CN1847475A - Spun dyeing meta-aramid short fiber and its preparation process - Google Patents
Spun dyeing meta-aramid short fiber and its preparation process Download PDFInfo
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- CN1847475A CN1847475A CN 200610043660 CN200610043660A CN1847475A CN 1847475 A CN1847475 A CN 1847475A CN 200610043660 CN200610043660 CN 200610043660 CN 200610043660 A CN200610043660 A CN 200610043660A CN 1847475 A CN1847475 A CN 1847475A
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Abstract
The present invention relates to spun dyeing meta-aramid short fiber and its preparation process, and belongs to the field of aramid short fiber and its preparation technology. The preparation process includes the following steps: 1. synthesizing meta-aramatoc polyamide solution as the spinning fluid; 2. pre-treating selected colorants, matching color and dispersing to obtain coloring fluid in proper concentration; 3. mixing the spinning fluid and the coloring fluid; 4. wet spinning the mixed fluid to form continuous tow by means of water solution coagulation bath at 10-35 deg.c; and 5. water washing, stoving, heat treatment, curling and cutting. The pigment of the present invention is treated into grain and agglomerate, whose maximum diameter determines the physical and mechanical performance, spinnability and post-processing performance of the fiber, and is water insoluble and organic solvent insoluble, resulting in no loss during the fiber production.
Description
One, affiliated technical field
The present invention relates to painted meta-aramid staple fibre and preparation method, belong to aramid fiber short fibre and preparation method thereof technical field.
Two, background technology
The meta-aramid that is used for spinning fibre is when carrying out wet method or dry spinning, the fiber of producing in order to make possesses acceptable physical and mechanical properties, must carry out hot drawing-off to fiber, promptly allow fiber make it produce to a certain degree crystallization reaching to heat-treat under the state of glass transition temperature of polymer.Though this fiber through the Overheating Treatment crystallization has improved some physical and mechanical properties of fiber, the dyeability of fiber is exerted an influence, make relatively difficulty of its dyeing, thereby meta-aramid fibers is restricted in the application of garment industry.
Three, summary of the invention
The object of the invention is the meta-aramid staple fibre that provides painted, this fiber is characterised in that painted meta-aramid solution is behind the process wet spinning, fiber not only has desired color, and has the better physical and mechanical properties of fiber than uncoloured fiber and process poststaining.
Spun dyeing meta-aramid short fiber preparation method of the present invention, special character is that its operation is:
1, synthetic a kind of earlier is that solvent comprises the meta-aromatic polyamide solution that mpd-i is a repetitive with the amide compound, gets spinning solution;
2, select suitable colouring agent, colouring agent preliminary treatment, colorant match, dispersion get the painted stoste of debita spissitudo;
3, spinning solution is mixed with painted stoste;
4, this mixed liquor is carried out wet spinning, the aqueous coagulation bath that by temperature is 10-35 ℃ is to form endless tow;
5, to its wash, oven dry, heat treatment and curl, cut off to make the meta-aramid staple fibre of original liquid coloring;
Wherein solvent is selected from dimethyl formamide or dimethylacetylamide;
Wherein poly solution logarithmic viscosity number is at least 2;
Be specially
1, in a kind of amide compound is the system of organic solvent, carries out polymerisation in solution, use anhydrous NH with monomer m-phthaloyl chloride (IPC) and monomer m-phenylene diamine (MPD) (MPDA)
3Carry out preneutralization, filter the gained ammonium chloride, add IPC, neutralization for the second time, get spinning solution;
The spinning solution that adopts before the wet spinning is the less salt spinning solution, adds m-phthaloyl chloride when carrying out polymerisation at twice, makes logarithmic viscosity number 〉=2 of spinning solution;
A, for the first time add m-phthaloyl chloride after, the controlling polymers solution viscosity adds anhydrous ammonia and carries out the hydrochloric acid that generates in the neutralization reaction, removes the ammonium chloride that neutralization reaction generates from the reactant mixture after the neutralization;
B, subsequently, in neutralization reaction solution, add m-phthaloyl chloride, and, making the spinning solution of less salt, and make logarithmic viscosity number 〉=2 of spinning solution by the amount of adjusting the m-phthaloyl chloride that adds with in calcium hydroxide, calcium oxide or other alkali compoundss and the acid that generates;
2, select suitable colouring agent, colouring agent preliminary treatment, colorant match, disperse the painted stoste of debita spissitudo;
The colouring agent that relates in this invention is the pigment of organic or inorganic, and it is to keep Stability Analysis of Structures, nondiscolouring in the clock time in 300 ℃, 5 minutes that selected pigment must satisfy in temperature;
The amount of adding pigment in the fiber depends on the type of the used pigment of desired color harmony, and the amount of the pigment that adds in the fiber is 0.1-4% (percentage by weight);
This pigment can be selected at least a in the following pigment, and these pigment are: AZO pigments, phthalocyanine pigment, heterocycle and condensed ring ketone pigment and some inorganic pigment, pigment be through after the milled processed, make its maximum gauge≤5 micron;
Be benzimidazolone heterocyclic pigment preferably in the AZO pigments;
Be copper phthalocyanine, halogenated copper phthalocyanine pigment preferably in the phthalocyanine pigment;
Heterocycle and condensed ring ketone pigment are two piperazine class pigment, 1 preferably, 4-diketopyrrolo-pyrrole class pigment;
Most of inorganic pigments are because have good durability and heat endurance can be applicable to produce the painted staple fibre of meta-aramid;
3, spinning solution mixes with proper proportion with the painted stoste of debita spissitudo;
Mix to obtain the spinning mixture of homogeneous 10% (weight) of painted stoste before wherein the poly polymer content is at least and spins with meeting the requirements of pigment and poly solution;
4, through wet spinning, cleaning, heat treatment, curl, cut off, packing;
With the spinning mixture deaeration and by diameter is that the spinning head of the spinneret orifice of 0.04-0.1 millimeter is extruded, and be that 10-35 ℃ aqueous coagulation bath forms long filament by temperature, drawing-off doubly makes it have the certain physical mechanical performance through 1.5-6 in containing the aqueous solution that a kind of amide compound is a solvent again, washing, it is heat-treated after drying fibrous, thereby further promote the physical and mechanical properties of fiber; Fiber after heat treatment can curl, cuts off and pack.
In the method for the invention, pigment is to exist with particle and condensation product form in fiber after handling, and the maximum gauge of particle and condensation product has directly determined physical and mechanical properties and the spinning property and the back processing characteristics of fiber; The particle and the condensation product particle diameter that experiment showed, pigment are big more, and the spinning property of fiber is poor more, easy more lousiness, the fracture of wire phenomenon of occurring in the spinning process; When the maximum particle diameter of pigment in fiber is less than 5 microns, the physical and mechanical properties of fiber significantly better than the raw white meta-aramid fibers and dyeing after meta-aramid fibers; Among the present invention used pigment water insoluble, be insoluble in the organic solvent, do not have pigment to be lost in aqueous coagulation bath and other baths in the fiber production process.
Four, description of drawings
Fig. 1: specific embodiment of the invention continuous processing flow chart.
Five, the specific embodiment
Provide specific embodiments of the invention below in order to explanation the present invention, but should not regard limitation of the present invention as.
According to shown in Figure 1, present embodiment spun dyeing meta-aramid short fiber preparation method, implement according to following operation:
1, in a kind of amide compound is the system of organic solvent, carries out polymerisation in solution, use anhydrous NH with monomer m-phenylene diamine (MPD) and monomer m-phthaloyl chloride (IPC)
3Carry out preneutralization, filter the gained ammonium chloride, add IPC, neutralization for the second time, get spinning solution;
The spinning solution that adopts before the wet spinning is the less salt spinning solution, adds m-phthaloyl chloride when carrying out polymerisation at twice, makes logarithmic viscosity number 〉=2 of spinning solution;
A, for the first time add m-phthaloyl chloride after, control stoste viscosity adds anhydrous ammonia and carries out the hydrochloric acid that generates in the neutralization reaction, removes the ammonium chloride that neutralization reaction generates from the reactant mixture after the neutralization;
B, subsequently, in neutralization reaction solution, add m-phthaloyl chloride, and, making the spinning solution of less salt, and make logarithmic viscosity number 〉=2 of spinning solution by the amount of adjusting the m-phthaloyl chloride that adds with in calcium hydroxide, calcium oxide or other alkali compoundss and the acid that generates;
2, select suitable colouring agent, colouring agent preliminary treatment, colorant match, disperse the painted stoste of debita spissitudo;
Colouring agent is the pigment of organic or inorganic, and it is to keep Stability Analysis of Structures, nondiscolouring in the clock time in 300 ℃, 5 minutes that pigment satisfies in temperature; The amount of adding pigment in the fiber depends on the type of the used pigment of desired color harmony, and the amount of the pigment that adds in the fiber is 0.1-4% (percentage by weight); This pigment can be selected at least a in the following pigment, and these pigment are: AZO pigments, phthalocyanine pigment, heterocycle and condensed ring ketone pigment and some inorganic pigment, pigment be through after the milled processed, make its maximum gauge≤5 micron;
3, spinning solution mixes with proper proportion with the painted stoste of debita spissitudo;
Mix to obtain the spinning mixture of homogeneous 10% (weight) of painted stoste before wherein the poly polymer content is at least and spins with meeting the requirements of pigment and poly solution;
4, through wet spinning, cleaning, heat treatment, curl, cut off, packing;
With the spinning mixture deaeration and by diameter is that the spinning head of the spinneret orifice of 0.04-0.1 millimeter is extruded, and be that 10-35 ℃ aqueous coagulation bath forms long filament by temperature, drawing-off doubly makes it have the certain physical mechanical performance through 1.5-6 in containing the aqueous solution that a kind of amide compound is a solvent again, washing, it is heat-treated after drying fibrous, thereby further promote the physical and mechanical properties of fiber; Fiber after heat treatment can curl, cuts off and pack.
In the method for embodiment, pigment is to exist with particle and condensation product form in fiber after handling, and the maximum gauge of particle and condensation product has directly determined physical and mechanical properties and the spinning property and the back processing characteristics of fiber; The particle and the condensation product particle diameter that experiment showed, pigment are big more, and the spinning property of fiber is poor more, easy more lousiness, the fracture of wire phenomenon of occurring in the spinning process; When the maximum particle diameter of pigment in fiber was less than 5 microns, the physical and mechanical properties of fiber was significantly better than the meta-aramid fibers of raw white meta-aramid fibers and process poststaining; Among the present invention used pigment water insoluble, be insoluble in the selected organic solvent, do not have pigment to be lost in aqueous coagulation bath and other baths in the fiber production process.
Test and test
Logarithmic viscosity number: η
Inh=Ln (t
1/ t
2)/c
t
1: the delivery time (s) of solution in viscosimeter
t
2: the delivery time (s) of solvent in viscosimeter
C: the concentration of polymer solution (g/ml)
Polymer concentration: be this polymer of benchmark with this polymer solution gross weight weight %, i.e. (polymer weight/polymer dope gross weight) * 100%.
The physical index of fiber (line density, brute force, elongation, intensity) adopts LENZINGVIBROSKOP400C type filament line density tester and LENZING VIBRODYN400C type monofilament strength tester to test.
Table 1
| Test event | Unit | Fiber color | ||||
| Raw white | Painted navy before spinning | Painted Chinese red before spinning | Painted black before spinning | The poststaining navy | ||
| Specification | dtex× mm | 2.22×51 | 2.22×51 | 2.22×51 | 2.22×51 | 2.22×51 |
| Fiber number | dtex | 2.29 | 2.25 | 2.18 | 2.25 | 2.23 |
| Ultimate strength | CN | 9.32 | 10.8 | 11.53 | 12.51 | 8.90 |
| Extension at break | ％ | 30.7 | 34.3 | 35.56 | 33.80 | 30.0 |
| Fracture strength | CN/dtex | 4.07 | 4.8 | 5.32 | 5.57 | 3.99 |
Claims (10)
1, spun dyeing meta-aramid short fiber preparation method is characterized in that its operation is:
(1), synthesizing a kind of earlier is that solvent comprises the meta-aromatic polyamide solution that mpd-i is a repetitive with the amide compound, gets spinning solution;
(2), select suitable colouring agent, colouring agent preliminary treatment, colorant match, dispersion, the painted stoste of debita spissitudo;
(3), spinning solution is mixed with painted stoste;
(4), this mixed liquor is carried out wet spinning, be that 10-30 ℃ aqueous coagulation bath is to form endless tow by temperature;
(5), to its wash, oven dry, heat treatment and curl, cut off to make the meta-aramid staple fibre of original liquid coloring.
2,, it is characterized in that described solvent is selected from dimethyl formamide or dimethylacetylamide according to the described spun dyeing meta-aramid short fiber preparation method of claim 1.
3,, it is characterized in that described poly solution logarithmic viscosity number is at least 2 according to the described spun dyeing meta-aramid short fiber preparation method of claim 1.
4,, it is characterized in that described spinning solution makes by the following method according to the described spun dyeing meta-aramid short fiber preparation method of claim 1
In the system that with the amide compound is organic solvent, carry out polymerisation in solution, through preneutralization, filter, add IPC, neutralization for the second time, get spinning solution with monomer m-phthaloyl chloride and m-phenylene diamine (MPD);
This spinning solution is the less salt spinning solution, adds m-phthaloyl chloride when carrying out polymerisation at twice, makes logarithmic viscosity number 〉=2 of spinning solution;
A, for the first time add m-phthaloyl chloride after, control former fluid viscosity, add anhydrous ammonia and carry out the hydrochloric acid that generates in the neutralization reaction, from the reactant mixture after the neutralization, remove the ammonium chloride that generates after the neutralization reaction;
B, subsequently, add m-phthaloyl chloride in the solution after neutralization reaction, and, making the spinning solution of less salt, and make logarithmic viscosity number 〉=2 of spinning solution by the amount of adjusting the m-phthaloyl chloride that adds with in calcium hydroxide, calcium oxide or other alkali compoundss and the acid that generates.
5, according to the described spun dyeing meta-aramid short fiber preparation method of claim 1, it is characterized in that described colouring agent is the pigment of organic or inorganic, it is to keep Stability Analysis of Structures, nondiscolouring in the clock time in 300 ℃, 5 minutes that pigment satisfies in temperature;
The amount of adding pigment in the fiber depends on the type of the used pigment of desired color harmony, the amount of the pigment that adds in the fiber 0.1-4% that is weight percentage.
6, according to claim 1 or 5 described spun dyeing meta-aramid short fiber preparation methods, it is characterized in that described this pigment can select at least a in the following pigment: AZO pigments, phthalocyanine pigment, heterocycle and condensed ring ketone pigment and inorganic pigment, pigment is through after the milled processed, make its maximum gauge≤5 micron.
7,, it is characterized in that being preferably in the described AZO pigments benzimidazolone heterocyclic pigment according to the described spun dyeing meta-aramid short fiber preparation method of claim 6; Be copper phthalocyanine, halogenated copper phthalocyanine pigment preferably in the phthalocyanine pigment; Heterocycle and condensed ring ketone pigment are two mouthfuls of oxazines class pigment, 1 preferably, 4-diketopyrrolo-pyrrole class pigment.
8, according to the described spun dyeing meta-aramid short fiber preparation method of claim 1, it is characterized in that described spinning solution mixes with painted stoste, be to meet the requirements of pigment and poly solution to mix, before wherein the poly polymer content is at least and spins 10% of painted stoste weight to obtain the spinning mixture of homogeneous.
9, according to the described spun dyeing meta-aramid short fiber preparation method of claim 1, it is characterized in that described is to be that the spinning head of the spinneret orifice of 0.04-0.1 millimeter is extruded with the spinning mixture deaeration and by diameter through wet spinning, and be that 10-35 ℃ aqueous coagulation bath forms long filament by temperature, drawing-off doubly makes it have the certain physical mechanical performance through 1.5-6 in containing the aqueous solution that a kind of amide compound is a solvent again.
10, spun dyeing meta-aramid short fiber is characterized in that it being to make according to the described spun dyeing meta-aramid short fiber preparation method of arbitrary claim among the claim 1-9.
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| CN101876092A (en) * | 2010-07-16 | 2010-11-03 | 四川辉腾科技有限公司 | Method for producing polymetaphenylene isophthamide spinning solution |
| CN102154726A (en) * | 2011-05-23 | 2011-08-17 | 蓝星（成都）新材料有限公司 | Middle modulus poly (p-phenyl-terephthalamide) fiber and preparation method thereof |
| CN102400242A (en) * | 2011-11-21 | 2012-04-04 | 圣欧（苏州）安全防护材料有限公司 | Method for preparing colored poly-m-phenyleneisophthalamide (PMIA) fibers |
| CN102534839A (en) * | 2010-12-09 | 2012-07-04 | 烟台泰和新材料股份有限公司 | Method for preparing meta-aramid fiber |
| CN101611182B (en) * | 2006-12-15 | 2012-08-01 | 帝人高科技产品株式会社 | Heterocyclic ring-containing aromatic polyamide fiber, method for producing the same, fabric comprising the fiber, fiber-reinforced composite material reinforced with the fiber |
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|---|---|---|---|---|
| JPS6414317A (en) * | 1987-06-18 | 1989-01-18 | Du Pont | Colored aramid fiber |
| CN1027655C (en) * | 1988-08-01 | 1995-02-15 | 纳幕尔杜邦公司 | Colored aramid fibers |
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