rinsing 3 times, flushing liquid is carried out to titration with hydrochloric acid standard solution, carry out the ammonia content in calculation sample.
2. the method for testing of ammonia content in polyacrylonitrile polymer as claimed in claim 1, is characterized in that, is specially:
Step 1: polyacrylonitrile polymer to be measured is poured in measuring cup, by decrement method ten thousand/ analytical balance on take testing sample 1.0-2.0g in circular glass sheet in the heart, be accurate to 0.0001g, be designated as M;
Step 2: being pressed in to drip with an identical glass sheet again has on the glass sheet of sample, and 2 blocks of glass sheet overlap, and with pointing the slurries that push gently in glass sheet, are squeezed into a circle, and circular one side and one side of glass sheet overlap, and the slurries that are pressed into are thin;
Step 3: rotate a glass sheet 180 and spend, 2 blocks of glass sheet point-blank, outwards draw 2 blocks of glass sheet gently, until 2 blocks of glass sheet separate;
Step 4: with the slurries on pure water rinsing glass sheet, be flushed in the beaker of a 500ml, attention can not spill, slurries are met after water, the film forming of can condensing, the one side of clamping film with tweezers, take off gently film, film is put into the beaker of wash-down water, soaked one minute, then wash-down water is poured in conical flask;
Step 5: pure water is poured in beaker, soaked film one minute, then water is poured in the conical flask of step 4 into 3 times so repeatedly;
Step 6: drip 2 methyl red-methylene blue indicator in conical flask, with the solution in Hydrochloric Standard Titration titration conical flask, being titrated to solution colour purpling look is terminal, writes down volume V;
Step 7: according to formula
calculate the ammonia content wt% in polyacrylonitrile polymer;
In formula: wt% is the ammonia content in polyacrylonitrile polymer to be measured, V is that titration consumes the volume of hydrochloric acid standard solution, the concentration that C is Hydrochloric Standard Titration, and M is the quality of the polyacrylonitrile polymer to be measured that takes, 17.03---the molal weight of ammonia.
3. the method for testing of ammonia content in polyacrylonitrile polymer as claimed in claim 2, is characterized in that: circular glass sheet diameter is 9cm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458732A (en) * | 2014-12-15 | 2015-03-25 | 内蒙古包钢钢联股份有限公司 | Method for calibrating hydrochloric acid and sulfuric acid standard liquids by adopting sodium carbonate reference |
| CN105527373A (en) * | 2016-01-08 | 2016-04-27 | 中简科技股份有限公司 | Detection method for ammonia content of polyacrylonitrile-based carbon fiber spinning solution |
| CN106370773A (en) * | 2016-08-17 | 2017-02-01 | 中简科技股份有限公司 | Determination method for content of residual acrylonitrile monomer in spinning solution of carbon fiber production |
| CN110672781A (en) * | 2019-10-17 | 2020-01-10 | 中复神鹰碳纤维有限责任公司 | Detection method for polyacrylonitrile spinning liquid ammonia ion replacement rate |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458732A (en) * | 2014-12-15 | 2015-03-25 | 内蒙古包钢钢联股份有限公司 | Method for calibrating hydrochloric acid and sulfuric acid standard liquids by adopting sodium carbonate reference |
| CN105527373A (en) * | 2016-01-08 | 2016-04-27 | 中简科技股份有限公司 | Detection method for ammonia content of polyacrylonitrile-based carbon fiber spinning solution |
| CN106370773A (en) * | 2016-08-17 | 2017-02-01 | 中简科技股份有限公司 | Determination method for content of residual acrylonitrile monomer in spinning solution of carbon fiber production |
| CN106370773B (en) * | 2016-08-17 | 2019-04-16 | 中简科技股份有限公司 | A kind of determination method of spinning solution remaining propylene nitrile monomer content in carbon fiber production process |
| CN110672781A (en) * | 2019-10-17 | 2020-01-10 | 中复神鹰碳纤维有限责任公司 | Detection method for polyacrylonitrile spinning liquid ammonia ion replacement rate |
| CN110672781B (en) * | 2019-10-17 | 2021-11-02 | 中复神鹰碳纤维股份有限公司 | Detection method for polyacrylonitrile spinning liquid ammonia ion replacement rate |
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