CN108589269A - A kind of special stiffening agent of cotton fabric - Google Patents
A kind of special stiffening agent of cotton fabric Download PDFInfo
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- CN108589269A CN108589269A CN201810397870.5A CN201810397870A CN108589269A CN 108589269 A CN108589269 A CN 108589269A CN 201810397870 A CN201810397870 A CN 201810397870A CN 108589269 A CN108589269 A CN 108589269A
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- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/80—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with boron or compounds thereof, e.g. borides
- D06M11/81—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with boron or compounds thereof, e.g. borides with boron; with boron halides; with fluoroborates
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- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/02—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of natural origin
- D06M14/04—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of natural origin of vegetal origin, e.g. cellulose or derivatives thereof
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/327—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
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- D06M23/12—Processes in which the treating agent is incorporated in microcapsules
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Abstract
The invention discloses a kind of special stiffening agents of cotton fabric, belong to macromolecule polymeric material technical field.It counts in parts by weight, 80~120 parts of mix monomers are weighed successively, 0.5~2.0 part of initiator, 8~15 parts of emulsifiers, 70~100 parts of deionized waters, 18~30 parts of property-modifying additives, 2~8 portions of anion surfactants, 8~12 parts of pretreatment micro-capsules and 2~3 parts of boraxs, mix monomer is mixed with water, and initiator and emulsifier is added, after being stirred, obtain blank, blank is mixed with anion surfactant, and sequentially adds borax, pre-processes micro-capsule and property-modifying additive, it is stirred, obtains the special stiffening agent of cotton fabric.Products obtained therefrom of the present invention can make cotton fiber retain preferable ultimate strength, and stiffening effect is preferable after handling cotton fiber.
Description
Technical field
The invention discloses a kind of special stiffening agents of cotton fabric, belong to macromolecule polymeric material technical field.
Background technology
Fabric hard finishing is a kind of important style arrangement, assigns fabric well-pressed, thick and solid, plentiful feel, mainly answers
In process for fabrics such as curtain, luggage, tent, lining cloth, footwear material and warp knits.It is commonly used in conventional processes
Melamine resin, Lauxite and cornstarch carry out stiffening processing.Formaldehyde is generated in process containing urea formaldehyde,
Workers ' health is seriously affected, part formaldehyde is combined with chemical bond form with resin macromolecular after arrangement, long-term in placement process
Release, it is easy to formaldehyde, market capacity be caused to reduce year by year；Cornstarch material is inconvenient, and fabric is easy mould after arrangement
Become, when handling colored fabric, easy tos produce the disadvantage of color and luster dimness, be often used together with other chemical synthesis class stiffening agents.
The dosage of continuous improvement with people to environmental requirement, environmental-friendly stiffening agent increases year by year, and major product type has
3 type of polyvinyl acetate, polyacrylate and polyurethane.Vinyl acetate and acrylate raw material are easy to get, polymerization technique at
Ripe, finished product affordable, market coverage is wide；Polyurethane is of high cost, is mainly used for high-end arrangement, fabric can be made to be endured with all one's will
And flexible feel, without folding line after cloth cover folding, and polyvinyl acetate and acrylate type stiffening agent use rear cloth
Face is also easy to produce folding line.
The fabric stiffening agent product of the prior art mainly has the fabric stiffening agent of virgin pp acid esters or melamine class, but
It is fabric stiffening agent product generally existing stiffening agent solvent resistance in use, stability, the deficiency of weatherability of the prior art,
And do not have uvioresistant, water repellent and flame retarding function, in formula containing formaldehyde, the emulsifier used not environmentally the problems such as.
Therefore, researching and developing novel fabric stiffening agent has very vast market prospect.
Invention content
The technical problem to be solved by the present invention is to：It is bad for fabric stiffening agent treatment effect used at present, and locate
Finished tensile strength is low after reason, and the poor problem of feel, the present invention provides a kind of special stiffening agents of cotton fabric.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of special stiffening agent of cotton fabric, is made of the raw material of following parts by weight：
80~120 parts of mix monomer
0.5~2.0 part of initiator
8~15 parts of emulsifier
70~100 parts of deionized water
18~30 parts of property-modifying additive
2~8 parts of anion surfactant
Pre-process 8~12 parts of micro-capsule
2~3 parts of borax
The preparation method of the property-modifying additive is：
It will（N- amidino groups）Dodecylacrylamide and polyethyleneglycol derivative in mass ratio 2：1~1：1 mixing, and poly- second is added
The ferrocene of 0.08~0.12 times of the paracide and polyethyleneglycol derivative quality that 0.1~0.2 times of diol, derivatives quality, is stirred
Mixing is mixed, additive is obtained, by additive dopamine in mass ratio 10：1~15：1 mixing, and pH to 7.5~8.2 is adjusted, it stirs
After mixing, filtering obtains pretreatment additive, by pretreatment additive and chitosan solution in mass ratio 1：1~1：2 mixing, mistake
Filter, obtains filter cake, by filter cake and graphene oxide mixture in mass ratio 1：8~1：10 mixing, filtering obtain pre- property-modifying additive,
By pre- property-modifying additive and natural rubber latex in mass ratio 1：8~1：10 mixing, and be added natural rubber latex quality 0.1~
0.2 times of zinc stearate, the sulphur and natural rubber latex quality 0.4~0.5 that 0.02~0.12 times of natural rubber latex quality
Coupling agent again, after being stirred, filtering obtains property-modifying additive；
It is described pretreatment micro-capsule preparation method be：
By polyvinyl alcohol and gelatin solution in mass ratio 1：3~1：5 mixing, and the sulfuric acid of 10~15 times of gelatin solution quality is added
Sodium solution, after being stirred, cooling obtains gelatin mixture, by gelatin mixture and formalin in mass ratio 50：1~80：1
Mixing, and pH to 9.0~9.5 is adjusted, under conditions of being 10~15 DEG C in temperature after 30~40min of solidification, washing is filtered, is obtained micro-
Micro-capsule is freeze-dried by capsule, obtains pretreatment micro-capsule.
The preparation method of the special stiffening agent of cotton fabric is to form to weigh each component by raw material, and mix monomer and water are mixed
It closes, and initiator and emulsifier is added, after being stirred, obtain blank, blank is mixed with anion surfactant, and successively
Borax is added, pre-processes micro-capsule and property-modifying additive, is stirred, obtains the special stiffening agent of cotton fabric.
The mix monomer is by vinyl acetate and methacrylate in mass ratio 6：1~8：1 mixing, and acetic acid is added
The acrylamide of 0.06~0.08 times of the methyl acrylate and vinyl acetate quality that 0.1~0.2 times of Ethylene mass, is stirred,
Obtain mix monomer.
The initiator is potassium peroxydisulfate, any one in sodium peroxydisulfate or ammonium persulfate.
The emulsifier is emulsifier op-10, any one in Tween-80 or Arlacel-80.
The anion surfactant is neopelex, fatty alcohol polyoxyethylene ether or fatty alcohol polyoxy second
Any one in alkene sodium sulphate.
The preparation method of the chitosan solution is by chitosan and acetic acid solution in mass ratio 1：3~1：5 mixing, are adjusted
PH to 4.0~4.5, is stirred, and obtains chitosan solution.
The preparation method of the graphene oxide mixture is by graphene oxide and water in mass ratio 1：100~1：200
It mixes, after sonic oscillation, adjusts pH to neutrality, obtain graphene oxide mixture.
The polyethyleneglycol derivative is any one in polyethylene glycol-p-methyl benzenesulfonic acid ester or polyethylene glycol salicylate
Kind.
The coupling agent is any one in γ propyltrimethoxy silane or γ-aminopropyl triethoxysilane.
The beneficial effects of the invention are as follows：
Property-modifying additive is added when preparing the special stiffening agent of cotton fabric in the present invention, and first, property-modifying additive adsorption is aerobic
Graphite alkene and chitosan, chitosan has preferable biocompatibility, and antibiotic property is preferable, after being added in product, can make
Product has preferable antibacterial effect, and surface of graphene oxide is rich in active group, and lubricity is preferable, in product is added
Afterwards, property-modifying additive can be brought into fibrous inside during product use, and forms hydrogen bond with the hydroxyl on cotton fiber surface and inhales
It is attached, to make interfibrous hole reduce, and then the stiffening effect of product is made to improve, secondly, graphite oxide in property-modifying additive
Alkene and Chitosan-coated can improve fiber on imitated vesicle structure during product use while fiberfill fibers hole
Between binding force make cotton fiber that there is preferable intensity, and due to property-modifying additive to make product after handling cotton fiber
Surface also carries rubber macromolecule segment, and the cotton fiber after product treatment can be made to possess preferable flexibility and fracture by force successively
Degree.
Specific implementation mode
The acetic acid solution in mass ratio 1 for being 5~10% by chitosan and mass fraction：3~1：5 mixing, are used in combination mass fraction
The pH to 4.0~4.5 of chitosan and acetate mixture is adjusted for 10~12% hydrochloric acid, is 40~50 DEG C in temperature, rotating speed is
After being stirred 15~30min under conditions of 200~300r/min, chitosan solution is obtained；Graphene oxide and water are pressed into quality
Than 1：100~1：200 mix, and under conditions of frequency is 55~65kHz after 15~30min of sonic oscillation, are with mass fraction
10~12% sodium hydroxide solution adjusts the mixture pH to 7.0~7.4 of graphene oxide and water, obtains graphene oxide mixing
Object；It will（N- amidino groups）Dodecylacrylamide and polyethyleneglycol derivative in mass ratio 2：1~1：1 is mixed in beaker, and
Be added into beaker 0.1~0.2 times of polyethyleneglycol derivative quality paracide and polyethyleneglycol derivative quality 0.08~
0.12 times of ferrocene is 45~65 DEG C in temperature, and rotating speed is stirred 40~65min under conditions of being 220~300r/min
Afterwards, additive is obtained, by additive and dopamine in mass ratio 10：1~15：1 mixing, it is 10~12% hydrogen that mass fraction, which is used in combination,
Sodium hydroxide solution adjusts pH to 7.5~8.2, is 40~50 DEG C in temperature, rotating speed stirs mixed under conditions of being 200~300r/min
After closing 25~60min, filtering obtains pretreatment additive, by pretreatment additive and chitosan solution in mass ratio 1：1~1：2
Mixing filters after impregnating 15~30min under room temperature, obtains filter cake, in mass ratio with graphene oxide mixture by filter cake
1：8~1：10 mixing, under room temperature impregnate 15~20min after filter, obtain pre- property-modifying additive, by pre- property-modifying additive with
Natural rubber latex in mass ratio 1：8~1：10 mixing, and add into the mixture of pre- property-modifying additive and natural rubber latex
Enter the zinc stearate of 0.1~0.2 times of natural rubber latex quality, the sulphur and day of 0.02~0.12 times of natural rubber latex quality
The coupling agent that 0.4~0.5 times of T PNR latex quality is 45~65 DEG C in temperature, and rotating speed is under conditions of 250~350r/min
After being stirred 45~80min, filtering obtains property-modifying additive；The gelatin solution that polyvinyl alcohol is 3~5% with mass fraction is pressed
Mass ratio 1：3~1：5 mixing are 90~95 DEG C in temperature, under conditions of rotating speed is 200~300r/min, it is stirred 20~
After 30min, the mixture of polyvinyl alcohol and gelatin is cooled to 50~60 DEG C, and add into the mixture of polyvinyl alcohol and gelatin
Enter the metabisulfite solution that the mass fraction of 10~15 times of gelatin solution quality is 20~30%, is 50~60 DEG C in temperature, rotating speed is
After being stirred 30~50min under conditions of 250~380r/min, pretreatment gelatin mixture is obtained, pretreatment gelatin is mixed
Object is cooled to 15~20 DEG C, obtains gelatin mixture, and the formalin that gelatin mixture and mass fraction are 30~35% is pressed quality
Than 50：1~80：The sodium hydroxide solution adjusting gelatin mixture and formalin of mass fraction 10~15% be used in combination in 1 mixing
PH to 9.0~9.5 filters washing, obtains micro-capsule under conditions of being 10~15 DEG C in temperature after 30~40min of solidification, and micro-capsule is cold
It is lyophilized dry, obtains pretreatment micro-capsule；It counts in parts by weight, weighs 80~120 parts of mix monomers successively, 0.5~2.0 part of initiator, 8
~15 parts of emulsifiers, 70~100 parts of deionized waters, 18~30 parts of property-modifying additives, 2~8 portions of anion surfactants, 8~
Mix monomer and water are mixed in beaker, and sequentially add initiation into beaker by 12 parts of pretreatment micro-capsules and 2~3 parts of boraxs
Agent and emulsifier, in temperature be 65~75 DEG C, rotating speed be 200~300r/min under conditions of be stirred 1~2h after, then at temperature
Degree is 80~85 DEG C, and rotating speed is stirred 2~3h under conditions of being 220~340r/min, blank is obtained, by blank and anion table
Face activating agent is mixed in blender, and borax is added into blender successively, micro-capsule and property-modifying additive is pre-processed, in temperature
It is 40~50 DEG C, after rotating speed is stirred 15~30min under conditions of being 200~300r/min, obtains the special stiffening agent of cotton fabric.
The mix monomer is by vinyl acetate and methacrylate in mass ratio 6：1~8：1 mixing, and vinyl acetate quality is added
The acrylamide of 0.1~0.2 times of 0.06~0.08 times of methyl acrylate and vinyl acetate quality, is stirred, and must mix single
Body.The initiator is potassium peroxydisulfate, any one in sodium peroxydisulfate or ammonium persulfate.The emulsifier is emulsifier op-10,
Any one in Tween-80 or Arlacel-80.The anion surfactant is neopelex, fatty alcohol polyoxy
Any one in vinethene or aliphatic alcohol polyethenoxy sodium sulphate.The polyethyleneglycol derivative is polyethylene glycol-to toluene sulphur
Any one in acid esters or polyethylene glycol salicylate.The coupling agent is γ propyltrimethoxy silane or γ-aminopropyl
Any one in triethoxysilane.
The acetic acid solution in mass ratio 1 for being 10% by chitosan and mass fraction：5 mixing, it is 12% that mass fraction, which is used in combination,
Hydrochloric acid adjusts the pH to 4.5 of chitosan and acetate mixture, is 50 DEG C in temperature, rotating speed stirs mixed under conditions of being 300r/min
After closing 30min, chitosan solution is obtained；By graphene oxide and water in mass ratio 1：200 mixing, in the condition that frequency is 65kHz
After lower sonic oscillation 30min, the sodium hydroxide solution for being 12% with mass fraction adjust the mixture pH of graphene oxide and water to
7.4, obtain graphene oxide mixture；It will（N- amidino groups）Dodecylacrylamide and polyethyleneglycol derivative in mass ratio 1：1
It is mixed in beaker, and the paracide and polyethyleneglycol derivative of 0.2 times of polyethyleneglycol derivative quality is added into beaker
The ferrocene that 0.12 times of quality is 65 DEG C in temperature, after rotating speed is stirred 65min under conditions of being 300r/min, must add
Agent, by additive and dopamine in mass ratio 15：1 mixing, be used in combination mass fraction be 12% sodium hydroxide solution adjusting pH to
8.2, it is 50 DEG C in temperature, after rotating speed is stirred 60min under conditions of being 300r/min, filtering obtains pretreatment additive, will
Pretreatment additive and chitosan solution in mass ratio 1：2 mixing, filter after impregnating 30min under room temperature, obtain filter cake, will
Filter cake and graphene oxide mixture in mass ratio 1：10 mixing, filter after impregnating 20min under room temperature, obtain pre- modification and add
Add agent, by pre- property-modifying additive and natural rubber latex in mass ratio 1：10 mixing, and to pre- property-modifying additive and natural rubber
The zinc stearate of 0.2 times of natural rubber latex quality, the sulphur that 0.12 times of natural rubber latex quality are added in the mixture of latex
The coupling agent of 0.5 times of sulphur and natural rubber latex quality is 65 DEG C in temperature, and rotating speed is stirred under conditions of being 350r/min
After 80min, filtering obtains property-modifying additive；The gelatin solution in mass ratio 1 for being 5% by polyvinyl alcohol and mass fraction：5 mixing,
In temperature be 95 DEG C, rotating speed be 300r/min under conditions of, after being stirred 30min, by the mixture of polyvinyl alcohol and gelatin
60 DEG C are cooled to, and it is 30% that the mass fraction of 15 times of gelatin solution quality, which is added, into the mixture of polyvinyl alcohol and gelatin
Metabisulfite solution is 60 DEG C in temperature, after rotating speed is stirred 50min under conditions of being 380r/min, it is mixed must to pre-process gelatin
Object is closed, pretreatment gelatin mixture is cooled to 20 DEG C, obtains gelatin mixture, is 35% by gelatin mixture and mass fraction
Formalin in mass ratio 80：1 mixing is used in combination the sodium hydroxide solution adjusting gelatin mixture of mass fraction 15% and formaldehyde molten
The pH to 9.5 of liquid filters washing, obtains micro-capsule, micro-capsule is freeze-dried, obtain under conditions of being 15 DEG C in temperature after solidification 40min
Pre-process micro-capsule；It counts in parts by weight, weighs 120 parts of mix monomers successively, 2.0 parts of initiators, 15 parts of emulsifiers, 100 parts are gone
30 parts of property-modifying additives of ionized water, 8 portions of anion surfactants, 12 parts of pretreatment micro-capsules and 3 parts of boraxs, by mix monomer with
Water is mixed in beaker, and initiator and emulsifier are sequentially added into beaker, is 75 DEG C in temperature, rotating speed is 300r/min's
Under the conditions of be stirred 2h after, then at temperature be 85 DEG C, rotating speed be 340r/min under conditions of be stirred 3h, obtain blank, will
Blank is mixed in anion surfactant in blender, and borax is added into blender successively, is pre-processed micro-capsule and is changed
Property additive, be 50 DEG C in temperature, after rotating speed is stirred 30min under conditions of being 300r/min, it is special stiffening to obtain cotton fabric
Agent.The mix monomer is by vinyl acetate and methacrylate in mass ratio 8：1 mixing, and vinyl acetate quality is added
The acrylamide of 0.2 times of 0.08 times of methyl acrylate and vinyl acetate quality, is stirred, obtains mix monomer.The initiation
Agent is potassium peroxydisulfate.The emulsifier is emulsifier op-10.The anion surfactant is neopelex.
The polyethyleneglycol derivative is polyethylene glycol-p-methyl benzenesulfonic acid ester.The coupling agent is γ propyltrimethoxy silane.
It will（N- amidino groups）Dodecylacrylamide and polyethyleneglycol derivative in mass ratio 1：1 is mixed in beaker, and
The paracide of 0.2 times of polyethyleneglycol derivative quality and two cyclopentadienyls of 0.12 times of polyethyleneglycol derivative quality are added into beaker
Iron is 65 DEG C in temperature, after rotating speed is stirred 65min under conditions of being 300r/min, additive is obtained, by additive and DOPA
Amine in mass ratio 15：1 mixing is used in combination the sodium hydroxide solution that mass fraction is 12% to adjust pH to 8.2, is 50 DEG C in temperature, turns
After speed is stirred 60min under conditions of being 300r/min, filtering obtains pretreatment additive, by pretreatment additive and naturally
Rubber latex in mass ratio 1：10 mixing, and natural rubber is added into the mixture of pretreatment additive and natural rubber latex
0.5 times of the zinc stearate that 0.2 times of latex quality, the sulphur that 0.12 times of natural rubber latex quality and natural rubber latex quality
Coupling agent is 65 DEG C in temperature, and after rotating speed is stirred 80min under conditions of being 350r/min, filtering obtains property-modifying additive；
The gelatin solution in mass ratio 1 for being 5% by polyvinyl alcohol and mass fraction：5 mixing, in temperature be 95 DEG C, rotating speed 300r/min
Under conditions of, after being stirred 30min, the mixture of polyvinyl alcohol and gelatin is cooled to 60 DEG C, and to polyvinyl alcohol with it is bright
The metabisulfite solution that the mass fraction of 15 times of gelatin solution quality is 30% is added in the mixture of glue, in temperature be 60 DEG C, rotating speed
After being stirred 50min under conditions of 380r/min, pretreatment gelatin mixture is obtained, pretreatment gelatin mixture is cooled to
20 DEG C, gelatin mixture is obtained, the formalin in mass ratio 80 for being 35% by gelatin mixture and mass fraction：1 mixing, is used in combination
The sodium hydroxide solution of mass fraction 15% adjusts the pH to 9.5 of gelatin mixture and formalin, the condition for being 15 DEG C in temperature
After lower solidification 40min, washing is filtered, micro-capsule is obtained, micro-capsule is freeze-dried, obtain pretreatment micro-capsule；It counts, claims successively in parts by weight
Take 120 parts of mix monomers, 2.0 parts of initiators, 15 parts of emulsifiers, 100 parts of deionized waters, 30 parts of property-modifying additives, 8 parts of anion
Surfactant, 12 parts of pretreatment micro-capsules and 3 parts of boraxs, mix monomer and water are mixed in beaker, and successively into beaker
Initiator and emulsifier is added, is 75 DEG C in temperature, after rotating speed is stirred 2h under conditions of being 300r/min, is then at temperature
85 DEG C, rotating speed is stirred 3h under conditions of being 340r/min, obtains blank, blank is mixed in anion surfactant and is stirred
It mixes in machine, and borax is added into blender successively, pre-process micro-capsule and property-modifying additive, be 50 DEG C in temperature, rotating speed is
After being stirred 30min under conditions of 300r/min, the special stiffening agent of cotton fabric is obtained.The mix monomer be by vinyl acetate with
Methacrylate in mass ratio 8：1 mixing, and the methyl acrylate and vinyl acetate quality of 0.2 times of vinyl acetate quality is added
0.08 times of acrylamide, is stirred, and obtains mix monomer.The initiator is potassium peroxydisulfate.The emulsifier is emulsifier
OP-10.The anion surfactant is neopelex.The polyethyleneglycol derivative is that polyethylene glycol-is right
Tosylate.The coupling agent is γ propyltrimethoxy silane.
The acetic acid solution in mass ratio 1 for being 10% by chitosan and mass fraction：5 mixing, it is 12% that mass fraction, which is used in combination,
Hydrochloric acid adjusts the pH to 4.5 of chitosan and acetate mixture, is 50 DEG C in temperature, rotating speed stirs mixed under conditions of being 300r/min
After closing 30min, chitosan solution is obtained；By graphene oxide and water in mass ratio 1：200 mixing, in the condition that frequency is 65kHz
After lower sonic oscillation 30min, the sodium hydroxide solution for being 12% with mass fraction adjust the mixture pH of graphene oxide and water to
7.4, obtain graphene oxide mixture；It will（N- amidino groups）Dodecylacrylamide and polyethyleneglycol derivative in mass ratio 1：1
It is mixed in beaker, and the paracide and polyethyleneglycol derivative of 0.2 times of polyethyleneglycol derivative quality is added into beaker
The ferrocene that 0.12 times of quality is 65 DEG C in temperature, after rotating speed is stirred 65min under conditions of being 300r/min, must add
Agent, by additive and dopamine in mass ratio 15：1 mixing, be used in combination mass fraction be 12% sodium hydroxide solution adjusting pH to
8.2, it is 50 DEG C in temperature, after rotating speed is stirred 60min under conditions of being 300r/min, filtering obtains pretreatment additive, will
Pretreatment additive and chitosan solution in mass ratio 1：2 mixing, filter after impregnating 30min under room temperature, obtain filter cake, will
Filter cake and graphene oxide mixture in mass ratio 1：10 mixing, filter after impregnating 20min under room temperature, obtain modified addition
Agent；The gelatin solution in mass ratio 1 for being 5% by polyvinyl alcohol and mass fraction：5 mixing, in temperature be 95 DEG C, rotating speed 300r/
Under conditions of min, after being stirred 30min, the mixture of polyvinyl alcohol and gelatin is cooled to 60 DEG C, and to polyvinyl alcohol with
The metabisulfite solution that the mass fraction of 15 times of gelatin solution quality is 30% is added in the mixture of gelatin, is 60 DEG C in temperature, turns
After speed is stirred 50min under conditions of being 380r/min, pretreatment gelatin mixture is obtained, by pretreatment gelatin mixture cooling
To 20 DEG C, gelatin mixture is obtained, the formalin in mass ratio 80 for being 35% by gelatin mixture and mass fraction：1 mixing, and
The pH to 9.5 that gelatin mixture and formalin are adjusted with the sodium hydroxide solution of mass fraction 15%, the item for being 15 DEG C in temperature
After curing 40min under part, washing is filtered, micro-capsule is obtained, micro-capsule is freeze-dried, obtain pretreatment micro-capsule；It counts in parts by weight, successively
Weigh 120 parts of mix monomers, 2.0 parts of initiators, 15 parts of emulsifiers, 100 parts of deionized waters, 30 parts of property-modifying additives, 8 parts of the moon from
Sub- surfactant, 12 parts of pretreatment micro-capsules and 3 parts of boraxs, mix monomer and water are mixed in beaker, and into beaker according to
Secondary addition initiator and emulsifier, in temperature be 75 DEG C, rotating speed be 300r/min under conditions of be stirred 2h after, then at temperature
It it is 85 DEG C, rotating speed is stirred 3h under conditions of being 340r/min, obtains blank, blank and anion surfactant are mixed in
In blender, and borax is added into blender successively, pre-processes micro-capsule and property-modifying additive, is 50 DEG C in temperature, rotating speed is
After being stirred 30min under conditions of 300r/min, the special stiffening agent of cotton fabric is obtained.The mix monomer be by vinyl acetate with
Methacrylate in mass ratio 8：1 mixing, and the methyl acrylate and vinyl acetate quality of 0.2 times of vinyl acetate quality is added
0.08 times of acrylamide, is stirred, and obtains mix monomer.The initiator is potassium peroxydisulfate.The emulsifier is emulsifier
OP-10.The anion surfactant is neopelex.The polyethyleneglycol derivative is that polyethylene glycol-is right
Tosylate.
The acetic acid solution in mass ratio 1 for being 10% by chitosan and mass fraction：5 mixing, it is 12% that mass fraction, which is used in combination,
Hydrochloric acid adjusts the pH to 4.5 of chitosan and acetate mixture, is 50 DEG C in temperature, rotating speed stirs mixed under conditions of being 300r/min
After closing 30min, chitosan solution is obtained；By graphene oxide and water in mass ratio 1：200 mixing, in the condition that frequency is 65kHz
After lower sonic oscillation 30min, the sodium hydroxide solution for being 12% with mass fraction adjust the mixture pH of graphene oxide and water to
7.4, obtain graphene oxide mixture；It will（N- amidino groups）Dodecylacrylamide and polyethyleneglycol derivative in mass ratio 1：1
It is mixed in beaker, and the paracide and polyethyleneglycol derivative of 0.2 times of polyethyleneglycol derivative quality is added into beaker
The ferrocene that 0.12 times of quality is 65 DEG C in temperature, after rotating speed is stirred 65min under conditions of being 300r/min, must add
Agent, by additive and dopamine in mass ratio 15：1 mixing, be used in combination mass fraction be 12% sodium hydroxide solution adjusting pH to
8.2, it is 50 DEG C in temperature, after rotating speed is stirred 60min under conditions of being 300r/min, filtering obtains pretreatment additive, will
Pretreatment additive and chitosan solution in mass ratio 1：2 mixing, filter after impregnating 30min under room temperature, obtain filter cake, will
Filter cake and graphene oxide mixture in mass ratio 1：10 mixing, filter after impregnating 20min under room temperature, obtain pre- modification and add
Add agent, by pre- property-modifying additive and natural rubber latex in mass ratio 1：10 mixing, and to pre- property-modifying additive and natural rubber
The zinc stearate of 0.2 times of natural rubber latex quality, natural rubber latex quality 0.02~0.12 are added in the mixture of latex
The coupling agent of 0.5 times of sulphur and natural rubber latex quality again is 65 DEG C in temperature, and rotating speed stirs under conditions of being 350r/min
After mixing mixing 80min, filtering obtains property-modifying additive；It counts in parts by weight, weighs 120 parts of mix monomers, 2.0 parts of initiations successively
Agent, 15 parts of emulsifiers, 100 parts of deionized waters, 30 parts of property-modifying additives, 8 portions of anion surfactants and 3 parts of boraxs, will mix
It closes monomer to be mixed in beaker with water, and sequentially adds initiator and emulsifier into beaker, be 75 DEG C in temperature, rotating speed is
It is 85 DEG C then at temperature after being stirred 2h under conditions of 300r/min, rotating speed is stirred 3h under conditions of being 340r/min,
Blank is obtained, blank and anion surfactant are mixed in blender, and borax and modification is added into blender successively
Additive is 50 DEG C in temperature, after rotating speed is stirred 30min under conditions of being 300r/min, obtains the special stiffening agent of cotton fabric.
The mix monomer is by vinyl acetate and methacrylate in mass ratio 8：1 mixing, and 0.2 times of vinyl acetate quality is added
0.08 times of methyl acrylate and vinyl acetate quality acrylamide, be stirred, obtain mix monomer.The initiator was
Potassium sulfate.The emulsifier is emulsifier op-10.The anion surfactant is neopelex.It is described poly-
Ethylene glycol derivative is polyethylene glycol-p-methyl benzenesulfonic acid ester.The coupling agent is γ propyltrimethoxy silane.
Comparative example：The fabric stiffening agent of Beijing scientific ＆ technical corporation production.
Cotton fiber is subjected to two leachings two with example 1 to 4 gained stiffening agent of example and comparative example respectively and rolls arrangement, and will be arranged
Cotton fiber afterwards is tested as follows
1. fracture strength：It is tested with reference to ISO 13934.1, specific testing result is as shown in table 1：
2. stiffening effect and washability test：It is tested with reference to GB/T 7689.4, the anti-of arrangement product is measured on Stiffness Tester
Curved length；By the measurement of fabric bending resistance length before and after washing, the washability for enduring with all one's will effect, specific testing result such as table 1 are evaluated
It is shown：
Table 1：Fracture strength endures with all one's will effect and the specific testing result of washability
By 1 testing result of table it is found that products obtained therefrom of the present invention is after handling cotton fiber, cotton fiber can be made to retain preferable fracture strong
Power, and stiffening effect is preferable.
Claims (10)
1. a kind of special stiffening agent of cotton fabric, which is characterized in that be made of the raw material of following parts by weight：
80~120 parts of mix monomer
0.5~2.0 part of initiator
8~15 parts of emulsifier
70~100 parts of deionized water
18~30 parts of property-modifying additive
2~8 parts of anion surfactant
Pre-process 8~12 parts of micro-capsule
2~3 parts of borax
The preparation method of the property-modifying additive is：
It will（N- amidino groups）Dodecylacrylamide and polyethyleneglycol derivative in mass ratio 2：1~1：1 mixing, and poly- second is added
The ferrocene of 0.08~0.12 times of the paracide and polyethyleneglycol derivative quality that 0.1~0.2 times of diol, derivatives quality, is stirred
Mixing is mixed, additive is obtained, by additive dopamine in mass ratio 10：1~15：1 mixing, and pH to 7.5~8.2 is adjusted, it stirs
After mixing, filtering obtains pretreatment additive, by pretreatment additive and chitosan solution in mass ratio 1：1~1：2 mixing, mistake
Filter, obtains filter cake, by filter cake and graphene oxide mixture in mass ratio 1：8~1：10 mixing, filtering obtain pre- property-modifying additive,
By pre- property-modifying additive and natural rubber latex in mass ratio 1：8~1：10 mixing, and be added natural rubber latex quality 0.1~
0.2 times of zinc stearate, the sulphur and natural rubber latex quality 0.4~0.5 that 0.02~0.12 times of natural rubber latex quality
Coupling agent again, after being stirred, filtering obtains property-modifying additive；
It is described pretreatment micro-capsule preparation method be：
By polyvinyl alcohol and gelatin solution in mass ratio 1：3~1：5 mixing, and the sulfuric acid of 10~15 times of gelatin solution quality is added
Sodium solution, after being stirred, cooling obtains gelatin mixture, by gelatin mixture and formalin in mass ratio 50：1~80：1
Mixing, and pH to 9.0~9.5 is adjusted, under conditions of being 10~15 DEG C in temperature after 30~40min of solidification, washing is filtered, is obtained micro-
Micro-capsule is freeze-dried by capsule, obtains pretreatment micro-capsule.
2. the special stiffening agent of a kind of cotton fabric according to claim 1, it is characterised in that：The special stiffening agent of cotton fabric
Preparation method be by raw material form weigh each component, mix monomer is mixed with water, and initiator and emulsifier is added, stirring
After mixing, blank is obtained, blank is mixed with anion surfactant, and sequentially add borax, pretreatment micro-capsule and modification add
Add agent, be stirred, obtains the special stiffening agent of cotton fabric.
3. the special stiffening agent of a kind of cotton fabric according to claim 1, it is characterised in that：The mix monomer is by acetic acid
Ethylene and methacrylate in mass ratio 6：1~8：1 mixing, and the acrylic acid first of 0.1~0.2 times of vinyl acetate quality is added
The acrylamide of 0.06~0.08 times of ester and vinyl acetate quality, is stirred, obtains mix monomer.
4. the special stiffening agent of a kind of cotton fabric according to claim 1, it is characterised in that：The initiator is persulfuric acid
Any one in potassium, sodium peroxydisulfate or ammonium persulfate.
5. the special stiffening agent of a kind of cotton fabric according to claim 1, it is characterised in that：The emulsifier is emulsifier
Any one in OP-10, Tween-80 or Arlacel-80.
6. the special stiffening agent of a kind of cotton fabric according to claim 1, it is characterised in that：The anion surfactant
For neopelex, any one in fatty alcohol polyoxyethylene ether or aliphatic alcohol polyethenoxy sodium sulphate.
7. the special stiffening agent of a kind of cotton fabric according to claim 1, it is characterised in that：The preparation of the chitosan solution
Method is by chitosan and acetic acid solution in mass ratio 1：3~1：5 mixing, adjust pH to 4.0~4.5, are stirred, and it is poly- to obtain shell
Sugar juice.
8. the special stiffening agent of a kind of cotton fabric according to claim 1, it is characterised in that：The graphene oxide mixture
Preparation method be by graphene oxide and water in mass ratio 1：100~1：200 mix, after sonic oscillation, adjusting pH to neutrality,
Obtain graphene oxide mixture.
9. the special stiffening agent of a kind of cotton fabric according to claim 1, it is characterised in that：The polyethyleneglycol derivative is
Any one in polyethylene glycol-p-methyl benzenesulfonic acid ester or polyethylene glycol salicylate.
10. the special stiffening agent of a kind of cotton fabric according to claim 1, it is characterised in that：The coupling agent is γ-propyl
Any one in trimethoxy silane or γ-aminopropyl triethoxysilane.
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| CN201810397870.5A CN108589269A (en) | 2018-04-28 | 2018-04-28 | A kind of special stiffening agent of cotton fabric |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113209726A (en) * | 2021-03-31 | 2021-08-06 | 南京际华三五二一环保科技有限公司 | Preparation method of stiff filter material for pleated filter bag |
| CN114182433A (en) * | 2021-12-06 | 2022-03-15 | 江苏金太阳纺织科技股份有限公司 | Preparation method of modified cotton wadding |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1025562A (en) * | 1961-11-01 | 1966-04-14 | Styrene Co Polymers Ltd | New copolymers for treatment of fibrous materials |
| CN102433750A (en) * | 2011-11-30 | 2012-05-02 | 浙江传化股份有限公司 | Environmental-friendly stiffening agent and preparation method thereof |
| CN107313252A (en) * | 2017-07-28 | 2017-11-03 | 苏州井村服饰有限公司 | A kind of cowboy's antibacterial stiffening agent and preparation method thereof |
-
2018
- 2018-04-28 CN CN201810397870.5A patent/CN108589269A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1025562A (en) * | 1961-11-01 | 1966-04-14 | Styrene Co Polymers Ltd | New copolymers for treatment of fibrous materials |
| CN102433750A (en) * | 2011-11-30 | 2012-05-02 | 浙江传化股份有限公司 | Environmental-friendly stiffening agent and preparation method thereof |
| CN107313252A (en) * | 2017-07-28 | 2017-11-03 | 苏州井村服饰有限公司 | A kind of cowboy's antibacterial stiffening agent and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113209726A (en) * | 2021-03-31 | 2021-08-06 | 南京际华三五二一环保科技有限公司 | Preparation method of stiff filter material for pleated filter bag |
| CN113209726B (en) * | 2021-03-31 | 2022-06-14 | 南京际华三五二一环保科技有限公司 | Preparation method of stiff filter material for pleated filter bag |
| CN114182433A (en) * | 2021-12-06 | 2022-03-15 | 江苏金太阳纺织科技股份有限公司 | Preparation method of modified cotton wadding |
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