CN105133319A - Preparation method of molten-drop-resisting polyamide fiber or fabric - Google Patents
Preparation method of molten-drop-resisting polyamide fiber or fabric Download PDFInfo
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- CN105133319A CN105133319A CN201510613344.4A CN201510613344A CN105133319A CN 105133319 A CN105133319 A CN 105133319A CN 201510613344 A CN201510613344 A CN 201510613344A CN 105133319 A CN105133319 A CN 105133319A
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- 239000004744 fabric Substances 0.000 title claims abstract description 113
- 239000000835 fiber Substances 0.000 title claims abstract description 108
- 239000004952 Polyamide Substances 0.000 title claims abstract description 51
- 229920002647 polyamide Polymers 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 239000000178 monomer Substances 0.000 claims abstract description 28
- 239000007864 aqueous solution Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 239000003112 inhibitor Substances 0.000 claims abstract description 10
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 9
- 229920001519 homopolymer Polymers 0.000 claims abstract description 5
- 150000001875 compounds Chemical class 0.000 claims abstract description 3
- 238000010894 electron beam technology Methods 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- CCJAYIGMMRQRAO-UHFFFAOYSA-N 2-[4-[(2-hydroxyphenyl)methylideneamino]butyliminomethyl]phenol Chemical compound OC1=CC=CC=C1C=NCCCCN=CC1=CC=CC=C1O CCJAYIGMMRQRAO-UHFFFAOYSA-N 0.000 claims description 7
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims description 7
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 7
- VLCAYQIMSMPEBW-UHFFFAOYSA-N methyl 3-hydroxy-2-methylidenebutanoate Chemical compound COC(=O)C(=C)C(C)O VLCAYQIMSMPEBW-UHFFFAOYSA-N 0.000 claims description 7
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 5
- 238000004132 cross linking Methods 0.000 claims description 5
- 150000001261 hydroxy acids Chemical group 0.000 claims description 5
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 4
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 4
- 239000011976 maleic acid Substances 0.000 claims description 4
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 238000002386 leaching Methods 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 2
- 239000004753 textile Substances 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000005855 radiation Effects 0.000 abstract description 4
- 230000006378 damage Effects 0.000 abstract description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract 1
- 238000005470 impregnation Methods 0.000 abstract 1
- 238000005096 rolling process Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 description 20
- 239000003610 charcoal Substances 0.000 description 15
- 238000002485 combustion reaction Methods 0.000 description 15
- 239000000463 material Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 239000011159 matrix material Substances 0.000 description 8
- 239000003063 flame retardant Substances 0.000 description 7
- 238000002844 melting Methods 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 229920000578 graft copolymer Polymers 0.000 description 4
- 238000012876 topography Methods 0.000 description 4
- 239000011260 aqueous acid Substances 0.000 description 3
- 230000001965 increasing effect Effects 0.000 description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 2
- 239000001099 ammonium carbonate Substances 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000012209 synthetic fiber Substances 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 239000004953 Aliphatic polyamide Substances 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 229920003231 aliphatic polyamide Polymers 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 201000007094 prostatitis Diseases 0.000 description 1
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- 230000002787 reinforcement Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 238000012549 training Methods 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a preparation method of molten-drop-resisting polyamide fiber or fabric. Under a normal temperature air condition, the fiber or fabric is radiated by virtue of electronic beams, then the fiber or fabric is placed into a monomer aqueous solution containing carboxyl groups to be under pre-reaction, and the fiber or fabric is enabled to be self-cross linked; then the fiber or fabric is padded in a polymerization inhibitor and a compound aqueous solution consisting of two monomers containing reactive double bonds, and the electronic beam radiation grafting is carried out after twice impregnation and twice rolling; after the grafting reaction is completed, the fiber or fabric can be boiled by virtue of treatment liquid so as to remove a grafted homopolymer to obtain the molten-drop-resisting polyamide fiber or fabric. The preparation method is simple and easy to operate and capable of implementing the industrialized production, and during a burning process of the prepared molten-drop-resisting polyamide fiber or fabric, a carbonized supporting layer can be rapidly formed on the surface of the fiber or fabric, so that the formation of molten drops is effectively inhibited, and the secondary harm caused by a high-temperature flame dropping object is avoided, and the situation threatening the human life can be prevented.
Description
Technical field
The present invention relates to the preparation method of a kind of fiber or fabric, especially relate to the preparation method of a kind of anti-dropping polyamide fiber or fabric.
Background technology
Polyamide fiber is a kind of synthetic fiber comparatively early realizing suitability for industrialized production, and its output occupies the prostatitis of each synthetic fiber always, has the performances such as good elasticity, brute force, rub resistance have a wide range of applications in relevant industries such as weavings because of it.
Along with the development of social production and people are to the higher pursuit of quality of the life, propose harsher requirement to traditional weaving composite fibre materials, as all required under a lot of occasion, it has certain fire resistance.Aliphatic polyamide fiber belongs to combustible, and the value of its limited oxygen index is approximately 20 ~ 21.5, with serious drip phenomenon during burning.These high temperature droppings easily ignite other material, accelerate flame propagation, expand fire scale; If dropping on human body skin to cause serious scald even to burn, bring secondary injury, significantly limit its underwear, protective clothing, military training clothes and some skyscrapers on application.
For the inflammable problem of fiber, carry out copolymerization or co-blended spinning by adding fire retardant in fiber synthesis phase or melt spinning process and flame-retardant after-finishing is carried out to fabric, can substantially realize the fire-retardant of fiber.But effective solution is not had for molten drop problem, and the fire-retardant mechanism of many products is all be based upon on the basis of molten drop on market, attempt by reducing fusing point, reinforcement melting drippage makes Combustion Source disengaging reach fire-retardant object, therefore the molten drop problem solved in fibrous material combustion process seems particularly urgent.
Preparation has polyamide fiber or the crucial mobility being to reduce melt in combustion process of fabric of anti-dropping effect, improve the intensity of melt, through the joint efforts of Chinese scholars, object that is glutinous, that become charcoal effect, reach anti-dropping in mechanism such as fiber surface formation supporting layer and change material structures can be increased by physics at present.The viscosity that polytetrafluorethylepowder powder, clay, talcum powder etc. increase melt as added in fiber, reduces the mobility of melt, although the method can reduce the number of molten drop, for the flammability of molten drop without improvement; Utilize the condensed phase charcoal forming machine of some fire retardants to manage, promote that matrix becomes charcoal in combustion, improve the anti-dropping performance of material, but there is fire-retardant FRW complex process, the problem that development cost is high.
Summary of the invention
The object of this invention is to provide the preparation method of a kind of anti-dropping polyamide fiber or fabric, the method have process evenly, efficiency is high, pollute less, technological process is simple and be easy to realize the features such as industrialization, prepared fiber or fabric anti-dropping excellent performance, stable and durable effect, washability is good.
The present invention adopts technical scheme as follows:
(1) under normal temperature air condition, synthetic polyamide fiber or fabric are carried out electron beam irradiation, the monomer solution put into immediately after irradiation containing hydroxy-acid group carries out pre-reaction at constant temperature 60 ~ 80 DEG C, makes, between polyamide molecule, self-crosslinking occurs;
(2) by the fiber after pre-reaction or textile pad at polymerization inhibitor with the compound water solution be made up of two kinds of monomers containing reactive double bond, after two leachings two are rolled, make the liquid carrying rate of described fiber or fabric be 60 ~ 100%, then carry out electron beam irradiation grafting;
Polymerization inhibitor adopts Fe
2sO
4, the mass percentage concentration of polymerization inhibitor is 0.05 ~ 0.15%; Two kinds of monomers containing reactive double bond are respectively a kind of and hydroxyethyl methylacrylate in acrylamide and N hydroxymethyl acrylamide and the one in hydroxypropyl acrylate, and the mass percentage concentration ratio between two kinds of monomers is respectively 10 ~ 20%:5 ~ 10%;
(3), after graft reaction completes, with treatment fluid fiber obtained above or fabric boiled and boil, to remove graft homopolymer, namely obtain described anti-dripping fibre or fabric.
In described step (1), thermostat temperature preferably can be 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C or 80 DEG C.
In described step (1), the irradiation dose of electron beam irradiation is 80 ~ 120kGy.Preferably can be 80kGy, 100kGy or 120kGy.
The preferred concentration of described polymerization inhibitor can be 0.05%, 0.10% or 0.15%.
Described two kinds of preferred concentration of monomer can be respectively 10%:5%, 10%:10%, 15%:5%, 15%:10%, 20%:5% or 20%:10%.
In described step (1), the described monomer containing hydroxy-acid group is the one in acrylic acid, methacrylic acid, maleic acid or itaconic acid, and the mass percentage concentration of monomer solution is 10%.
The pre-reaction of described step (1) is carried out in thermostat water bath, and reaction temperature is 60 ~ 80 DEG C.
Described step (2) two is soaked in two roll process, and the pressure between two roller is 0.1 ~ 0.3Mpa, specifically can be 0.1MPa, 0.2MPa or 0.3MPa, and rotating speed is 6m/min.
The irradiation dose of described step (2) electron beam irradiation graft reaction is 90 ~ 180kGy, preferably can be 90kGy, 135kGy or 180kGy.
Described treatment fluid is a kind of aqueous solution in NaOH, sodium carbonate, sodium bicarbonate, sodium phosphate, carbonic hydroammonium, and the mass percentage concentration for the treatment of fluid is 1 ~ 4%, preferably can be 1%, 2% or 4%.
Described fiber or fabric are fiber or the fabric of synthesizing polyamides.
Described fabric can be PURE YARN FABRIC or the BLENDED FABRIC of above-mentioned polyamide fiber, specifically can be woven fabric, knitted fabric and nonwoven fabric.
What the technical method adopted in the present invention realized the anti-dropping utilization of polyamide fiber or fabric is following principle: the class monomer containing hydroxy-acid group under certain reaction condition can promote being cross-linked between polyamide molecule, and cross-linked structure can realize the not melting of material; The graft polymers of monomer and the large intermolecular formation of polyamide in graft reaction, decomposing prior to matrix when being heated and forming coke layer is that fiber melt provides support, in addition, it also has the effect promoting that matrix becomes charcoal, the melting behavior of matrix material is converted into into charcoal process, can be specifically described by accompanying drawing in the embodiment of these principles below.
Mainly irradiation crosslinking technological is applied in anti-dropping aspect in existing radiation processing technology, by add crosslinking agent in material after, be aided with irradiation, material internal produced crosslinked, change thermosetting into by thermoplasticity, thus realize not melting, but mainly still concentrate on plastic industry at present.The present invention utilizes the inductive effect of electron beam to cause some monomers with charcoal effect to carry out graft reaction, promotes the one-tenth charcoal of matrix material, the melting behavior of matrix is converted into into charcoal process.Along with the maturation gradually of radiation processing technology, the application of the present invention in fabric modifying has very large potentiality.
The present invention compared to existing technology method creates following different know-why, has following beneficial effect:
The effect of anti-dropping depends on the grafting efficiency of monomer and the removal efficiency of grafting accessory substance to a great extent, mean and will improve monomer concentration, and concentration certainly will cause the autohemagglutination between monomer to aggravate while increasing, be unfavorable for the removal of grafting accessory substance, the method used in the present invention controls the generation of monomer homopolymers effectively, farthest improve the grafting efficiency of monomer, be mainly reflected in following three aspects:
A) the present invention uses the method for pre-irradiation to carry out cross-linking radiation to fiber or fabric, in the inventive method, monomer is not by the irradiation of electron beam, the probability that autohemagglutination occurs between monomer is low, because this reacting phase is to gentleness, can avoids excessively crosslinked between polyamide molecule and affect the serviceability of material;
B) the present invention introduces polymerization inhibitor first in grafting system, and the polymerization inhibitor obtaining described concentration by continuous experimental exploring can suppress the autohemagglutination between monomer effectively, improves the grafting efficiency of graft reaction;
C) to boil to the reaction fiber of gained or fabric with treatment fluid and boil, the removal efficiency of the method to monomer homopolymers is high, and the fiber processed or fabric have good feel.
The preparation method related in the present invention carries out after spinning, does not change the original production technology of fiber, and destroys less to fiber molecule agent structure, and cross-linking effect is better, farthest retains the original performance of fiber or fabric, as intensity, feel etc.; By covalently bound mode monomer introduced the persistence that ensure that modification in the side chain of fiber molecule.
Preparation method provided by the invention is simple, be easy to realize industrialization produce, the anti-dripping fibre of preparation or fabric in combustion surface energy form charing supporting layer fast, not molten drop, the harm that high temperature molten drop thing brings can be avoided, stop the situation jeopardizing people's life to occur.
Accompanying drawing explanation
Fig. 1 is the thermogravimetric curve figure of polyamide anti-dropping fabric prepared by the present invention.
Fig. 2 is the surface topography of residue after the polyamide anti-dropping fabric prepared of the present invention and calcination thereof.
Detailed description of the invention
Below in conjunction with drawings and Examples, the invention will be further described.
The experimental technique used in following embodiment if no special instructions, is conventional method.
Material used in following embodiment, reagent etc., as without Special Statement, all can obtain from commercial channels.
Percentage composition described in following embodiment is mass percentage.
Embodiments of the invention are as follows:
Embodiment 1:
Under normal temperature air condition, first electron beam irradiation is carried out to polyamide fiber, dosage is made to reach 80kGy, 10% acrylic acid aqueous solution put into immediately by fiber after irradiation, and 1h is reacted at 60 DEG C, reaction after washing is clean, and polyamide fiber, without obvious weightening finish, then pads at the Fe by the acrylamide of 10% and the hydroxyethyl methylacrylate of 5% and 0.05% by fiber
2sO
4mixed aqueous solution in a period of time, fiber is allowed to pass through padding machine, pressure between two roller is 0.3Mpa, make fiber liquid carrying rate reach 60%, then carry out electron beam irradiation grafting, make irradiation dose reach 135kGy, after irradiation grafting, with 1% sodium hydroxide solution fiber boiled and boils 20min, after washing clean, percent grafting is 11.4%.
In combustion, surface carbonizes rapidly the present embodiment gained fiber, does not drip, and illustrates that the fiber of preparation has the characteristic of anti-dropping.
Embodiment 2:
Under normal temperature air condition, first electron beam irradiation is carried out to polyamide fiber, dosage is made to reach 120kGy, 10% metering system aqueous acid put into immediately by fiber after irradiation, and 1h is reacted at 70 DEG C, reaction after washing is clean, and polyamide fiber, without obvious weightening finish, then pads at the Fe by the acrylamide of 12% and the hydroxypropyl acrylate of 8% and 0.05% by fiber
2sO
4mixed aqueous solution in a period of time, fiber is allowed to pass through padding machine, pressure between two roller is 0.2Mpa, make fiber liquid carrying rate reach 80%, then carry out electron beam irradiation grafting, make irradiation dose reach 180kGy, after irradiation grafting, with 2% sodium carbonate liquor fiber boiled and boils 20min, after washing clean, percent grafting is 15.6%.
In combustion, surface carbonizes rapidly the present embodiment gained fiber, does not drip, and illustrates that the fiber of preparation has the characteristic of anti-dropping.
Embodiment 3:
Under normal temperature air condition, first electron beam irradiation is carried out to polyamide fiber, dosage is made to reach 100kGy, the 10% itaconic acid aqueous solution put into immediately by fiber after irradiation, and 1h is reacted at 65 DEG C, reaction after washing is clean, and polyamide fiber, without obvious weightening finish, then pads at the Fe by the N hydroxymethyl acrylamide of 20% and the hydroxypropyl acrylate of 5% and 0.10% by fiber
2sO
4mixed aqueous solution in a period of time, fiber is allowed to pass through padding machine, pressure between two roller is 0.3Mpa, make fiber liquid carrying rate reach 60%, then carry out electron beam irradiation grafting, make irradiation dose reach 90kGy, after irradiation grafting, with 4% sodium bicarbonate solution fiber boiled and boils 20min, after washing clean, percent grafting is 13.4%.
In combustion, surface carbonizes rapidly the present embodiment gained fiber, does not drip, and illustrates that the fiber of preparation has the characteristic of anti-dropping.
Embodiment 4:
Under normal temperature air condition, first electron beam irradiation is carried out to polyamide fiber, dosage is made to reach 120kGy, 10% metering system aqueous acid put into immediately by fiber after irradiation, and 1h is reacted at 80 DEG C, reaction after washing is clean, and polyamide fiber, without obvious weightening finish, then pads at the Fe by the N hydroxymethyl acrylamide of 20% and the hydroxypropyl acrylate of 10% and 0.15% by fiber
2sO
4mixed aqueous solution in a period of time, fiber is allowed to pass through padding machine, pressure between two roller is 0.1Mpa, make fiber liquid carrying rate reach 100%, then carry out electron beam irradiation grafting, make irradiation dose reach 180kGy, after irradiation grafting, with 2% sodium radio-phosphate,P-32 solution fiber boiled and boils 20min, after washing clean, percent grafting is 19.1%.
In combustion, surface carbonizes rapidly the present embodiment gained fiber, does not drip, and illustrates that the fiber of preparation has the characteristic of anti-dropping.
Embodiment 5:
Under normal temperature air condition, first electron beam irradiation is carried out to polyamide fiber, dosage is made to reach 80kGy, 10% aqueous maleic acid put into immediately by fiber after irradiation, and 1h is reacted at 75 DEG C, reaction after washing is clean, and polyamide fiber, without obvious weightening finish, then pads at the Fe by the acrylamide of 10% and the hydroxyethyl methylacrylate of 10% and 0.05% by fiber
2sO
4mixed aqueous solution in a period of time, fiber is allowed to pass through padding machine, pressure between two roller is 0.1Mpa, make fiber liquid carrying rate reach 80%, then carry out electron beam irradiation grafting, make irradiation dose reach 135kGy, after irradiation grafting, with 1% ammonium bicarbonate soln fiber boiled and boils 20min, after washing clean, percent grafting is 14.6%.
In combustion, surface carbonizes rapidly the present embodiment gained fabric, does not drip, and illustrates that the fiber of preparation has the characteristic of anti-dropping.
Embodiment 6:
Under normal temperature air condition, first electron beam irradiation is carried out to polyamide fabric, dosage is made to reach 120kGy, fabric after irradiation puts into 10% metering system aqueous acid immediately, and 1h is reacted at 80 DEG C, reaction after washing is clean, and polyamide fabric, without obvious weightening finish, is then padded at the Fe by the N hydroxymethyl acrylamide of 20% and the hydroxyethyl methylacrylate of 5% and 0.10% by fabric
2sO
4mixed aqueous solution in a period of time, fabric is allowed to pass through padding machine, pressure between two roller is 0.3Mpa, make fabric liquid carrying rate reach 60%, then carry out electron beam irradiation grafting, make irradiation dose reach 135kGy, after irradiation grafting, with 4% ammonium bicarbonate soln fabric boiled and boils 20min, after washing clean, percent grafting is 16.7%.
In combustion, surface carbonizes rapidly the present embodiment gained fabric, does not drip, and illustrates that the fabric of preparation has the characteristic of anti-dropping.
Embodiment 7:
Under normal temperature air condition, first electron beam irradiation is carried out to polyamide fabric, dosage is made to reach 120kGy, fabric after irradiation puts into the 10% itaconic acid aqueous solution immediately, and 1h is reacted at 60 DEG C, reaction after washing is clean, and polyamide fabric, without obvious weightening finish, is then padded at the Fe by the acrylamide of 14% and the hydroxyethyl methylacrylate of 6% and 0.10% by fabric
2sO
4mixed aqueous solution in a period of time, fabric is allowed to pass through padding machine, pressure between two roller is 0.2Mpa, make fabric liquid carrying rate reach 80%, then carry out electron beam irradiation grafting, make irradiation dose reach 135kGy, after irradiation grafting, with 4% sodium bicarbonate solution fabric boiled and boils 20min, after washing clean, percent grafting is 16.3%.
In combustion, surface carbonizes rapidly the present embodiment gained fabric, does not drip, and illustrates that the fabric of preparation has the characteristic of anti-dropping.
Embodiment 8:
Under normal temperature air condition, first electron beam irradiation is carried out to polyamide fabric, dosage is made to reach 80kGy, fabric after irradiation puts into 10% acrylic acid aqueous solution immediately, and 1h is reacted at 65 DEG C, reaction after washing is clean, and polyamide fabric, without obvious weightening finish, is then padded at the Fe by the N hydroxymethyl acrylamide of 20% and the hydroxypropyl acrylate of 10% and 0.15% by fabric
2sO
4mixed aqueous solution in a period of time, fabric is allowed to pass through padding machine, pressure between two roller is 0.1Mpa, make fabric liquid carrying rate reach 100%, then carry out electron beam irradiation grafting, make irradiation dose reach 180kGy, after irradiation grafting, with 2% sodium radio-phosphate,P-32 solution fabric boiled and boils 20min, after washing clean, percent grafting is 19.7%.
In combustion, surface carbonizes rapidly the present embodiment gained fabric, does not drip, and illustrates that the fabric of preparation has the characteristic of anti-dropping.
Embodiment 9:
Under normal temperature air condition, first electron beam irradiation is carried out to polyamide fabric, dosage is made to reach 100kGy, fabric after irradiation puts into 10% aqueous maleic acid immediately, and 1h is reacted at 75 DEG C, reaction after washing is clean, and polyamide fabric, without obvious weightening finish, is then padded at the Fe by the acrylamide of 10% and the hydroxypropyl acrylate of 5% and 0.05% by fabric
2sO
4mixed aqueous solution in a period of time, fabric is allowed to pass through padding machine, pressure between two roller is 0.1Mpa, make fabric liquid carrying rate reach 100%, then carry out electron beam irradiation grafting, make irradiation dose reach 180kGy, after irradiation grafting, with 1% sodium hydroxide solution fabric boiled and boils 20min, after washing clean, percent grafting is 13.3%.
In combustion, surface carbonizes rapidly the present embodiment gained fabric, does not drip, and illustrates that the fabric of preparation has the characteristic of anti-dropping.
Embodiment 10:
Under normal temperature air condition, first electron beam irradiation is carried out to polyamide fabric, dosage is made to reach 80kGy, fabric after irradiation puts into 10% acrylic acid aqueous solution immediately, and 1h is reacted at 70 DEG C, reaction after washing is clean, and polyamide fabric, without obvious weightening finish, is then padded at the Fe by the N hydroxymethyl acrylamide of 10% and the hydroxyethyl methylacrylate of 10% and 0.05% by fabric
2sO
4mixed aqueous solution in a period of time, fabric is allowed to pass through padding machine, pressure between two roller is 0.3Mpa, make fabric liquid carrying rate reach 60%, then carry out electron beam irradiation grafting, make irradiation dose reach 90kGy, after irradiation grafting, with 2% sodium carbonate liquor fabric boiled and boils 20min, after washing clean, percent grafting is 11.2%.
In combustion, surface carbonizes rapidly the present embodiment gained fabric, does not drip, and illustrates that the fabric of preparation has the characteristic of anti-dropping.
As shown in Figure 1, wherein square represents polyamide fabric former state to the thermogravimetric curve of anti-dropping fabric sample prepared in above-described embodiment 8, and triangle represents the fabric sample prepared in the present embodiment; In prepared anti-dropping fabric sample fiber surface topography and in high temperature Muffle furnace calcination gained residue after 20 minutes surface topography as shown in Figure 2, wherein (a) and (c) is fabric former state, (b) and (d) fabric sample for preparing in the present embodiment.
As can be seen from the thermogravimetric curve of Fig. 1 fabric sample, the temperature of initial decomposition of fabric former state is at 372 DEG C, in the present embodiment, fabric sample temperature of initial decomposition is advanced to 173 DEG C, mainly the decomposition in advance of graft polymers causes, the introducing of graft polymers facilitates the decomposition of matrix, in addition, the charcoal residual rate of sample at 800 DEG C is increased to 8.6% by 3.5% of fabric former state, increase 1.5 times, show the fabric sample using the preparation method in this patent to prepare, its carbon-forming performance obviously promotes, most for matrix melting behavior can be converted into harmless one-tenth charcoal process.
Fiber in the anti-dropping fabric of preparation in embodiment 8 is observed surface topography under a scanning electron microscope, as can be seen from Fig. 2 (a), for fabric former state, its fiber surface is smooth and smooth, arrange loose between fiber, interfibrous space is high-visible.And in sample after grafting, as shown in Fig. 2 (b), fiber surface becomes coarse and covers has gone up one deck graft polymers, between fiber, had the trend of entanglement, arranging situation also more non-grafting time more tight.Can find out the layer of charcoal surface relatively flat of fabric former state from Fig. 2 (c), layer of charcoal intensity of loosening is not high.For grafting samples, as shown in Fig. 2 (d), layer of charcoal surface presentation goes out similar cellular cross-linked structure, illustrate that the fabric sample inside in the present embodiment there occurs crosslinked, and layer of charcoal is more closely abundant, cross-linked structure can improve the intensity of layer of charcoal, for fiber melt provides a supporting role, suppress its melting to be dripped, more than it serves to show that the present invention has outstanding significant technique effect.
The specific embodiment of above-mentioned detailed description of the invention is used for explaining and the present invention is described, but not limits the invention, and in the protection domain of spirit of the present invention and claim, any amendment make the present invention and change, all fall into protection scope of the present invention.
Claims (9)
1. a preparation method for anti-dropping polyamide fiber or fabric, comprises the steps:
(1) under normal temperature air condition, synthetic polyamide fiber or fabric are carried out electron beam irradiation, the monomer solution put into immediately after irradiation containing hydroxy-acid group carries out pre-reaction at constant temperature 60 ~ 80 DEG C, makes, between polyamide molecule, self-crosslinking occurs;
(2) fiber after pre-reaction or textile pad are being added in the compound water solution be made up of two kinds of monomers containing reactive double bond by polymerization inhibitor, after two leachings two are rolled, make the liquid carrying rate of described fiber or fabric be 60 ~ 100%, then carry out electron beam irradiation grafting;
Polymerization inhibitor adopts Fe
2sO
4, the mass percentage concentration of polymerization inhibitor is 0.05 ~ 0.15%; Two kinds of monomers containing reactive double bond are respectively a kind of and hydroxyethyl methylacrylate in acrylamide and N hydroxymethyl acrylamide and the one in hydroxypropyl acrylate, and the mass percentage concentration ratio between two kinds of monomers is respectively 10 ~ 20%:5 ~ 10%;
(3), after graft reaction completes, with treatment fluid fiber obtained above or fabric boiled and boil, to remove graft homopolymer, namely obtain described anti-dripping fibre or fabric.
2. the preparation method of a kind of anti-dropping polyamide fiber according to claim 1 or fabric, is characterized in that: in described step (1), the irradiation dose of electron beam irradiation is 80 ~ 120kGy.
3. the preparation method of a kind of anti-dropping polyamide fiber according to claim 1 or fabric, it is characterized in that: in described step (1), the described monomer containing hydroxy-acid group is the one in acrylic acid, methacrylic acid, maleic acid or itaconic acid, and the mass percentage concentration of monomer solution is 10%.
4. the preparation method of a kind of anti-dropping polyamide fiber according to claim 1 or fabric, it is characterized in that: the pre-reaction of described step (1) is carried out in thermostat water bath, reaction temperature is 60 ~ 80 DEG C.
5. the preparation method of a kind of anti-dropping polyamide fiber according to claim 1 or fabric, is characterized in that: described step (2) two is soaked in two roll process, and the pressure between two roller is 0.1 ~ 0.3Mpa, and rotating speed is 6m/min.
6. the preparation method of a kind of anti-dropping polyamide fiber according to claim 1 or fabric, is characterized in that: the irradiation dose of described step (2) electron beam irradiation graft reaction is 90 ~ 180kGy.
7. the preparation method of a kind of anti-dropping polyamide fiber according to claim 1 or fabric, it is characterized in that: described treatment fluid is a kind of aqueous solution in NaOH, sodium carbonate, sodium bicarbonate, sodium phosphate, carbonic hydroammonium, the mass percentage concentration for the treatment of fluid is 1 ~ 4%.
8. the preparation method of a kind of anti-dropping polyamide fiber according to claim 1 or fabric, is characterized in that: described fabric is PURE YARN FABRIC or the BLENDED FABRIC of polyamide fiber.
9. the anti-dripping fibre prepared according to described method arbitrary in claim 1-8 or fabric.
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| CN107177979A (en) * | 2017-06-30 | 2017-09-19 | 四川东材科技集团股份有限公司 | One kind is without molten drop flame retardant polyester fiber/fabric and preparation method thereof |
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