CN103451759A - Preparation method of polyisophthaloyl metaphenylene diamine fibrid - Google Patents
Preparation method of polyisophthaloyl metaphenylene diamine fibrid Download PDFInfo
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- CN103451759A CN103451759A CN2013103117277A CN201310311727A CN103451759A CN 103451759 A CN103451759 A CN 103451759A CN 2013103117277 A CN2013103117277 A CN 2013103117277A CN 201310311727 A CN201310311727 A CN 201310311727A CN 103451759 A CN103451759 A CN 103451759A
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Abstract
The invention discloses a preparation method of a polyisophthaloyl metaphenylene diamine fibrid. The preparation method comprises the steps of preparing a polyisophthaloyl metaphenylene diamine colloid polymer by primarily polymerizing metaphenylene diamine and m-phthaloyl chloride at polymerization temperature of 20-40 DEG C; preparing a precipitation solution; dispersing the polyisophthaloyl metaphenylene diamine colloid polymer in the precipitation solution and performing precipitation in a precipitator; causing a precipitated mixture solution to pass through a washing filter so as to remove solvents, auxiliaries and water, and thus obtaining polyisophthaloyl metaphenylene diamine fibrid. The preparation method disclosed by the invention is a production method capable of forming in one step in the absence of secondary fine pulping, and has the advantages of low production equipment investment, stable production process and less processing points and controlling points.
Description
Technical field:
The present invention relates to the fibrid technical field, relate in particular to a kind of preparation method of poly(isophthaloyl metaphenylene diamine) fibrid.
Background technology:
The high-performance aramid fiber has high strength, low distortion, high temperature resistant, resistance to chemical attack and the good characteristics such as insulating properties, in fields such as Aero-Space, military affairs, electronics and machineries, is widely used.Fanglun 1313 (aramid fiber 1313 fiber) is a kind of fiber had practical value most in aramid fiber, the basic aramid fiber 1313 fibrid that adopts is as viscose fibre, its strand is arranged indentation, there is outstanding high-temperature insulation performance, be mainly used in special protecting clothing, high-temperature-resistant filtering material, insulating material, cellular structural material etc.The poly(isophthaloyl metaphenylene diamine) fibrid has conventional structure and the performance of fibrid, and outer appearnce, like lumber fibre, has excellent wet processing characteristics and strengthens the property, good dispersion in water, and average specific surface area is about 5-20m
2/ g, draw ratio is large, and intensity is high, is one of important viscose fibre of aramid fiber wet papermaking.
Summary of the invention:
The preparation method who the purpose of this invention is to provide a kind of poly(isophthaloyl metaphenylene diamine) fibrid, fibrid stable performance, good quality.
Purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of poly(isophthaloyl metaphenylene diamine) fibrid comprises the following steps:
(1) prepare the poly(isophthaloyl metaphenylene diamine) colloidal polymer by m-phenylene diamine (MPD) and m-phthaloyl chloride through a polymerization, polymerization temperature is 20-40 ℃;
(2) preparation precipitating solution;
(3) the poly(isophthaloyl metaphenylene diamine) colloidal polymer is dispersed in precipitating solution, carries out precipitating in precipitation machine;
(4) mixed liquor after precipitating in step (3) is passed through to washing filter, except desolventizing, auxiliary agent and moisture, obtain the poly(isophthaloyl metaphenylene diamine) fibrid.
As technique scheme preferably, the concentration=8-15% of described poly(isophthaloyl metaphenylene diamine) colloidal polymer, viscosity=1.2-2.0, temperature=20-50 ℃.
As technique scheme preferably, the temperature of described precipitating solution is 20-50 ℃.
As technique scheme preferably, the mass ratio of described poly(isophthaloyl metaphenylene diamine) colloidal polymer and precipitating liquid is 1:5-20.
As technique scheme preferably, described precipitating solution is the mixture of amide-type polar organic solvent, alcohol organic solvent, cosolvent and water.
As technique scheme preferably, described amide-type polar organic solvent is DMA or METHYLPYRROLIDONE.
As technique scheme preferably, described alcohol organic solvent is one or several mixtures in glycerine, BDO and ethylene glycol.
As technique scheme preferably, described cosolvent is one or more mixtures in sodium chloride, calcium chloride, magnesium chloride, aluminium chloride.
As technique scheme preferably, the percentage by weight of described amide-type organic solvent is 0-40%, the percentage by weight of alcohols class organic solvent is 60-95%, the percentage by weight of cosolvent is 0-30%, all the other are water.
As technique scheme preferably, described precipitation machine is the equipment that can stir of sealing, speed is 1000-4000rpm.
Beneficial effect of the present invention is: poly(isophthaloyl metaphenylene diamine) fibrid preparation method provided by the invention is the production method that does not need the meticulous making beating of secondary, one-step shaping, small investment of production equipment, and stable production process, the process point control point is few.
The specific embodiment:
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, and this embodiment only, for explaining the present invention, does not form limiting the scope of the present invention.
Embodiment 1-15: by m-phenylene diamine (MPD) and m-phthaloyl chloride, through a polymerization, prepare the poly(isophthaloyl metaphenylene diamine) colloidal polymer, polymerization temperature is 20-40 ℃, in Table 1(embodiment 18 as a comparison, polymer concentration is 18.3wt% for polymer concentration and logarithmic viscosity number); By DMA (DMAC), glycerine, calcium chloride and water preparation precipitating solution, the percentage by weight of each component is in Table 1, and the mass ratio of poly(isophthaloyl metaphenylene diamine) colloidal polymer and precipitating liquid is 1:10; The poly(isophthaloyl metaphenylene diamine) colloidal polymer of 20-50 ℃ is dispersed in the precipitating solution of 20-50 ℃, carry out precipitating in the precipitation machine that can stir in sealing, the precipitation machine rotating speed be 1000-4000rpm(embodiment 12 as a comparison, rotating speed is 800rpm), different embodiment rotating speeds are in Table 1; Mixed liquor after above-mentioned precipitating, by washing filter, except desolventizing, auxiliary agent and moisture, is obtained to the poly(isophthaloyl metaphenylene diamine) fibrid, and to the poly(isophthaloyl metaphenylene diamine) fibrid test beating degree obtained, result is listed in table 1 respectively.
Table 1
Other conditions are basic identical, the embodiment analysis that precipitating solution component is different: can find out to only have in the situation of DMAC from the data of embodiment 1-8, very low in the situation beating degree of 3000rpm, the one-tenth paper binding ability extreme difference of fibrid is described, does not reach instructions for use; And used the fibrid of glycerine, effect out is fine, basically well meets the manufacture requirement of page; Added the fibrid of calcium chloride, effect out is better.
The embodiment analysis that the precipitation machine rotating speed is different: from the data of embodiment 7 and 9-12, can find out, in the situation that the precipitating solution phase is same, the raising of rotating speed contributes to the raising of beating degree, but high again, and the processing request of equipment improves, and obviously there is no need.Speed is lower than 1000, and fibrid out has a lot of bulks, is not suitable as papermaking and uses.
The embodiment analysis of different colloidal polymer concentration: can find out from the data of embodiment 7 and 13-15, the concentration low spot of colloidal polymer, contribute to improve beating degree, but be also worthless lower than 8, because this can cause the unit production capacity very low, and produce a large amount of fiber fines and be lost in the process of washing or copy paper, loss is serious; Concentration improves, and beating degree can descend, and the poor performance of copy paper is also unaccommodated.
Claims (10)
1. the preparation method of a poly(isophthaloyl metaphenylene diamine) fibrid is characterized in that: comprise the following steps:
(1) prepare the poly(isophthaloyl metaphenylene diamine) colloidal polymer by m-phenylene diamine (MPD) and m-phthaloyl chloride through a polymerization, polymerization temperature is 20-40 ℃;
(2) preparation precipitating solution;
(3) the poly(isophthaloyl metaphenylene diamine) colloidal polymer is dispersed in precipitating solution, carries out precipitating in precipitation machine;
(4) mixed liquor after precipitating in step (3) is passed through to washing filter, except desolventizing, auxiliary agent and moisture, obtain the poly(isophthaloyl metaphenylene diamine) fibrid.
2. the preparation method of poly(isophthaloyl metaphenylene diamine) fibrid according to claim 1, is characterized in that: the concentration=8-15% of described poly(isophthaloyl metaphenylene diamine) colloidal polymer, viscosity=1.2-2.0, temperature=20-50 ℃.
3. the preparation method of poly(isophthaloyl metaphenylene diamine) fibrid according to claim 1, it is characterized in that: the temperature of described precipitating solution is 20-50 ℃.
4. the preparation method of poly(isophthaloyl metaphenylene diamine) fibrid according to claim 1, it is characterized in that: the mass ratio of described poly(isophthaloyl metaphenylene diamine) colloidal polymer and precipitating liquid is 1:5-20.
5. the preparation method of poly(isophthaloyl metaphenylene diamine) fibrid according to claim 1, it is characterized in that: described precipitating solution is the mixture of amide-type polar organic solvent, alcohol organic solvent, cosolvent and water.
6. the preparation method of poly(isophthaloyl metaphenylene diamine) fibrid according to claim 5, it is characterized in that: described amide-type polar organic solvent is DMA or METHYLPYRROLIDONE.
7. the preparation method of poly(isophthaloyl metaphenylene diamine) fibrid according to claim 5, it is characterized in that: described alcohol organic solvent is one or several mixtures in glycerine, BDO and ethylene glycol.
8. the preparation method of poly(isophthaloyl metaphenylene diamine) fibrid according to claim 5, it is characterized in that: described cosolvent is one or more mixtures in sodium chloride, calcium chloride, magnesium chloride, aluminium chloride.
9. the preparation method of poly(isophthaloyl metaphenylene diamine) fibrid according to claim 5, it is characterized in that: the percentage by weight of described amide-type organic solvent is 0-40%, the percentage by weight of alcohols class organic solvent is 60-95%, the percentage by weight of cosolvent is 0-30%, and all the other are water.
10. the preparation method of poly(isophthaloyl metaphenylene diamine) fibrid according to claim 1 is characterized in that: described precipitation machine is the equipment that can stir of sealing, and speed is 1000-4000rpm.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104630924A (en) * | 2015-01-12 | 2015-05-20 | 烟台泰和新材料股份有限公司 | Method for preparing aromatic polyamide membrane type fibrid |
| CN104831577A (en) * | 2015-04-14 | 2015-08-12 | 深圳昊天龙邦复合材料有限公司 | Wave-absorption and long-service life composite paper and preparation method thereof |
| CN105506769A (en) * | 2016-01-07 | 2016-04-20 | 江苏先诺新材料科技有限公司 | Polyamide acid fibrid, polyimide fibrid and preparation method of polyamide acid fibrid |
| CN106637473A (en) * | 2016-10-11 | 2017-05-10 | 四川辉腾科技股份有限公司 | Method for environment-friendly production of meta-position aramid fiber fibrid |
| CN110129912A (en) * | 2019-06-10 | 2019-08-16 | 黄河三角洲京博化工研究院有限公司 | A kind of p-aramid fiber fibrid and its continuous producing method |
| CN110184677A (en) * | 2019-06-03 | 2019-08-30 | 江苏扬农化工集团有限公司 | A kind of preparation method of PPTA-MPIA In-situ reaction fibrid |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104630924A (en) * | 2015-01-12 | 2015-05-20 | 烟台泰和新材料股份有限公司 | Method for preparing aromatic polyamide membrane type fibrid |
| CN104831577A (en) * | 2015-04-14 | 2015-08-12 | 深圳昊天龙邦复合材料有限公司 | Wave-absorption and long-service life composite paper and preparation method thereof |
| CN105506769A (en) * | 2016-01-07 | 2016-04-20 | 江苏先诺新材料科技有限公司 | Polyamide acid fibrid, polyimide fibrid and preparation method of polyamide acid fibrid |
| CN105506769B (en) * | 2016-01-07 | 2019-11-08 | 江苏先诺新材料科技有限公司 | A kind of polyamic acid fibrid and polyimides fibrid and preparation method thereof |
| CN106637473A (en) * | 2016-10-11 | 2017-05-10 | 四川辉腾科技股份有限公司 | Method for environment-friendly production of meta-position aramid fiber fibrid |
| CN110184677A (en) * | 2019-06-03 | 2019-08-30 | 江苏扬农化工集团有限公司 | A kind of preparation method of PPTA-MPIA In-situ reaction fibrid |
| CN110184677B (en) * | 2019-06-03 | 2021-11-26 | 江苏瑞盛新材料科技有限公司 | Preparation method of PPTA-MPIA in-situ composite fibrid |
| CN110129912A (en) * | 2019-06-10 | 2019-08-16 | 黄河三角洲京博化工研究院有限公司 | A kind of p-aramid fiber fibrid and its continuous producing method |
| CN110129912B (en) * | 2019-06-10 | 2021-10-26 | 黄河三角洲京博化工研究院有限公司 | Para-aramid fibrid and continuous production method thereof |
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