CN104630924A - Method for preparing aromatic polyamide membrane type fibrid - Google Patents
Method for preparing aromatic polyamide membrane type fibrid Download PDFInfo
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- CN104630924A CN104630924A CN201510012906.XA CN201510012906A CN104630924A CN 104630924 A CN104630924 A CN 104630924A CN 201510012906 A CN201510012906 A CN 201510012906A CN 104630924 A CN104630924 A CN 104630924A
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Abstract
The invention discloses a method for preparing an aromatic polyamide membrane type fibrid. The method comprises the following steps: (1) preparing a stock solution of aromatic polyamide, namely polymerizing aromatic diamine and aromatic benzenedicarbonyl chloride in a solvent, neutralizing and filtering to prepare the stock solution of aromatic polyamide; (2) preparing a precipitation solvent, namely mixing and compounding water, DMAC and chlorate, and uniformly stirring; (3) preparing fibrid, namely introducing the stock solution of aromatic polyamide and the precipitation solvent into precipitation equipment, cutting at high speed by virtue of the precipitation equipment to form fibrid, and discharging into a discharge tank for further cooling and molding; (4) post-treating fibrid, namely washing the cooled and molded precipitation fiber mixed material containing the solvent, and removing the solvent to obtain the precipitation fiber finished product. The aromatic polyamide fibrid has excellent dispersion, rich shape and leather, little equipment investment and simple and effective process.
Description
Technical field
The present invention relates to a kind of fibre manufacture, particularly relate to preparation method of a kind of aromatic polyamide fibrid and products thereof.
Background technology
In tec fiber material, aromatic polyamide fibre (abbreviation aramid fiber) occupies very outstanding status.Aramid fiber mainly divides meta-aramid and p-aramid fiber two kinds.Aramid fiber is succeeded in developing by du pont company, and achieves industrialization production the sixties in 20th century, and at present, the production capacity of E.I.Du Pont Company's aramid fiber is still in occupation of the position in the whole world first.Because cost of investment is large, technology barriers are high, meta-aramid is produced by only a few business monopolies such as the U.S. and Japan for a long time, and technical matters holds in close confidence.
Meta-aramid has the good characteristic such as high temperature resistant, inherent flame retardant, electric insulation, radioresistance, resistance to chemical attack, the speciality paper made with aramid fiber, has the premium properties such as high strength, low deformation, high temperature resistant, fire-retardant and electric insulation.
Position Nomex paper between meta-position aramid fiber paper also claims is formed through Top wire former, squeezing, drying, high temperature press polish by the slurry containing aramid short fiber and fibrid.Fibrid is the paper slurry fiber that filoplume enriches, and is the critical materials producing aramid paper.Meta-position aramid fiber paper has high strength, low distortion, high temperature resistant, resistance to chemical attack, fire-retardant and excellent electrical insulation capability, is widely used in the fields such as Aero-Space, communications and transportation and electric insulation.
Therefore, successively similar fibrid technology is studied by You Duo company and mechanism.
Patent US3018091 discloses a kind of structure of precipitating equipment, the preparation technology that wherein to refer to water and DMF be the fibrid of precipitating solvent.
Patent US3756908 discloses a kind of technology of preparing of aromatic polyamide paper, manufactures paper fibrid used and also uses technology in 3018091.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of fibrid favorable dispersibility, form filoplume enriches, equipment investment is few, the preparation method of the simple and effective aromatic polyamide fibrid of technique.
A preparation method for aromatic polyamide fibrid, comprises the steps:
(1) preparation of aromatic polyamide stoste: aromatic diamine and aromatic dimethyl chloride are polymerized in a solvent, obtained aromatic polyamide stoste after neutralization, filtration;
(2) allotment of precipitating solvent: by composite for the mixing of water, DMAC and chlorate, stir after mixing;
(3) preparation of fibrid: pass in precipitating equipment by described aromatic polyamide stoste and described precipitating solvent, forms fibrid through precipitating equipment high speed shear, then enters further cooling forming in discharge tank;
(4) post processing of fibrid: the fibrid compound containing solvent after cooling forming is removed desolventizing after washing, obtains fibrid finished product.
The preparation method of aromatic polyamide fibrid of the present invention, wherein described in step (1), solvent is DMAC, and in described aromatic polyamide stoste, poly(isophthaloyl metaphenylene diamine) polymer content is 5 ~ 20%.
The preparation method of aromatic polyamide fibrid of the present invention, wherein said aromatic diamine is m-phenylene diamine (MPD), described aromatic dimethyl chloride is m-phthaloyl chloride, the mol ratio that two kinds of raw materials add is 1:1, the concentration of described poly(isophthaloyl metaphenylene diamine) polymer solution is 5-20%, and inherent viscosity is 1.4-1.9.
The preparation method of aromatic polyamide fibrid of the present invention, wherein precipitating solvent described in step (2) mixes composite forming by the material of following parts by mass: the water being less than or equal to 60 parts, be less than or equal to the DMAC of 60 parts, the chlorate of 1 ~ 10 part; Stir after mixing composite good solvent, be cooled to 0-20 DEG C for subsequent use.
The preparation method of aromatic polyamide fibrid of the present invention, wherein said chlorate is one or both the mixture in lithium chloride, calcium chloride, magnesium chloride.
The preparation method of aromatic polyamide fibrid of the present invention, wherein in step (3), in step (3), described aromatic polyamide stoste and precipitating solvent are passed in precipitating equipment with the amount of 10-200kg/h and 500-2000kg/h respectively and forms fibrid through precipitating equipment high speed shear, the rotating speed of described precipitating equipment is 500-3000 rev/min, the material reaction time is in a device 1-2min, then enters further cooling forming in discharge tank.
The preparation method of aromatic polyamide fibrid of the present invention, the mass ratio of wherein said aromatic polyamide stoste and described precipitating solvent is 1:5-50.
The preparation method of aromatic polyamide fibrid of the present invention, the solvent in wherein said fibrid finished product is less than 0.01%.
Preparation method's difference from prior art of aromatic polyamide fibrid of the present invention is:
The preparation method of aromatic polyamide fibrid of the present invention have employed and mixes composite precipitating solvent by water, DMAC and chlorate, especially chlorate formula is added, be conducive to forming film-form or fibrous fibrid, fibrid can be made in paper-making process better to play cementation; In the forming process of fibrid, precipitating solvent plays conclusive effect, and this formula has obvious difference with the performance of other patent formulation solvent for use and solvent.
The method of the invention under stable lower temperature by meta-aromatic polyamide stoste and a certain proportion of precipitating solvent delivery to precipitating equipment, stoste is solidified and is formed the abundant fiber fines of filoplume and fibrid under the high speed shear effect of precipitating equipment, and the fibrid of shaping removes desolventizing through cooling forming, washing.Manufactured fibrid favorable dispersibility, form filoplume are abundant, equipment investment is few, technique is simply effective.
Below in conjunction with accompanying drawing, the preparation method to aromatic polyamide fibrid of the present invention is described further.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the preparation method of aromatic polyamide fibrid of the present invention.
Detailed description of the invention
Embodiment 1
As shown in Figure 1, the preparation method of aromatic polyamide fibrid of the present invention comprises the steps:
(1) prepare meta-aromatic polyamide stoste, m-phenylene diamine (MPD) and m-phthaloyl chloride are polymerized in solvent DMAC obtaining poly(isophthaloyl metaphenylene diamine) solution, the inherent viscosity controlling polymer is 1.5, and concentration is 15%.Obtain transparent polymer dope through process such as neutralization, filtrations, the mol ratio that m-phenylene diamine (MPD) and m-phthaloyl chloride two kinds of raw materials add is 1:1.
(2) allocate precipitating solvent, by composite for the mixing of water, DMAC and lithium chloride, the amount of water is 40%, DMAC is 50%, and lithium chloride is 10%.Stir after mixing, be cooled to 10 DEG C for subsequent use.
(3) fibrid is prepared, poly(isophthaloyl metaphenylene diamine) stoste and precipitating solvent are respectively with the flow of 100kg/h and 1000kg/h, continous-stable enter precipitating equipment, fibrid is formed through precipitating equipment high speed shear, the rotating speed of precipitating equipment is 1000 revs/min, the material reaction time is in a device 2min, is then entered in discharge tank by fibrid.
(4) carry out post processing to fibrid, enter in discharge tank by the fibrid compound containing solvent, then beat on separation equipment by pump, through cyclic washing except desolventizing, the content of solvent should be less than 0.01%, obtains fibrid finished product.
The form of gained fibrid is tiny, and be translucent shape fiber or film, and fiber beating degree is 28 ° of SR.
Embodiment 2
As shown in Figure 1, the preparation method of aromatic polyamide fibrid of the present invention comprises the steps:
(1) prepare meta-aromatic polyamide stoste, m-phenylene diamine (MPD) and m-phthaloyl chloride are polymerized in solvent DMAC obtaining poly(isophthaloyl metaphenylene diamine) solution, the inherent viscosity controlling polymer is 1.5, and concentration is 10%.Obtain transparent polymer dope through process such as neutralization, filtrations, the mol ratio that m-phenylene diamine (MPD) and m-phthaloyl chloride two kinds of raw materials add is 1:1.
(2) allocate precipitating solvent, by composite for the mixing of water, DMAC and calcium chloride, the amount of water is 45%, DMAC is 50%, and calcium chloride is 5%.Stir after mixing, be cooled to 10 DEG C for subsequent use.
(3) fibrid is prepared, poly(isophthaloyl metaphenylene diamine) stoste and precipitating solvent are respectively with the flow of 200kg/h and 2000kg/h, continous-stable enter precipitating equipment, fibrid is formed through precipitating equipment high speed shear, the rotating speed of precipitating equipment is 3000 revs/min, the material reaction time is in a device 1min, is then entered in discharge tank by fibrid.
(4) carry out post processing to fibrid, enter in discharge tank by the fibrid compound containing solvent, then beat on separation equipment by pump, through cyclic washing except desolventizing, the content of solvent should be less than 0.01%, obtains fibrid finished product.
The form of gained fibrid is tiny, and be translucent shape fiber or film, and fiber beating degree is 36 ° of SR.
Embodiment 3
As shown in Figure 1, the preparation method of aromatic polyamide fibrid of the present invention comprises the steps:
(1) prepare meta-aromatic polyamide stoste, m-phenylene diamine (MPD) and m-phthaloyl chloride are polymerized in solvent DMAC obtaining poly(isophthaloyl metaphenylene diamine) solution, the inherent viscosity controlling polymer is 1.5, and concentration range is 15%.Obtain transparent polymer dope through process such as neutralization, filtrations, the mol ratio that m-phenylene diamine (MPD) and m-phthaloyl chloride two kinds of raw materials add is 1:1.
(2) allocate precipitating solvent, by composite for the mixing of water, DMAC and magnesium chloride, the amount of water is 50%, DMAC is 45%, and magnesium chloride is 5%.Stir after mixing, be cooled to 10 DEG C for subsequent use.
(3) fibrid is prepared, poly(isophthaloyl metaphenylene diamine) stoste and precipitating solvent are respectively with the flow of 10kg/h and 500kg/h, continous-stable enter precipitating equipment, fibrid is formed through precipitating equipment high speed shear, the rotating speed of precipitating equipment is 2500 revs/min, the material reaction time is in a device 1min, is then entered in discharge tank by fibrid.
(4) post processing is carried out to fibrid, fibrid compound containing solvent is entered in discharge tank, then beats on separation equipment by pump, through cyclic washing squeezing except desolventizing, the content of solvent should be less than 0.01%, obtains fibrid finished product.
The form of gained fibrid is tiny, and be translucent shape fiber or film, and fiber beating degree is 38 ° of SR.
Embodiment 4
As shown in Figure 1, the preparation method of aromatic polyamide fibrid of the present invention comprises the steps:
(1) prepare meta-aromatic polyamide stoste, m-phenylene diamine (MPD) and m-phthaloyl chloride are polymerized in solvent DMAC obtaining poly(isophthaloyl metaphenylene diamine) solution, the inherent viscosity controlling polymer is 1.5, and concentration range is 15%.Obtain transparent polymer dope through process such as neutralization, filtrations, the mol ratio that m-phenylene diamine (MPD) and m-phthaloyl chloride two kinds of raw materials add is 1:1.
(2) allocate precipitating solvent, by composite for the mixing of water, DMAC and chlorate, the amount of water is 45%, DMAC is 45%, and calcium chloride and lithium chloride are respectively 5%.Stir after mixing, be cooled to 10 DEG C for subsequent use.
(3) fibrid is prepared, poly(isophthaloyl metaphenylene diamine) stoste and precipitating solvent are respectively with the flow of 100kg/h and 1000kg/h, continous-stable enter precipitating equipment, fibrid is formed through precipitating equipment high speed shear, the rotating speed of precipitating equipment is 500 revs/min, the material reaction time is in a device 2min, is then entered in discharge tank by fibrid.
(4) carry out post processing to fibrid, enter in discharge tank by the fibrid compound containing solvent, then beat on separation equipment by pump, through washing is except desolventizing repeatedly, the content of solvent should be less than 0.01%, obtains fibrid finished product.
The form of gained fibrid is tiny, and be translucent shape fiber or film, and fiber beating degree is 40 ° of SR.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.
Claims (8)
1. a preparation method for aromatic polyamide fibrid, is characterized in that: comprise the steps:
(1) preparation of aromatic polyamide stoste: aromatic diamine and aromatic dimethyl chloride are polymerized in a solvent, obtained aromatic polyamide stoste after neutralization, filtration;
(2) allotment of precipitating solvent: by composite for the mixing of water, DMAC and chlorate, stir after mixing;
(3) preparation of fibrid: pass in precipitating equipment by described aromatic polyamide stoste and described precipitating solvent, forms fibrid through precipitating equipment high speed shear, then enters further cooling forming in discharge tank;
(4) post processing of fibrid: the fibrid compound containing solvent after cooling forming is removed desolventizing after washing, obtains fibrid finished product.
2. the preparation method of aromatic polyamide fibrid according to claim 1, it is characterized in that: described in step (1), solvent is DMAC, in described aromatic polyamide stoste, poly(isophthaloyl metaphenylene diamine) polymer content is 5 ~ 20%.
3. the preparation method of aromatic polyamide fibrid according to claim 2, it is characterized in that: described aromatic diamine is m-phenylene diamine (MPD), described aromatic dimethyl chloride is m-phthaloyl chloride, the mol ratio that two kinds of raw materials add is 1:1, the concentration of described poly(isophthaloyl metaphenylene diamine) polymer solution is 5-20%, and inherent viscosity is 1.4-1.9.
4. the preparation method of aromatic polyamide fibrid according to claim 3, it is characterized in that: precipitating solvent described in step (2) mixes composite forming by the material of following parts by mass: the water being less than or equal to 60 parts, be less than or equal to the DMAC of 60 parts, the chlorate of 1 ~ 10 part; Stir after mixing composite good solvent, be cooled to 0-20 DEG C for subsequent use.
5. the preparation method of aromatic polyamide fibrid according to claim 4, is characterized in that: described chlorate is one or both the mixture in lithium chloride, calcium chloride, magnesium chloride.
6. the preparation method of aromatic polyamide fibrid according to claim 5, it is characterized in that: in step (3), described aromatic polyamide stoste and precipitating solvent are passed in precipitating equipment with the amount of 10-200kg/h and 500-2000kg/h respectively and forms fibrid through precipitating equipment high speed shear, the rotating speed of described precipitating equipment is 500-3000 rev/min, the material reaction time is in a device 1-2min, then enters further cooling forming in discharge tank.
7. the preparation method of aromatic polyamide fibrid according to claim 6, is characterized in that: the mass ratio of described aromatic polyamide stoste and described precipitating solvent is 1:5-1:50.
8. the preparation method of aromatic polyamide fibrid according to claim 7, is characterized in that: the solvent in described fibrid finished product is less than 0.01%.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105239196A (en) * | 2015-11-10 | 2016-01-13 | 东华大学 | Method for preparing polyamideimide precipitation fibers |
| CN105481650A (en) * | 2015-12-11 | 2016-04-13 | 烟台泰和新材料股份有限公司 | Separation and recovery method of aramid fibrid multicomponent solvent |
| CN106436440A (en) * | 2016-10-11 | 2017-02-22 | 四川辉腾科技股份有限公司 | Fiber forming control production method for poly-m-phenyleneisophthalamide precipitation fiber |
| CN106592000A (en) * | 2016-12-21 | 2017-04-26 | 四川辉腾科技股份有限公司 | Method for producing aramid fiber III 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 |
| CN106832263A (en) * | 2017-02-15 | 2017-06-13 | 烟台泰和新材料股份有限公司 | A kind of high-melting-point ternary aromatic polyamides condensate and the method that fibrid is prepared using it |
| CN110205697A (en) * | 2019-06-21 | 2019-09-06 | 赣州龙邦材料科技有限公司 | A kind of fibrid and preparation method thereof |
| CN110230116A (en) * | 2019-06-21 | 2019-09-13 | 赣州龙邦材料科技有限公司 | A kind of aramid fiber superbhort fiber and preparation method thereof |
| CN110229350A (en) * | 2019-06-21 | 2019-09-13 | 赣州龙邦材料科技有限公司 | A kind of aramid fiber fibrid and preparation method thereof |
| CN112143226A (en) * | 2020-10-20 | 2020-12-29 | 株洲时代新材料科技股份有限公司 | Preparation method of fibrid reinforced nylon composite material |
| CN112688023A (en) * | 2020-12-30 | 2021-04-20 | 河北金力新能源科技股份有限公司 | Aromatic polyamide coating diaphragm and preparation method thereof |
| CN113668089A (en) * | 2020-05-13 | 2021-11-19 | 中蓝晨光化工有限公司 | Preparation method of aromatic polyamide film-shaped fibrid |
| CN115369505A (en) * | 2022-07-08 | 2022-11-22 | 株洲时代新材料科技股份有限公司 | Multistage dispersion disc precipitation forming device and forming process, precipitation fiber precipitation purification device and process |
| CN115369505B (en) * | 2022-07-08 | 2024-05-03 | 株洲时代新材料科技股份有限公司 | Multistage dispersion plate precipitation forming device and forming process, fibrid precipitation purifying device and technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105239196A (en) * | 2015-11-10 | 2016-01-13 | 东华大学 | Method for preparing polyamideimide precipitation fibers |
| CN105239196B (en) * | 2015-11-10 | 2017-10-24 | 东华大学 | A kind of preparation method of polyamidoimide fibrid |
| CN105481650A (en) * | 2015-12-11 | 2016-04-13 | 烟台泰和新材料股份有限公司 | Separation and recovery method of aramid fibrid multicomponent solvent |
| CN105481650B (en) * | 2015-12-11 | 2017-08-22 | 烟台泰和新材料股份有限公司 | A kind of separation and recovery method of aramid fiber fibrid multicomponent solvent |
| CN106436440A (en) * | 2016-10-11 | 2017-02-22 | 四川辉腾科技股份有限公司 | Fiber forming control production method for poly-m-phenyleneisophthalamide precipitation fiber |
| 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 |
| CN106436440B (en) * | 2016-10-11 | 2018-12-07 | 四川辉腾科技股份有限公司 | The fiberizing of meta-aramid fibre fibrid controls production method |
| CN106592000A (en) * | 2016-12-21 | 2017-04-26 | 四川辉腾科技股份有限公司 | Method for producing aramid fiber III fibrid |
| CN106592000B (en) * | 2016-12-21 | 2018-12-25 | 四川辉腾科技股份有限公司 | A method of producing aramid fiber III fibrid |
| CN106832263A (en) * | 2017-02-15 | 2017-06-13 | 烟台泰和新材料股份有限公司 | A kind of high-melting-point ternary aromatic polyamides condensate and the method that fibrid is prepared using it |
| CN110205697A (en) * | 2019-06-21 | 2019-09-06 | 赣州龙邦材料科技有限公司 | A kind of fibrid and preparation method thereof |
| CN110230116A (en) * | 2019-06-21 | 2019-09-13 | 赣州龙邦材料科技有限公司 | A kind of aramid fiber superbhort fiber and preparation method thereof |
| CN110229350A (en) * | 2019-06-21 | 2019-09-13 | 赣州龙邦材料科技有限公司 | A kind of aramid fiber fibrid and preparation method thereof |
| CN113668089A (en) * | 2020-05-13 | 2021-11-19 | 中蓝晨光化工有限公司 | Preparation method of aromatic polyamide film-shaped fibrid |
| CN113668089B (en) * | 2020-05-13 | 2023-07-28 | 中蓝晨光化工有限公司 | Preparation method of aromatic polyamide membranous fibrid |
| CN112143226A (en) * | 2020-10-20 | 2020-12-29 | 株洲时代新材料科技股份有限公司 | Preparation method of fibrid reinforced nylon composite material |
| CN112143226B (en) * | 2020-10-20 | 2023-03-31 | 株洲时代新材料科技股份有限公司 | Preparation method of fibrid reinforced nylon composite material |
| CN112688023A (en) * | 2020-12-30 | 2021-04-20 | 河北金力新能源科技股份有限公司 | Aromatic polyamide coating diaphragm and preparation method thereof |
| CN115369505A (en) * | 2022-07-08 | 2022-11-22 | 株洲时代新材料科技股份有限公司 | Multistage dispersion disc precipitation forming device and forming process, precipitation fiber precipitation purification device and process |
| CN115369505B (en) * | 2022-07-08 | 2024-05-03 | 株洲时代新材料科技股份有限公司 | Multistage dispersion plate precipitation forming device and forming process, fibrid precipitation purifying device and technology |
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