CN102400242A - Method for preparing colored poly-m-phenyleneisophthalamide (PMIA) fibers - Google Patents
Method for preparing colored poly-m-phenyleneisophthalamide (PMIA) fibers Download PDFInfo
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Abstract
The invention discloses a method for preparing colored poly-m-phenyleneisophthalamide (PMIA) fibers. The method comprises the following steps of: dissolving m-phenylenediamine into a polar organic solvent, cooling, adding m-phthaloyl chloride, performing low-temperature solution polymerization, neutralizing the solution by using calcium hydroxide and thus obtaining a PMIA spinning solution, and defoaming; dispersing a coloring agent into a polar organic solvent to prepare a coloring agent solution; adding the spinning solution and the coloring agent solution into the head of a split double-screw extruder at the same time, and mixing; and directly feeding the mixture into a coagulation bath because the split double-screw extruder is directly connected with a spinning jet, performing thermal stretching, curving, cutting, packing, and thus obtaining the colored PMIA fibers. The coloring agent solution and the spinning solution are mixed by adopting the split double-screw extruder in the method, and the split double-screw extruder is directly connected with the spinning jet for spinning. According to the method, when the color is changed, the cylinder can be quickly opened in a few minutes and is artificially cleaned, so that a cleaning material is not used or a small quantity of cleaning material is used, the cost is saved, and the environmental pollution is reduced.
Description
Technical field
The present invention relates to a kind of preparation method of meta-aramid fibers, relate in particular to a kind of preparation method of coloured meta-aramid fibers.
Background technology
Meta-aramid, the full name poly is claimed aramid fiber 1313 again, is a kind of high-temperature fibre kind wide, that output is big, development is fast of developing early, use, its total amount occupies second of special fibre.Be to arrange the regular big molecule of sawtooth pattern, before fusion, just decompose that vitrification point Tg is 270 ℃, significantly decomposition and carbonization can not take place below 350 ℃.When temperature surpassed 400 ℃, fiber embrittlement, charing gradually still can not produce molten drop until decomposition; In flame, do not prolong combustion, have anti-flammability preferably, limited oxygen index LOI is 29%-32%, and performance is splendid.
At present; Meta-aramid fibers dyeing difficulty; Limited the application of meta-aramid fibers, carried out spinning in the poly (m-phenylene isophthalmide) spinning dope more, prepared coloured meta-aramid fibers so meta-aramid fibers adopts pigment directly added at garment industry.
At the disclosed related patent U.S. Patent No. CN1847475A of China, CN1740412A and CN1004224
Among the 01C, all exist poly (m-phenylene isophthalmide) spinning dope and pigment slurry mixing procedure long, complex process during color replacement, slurries wastes is serious, cleans shortcoming such as waste time and energy.
Therefore, press for the preparation method that a kind of coloured meta-aramid fibers can be provided, can overcome above-mentioned disadvantage.
Summary of the invention
The technical problem that the present invention solves provides a kind of preparation method of coloured meta-aramid fibers, to overcome the above-mentioned defective that prior art exists.
A kind of preparation method of coloured meta-aramid fibers, be made up of following step:
(1) preparation spinning solution: m-phenylene diamine (MPD) is dissolved in the polar organic solvent, and cooling adds m-phthaloyl chloride and carries out low temperature solution polymerization, with the calcium hydroxide neutralization, obtains poly (m-phenylene isophthalmide) spinning dope, deaeration;
(2) configuration colourant solution: colouring agent is dispersed in the polar organic solvent, makes colourant solution;
(3) spinning solution and colouring agent mix: step (1) spinning solution that makes and the colourant solution that step (2) makes are added the mixing of dissection type double screw extruder head simultaneously; The mass ratio of said spinning solution and colourant solution is 3000:1-65:1, preferably 1000:1-100:1;
(4) spinning: the dissection type double screw extruder directly connects spinning head and directly gets into coagulating bath, hot-stretch, curl, cut off, packing, make coloured meta-aramid fibers;
Wherein step (1) is identical with the polar organic solvent of step (2).
The waste of the spinning slurry when reducing colour changing, the present invention adds colouring agent when spinning, be employed in mixed colorant solution and spinning solution in the dissection type double screw extruder.This mixed method makes the colourant solution distance short, is easy to color and luster alternately, helps the coloured aramid fiber production of many kinds.
The screw rod of dissection type double screw extruder main frame, machine barrel all adopt advanced " building block system " design, and screw rod is combined by the various forms of spiral shell pieces that are sleeved on the mandrel, can disassembled simply; When changing color; As long as time a few minutes just can be opened machine barrel fast, carry out manual work and clean, so just can use no or little and clean material; Practice thrift cost, reduce environmental pollution.Another advantage of " building block system " design is can carry out local replacing for screw rod and cylindrical shell element that wearing and tearing have taken place, has avoided scrapping of whole screw rod or cylindrical shell, greatly reduces maintenance cost.
Preferably,
M-phenylene diamine (MPD) and m-phthaloyl chloride mol ratio are 1:1 in the said step (1), and the mol ratio of calcium hydroxide and m-phenylene diamine (MPD) is 1:1.002.
The polar organic solvent of said step (1) and step (2) is DMAC N,N or N-Methyl pyrrolidone.
The logarithmic viscosity number of spinning solution is at 2-2.5 in the said step (1), and the mass percent concentration of poly is 15-19% in the spinning solution.
Colouring agent is an inorganic pigment in the said step (2), preferably 10min nondiscolouring under 350 degree, and water insoluble, DMAC N,N and N-Methyl pyrrolidone.Inorganic pigment is a graininess, greater than 2000 orders.Be inorganic compounding pigment preferably in the inorganic pigment, color is vivid, and function admirable has favorable durability.
The mass percent concentration of colouring agent is 25-46% in the colourant solution in the said step (2).
Spinning solution and colourant solution are 3-15min in the time of staying of dissection type double screw extruder in the said step (3), and extruding slurry temperature is 0-70 ℃, is preferably 40-60 ℃.
Coagulation bath temperature is 20-50 ℃ described in the said step (4); Coagulating bath is the aqueous solution of polar organic solvent; Said polar organic solvent is identical with the polar organic solvent of step (1) and step (2), and polar organic solvent mass percent concentration described in the said coagulating bath is 35-50%.
In the said step (4) in the hot drawing-off hot drafting multiple be 3-6 doubly, to improve the physical and mechanical properties of fiber.
The preparation method of coloured meta-aramid fibers of the present invention adopts dissection type double screw extruder mixed colorant and spinning solution, and the dissection type double screw extruder directly connects spinning head, carries out spinning.When this method is changed color,, carry out manual work and clean, so just can use no or little and clean material, practice thrift cost, reduce environmental pollution as long as time a few minutes just can be opened machine barrel fast.
Through embodiment the present invention is described further below, but embodiment does not limit protection scope of the present invention.
The specific embodiment
Embodiment 1
Present embodiment original liquid coloring fibre manufacture adopts the polymerization production line of producing 500kg daily, implements according to following operation:
(1) preparation spinning solution: m-phenylene diamine (MPD) is dissolved in the DMAC N,N, and cooling adds m-phthaloyl chloride and carries out low temperature solution polymerization, with the calcium hydroxide neutralization, obtains poly (m-phenylene isophthalmide) spinning dope, deaeration; Said m-phenylene diamine (MPD) and m-phthaloyl chloride mol ratio are 1:1; The mol ratio of calcium hydroxide and m-phenylene diamine (MPD) is 1:1.002; The logarithmic viscosity number of the spinning solution of preparation is 2.3, and the mass percent concentration of poly is 18% in the spinning solution.
(2) configuration colourant solution: inorganic pigment is dispersed in the DMAC N,N, makes colourant solution, wherein the mass percent concentration of colouring agent is 35%.Used inorganic pigment is yellow inorganic compounding pigment, fineness 3000 orders.
(3) spinning solution and colouring agent mix: step (1) spinning solution that makes and the colourant solution that step (2) makes are added the mixing of dissection type double screw extruder head simultaneously, and the mass ratio of said spinning solution and colourant solution is 130:1; Wherein, spinning solution and colourant solution are 7min in the time of staying of dissection type double screw extruder, and the dissection type double screw extruder designs for jacket type, and extruding slurry temperature is 50 ℃.
(4) spinning: the dissection type double screw extruder directly connects spinning head and directly gets into coagulating bath, hot-stretch, curl, cut off, packing, make coloured meta-aramid fibers;
Wherein, said coagulation bath temperature is 40 ℃, and coagulating bath is the aqueous solution of DMAC N,N, and DMAC N,N mass percent concentration described in the said coagulating bath is 40%.Hot drafting multiple is 5 times in the hot drawing-off, to improve the physical and mechanical properties of fiber.
Pigment content is 1.5% in the obtained coloured meta-aramid fibers of present embodiment, and fiber number is 2.2dtex, and fracture strength is greater than 4cN/dtex.
Embodiment 2
Present embodiment original liquid coloring fibre manufacture adopts the polymerization production line of producing 500kg daily, implements according to following operation:
(1) preparation spinning solution: m-phenylene diamine (MPD) is dissolved in the N-Methyl pyrrolidone, and cooling adds m-phthaloyl chloride and carries out low temperature solution polymerization, with the calcium hydroxide neutralization, obtains poly (m-phenylene isophthalmide) spinning dope, deaeration; Said m-phenylene diamine (MPD) and m-phthaloyl chloride mol ratio are 1:1; The mol ratio of calcium hydroxide and m-phenylene diamine (MPD) is 1:1.002; The logarithmic viscosity number of the spinning solution of preparation is 2.5, and the mass percent concentration of poly is 15% in the spinning solution.
(2) configuration colourant solution: inorganic pigment is dispersed in the N-Methyl pyrrolidone, makes colourant solution, wherein the mass percent concentration of colouring agent is 40%.Used inorganic pigment is a black inorganic compounding pigment, fineness 3000 orders.
(3) spinning solution and colouring agent mix: step (1) spinning solution that makes and the colourant solution that step (2) makes are added the mixing of dissection type double screw extruder head simultaneously, and the mass ratio of said spinning solution and colourant solution is 500:1; Wherein, spinning solution and colourant solution are 7min in the time of staying of dissection type double screw extruder, and the dissection type double screw extruder designs for jacket type, and extruding slurry temperature is 50 ℃.
(4) spinning: the dissection type double screw extruder directly connects spinning head and directly gets into coagulating bath, hot-stretch, curl, cut off, packing, make coloured meta-aramid fibers;
Wherein, said coagulation bath temperature is 40 ℃, and coagulating bath is the aqueous solution of N-Methyl pyrrolidone, and N-Methyl pyrrolidone mass percent concentration described in the said coagulating bath is 40%.Hot drafting multiple is 5 times in the hot drawing-off, to improve the physical and mechanical properties of fiber.
Pigment content is 0.5% in the obtained coloured meta-aramid fibers of present embodiment, and fiber number is 2.2dtex, and fracture strength is greater than 4.3cN/dtex.
The waste of the spinning slurry when reducing colour changing, the present invention adds colouring agent when spinning, be employed in mixed colorant solution and spinning solution in the dissection type double screw extruder.This mixed method makes the colourant solution distance short, is easy to color and luster alternately, helps the coloured aramid fiber production of many kinds.
The screw rod of dissection type double screw extruder main frame, machine barrel all adopt advanced " building block system " design, and screw rod is combined by the various forms of spiral shell pieces that are sleeved on the mandrel, can disassembled simply;, when changing color, as long as time a few minutes just can open machine barrel fast; Carrying out manual work cleans; So just can use no or little and clean material, practice thrift cost, reduce environmental pollution.Another advantage of " building block system " design is can carry out local replacing for screw rod and cylindrical shell element that wearing and tearing have taken place, has avoided scrapping of whole screw rod or cylindrical shell, greatly reduces maintenance cost.
In a word, the present invention can also have multiple conversion and remodeling, is not limited to the concrete structure of above-mentioned embodiment, and protection scope of the present invention should comprise those conspicuous to those skilled in the art conversion or substitute and remodeling.
Claims (10)
1. the preparation method of a coloured meta-aramid fibers is characterized in that, is made up of following step:
(1) preparation spinning solution: m-phenylene diamine (MPD) is dissolved in the polar organic solvent, and cooling adds m-phthaloyl chloride and carries out low temperature solution polymerization, with the calcium hydroxide neutralization, obtains poly (m-phenylene isophthalmide) spinning dope, deaeration;
(2) configuration colourant solution: colouring agent is dispersed in the polar organic solvent, makes colourant solution;
(3) spinning solution and colouring agent mix: step (1) spinning solution that makes and the colourant solution that step (2) makes are added the mixing of dissection type double screw extruder head simultaneously, and the mass ratio of said spinning solution and colourant solution is 3000:1-65:1;
(4) spinning: the dissection type double screw extruder directly connects spinning head and directly gets into coagulating bath, hot-stretch, curl, cut off, packing, make coloured meta-aramid fibers;
Wherein step (1) is identical with the polar organic solvent of step (2).
2. the preparation method of coloured meta-aramid fibers as claimed in claim 1 is characterized in that: m-phenylene diamine (MPD) and m-phthaloyl chloride mol ratio are 1:1 in the said step (1), and the mol ratio of calcium hydroxide and m-phenylene diamine (MPD) is 1:1.002.
3. the preparation method of coloured meta-aramid fibers as claimed in claim 1, it is characterized in that: the polar organic solvent of said step (1) and step (2) is DMAC N,N or N-Methyl pyrrolidone.
4. the preparation method of coloured meta-aramid fibers as claimed in claim 1 is characterized in that: the logarithmic viscosity number of spinning solution is at 2-2.5 in the said step (1), and the mass percent concentration of poly is 15-19% in the spinning solution.
5. the preparation method of coloured meta-aramid fibers as claimed in claim 1 is characterized in that: colouring agent is an inorganic pigment in the said step (2).
6. the preparation method of coloured meta-aramid fibers as claimed in claim 1, it is characterized in that: the mass percent concentration of colouring agent is 25-46% in the colourant solution in the said step (2).
7. the preparation method of coloured meta-aramid fibers as claimed in claim 1 is characterized in that: spinning solution and colourant solution are 3-15min in the time of staying of dissection type double screw extruder in the said step (3), and extruding slurry temperature is 0-70 ℃.
8. the preparation method of coloured meta-aramid fibers as claimed in claim 1, it is characterized in that: in the said step (3), the mass ratio of said spinning solution and colourant solution is 1000:1-100:1.
9. the preparation method of coloured meta-aramid fibers as claimed in claim 1; It is characterized in that: coagulation bath temperature is 20-50 ℃ described in the said step (4); Coagulating bath is the aqueous solution of polar organic solvent; Said polar organic solvent is identical with the polar organic solvent of step (1) and step (2), and polar organic solvent mass percent concentration described in the said coagulating bath is 35-50%.
10. the preparation method of coloured meta-aramid fibers as claimed in claim 1 is characterized in that: in the said step (4) in the hot drawing-off hot drafting multiple be 3-6 doubly.
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Cited By (5)
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| CN105862496A (en) * | 2015-01-20 | 2016-08-17 | 圣欧芳纶（江苏）股份有限公司 | Method for preparing colored m-aramid fiber paper |
| CN107227496A (en) * | 2017-06-20 | 2017-10-03 | 义乌华鼎锦纶股份有限公司 | A kind of preparation method and equipment of polyamide coloured fiber |
| CN113981560A (en) * | 2021-10-29 | 2022-01-28 | 烟台泰和新材料股份有限公司 | Antibacterial meta-aramid fiber and preparation method thereof |
| CN114197072A (en) * | 2021-12-08 | 2022-03-18 | 上海鑫茗企业管理有限公司 | Spinning method of meta-aramid fiber |
| CN116837484A (en) * | 2023-07-21 | 2023-10-03 | 江苏新视界先进功能纤维创新中心有限公司 | Polymer coloring method, spinning solution and colored fiber |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104593898B (en) * | 2014-12-27 | 2016-08-17 | 烟台泰和新材料股份有限公司 | The preparation method of coloring para-aramid fiber before a kind of |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105862496A (en) * | 2015-01-20 | 2016-08-17 | 圣欧芳纶（江苏）股份有限公司 | Method for preparing colored m-aramid fiber paper |
| CN107227496A (en) * | 2017-06-20 | 2017-10-03 | 义乌华鼎锦纶股份有限公司 | A kind of preparation method and equipment of polyamide coloured fiber |
| CN113981560A (en) * | 2021-10-29 | 2022-01-28 | 烟台泰和新材料股份有限公司 | Antibacterial meta-aramid fiber and preparation method thereof |
| CN114197072A (en) * | 2021-12-08 | 2022-03-18 | 上海鑫茗企业管理有限公司 | Spinning method of meta-aramid fiber |
| CN116837484A (en) * | 2023-07-21 | 2023-10-03 | 江苏新视界先进功能纤维创新中心有限公司 | Polymer coloring method, spinning solution and colored fiber |
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Address after: Friendship Industrial Zone Wujiang City Lingzhen Suzhou City, Jiangsu province 215222 Applicant after: SRO ARAMID FIBER (JIANGSU) CO., LTD. Address before: Friendship Industrial Zone Wujiang City Lingzhen Suzhou City, Jiangsu province 215222 Applicant before: Shengou(Suzhou) Safety Protection Material Co., Ltd. |
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Address after: 215222 Friendship Road 79, Wujiang District, Jiangsu, Suzhou Patentee after: Super Gomez new materials Limited by Share Ltd Address before: Friendship Industrial Zone Wujiang City Lingzhen Suzhou City, Jiangsu province 215222 Patentee before: SRO ARAMID FIBER (JIANGSU) CO., LTD. |