CN102154725A - Ultrahigh flame-retardant AN-VDC copolymer fiber and production method thereof - Google Patents
Ultrahigh flame-retardant AN-VDC copolymer fiber and production method thereof Download PDFInfo
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- CN102154725A CN102154725A CN 201110046972 CN201110046972A CN102154725A CN 102154725 A CN102154725 A CN 102154725A CN 201110046972 CN201110046972 CN 201110046972 CN 201110046972 A CN201110046972 A CN 201110046972A CN 102154725 A CN102154725 A CN 102154725A
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Abstract
The invention discloses an ultrahigh flame-retardant AN-VDC copolymer fiber and a production method thereof. Chemical compositions of the copolymer fiber contain acrylonitrile, vinylidene chloride, acrylamide methyl propane sodium sulfonate, antimony peroxide and decabromdiphenylethane, wherein the weight ratio of the antimony peroxide in the fiber is 6.5 to 10%, and the weight ratio of the decabromdiphenylethane in the fiber is 5.5 to 10%. The production method of the fiber comprises the following steps of: fully mixing the decabromdiphenylethane, a polymerizing liquid and dimethyl fomamide which are ground and filtered to be prepared into a decabromdiphenylethane solution; adding an antimony peroxide colloidal solution and a dimethyl fomamide aqueous solution into polymerizing liquid undegoing demonomerisation, filtering the mixed liquor after being fully mixed, and then continuously adding the prepared decabromdiphenylethane solution on line to the mixed liquor, and finally sending the mixed liquor to a spinning working procedure. As the ultrahigh flame-retardant AN-VDC copolymer fiber has excellent fire resistance, environmental protection and combination properties, the fiber is increasingly and widely applied in various fields, in particular to the field of a specific flame-retardant fabric.
Description
Technical field:
The present invention relates to a kind of polyacrylic and polyester fiber, relate in particular to fire-retardant polyacrylic and polyester fiber of a kind of superelevation and its production method.
Background technology:
Polyacrylic and polyester fiber claims modified acrylic fibres again, be meant that acrylonitrile content (refers to weight content ratio, with implication hereinafter herewith) be 35～85% fibre-forming material, its chemical constitution is to be formed by acrylonitrile (ACN) monomer, vinylidene chloride (VDC) monomer and acrylamido methyl propane sulfonic acid sodium (SAMPS) monomer three copolymerization.Characteristics of polyacrylic and polyester fiber are the natural soft hand feeling with similar natural fabric, excellent water imbibition performance and good comfort, and the physical property of its wool type fiber is similar to animal wool, and feel is smooth, resilience good, warmth retention property is better than wool; It is that dyeability is also very good that polyacrylic and polyester fiber also has characteristics, and its dye uptake height, lovely luster, COLOR FASTNESS are good, sun-resistant; Another characteristics of polyacrylic and polyester fiber are that chemical stability is good, have excellent acid alkalescence and anti-other chemical agent performance; And the maximum characteristics of polyacrylic and polyester fiber are to possess excellent flame-retardant, its limited oxygen index (refer to textile fabric in the mist of oxygen and nitrogen, keep the burning required oxygen concentration lowest percentage, abbreviation LOI) reach 26-30%, and general burnable fiber has only 21-24% (the limited oxygen index numerical value of each fibrid sees the following form):
Because polyacrylic and polyester fiber possesses above-mentioned many distinctive advantages, therefore it is not only a kind of grade textiles fiber, also be a kind of functional fiber simultaneously, so not only be widely used in household textiles, Fake Furs, insulation garment, carpet etc. at home and abroad, but also be used to flame-retardant textile such as aviation blanket, cabin cover for seat, interior trim and high-performance apparel, filter cloth, parasols etc., even as the interpolation material of accumulator plate.
The main body of polyacrylic and polyester fiber molecular structure is acrylonitrile (ACN), in order to improve fire resistance, in polymer, added vinylidene chloride (VDC) as second monomer, in order to improve dyeability, in polymer, added acrylamido methyl propane sulfonic acid sodium (SAMPS) again as the 3rd monomer.Three kinds of monomers of polymer are not that ternary directly is polymerized, but by ACN and VDC polymerization, ACN and SAMPS polymerization obtain polymer " V " and " S " respectively, and two kinds of polymer are mixed into the MDC polymer fluid again.Polymerization process and spinning process all with dimethyl formamide (DMF) as solvent, therefore polymerization process is a homogeneous reaction, ACN, the VDC monomer of failing in the course of reaction to participate in reacting are reclaimed use after thin film evaporator takes off list, the polymer solution of gained enters spinning process after filtering, obtains finished fiber.
It is owing to added vinylidene in its macromolecular structure that polyacrylic and polyester fiber possesses fire resistance, promptly contains the chlorine element, so it has permanent fire retardant.The fire resistance of polyacrylic and polyester fiber is relevant with the content of chlorine element, and content of Cl element is high more, and its LOI (limited oxygen index) value is also high more, and fire resistance is just good more.For further improving the fire resistance of fiber, just need improve constantly the content of Cl element in the fiber, that is to say the addition that will improve vinylidene in the polymer.Along with the consumption that increases vinylidene, though the limited oxygen index of fiber (LOI) value can increase, the gloss of fiber, feel, dyeability and spinning property but obviously descend, thereby have a strong impact on the quality of polyacrylic and polyester fiber.Therefore, improve the method for fiber anti-flammability, under the prerequisite that does not influence fiber quality, have certain limitation with the content that improves chlorine element in the fiber.At present, the main method that improves the polyacrylic and polyester fiber fire resistance is to add Diantimony Pentoxide Colloid solution in the polyacrylic and polyester fiber polymer fluid, utilize the cooperative flame retardant effect of chloro-antimony to improve the LOI of fiber, increase along with antimony pentoxide content, the LOI of fiber also increases gradually, but be increased to a certain amount of after, just not obvious to the impact effect of fiber LOI, the highest of the LOI value of fiber reaches 32%.
Progress along with expanding economy and science and technology, the Application Areas of polyacrylic and polyester fiber is more and more wideer, the market potential is increasing to the demand of flame retardant polyacrylic and polyester fiber, but the requirement to quality is also harsh more, especially higher in the job that requires special skills field to the requirement of fire resistance, along with the terminal use is more and more higher to the requirement of the combination property of fabric, the ratio of BLENDED FABRIC is increasing, for under the prerequisite that guarantees the fabrics flame resistance performance, strengthen blending rate with other fiber, just must the higher fire resistance fibre of operating limit oxygen index (OI), thereby the polyacrylic and polyester fiber that development has a better anti-flammability has just become urgent task.
Summary of the invention:
Technical problem to be solved by this invention is to overcome common polyacrylic and polyester fiber to improve the difficulty that fire resistance is limited to, provide a kind of superelevation fire-retardant polyacrylic and polyester fiber, not only contain antimony pentoxide in its copolymer, and contain TDE, thereby increase substantially its limited oxygen index, and in the fortifying fibre fire resistance, keep other performance of fiber.
The present invention's another technical problem to be solved simultaneously provides a kind of new production method of making the fire-retardant polyacrylic and polyester fiber of above-mentioned superelevation.
In order to solve the problems of the technologies described above, the technical scheme that the present invention takes is:
The fire-retardant polyacrylic and polyester fiber of a kind of superelevation contains acrylonitrile, vinylidene chloride and acrylamido methyl propane sulfonic acid sodium in the chemical analysis of its copolymerization, it is characterized in that: also contain antimony pentoxide and TDE in the copolymerization chemical analysis of described fiber.
In the fire-retardant polyacrylic and polyester fiber of superelevation of the present invention, described antimony pentoxide contained weight ratio in fiber is 6.5～10%, and described TDE contained weight ratio in fiber is 5.5～10%.
A kind of production method of making the fire-retardant polyacrylic and polyester fiber of described superelevation includes and takes off single and the filtration operation, it is characterized in that: TDE, polymer fluid and dimethyl formamide are fully mixed, and be prepared into TDE solution by grinding and filtration; Add the Diantimony Pentoxide Colloid solution and the dimethyl formamide aqueous solution in the polymer fluid after taking off list, filter after fully mixing, on-line continuous adds the above-mentioned TDE solution that is prepared into then, delivers to spinning process at last.
In the production method of the fire-retardant polyacrylic and polyester fiber of manufacturing superelevation of the present invention, the raw material for preparing described TDE solution is 40～60 kilograms of 40～50 kilograms of TDEs, 50～70 kilograms of polymer fluids and dimethyl formamides; The hybrid technique step of adding Diantimony Pentoxide Colloid solution is:
(1) starts vacuum system, make basin be in negative pressure state;
(2) barreled Diantimony Pentoxide Colloid solution is pumped in the basin, basin is forced into 1.1Mpa;
(3) with Diantimony Pentoxide Colloid solution through electromagnetic flowmeter, be added in the impeller by certain ratio, fully mix with the polymer fluid and the dimethyl formamide aqueous solution;
(4) polymer fluid that will be mixed with antimony pentoxide filters.
Compare with existing flame retardant polyacrylic and polyester fiber, not not being both of the fire-retardant polyacrylic and polyester fiber of superelevation of the present invention, flame retardant polyacrylic and polyester fiber is by contain the limited oxygen index that antimony pentoxide improves fiber in fiber-forming polymer, and the fire-retardant polyacrylic and polyester fiber of superelevation not only contains the fire retardant antimony pentoxide, but also contain another TDE, thereby the cooperative flame retardant effect of utilizing chloro-bromo-antimony has increased substantially the limited oxygen index (LOI) of fiber, its peak has surpassed 36%, thereby greatly promoted the fire resistance of described polyacrylic and polyester fiber, and make it to have permanent, the fire resistance of fiber manufactured goods can or permanent do not used etc. former thereby changes to some extent because of washing; Meanwhile, owing to do not improve the content of chlorine, so other performance indications of the fire-retardant polyacrylic and polyester fiber of superelevation have still kept original level, performance indications that have such as whiteness dyeability etc. are also significantly better than flame retardant polyacrylic and polyester fiber.The following table of comparisons has provided the fire-retardant polyacrylic and polyester fiber of described superelevation that obtains by conventional detection and the performance numerical value of flame retardant polyacrylic and polyester fiber:
| Index | The high flame retardant fiber | The superelevation fire resistance fibre |
| Whiteness | 90 | 92 |
| Dye uptake % | 90 | 96 |
| LOI％ | 32 | 36 |
What the production method of the fire-retardant polyacrylic and polyester fiber of manufacturing superelevation of the present invention was different with the production method of flame retardant polyacrylic and polyester fiber is, after in taking off single polymer fluid, adding antimony pentoxide, before entering spinning machine, increased the operation of on-line continuous adding TDE, make fire retardant Diantimony Pentoxide Colloid solution and TDE solution be evenly distributed in fibrous inside, thereby make described flame retardant polyacrylic and polyester fiber possess permanent superelevation fire resistance.
Beneficial effect of the present invention is, add TDE and Diantimony Pentoxide Colloid solution in the polymer fluid after taking off list, make it to mate with fiber-forming polymer, utilize the cooperative flame retardant effect of chloro-bromo-antimony, significantly improved the fire resistance of fiber, be the limited oxygen index of fiber, other performance indications still remain unchanged simultaneously, even significantly better than common fire resistance fibre.
Description of drawings:
Fig. 1 is the flow sheet of the fire-retardant polyacrylic and polyester fiber of superelevation of the present invention.
The specific embodiment:
The invention will be further described below in conjunction with specific embodiments and the drawings.
See also the flow sheet of the fire-retardant polyacrylic and polyester fiber of Fig. 1 superelevation of the present invention.
The production procedure of the fire-retardant polyacrylic and polyester fiber of superelevation of the present invention is divided into following five steps:
The first step, the preparation polymer fluid
In copolyreaction, based on acrylonitrile (ACN) first monomer, to improve anti-flammability, acrylamido methyl propane sulfonic acid sodium (SAMPS) is that the 3rd monomer is to improve dyeability to vinylidene chloride (VDC) as second monomer; By ACN and VDC, ACN and SAMPS polymerization respectively, obtain polymer " V " and " S " during reaction, two kinds of polymer are mixed into polymer fluid again.
Second step, preparation TDE solution
1, with TDE 40-50 kilogram, polymer fluid 50-70 kilogram, dimethyl formamide (DMF) 40-60 kilogram joins in the dispersion machine and fully mixes;
2, the mixed liquor that the 1st step was made ground 3-4 hour by sand mill;
3, the solution after will grinding filters and makes TDE solution.
In the 3rd step, add antimony pentoxide solution
The polymer fluid prepared by first step polymerisation enters thin film evaporator, sees also Fig. 1, after taking off single operation, enters impeller and adds Diantimony Pentoxide Colloid solution and dimethyl formamide (DMF) aqueous solution, filters after fully mixing;
The Diantimony Pentoxide Colloid solution that is added meets following requirement:
Granularity :≤0.02 micron
Density: 1.83 gram per centimeters
3
PH value: 4～6
Antimony pentoxide content: 48%
The moisture of polymer fluid is controlled at≤and 3%, the dried content of polymer fluid is controlled at≤and 23.5%;
The technological operation step of adding Diantimony Pentoxide Colloid solution is as follows:
(1) starts vacuum system, make basin be in negative pressure state;
(2) barreled Diantimony Pentoxide Colloid solution is pumped in the basin, basin is forced into 1.1Mpa;
(3) with Diantimony Pentoxide Colloid solution through electromagnetic flowmeter, be added in the impeller by certain ratio, fully mix with the polymer fluid and the DMF aqueous solution;
(4) polymer fluid that will be mixed with antimony pentoxide filters.
In the 4th step, add TDE solution
Before the polymer fluid of making through the 3rd step that contains antimony pentoxide is entering spinning process, add to on-line continuous the TDE solution that is prepared into by above-mentioned second step in proportion, the content that makes TDE in the fiber is 5.5～10%.
In the 5th step, be spun into the fire-retardant polyacrylic and polyester fiber of superelevation
To deliver to spinning machine through the polymer fluid that contains antimony pentoxide and TDE that the 4th step made at last and carry out spinning.
Except that the operation of above-mentioned interpolation antimony pentoxide and TDE, the technological parameter of other each production process still routinely polyacrylic and polyester fiber production be provided with and operate.
Contain acrylonitrile, vinylidene chloride, acrylamido methyl propane sulfonic acid sodium, antimony pentoxide and TDE in the copolymerization chemical analysis according to the fire-retardant polyacrylic and polyester fiber of superelevation of the present invention of aforementioned production method manufacturing, described antimony pentoxide contained weight ratio in fiber is 6.5～10%, described TDE contained weight ratio in fiber is 5.5～10%, and above-mentioned each composition is evenly distributed.
Because the cooperative flame retardant effect of chloro-bromo-antimony, the present invention has significantly improved the fire resistance of the fire-retardant polyacrylic and polyester fiber of described superelevation, its limited oxygen index value reaches as high as 36.4%, simultaneously, owing to do not improve the content of chlorine, so other performance indications of the fire-retardant polyacrylic and polyester fiber of described superelevation still can be kept the quality level of common Vinyon N fire resistance fibre, the index that has even can exceed previous level.
It below is the embodiment of the invention of fire retardant different content.
Example 1:
The contained weight ratio % 6.5 of antimony pentoxide in the fiber
The contained weight ratio % 6.5 of TDE in the fiber
Fiber limited oxygen index measured value: 35.8
Example 2:
The contained weight ratio % 7 of antimony pentoxide in the fiber
The contained weight ratio % 6.5 of TDE in the fiber
Fiber limited oxygen index measured value: 36.4
Example 3:
The contained weight ratio % 10 of antimony pentoxide in the fiber
The contained weight ratio % 6.5 of TDE in the fiber
Fiber limited oxygen index measured value: 36.4
Example 4:
The contained weight ratio % 6.5 of antimony pentoxide in the fiber
The contained weight ratio % 5.5 of TDE in the fiber
Fiber limited oxygen index measured value: 35.2
Example 5:
The contained weight ratio % 6.5 of antimony pentoxide in the fiber
The contained weight ratio % 7 of TDE in the fiber
Fiber limited oxygen index measured value: 36.4
Example 6:
The contained weight ratio % 6.5 of antimony pentoxide in the fiber
The contained weight ratio % 10 of TDE in the fiber
Fiber limited oxygen index measured value: 36.4
The fire-retardant polyacrylic and polyester fiber of superelevation of the present invention is on the index basis that keeps flame retardant polyacrylic and polyester, increased substantially the fire resistance of fiber, its good anti-flammability, the feature of environmental protection and combination property have satisfied the requirement that the user improves constantly the flame-retardant textile performance, thereby have obtained increasingly extensive application in every field.
Claims (5)
1. the fire-retardant polyacrylic and polyester fiber of superelevation contains acrylonitrile, vinylidene chloride and acrylamido methyl propane sulfonic acid sodium in the chemical analysis of its copolymerization, it is characterized in that: also contain antimony pentoxide and TDE in the copolymerization chemical analysis of described fiber.
2. the fire-retardant polyacrylic and polyester fiber of superelevation according to claim 1 is characterized in that: described antimony pentoxide contained weight ratio in fiber is 6.5～10%, and described TDE contained weight ratio in fiber is 5.5～10%.
3. production method of making claim 1 or the fire-retardant polyacrylic and polyester fiber of 2 described superelevation, include and take off single and the filtration operation, it is characterized in that: TDE, polymer fluid and dimethyl formamide are fully mixed, and be prepared into TDE solution by grinding and filtration; Add the Diantimony Pentoxide Colloid solution and the dimethyl formamide aqueous solution in the polymer fluid after taking off list, filter after fully mixing, on-line continuous adds the above-mentioned TDE solution that is prepared into then, delivers to spinning process at last.
4. the production method of the fire-retardant polyacrylic and polyester fiber of manufacturing superelevation according to claim 3 is characterized in that: the raw material for preparing described TDE solution is 40～60 kilograms of 40～50 kilograms of TDEs, 50～70 kilograms of polymer fluids and dimethyl formamides.
5. the production method of the fire-retardant polyacrylic and polyester fiber of manufacturing superelevation according to claim 3 is characterized in that: the hybrid technique step of adding Diantimony Pentoxide Colloid solution is:
(1) starts vacuum system, make basin be in negative pressure state;
(2) barreled Diantimony Pentoxide Colloid solution is pumped in the basin, basin is forced into 1.1Mpa;
(3) with Diantimony Pentoxide Colloid solution through electromagnetic flowmeter, be added in the impeller by certain ratio, fully mix with the polymer fluid and the dimethyl formamide aqueous solution;
(4) polymer fluid that will be mixed with antimony pentoxide filters.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104558392B (en) * | 2013-10-29 | 2016-08-31 | 台湾塑胶工业股份有限公司 | Manufacturing method of highly flame-retardant modified polyacrylonitrile, and flame-retardant fiber |
| CN106835318A (en) * | 2017-02-20 | 2017-06-13 | 南通市中和化纤有限公司 | The cellular porous MnO of high magnification2Composite nano fiber |
| CN115652461A (en) * | 2022-10-24 | 2023-01-31 | 南通谐好安全科技有限公司 | Flame-retardant acrylic fiber and preparation process and application thereof |
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| US4285900A (en) * | 1979-03-09 | 1981-08-25 | Snia Viscosa Societa' Nazionale Industria Applicazioni Viscosa S.P.A. | Process for manufacturing modacrylic fibers having high luster, thermal stability and flame resistance |
| CN1455034A (en) * | 2002-04-29 | 2003-11-12 | 中国石油化工股份有限公司 | Fire resistant acrylonitrile copolymer fiber and manufacturing method thereof |
| CN101021018A (en) * | 2007-03-09 | 2007-08-22 | 抚顺惠抚阻燃纤维有限公司 | Flame retardant polyacrylic and polyester fiber and its production process |
| CN101475717A (en) * | 2008-01-04 | 2009-07-08 | 金发科技股份有限公司 | Flame-retardant polypropelene composition and preparation thereof |
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2011
- 2011-02-25 CN CN 201110046972 patent/CN102154725A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4285900A (en) * | 1979-03-09 | 1981-08-25 | Snia Viscosa Societa' Nazionale Industria Applicazioni Viscosa S.P.A. | Process for manufacturing modacrylic fibers having high luster, thermal stability and flame resistance |
| CN1455034A (en) * | 2002-04-29 | 2003-11-12 | 中国石油化工股份有限公司 | Fire resistant acrylonitrile copolymer fiber and manufacturing method thereof |
| CN101021018A (en) * | 2007-03-09 | 2007-08-22 | 抚顺惠抚阻燃纤维有限公司 | Flame retardant polyacrylic and polyester fiber and its production process |
| CN101475717A (en) * | 2008-01-04 | 2009-07-08 | 金发科技股份有限公司 | Flame-retardant polypropelene composition and preparation thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104558392B (en) * | 2013-10-29 | 2016-08-31 | 台湾塑胶工业股份有限公司 | Manufacturing method of highly flame-retardant modified polyacrylonitrile, and flame-retardant fiber |
| CN106835318A (en) * | 2017-02-20 | 2017-06-13 | 南通市中和化纤有限公司 | The cellular porous MnO of high magnification2Composite nano fiber |
| CN115652461A (en) * | 2022-10-24 | 2023-01-31 | 南通谐好安全科技有限公司 | Flame-retardant acrylic fiber and preparation process and application thereof |
| CN115652461B (en) * | 2022-10-24 | 2024-03-12 | 南通谐好安全科技有限公司 | Flame-retardant acrylic fiber and preparation process and application thereof |
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Application publication date: 20110817 |