CN106769678A - PPTA molecular weight method for quick - Google Patents
PPTA molecular weight method for quick Download PDFInfo
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- CN106769678A CN106769678A CN201611089674.9A CN201611089674A CN106769678A CN 106769678 A CN106769678 A CN 106769678A CN 201611089674 A CN201611089674 A CN 201611089674A CN 106769678 A CN106769678 A CN 106769678A
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- Prior art keywords
- ppta
- quick
- condensate
- acid
- molecular weight
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
- G01N11/02—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material
- G01N11/04—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material through a restricted passage, e.g. tube, aperture
- G01N11/06—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material through a restricted passage, e.g. tube, aperture by timing the outflow of a known quantity
Abstract
The invention belongs to analysis technical field, and in particular to PPTA（PPTA）The method for quick of polymer molecular weight.PPTA is often sulfuric acid process with detection method, but dissolution time is more long, it is difficult to meet quality of production detection needs.The present invention utilizes condensate dissolution characteristics, and conventional sulfuric acid method is improved, and is substantially shorter detection time, meets PPTA production needs.The present invention is using can heated for controlling temperature magnetic stirring apparatus, heating bath stability contorting temperature range is in 55 85 DEG C, by 500 5000 rpms of magnetic agitation variable speed, condensate can be completely dissolved into the strong acid such as the concentrated sulfuric acid, oleum, chlorosulfonic acid or methanesulfonic acid within about 12 hours, viscosity measurements are carried out using the Ubbelohde viscometer of the 1.5mm of internal diameter 0.7, the quick detection of PPTA molecular weight is realized, Real-time Feedback contributes to quality of production control.
Description
Technical field
The invention belongs to analysis technical field, more particularly to PPTA in p-aramid fiber production process
（PPTA）Polymer molecule quantity measuring method, refers specifically to using specified temp control and solvent method quick detection PPTA molecules
Amount.
Background technology
Para-aramid fiber is high-strength, the high modulus fiber of currently fast-developing application, and other materials have prominent on year-on-year basis
The superiority for going out, is used widely in defence and military and civilian reinforcing material field, and certain fields have its irreplaceable
Property, the country increases several producers newly and carries out para-aramid fiber development ＆ production to break external monopolization, in recent years, and obtains obvious work
With the market share is also progressively opened.And produce the PPTA of molecular weight stabilizers（PPTA）Polymer is raw
Is produced from the basis of para-aramid fiber, is also to ensure that para-aramid fiber embodies the basic bar of different aspect characteristic in some fields
Part, during PPTA is produced, it is crucial problem that molecular weight is quickly determined, and will have influence on the stabilization sizing of polymerization process product,
It is the first step of whole product chain most critical.Polymer intrinsic viscosity method of testing, its original reference, stability all ten is divided into
Ripe reliability, different formulations and test parameter all can be in obvious contrast relationship with theoretical molecular, be applied in each technique productions straight
It is inherent viscosity to see, with its universality.
It is often sulfuric acid process with detection method that Chinese patent ZL201610147338.9 introduces PPTA, but dissolution time is more long,
It is difficult to meet quality of production detection needs.The near infrared spectrum detection method that the patent is proposed, although shorten detection time, but according to
Bad great amount of samples is modeled, and the stability and reappearance risk during polymer morphology to molecular weight detection are larger, the party
Method is more strict to the requirement such as sample fineness, structural stability, and is not cleaned saliferous, contains in production process major control
Machine solvent and the uneven condensate of proportioning, because when form and paradigmatic structure distribution are sheared by particle, being somebody's turn to do after finished product
Patented method can not be prevented effectively from its deviation unstable mutation, and the quick determination data of molecular weight offsets larger shortcoming.Therefore
This patent is started with from original method of testing, is carried out many experiments and is improved checking, it is determined that not disclosed dissolved form and parameter, side
Method simple economy is low to personnel specialty requirement, it is easy to operate, stability is big, and risk is minimum.
The content of the invention
The inventive method dissolution velocity, measuring stability, reappearance and it is comparative all show outstanding effect, solve
PPTA be difficult to dissolving and under the conditions of some degraded it is rotten it is serious caused by relative nature viscosity asking of being difficult to quick and precisely to detect
Topic.
The present invention proposes the method that quick detection para-aramid fiber produces each stage polymer molecular weight, using condensate
Dissolution characteristics, are improved to conventional sulfuric acid method.The present invention is used can heated for controlling temperature magnetic stirring apparatus, heating bath stability contorting temperature
Scope is swollen by appropriate thermosol and quickly divide by 500-5000 rpms of magnetic agitation variable speed in 55-85 DEG C
Under scattered acceleration effect, condensate can be completely dissolved to the concentrated sulfuric acid, oleum, chlorosulfonic acid or methanesulfonic acid within about 1-2 hours
In Deng strong acid, viscosity measurements are carried out using the Ubbelohde viscometer of internal diameter 0.7-1.5mm, realize the quick detection of PPTA molecular weight,
Real-time Feedback, contributes to production to adjust.
Specific embodiment
Example one, it is concretely comprised the following steps：
1st, using described in Chinese patent ZL200810225084.3 polymerization methodses, the original relative nature viscosity number of output polymer is
4-8.5dL/g, totally 45 batches carry out follow-on test contrast.
2nd, with conventional method, the concentrated sulfuric acid is carried out by 0.5g/100ml modes to every batch of polymer and is completely dissolved, plus magnetic force is stirred
Mix, it is average time-consuming 22 hours, using Ubbelohde viscometer internal diameter 1.07mm, test relative nature viscosity IV values；
3rd, while using this method, carrying out the concentrated sulfuric acid by 0.5g/100ml modes to identical sample polymer and being completely dissolved, averagely
It is time-consuming 2 hours, using Ubbelohde viscometer internal diameter 1.07mm, test relative nature viscosity IV values；
4th, relative nature viscosity is contrasted, method using effect is outstanding, and stability is high, shortens 20 hours testing times, can referred in real time
Lead production process product after stabilization.
Example two, it is concretely comprised the following steps：
1st, polymer carries out contrast test in taking adjacent 10 batches of production.
2nd, with conventional method, the concentrated sulfuric acid is carried out by 0.5g/100ml modes to every batch of polymer and is completely dissolved, plus magnetic force is stirred
Mix, it is average time-consuming 22 hours, using Ubbelohde viscometer internal diameter 1.07mm, test relative nature viscosity IV values；
3rd, while using this method, carrying out the concentrated sulfuric acid by 0.5g/100ml modes to identical sample polymer and being completely dissolved, averagely
It is time-consuming 2 hours, using Ubbelohde viscometer internal diameter 1.07mm, test relative nature viscosity IV values；
4th, instance data as shown in table 1, using the several months, meets production adjustment needs.Formulate this p-aramid fiber polymer molecule amount
Method for rapidly testing.And can be applied to other inherent viscosities it is higher and suitable for this dissolution mechanism polymer molecule amount detection.
The example polymer intrinsic viscosity example of table 1
Absolute deviation values are between 0.4, and production is in controllable, and fast method of the present invention is poly- suitable for p-aramid fiber
Compound production detection.
Claims (8)
1. a kind of method for quick of PPTA molecular weight, it is characterised in that the method includes following step
Suddenly：
（1）Condensate dissolves：PPTA condensate is mixed with solvent of strong in a heated condition, is used
Agitator after stirring a period of time, makes condensate be dissolved completely in solvent of strong under constant agitation speed, forms condensate
Solution；
（2）Condensate viscosity measurements：Viscosity measurements are carried out to the polymer solution after dissolving using viscosimeter.
2. method for quick according to claim 1, it is characterised in that the agitator is magnetic stirring apparatus.
3. method for quick according to claim 1, it is characterised in that the heating temperature range is 55-85 DEG C.
4. method for quick according to claim 1, it is characterised in that the mixing speed is 500-5000 revolutions per minute
Clock.
5. method for quick according to claim 1, it is characterised in that the mixing time is 1-2 hours.
6. method for quick according to claim 1, it is characterised in that the solvent of strong is the concentrated sulfuric acid, oleum
Acid, chlorosulfonic acid or methanesulfonic acid.
7. method for quick according to claim 1, it is characterised in that the viscosimeter internal diameter is 0.7-1.5mm.
8. method for quick according to claim 2, it is characterised in that the magnetic stirring apparatus gear is stepless
Speed change.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611089674.9A CN106769678A (en) | 2016-12-01 | 2016-12-01 | PPTA molecular weight method for quick |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611089674.9A CN106769678A (en) | 2016-12-01 | 2016-12-01 | PPTA molecular weight method for quick |
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| CN106769678A true CN106769678A (en) | 2017-05-31 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611089674.9A Pending CN106769678A (en) | 2016-12-01 | 2016-12-01 | PPTA molecular weight method for quick |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105699255A (en) * | 2016-03-15 | 2016-06-22 | 山东万圣博科技股份有限公司 | Method for rapidly detecting molecular weight of poly-p-phenylene terephthamide resin |
-
2016
- 2016-12-01 CN CN201611089674.9A patent/CN106769678A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105699255A (en) * | 2016-03-15 | 2016-06-22 | 山东万圣博科技股份有限公司 | Method for rapidly detecting molecular weight of poly-p-phenylene terephthamide resin |
Non-Patent Citations (5)
| Title |
|---|
| 岳阳石油化工总厂研究院芳纶II分析组: "聚对苯二甲酰对苯二胺粘度的快速测定", 《合成纤维工业》 * |
| 潘智存 等: "聚对苯二甲酰对苯二胺在浓硫酸中溶解规律的研究", 《合成纤维工业》 * |
| 王明德 等: "《物理化学实验》", 30 September 2013, 西安交通大学 * |
| 范奎城 等: "聚对苯二甲酰苯二胺硫酸液晶溶液流变性能的研究", 《高分子材料科学与工程》 * |
| 黎华明 等: "《高分子科学实验》", 31 December 2011, 湘潭大学出版社 * |
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