CN103526321B - A kind of preparation method of high-performance polyisophthaloyl metaphenylene diamine fiber - Google Patents
A kind of preparation method of high-performance polyisophthaloyl metaphenylene diamine fiber Download PDFInfo
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- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000000835 fiber Substances 0.000 title claims abstract description 53
- -1 polyisophthaloyl Polymers 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000001125 extrusion Methods 0.000 claims abstract description 13
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 13
- 238000009998 heat setting Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 150000001412 amines Chemical class 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 229940018564 m-phenylenediamine Drugs 0.000 claims description 64
- 229920000642 polymer Polymers 0.000 claims description 29
- 239000007788 liquid Substances 0.000 claims description 23
- 238000007711 solidification Methods 0.000 claims description 23
- 230000008023 solidification Effects 0.000 claims description 23
- WFKAJVHLWXSISD-UHFFFAOYSA-N isobutyramide Chemical compound CC(C)C(N)=O WFKAJVHLWXSISD-UHFFFAOYSA-N 0.000 claims description 21
- 238000009987 spinning Methods 0.000 claims description 21
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 16
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 16
- FDQSRULYDNDXQB-UHFFFAOYSA-N benzene-1,3-dicarbonyl chloride Chemical compound ClC(=O)C1=CC=CC(C(Cl)=O)=C1 FDQSRULYDNDXQB-UHFFFAOYSA-N 0.000 claims description 16
- 239000000084 colloidal system Substances 0.000 claims description 11
- BNUSXAUXIQINHI-UHFFFAOYSA-L C(C)(=O)N(C)C.[OH-].[Ca+2].[OH-] Chemical compound C(C)(=O)N(C)C.[OH-].[Ca+2].[OH-] BNUSXAUXIQINHI-UHFFFAOYSA-L 0.000 claims description 9
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 9
- 239000001110 calcium chloride Substances 0.000 claims description 9
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 235000011187 glycerol Nutrition 0.000 claims description 8
- 230000015271 coagulation Effects 0.000 claims description 7
- 238000005345 coagulation Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- 239000003495 polar organic solvent Substances 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 5
- 239000000920 calcium hydroxide Substances 0.000 claims description 5
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 4
- 239000006227 byproduct Substances 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 150000004985 diamines Chemical class 0.000 claims description 3
- 239000000243 solution Substances 0.000 description 26
- 238000005516 engineering process Methods 0.000 description 4
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000001788 irregular Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 1
- 241000293001 Oxytropis besseyi Species 0.000 description 1
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 1
- 244000046052 Phaseolus vulgaris Species 0.000 description 1
- 150000001263 acyl chlorides Chemical class 0.000 description 1
- 235000019994 cava Nutrition 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
Abstract
The invention discloses a kind of preparation method of high-performance polyisophthaloyl metaphenylene diamine fiber, comprise the steps such as two amine solvents, polymerized at normal temperature reaction, neutralization reaction, filtration and deaeration, extrusion molding, drawing-off, washing, oven dry, HEAT SETTING, the fiber that the present invention prepares has higher tensile strength and fracture strength, retaining power is stronger, and section dirty efficiency is higher.
Description
Technical field
The present invention relates to the technical field of producing of Fanglun 1313, especially relate to a kind of preparation method of high-performance polyisophthaloyl metaphenylene diamine fiber.
Background technology
In prior art, the production technology comparative maturity of Fanglun 1313, if Chinese invention patent application number is " 201110406292.5 ", patent name is the Chinese invention patent application of " method of continuous production of polyisophthaloyl metaphenylene diamine spinning stock solution ", and Chinese invention patent number is " 200810035666.5 ", patent name is for shown in the Chinese invention patent of " preparation method of polyisophthaloyl metaphenylene diamide pulp-shaped fiber ", the cross sectional shape of its Fanglun 1313 produced is regular, its cross sectional shape is circular for oval, in the same circumstances, such as, when equal in quality or same volume, the contact area of the Fanglun 1313 that the production technology of prior art is produced is less, retaining power is poor, cut dirty efficiency lower, be used in high-performance page aspect, the page of the Fanglun 1313 that prior art production technology is produced is in tensile strength, the poor-performing of fracture strength aspect.Therefore be necessary to be improved.
Summary of the invention
For the deficiency that prior art exists, the object of this invention is to provide a kind of preparation method of high-performance polyisophthaloyl metaphenylene diamine fiber, the fiber that it prepares has higher tensile strength and fracture strength, and retaining power is stronger, and section dirty efficiency is higher.
To achieve these goals, the technical solution adopted in the present invention is.
A preparation method for high-performance polyisophthaloyl metaphenylene diamine fiber, comprises the following steps,
Two amine solvents, m-phenylene diamine (MPD) selects polymer grade m-phenylene diamine (MPD), amide-type polar organic solvent selects dimethylacetamide solution, by the dimethylacetamide solution that the dimethylacetylamide of the drying of 6 ~ 8 weight portions is made, the polymer grade m-phenylene diamine (MPD) of 1 weight portion is joined dimethylacetamide solution, and solution temperature controls at 20 ~ 30 DEG C;
Polymerized at normal temperature reacts, and adds the polymer grade m-phthaloyl chloride of 1 ~ 3 weight portion continuously lentamente, carries out polymerisation, and reaction generates poly-m-phthaloyl chloride m-phenylene diamine (MPD) condensation polymer and byproduct hydrogen chloride;
Neutralization reaction, corresponding to the described m-phenylene diamine (MPD) of 1 weight portion, adds the calcium hydroxide dimethylacetamide solution of 0.5 ~ 0.7 weight portion, carries out neutralization reaction, controls solution temperature lower than 70 DEG C during reaction;
The poly-m-phthaloyl chloride m-phenylene diamine (MPD) polymer prepared, concentration=16 ~ 20wt%, [η]=1.3 ~ 2.2, pH value=6.5 ~ 7;
Filter and deaeration, filtered by filter medium, deaeration, be prepared into the colloid of applicable spinning, colloid is stored in the temperature environment of 40 ~ 100 DEG C;
Extrusion molding, colloid is extruded by spinning head, and in solidification liquid, directly extrude also coagulation forming is non-drawing of fiber;
Drawing-off, by the non-drawing of fiber of drawing machine drawing-off coagulation forming;
Washing;
Dry;
HEAT SETTING;
Finished product.
In further technical scheme, in described filtration and deaeration step, filter medium selects 600 ~ 1000 object paper filter material or sintering felt; In described extrusion molding step, spinning head selects aperture to be 0.05 ~ 0.15mm, hole count 1000 ~ 30000 sphere spinning head.
In further technical scheme, in described filtration and deaeration step, filter medium selects 800 object paper filter material or sintering felt; In described extrusion molding step, spinning head selects aperture to be the sphere spinning head of 0.09mm, and in described drafting step, drafting multiple is 4 times.
In further technical scheme, in described extrusion molding step, the temperature of solidification liquid is 70 ~ 120 DEG C, and solidification liquid comprises the glycerine of the dimethylacetylamide of 5 ~ 25% weight portions, the calcium chloride of 30 ~ 50% weight portions and 0 ~ 10% weight portion, and all the other are water.
In further technical scheme, in described extrusion molding step, the temperature of solidification liquid is 84 DEG C, and solidification liquid comprises the glycerine of the dimethylacetylamide of 25% weight portion, the calcium chloride of 45% weight portion and 2% weight portion, and all the other are water.
In further technical scheme, in described drafting step, drafting multiple is 2 ~ 5 times;
In described baking step, the temperature of oven dry is 120 ~ 160 DEG C;
Described heat setting step, the temperature of HEAT SETTING is 250 ~ 350 DEG C.
In further technical scheme, in described diamines dissolving step, by the dimethylacetamide solution that the dimethylacetylamide of the drying of 7.8 weight portions is made, the polymer grade m-phenylene diamine (MPD) of 1 weight portion is joined dimethylacetamide solution, solution temperature controls at 20 ~ 30 DEG C;
In described polymerized at normal temperature reactions steps, add the polymer grade m-phthaloyl chloride of 1.88 weight portions continuously lentamente;
In neutralization reaction step, corresponding to the described m-phenylene diamine (MPD) of 1 weight portion, add the calcium hydroxide dimethylacetamide solution of 0.68 weight portion, in calcium hydroxide dimethylacetamide solution, the weight ratio of calcium hydroxide and dimethylacetylamide is 1:2.
After adopting above-mentioned technique, the present invention compared to the prior art advantageously: the intensity of the high-performance polyisophthaloyl metaphenylene diamine fiber that the present invention prepares is very high, can reach more than 5.0cn/dtex, and modulus is 80 ~ 110cn/dtex; And its cross section is irregular, is not circle or the ellipse of rule, is applied to filtration aspect, in the same circumstances, the contact area of fiber of the present invention is larger, and its retaining power is stronger, and section dirty efficiency is higher; Be used in high-performance page aspect, the contact area also due to fiber of the present invention is larger, and fiber page has other allied fibers without superable premium properties in tensile strength, fracture strength.
Detailed description of the invention
The following stated is only preferred embodiment of the present invention, does not therefore limit protection scope of the present invention.
Embodiment one
A preparation method for high-performance polyisophthaloyl metaphenylene diamine fiber, comprises the following steps,
Two amine solvents, it is in the amide-type polar organic solvent of 20 ~ 60 DEG C that m-phenylene diamine (MPD) is added to temperature, and m-phenylene diamine (MPD) is dissolved in amide-type polar organic solvent; Particularly, m-phenylene diamine (MPD) selects polymer grade m-phenylene diamine (MPD), amide-type polar organic solvent selects dimethylacetamide solution, by the dimethylacetamide solution that the dimethylacetylamide of the drying of 6 ~ 8 weight portions is made, the polymer grade m-phenylene diamine (MPD) of 1 weight portion is joined dimethylacetamide solution, and solution temperature controls at 20 ~ 30 DEG C;
Polymerized at normal temperature reacts, and the solution temperature of diamines dissolving step gained controls to be 20 ~ 40 DEG C, adds m-phthaloyl chloride and carries out polymerisation, particularly, add the polymer grade m-phthaloyl chloride of 1 ~ 3 weight portion continuously lentamente; Reaction generates poly-m-phthaloyl chloride m-phenylene diamine (MPD) condensation polymer and byproduct hydrogen chloride;
Neutralization reaction, adds alkaline earth oxide or hydroxide, carries out neutralization reaction, controls solution temperature lower than 70 DEG C during reaction; Corresponding to the m-phenylene diamine (MPD) of 1 weight portion, add alkaline earth oxide or the hydroxide of 0.5 ~ 0.7 weight portion;
The poly-m-phthaloyl chloride m-phenylene diamine (MPD) polymer prepared, concentration=16 ~ 20wt%, [η]=1.3 ~ 2.2, pH value=6.5 ~ 7;
Filter and deaeration, filtered by filter medium, filter medium selects 600 ~ 1000 object paper filter material or sintering felt; Deaeration, is prepared into the colloid of applicable spinning, and colloid is stored in the temperature environment of 40 ~ 100 DEG C;
Extrusion molding, colloid is extruded by spinning head, and spinning head selects aperture to be 0.05 ~ 0.15mm, hole count 1000 ~ 30000 sphere spinning head; In solidification liquid, directly extrude also coagulation forming is non-drawing of fiber; The temperature of solidification liquid is 70 ~ 120 DEG C, and solidification liquid comprises the glycerine of the dimethylacetylamide of 5 ~ 25% weight portions, the calcium chloride of 30 ~ 50% weight portions and 0 ~ 10% weight portion, and all the other are water.
Drawing-off, by the non-drawing of fiber of drawing machine drawing-off coagulation forming; Drafting multiple is 2 ~ 5 times;
Washing;
Dry; The temperature of drying is 120 ~ 160 DEG C;
HEAT SETTING; The temperature of HEAT SETTING is 250 ~ 350 DEG C;
Finished product.
The preparation method of high-performance polyisophthaloyl metaphenylene diamine fiber of the present invention, a certain amount of dimethylacetylamide is added in polymeric kettle, two amine solvents are good, then the acyl chlorides of equimolar amounts is slowly added, reaction terminate after, add a certain amount of calcium hydroxide neutralization, in become reconciled after pass through filter media, again through deaeration, be prepared into the polymeric colloid of qualified applicable spinning.
Above-mentioned colloid by spray plate, inside solidification liquid, wire drawing is solidified, then drawing-off, again the fiber of drawing-off is passed through washing washes clean, delay unloading and press dry, enter baking zone drying, the temperature of dry section controls in the scope of 120 ~ 160 DEG C, then enter the heat setting machine sizing of 250 ~ 350 DEG C, obtain product afterwards.
The intensity of the high-performance polyisophthaloyl metaphenylene diamine fiber finally obtained is very high, even can reach more than 5.0cn/dtex, and modulus is 80 ~ 110cn/dtex; And fiber prepared by the present invention, cross section is not circle or the ellipse of rule, but irregular shape, its cross sectional shape is similar to shoestring, its two ends are close to circular arc, middle part caves inward or outwardly, is similar to the shape of broadband shape or waist beans, thus gives fiber and play an important role in different fields.
In situation of the same area, circular girth is the shortest; And under identical weight, the perimeter of section of erose fiber is longer, that is, fiber surface of the present invention is no matter under which kind of use occasion, and it is relatively large with the contact area of other things.The high-performance polyisophthaloyl metaphenylene diamine fiber that the present invention prepares is applied to filtration aspect, and in the same circumstances, the contact area of fiber of the present invention is larger, and its retaining power is stronger, and section dirty efficiency is higher; Be used in high-performance page aspect, the contact area also due to fiber of the present invention is larger, and fiber page has other allied fibers without superable premium properties in tensile strength, fracture strength.
Embodiment two
A preparation method for high-performance polyisophthaloyl metaphenylene diamine fiber, comprises the following steps,
Two amine solvents, m-phenylene diamine (MPD) selects polymer grade m-phenylene diamine (MPD), amide-type polar organic solvent selects dimethylacetamide solution, by the dimethylacetamide solution that the dimethylacetylamide of the drying of 7.8 weight portions is made, the polymer grade m-phenylene diamine (MPD) of 1 weight portion is joined dimethylacetamide solution, and solution temperature controls at 20 ~ 30 DEG C;
Polymerized at normal temperature reacts, and corresponding to the m-phenylene diamine (MPD) of 1 weight portion, adds the polymer grade m-phthaloyl chloride of 1.88 weight portions continuously lentamente;
Neutralization reaction, corresponding to the m-phenylene diamine (MPD) of 1 weight portion, adds alkaline earth oxide or the hydroxide of 0.68 weight portion; More specifically, add the calcium hydroxide dimethylacetamide solution of 0.68 weight portion, in calcium hydroxide dimethylacetamide solution, the weight ratio of calcium hydroxide and dimethylacetylamide is 1:2;
The poly-m-phthaloyl chloride m-phenylene diamine (MPD) polymer prepared,
Filter and deaeration, filter medium selects 800 object paper filter material or sintering felt;
Extrusion molding, spinning head selects aperture to be the sphere spinning head of 0.09mm, and the temperature of solidification liquid is 84 DEG C, and solidification liquid comprises the glycerine of the dimethylacetylamide of 25% weight portion, the calcium chloride of 45% weight portion and 2% weight portion, and all the other are water.
In drafting step, by the non-drawing of fiber of drawing machine drawing-off coagulation forming, drafting multiple is 4 times.
Washing;
Dry;
HEAT SETTING;
Finished product.
Embodiment three
A kind of preparation method of high-performance polyisophthaloyl metaphenylene diamine fiber, comprise the following steps, in the tank reactor with stirring and chuck, the polymer grade m-phenylene diamine (MPD) of 1 weight portion is added in the dimethylacetylamide of the drying of 7.8 weight portions, temperature is controlled at 20 ~ 30 DEG C, the continuous polymer grade m-phthaloyl chloride adding 1.88 weight portions slowly carries out polymerisation, the hydrogen chloride the generated calcium hydroxide dimethylacetamide solution of 0.68 weight portion, the ratio of calcium hydroxide and dimethylacetylamide is 1:2.The continuous neutralization reaction of solution, control temperature, lower than 70 DEG C, reacts the poly-m-phthaloyl chloride m-phenylene diamine (MPD) colloidal polymer generated, the concentration=18.2wt% of polymer, [η]=1.92, pH value=6.9; Polymer pale yellow transparent, quality is good.Polymer in 800 object filter media, deaeration; Then be 20000 by hole count, aperture is the spinning head of 0.09mm, solidifies in solidification liquid.The temperature of solidification liquid is 84 DEG C, and solidification liquid comprises the glycerine of the dimethylacetylamide of 25% weight portion, the calcium chloride of 45% weight portion and 2% weight portion, and all the other are water.
Fiber after solidifying through the drawing-off of 4 times, afterwards through washing, dry, HEAT SETTING, the fiber finally obtained, fiber number: 2.04Dtex, intensity is: 5.2cn/dtex, and percentage elongation is 32%.
In order to further illustrate the present invention, be described below in conjunction with comparison example.
Comparison example 1
Curing condition in example 1 is changed into: the temperature of solidification liquid is 84 DEG C, solidification liquid comprises the dimethylacetylamide of 20% weight portion and the calcium chloride of 42% weight portion, and all the other are water, and other are constant.The fiber finally obtained, fiber number: 2.06Dtex, intensity is: 3.9cn/dtex, and percentage elongation is 43%.
Comparison example 2
Drafting multiple in example 1 is changed into 3 times, and other are constant.The fiber finally obtained, fiber number: 2.2Dtex, intensity is: 4.1cn/dtex, and percentage elongation is 39%.
Comparison example 3
Curing condition in example 1 is changed into: the temperature of solidification liquid is 100 DEG C, solidification liquid comprises the dimethylacetylamide of 20% weight portion, the calcium chloride of 42% weight portion is the glycerine with 7% weight portion, and all the other are water, and other are constant.The fiber finally obtained, fiber number: 2.02Dtex, intensity is: 4.3cn/dtex, and percentage elongation is 34%.
Above content is only preferred embodiment of the present invention, and for those of ordinary skill in the art, according to thought of the present invention, all will change in specific embodiments and applications, this description should not be construed as limitation of the present invention.
Claims (8)
1. a preparation method for high-performance polyisophthaloyl metaphenylene diamine fiber, is characterized in that: comprise the following steps,
Two amine solvents, m-phenylene diamine (MPD) selects polymer grade m-phenylene diamine (MPD), amide-type polar organic solvent selects dimethylacetamide solution, by the dimethylacetamide solution that the dimethylacetylamide of the drying of 6 ~ 8 weight portions is made, the polymer grade m-phenylene diamine (MPD) of 1 weight portion is joined dimethylacetamide solution, and solution temperature controls at 20 ~ 30 DEG C;
Polymerized at normal temperature reacts, and adds the polymer grade m-phthaloyl chloride of 1 ~ 3 weight portion continuously lentamente, carries out polymerisation, and reaction generates poly-m-phthaloyl chloride m-phenylene diamine (MPD) condensation polymer and byproduct hydrogen chloride;
Neutralization reaction, corresponding to the described m-phenylene diamine (MPD) of 1 weight portion, adds the calcium hydroxide dimethylacetamide solution of 0.5 ~ 0.7 weight portion, carries out neutralization reaction, controls solution temperature lower than 70 DEG C during reaction;
The poly-m-phthaloyl chloride m-phenylene diamine (MPD) polymer prepared, concentration=16 ~ 20wt%, [η]=1.3 ~ 2.2, pH value=6.5 ~ 7;
Filter and deaeration, filtered by filter medium, deaeration, be prepared into the colloid of applicable spinning, colloid is stored in the temperature environment of 40 ~ 100 DEG C;
Extrusion molding, colloid is extruded by spinning head, and in solidification liquid, directly extrude also coagulation forming is non-drawing of fiber;
Drawing-off, by the non-drawing of fiber of drawing machine drawing-off coagulation forming;
Washing;
Dry;
HEAT SETTING;
Finished product.
2. the preparation method of a kind of high-performance polyisophthaloyl metaphenylene diamine fiber according to claim 1, is characterized in that: in described filtration and deaeration step, and filter medium selects 600 ~ 1000 object paper filter material or sintering felt; In described extrusion molding step, spinning head selects aperture to be 0.05 ~ 0.15mm, hole count 1000 ~ 30000 sphere spinning head.
3. the preparation method of a kind of high-performance polyisophthaloyl metaphenylene diamine fiber according to claim 1, is characterized in that: in described filtration and deaeration step, and filter medium selects 800 object paper filter material or sintering felt; In described extrusion molding step, spinning head selects aperture to be the sphere spinning head of 0.09mm, and in described drafting step, drafting multiple is 4 times.
4. the preparation method of a kind of high-performance polyisophthaloyl metaphenylene diamine fiber according to claim 1, it is characterized in that: in described extrusion molding step, the temperature of solidification liquid is 70 ~ 120 DEG C, solidification liquid comprises the glycerine of the dimethylacetylamide of 5 ~ 25% weight portions, the calcium chloride of 30 ~ 50% weight portions and 0 ~ 10% weight portion, and all the other are water.
5. the preparation method of a kind of high-performance polyisophthaloyl metaphenylene diamine fiber according to claim 1, it is characterized in that: in described extrusion molding step, the temperature of solidification liquid is 84 DEG C, solidification liquid comprises the glycerine of the dimethylacetylamide of 25% weight portion, the calcium chloride of 45% weight portion and 2% weight portion, and all the other are water.
6. the preparation method of a kind of high-performance polyisophthaloyl metaphenylene diamine fiber according to claim 1, is characterized in that: in described drafting step, drafting multiple is 2 ~ 5 times;
In described baking step, the temperature of oven dry is 120 ~ 160 DEG C;
Described heat setting step, the temperature of HEAT SETTING is 250 ~ 350 DEG C.
7. the preparation method of a kind of high-performance polyisophthaloyl metaphenylene diamine fiber according to claim 1, it is characterized in that: in described diamines dissolving step, by the dimethylacetamide solution that the dimethylacetylamide of the drying of 7.8 weight portions is made, the polymer grade m-phenylene diamine (MPD) of 1 weight portion is joined dimethylacetamide solution, and solution temperature controls at 20 ~ 30 DEG C;
In described polymerized at normal temperature reactions steps, add the polymer grade m-phthaloyl chloride of 1.88 weight portions continuously lentamente;
In neutralization reaction step, corresponding to the described m-phenylene diamine (MPD) of 1 weight portion, add the calcium hydroxide dimethylacetamide solution of 0.68 weight portion.
8. the preparation method of a kind of high-performance polyisophthaloyl metaphenylene diamine fiber according to claim 7, is characterized in that: in neutralization reaction step, in calcium hydroxide dimethylacetamide solution, the weight ratio of calcium hydroxide and dimethylacetylamide is 1: 2.
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| CN105970306A (en) * | 2016-07-15 | 2016-09-28 | 圣欧芳纶（淮安）有限公司 | Production process for optimizing fiber performance through heat treatment |
| CN106222764B (en) * | 2016-10-07 | 2018-04-06 | 上海会博新材料科技有限公司 | The device of meta-aramid fibers is prepared using dry spinning |
| CN107815741A (en) * | 2017-07-24 | 2018-03-20 | 烟台泰和新材料股份有限公司 | A kind of meta-aramid filament preparation process |
| CN110804767B (en) * | 2019-11-04 | 2022-04-26 | 赣州龙邦材料科技有限公司 | Aramid 1313 fiber and preparation method and application thereof |
| CN114703554B (en) * | 2022-04-27 | 2023-04-25 | 赣州龙邦材料科技有限公司 | Preparation method for aramid fiber primary pulp stretch solidification molding |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101250833A (en) * | 2008-04-03 | 2008-08-27 | 钟洲 | Method for manufacturing polyisophthaloyl metaphenylene diamide pulp-shaped fibre |
| CN101302649A (en) * | 2008-04-03 | 2008-11-12 | 圣欧（苏州）安全防护材料有限公司 | Making method of non-circular sectional special-shaped meta-position aromatic polyamide fiber |
| CN101724935A (en) * | 2009-12-14 | 2010-06-09 | 中蓝晨光化工研究院有限公司 | Polyphenylene terephthalamide fibre and preparation method thereof |
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