CN108978218A - A kind of preparation method of cotton fabric stiffening agent - Google Patents
A kind of preparation method of cotton fabric stiffening agent Download PDFInfo
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- 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
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Abstract
The invention discloses a kind of preparation methods of cotton fabric stiffening agent, belong to fabric finishing agent technical field.Acrylic acid is mixed with methyl methacrylate 2:1~3:1 in mass ratio, and 0.3~0.6 times of acrylic acid quality of hydroxyethyl methacrylate is added, the butyl acrylate that 0.2~0.4 times of acrylic acid quality, the water and 0.1~0.2 times of acrylic acid quality of emulsifier that 5~8 times of acrylic acid quality, after being stirred, blank must be mixed, mixing blank is mixed with modified phenylethylene 10:2~10:3 in mass ratio, and the additive of 0.2~0.3 times of blank quality of mixing is added, it is stirred, obtain blank, water is mixed with initiator 30:1~40:1 in mass ratio, obtain bottom liquid, blank is mixed with bottom liquid 8:3 in mass ratio, after being stirred to react, adjust pH to 6~7, obtain cotton fabric stiffening agent.The cotton fabric of technical solution of the present invention preparation stiffening agent has excellent stiffening effect, and has preferable waterproofness, and stiffening effect is lasting.
Description
Technical field
The invention discloses a kind of preparation methods of cotton fabric stiffening agent, belong to fabric finishing agent technical field.
Background technique
Hard finishing is one kind of fabric post-treatment, it by padding stiffening agent, make between the fiber in fabric yarn
Cementation is produced under certain condition, stiffening agent is between fibrous inside, fiber or the surface of fiber forms film or generates crosslinking,
To make fabric generate stiffening, thick and solid, plentiful feel.It is widely used in during the final finishing of drapery, especially window
The hard finishing of cord, suitcase cloth, knitted fabric and lining cloth.
The non-renewable of petroleum-based products and close fine fabric wearing comfort it is poor etc. due to, natural fiber is (such as
Cotton, hair, silk) advantage display again, the demand and consumption of natural fabric, which also show, to be risen year by year
Trend.The existing sizing agent applied to natural fiber is made a general survey of, starch is mostly important one of kind, accounts for spinning sizing agent
70% or so of total amount consumed.Starch is good to the sizing performance of natural fiber especially cellulose fibre, environmentally friendly, so
And global " crisis in food " is increasingly serious, provision price was even more to increase substantially in recent years, and the price water of starch rises ship
It is high；Polyvinyl alcohol (PVA) is also one of the main slurry for natural fiber, and consumption is only second to starch size, accounts for about weaving
The 20% of slurry total amount consumed.Since the biodegradable properties of PVA are very poor, be unfavorable for environmental protection, American-European some countries early in
The beginning of this century is just classified as " unclean slurry " and is disabled, currently, also starting to vigorously advocate in society to use no or little
PVA；And as the smallest polyacrylic size of dosage in three big slurries, although the elongation at break of its serous coat is higher, slurry
Film-strength is but very low, is referred to as " soft without heavily fortified point " by professional person.In addition, the moisture absorption of polyacrylic size glues phenomenon very again
Seriously, these defects make the slurry be typically only capable to that other main slurries is assisted to be used in mixed way with small scale.
The shortcomings that in order to overcome polyacrylic stiffening agent, therefore, it is small to research and develop novel hygroscopicity, endures with all one's will effect
Good polyacrylic stiffening agent has a vast market foreground.
Summary of the invention
The present invention solves the technical problem of: for traditional polyacrylic stiffening agent because hygroscopicity is big, and it is strong
Spend it is lower, caused by endure with all one's will ineffective problem, provide a kind of preparation method of cotton fabric stiffening agent.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of cotton fabric stiffening agent, specific preparation step are as follows:
(1) according to parts by weight, it successively weighs: 200~205 parts of toluene, 160~165 parts of TEPM, 40~42 parts of styrene and 2
Toluene is mixed with TEPM, and styrene and initiator is added by~4 parts of initiators, under nitrogen atmosphere, after being stirred to react, is obtained
Modified phenylethylene mixture mixes modified phenylethylene mixture with petroleum ether 1:2~1:3 in mass ratio, and filtering obtains modified benzene
Ethylene；
(2) carbon nanotube is mixed with dehydrated alcohol 1:80~1:100 in mass ratio, after ultrasonic disperse, adjusts pH to 8~10,
It is stirred to react, and adjusts pH to neutrality, filter washing, drying obtains pretreatment carbon nanotube, will pretreatment carbon nanotube and ethyl alcohol
Aqueous solution 1:200~1:250 in mass ratio mixing, ultrasonic disperse obtain pretreatment carbon nanotube mixture, will pre-process carbon nanometer
Pipe mixture is mixed with ammonium hydroxide 20:1~35:1 in mass ratio, and pretreatment carbon nanotube mixture matter is added dropwise under ultrasound condition
The ethyl orthosilicate mixture of 0.1~0.2 times of amount, after being stirred, obtains pre- modified carbon nano-tube mixture, pre- carbon modified is received
Nanotube mixture is mixed with Ethanol-Acetic Acid mixture 100:1~120:1 in mass ratio, and pre- modified carbon nano-tube mixing is added
The silane coupling agent that 0.05~0.08 times of amount of substance after being stirred, is filtered, is washed, dry, obtains modified carbon nano-tube；
(3) modified carbon nano-tube is mixed with modified epoxy soybean oil 5:1~8:1 in mass ratio, and modified carbon nano-tube is added
The organic solvent and 0.1~0.2 times of modified carbon nano-tube quality of dicyclohexyl diimine that 5~6 times of quality, after being stirred to react,
Filtering, obtains additive；
(4) acrylic acid is mixed with methyl methacrylate 2:1~3:1 in mass ratio, and acrylic acid quality 0.3~0.6 is added
Times hydroxyethyl methacrylate, the butyl acrylate that 0.2~0.4 times of acrylic acid quality, the water that 5~8 times of acrylic acid quality and
The emulsifier that 0.1~0.2 times of acrylic acid quality after being stirred, obtains mixing blank, and mixing blank and modified phenylethylene are pressed matter
Amount is mixed than 10:2~10:3, and the additive of 0.2~0.3 times of blank quality of mixing is added, and is stirred, is obtained blank, by water
It is mixed with initiator 30:1~40:1 in mass ratio, obtains bottom liquid, blank is mixed with bottom liquid 8:3 in mass ratio, after being stirred to react,
PH to 6~7 is adjusted, cotton fabric stiffening agent is obtained.
Step (1) TEPM is methacryloxypropyl.
The initiator is potassium peroxydisulfate, any one in sodium peroxydisulfate or azodiisobutyronitrile.
Step (2) the ethyl orthosilicate mixture is by ethyl orthosilicate and ethyl alcohol 1:8~1 in mass ratio；10 mixing,
Obtain ethyl orthosilicate mixture.
By ethyl alcohol, 1:1 is mixed step (2) the Ethanol-Acetic Acid mixture by volume with acetic acid, obtains Ethanol-Acetic Acid mixing
Object.
Step (2) silane coupling agent is silane resin acceptor kh-550, silane coupling agent KH-560 or silane coupling agent
Any one in KH-570.
Step (3) organic solvent is cyclohexanone, any one in dimethylbenzene or toluene.
Step (4) emulsifier is emulsifier op-10, any one in emulsifier AEO-7 or emulsifier 1303.
Step (3) modified epoxy soybean oil is to mix epoxidized soybean oil with hydrogen peroxide 5:1~8:1 in mass ratio,
And 0.2~0.3 times of Quaity of Epoxidized Soybean Oil of acetic acid is added, after being stirred to react, pretreatment epoxidized soybean oil is obtained, ring will be pre-processed
Oxygen soybean oil is mixed with nickel 30:1~50:1 in mass ratio, and under atmosphere of hydrogen, is stirred to react, and modified epoxy soybean oil is obtained.
The beneficial effects of the present invention are:
(1) modified phenylethylene is added when preparing cotton fabric stiffening agent in the present invention, firstly, after styrene is in addition product,
It can react and polymerize with the monomeric fashion of interiors of products in product preparation process, so that the crosslink density of product is improved, into
And after product use, the crosslinking degree of surface of cotton fabric is improved, the stiffening effect of product is improved, secondly, styrene is passing through
Modified, styrene-grafted organosilan is crossed, to make certain hydrophobic performance that has of product, and then reduces the anti-suction of product
Wet performance, makes that stiffening effect is lasting；
(2) additive is added when preparing cotton fabric stiffening agent in the present invention, on the one hand, contains modified carbon nano tube in additive
Pipe, can be in electrostatic force after being added in product due to carbon nano tube surface grafted amino group silica after being added in product
Under the action of be uniformly distributed in product, and since the presence of amino can be such that the adsorption capacity between product and cotton fabric enhances, from
And improve the adhesive force of product, and then improve the service life of product, and due to the addition of carbon nanotube, product can be made
The cross-linked network mechanical property of formation improves, and then improves the stiffening effect of product, and on the other hand, carbon modified is received in additive
Mitron is compound with modified epoxy soybean oil, so as to be grafted the epoxidized soybean oil containing hydroxyl on the carbon nanotubes, makes carbon nanometer
The dispersibility of pipe in the product improves, and since the epoxidized soybean oil containing hydroxyl can further be handed in product use process
Connection, so that the stiffening effect of product be made to improve.
Specific embodiment
Epoxidized soybean oil is mixed with hydrogen peroxide 5:1~8:1 in mass ratio, and the mixing to epoxidized soybean oil and hydrogen peroxide
0.2~0.3 times of Quaity of Epoxidized Soybean Oil of acetic acid is added in object, is 80~85 DEG C in temperature, revolving speed is 300~400r/min's
Under the conditions of, after being stirred to react 30~40min, pretreatment epoxidized soybean oil is obtained, in mass ratio with nickel by pretreatment epoxidized soybean oil
30:1~50:1 mixing, and hydrogen is passed through with the rate of 8~20mL/min into the mixture of pretreatment epoxidized soybean oil and nickel,
It is 50~70 DEG C in temperature, under conditions of revolving speed is 300~400r/min, after being stirred to react 1~2h, obtains modified epoxy soybean
Oil；According to parts by weight, it successively weighs: 200~205 parts of toluene, 160~165 parts of TEPM, 40~42 parts of styrene and 2~4 parts
Toluene and TEPM are mixed in four-hole boiling flask by initiator, and styrene and initiator are added into four-hole boiling flask, with 5~
The rate of 12mL/min is passed through nitrogen into four-hole boiling flask, is 80~90 DEG C in temperature, revolving speed is the condition of 300~400r/min
Under, after being stirred to react 3~4h, obtain modified phenylethylene mixture, by modified phenylethylene mixture and petroleum ether 1:2 in mass ratio~
1:3 mixing, in temperature be 40~60 DEG C, revolving speed be 300~400r/min under conditions of, after being stirred 30~40min, mistake
Filter, obtains modified phenylethylene；Carbon nanotube and dehydrated alcohol 1:80~1:100 in mass ratio are mixed in three-necked flask, Yu Pin
Under conditions of rate is 45~55kHz after 1~2h of ultrasonic disperse, three are adjusted with the potassium hydroxide solution that mass fraction is 16~17%
The pH to 8~10 of material in mouth flask, and be 80~88 DEG C in temperature, under conditions of revolving speed is 300~400r/min, stirring is anti-
After answering 7~8h, the pH for adjusting material in three-necked flask with the hydrochloric acid that mass fraction is 10~12% is filtered, must be pre-processed to neutrality
Carbon nanotube blank, will pretreatment carbon nanotube blank be washed with water 3~6 times after, and in temperature be 70 DEG C under conditions of vacuum
After dry 2~4h, pretreatment carbon nanotube is obtained, the ethanol water that carbon nanotube will be pre-processed and mass fraction is 50~60%
The mixing of 1:200~1:250 in mass ratio obtains pre- place under conditions of frequency is 45~55kHz after 60~70min of ultrasonic disperse
Carbon nanotube mixture is managed, the ammonium hydroxide 20:1 in mass ratio that carbon nanotube mixture will be pre-processed and mass fraction is 20~24%
~35:1 is mixed in flask, and in frequency be 45~55kHz ultrasound condition under with the rate of 8~18mL/min into flask
The ethyl orthosilicate mixture of 0.1~0.2 times of carbon nanotube mixture quality of pretreatment is added dropwise, after being added dropwise, is in temperature
35~45 DEG C, under conditions of revolving speed is 300~400r/min, after being stirred 15~18h, obtain pre- modified carbon nano-tube mixing
Pre- modified carbon nano-tube mixture and Ethanol-Acetic Acid mixture 100:1~120:1 in mass ratio are mixed in reaction kettle by object,
And the silane coupling agent of 0.05~0.08 times of pre- modified carbon nano-tube mixture quality is added into reaction kettle, in temperature be 35~
It 45 DEG C, after revolving speed is stirred 5~6h under conditions of being 300~400r/min, filters, obtains modified carbon nano tube blank, will change
Property carbon nanotube blank be washed with water 5~8 times after, in temperature be 70 DEG C under conditions of be dried in vacuo 2~3h after, obtain carbon modified and receive
Mitron；Modified carbon nano-tube is mixed with modified epoxy soybean oil 5:1~8:1 in mass ratio, and to modified carbon nano-tube with change
Property epoxidized soybean oil mixture in be added 5~6 times of modified carbon nano-tube quality organic solvent and modified carbon nano-tube quality
0.1~0.2 times of dicyclohexyl diimine is 60~80 DEG C in temperature, under conditions of revolving speed is 300~400r/min, stirs
After reacting 1~3h, filtering obtains additive；Acrylic acid is mixed with methyl methacrylate 2:1~3:1 in mass ratio, and to third
The hydroxyethyl methacrylate of 0.3~0.6 times of acrylic acid quality, propylene are added in the mixture of olefin(e) acid and methyl methacrylate
The butyl acrylate of 0.2~0.4 times of sour quality, the water and 0.1~0.2 times of acrylic acid quality of emulsification that 5~8 times of acrylic acid quality
Agent is 40~60 DEG C in temperature, after revolving speed is stirred 30~90min under conditions of being 300~400r/min, obtains mixing base
Mixing blank mix with modified phenylethylene 10:2~10:3 in mass ratio by material, and to mixing mixing for blank and modified phenylethylene
It closes and the additive for mixing 0.2~0.3 times of blank quality is added in object, be 30~45 DEG C in temperature, revolving speed is 300~450r/min
Under conditions of be stirred 20~30min after, obtain blank, water mixed with initiator 30:1~40:1 in mass ratio, in temperature
It is 30~40 DEG C, under conditions of revolving speed is 300~400r/min, after being stirred 20~40min, bottom liquid is obtained, by blank and bottom
Liquid 8:3 in mass ratio mixing is 80~85 DEG C in temperature, under conditions of revolving speed is 300~400r/min, is stirred to react 2~3h
Afterwards, cotton fabric stiffening agent blank is obtained, adjusts cotton fabric stiffening agent base with the sodium hydroxide solution that mass fraction is 5~10%
The pH to 6~7 of material, obtains cotton fabric stiffening agent.The TEPM is methacryloxypropyl.It is described to draw
Hair agent is potassium peroxydisulfate, any one in sodium peroxydisulfate or azodiisobutyronitrile.The ethyl orthosilicate mixture is by positive silicon
Acetoacetic ester and ethyl alcohol 1:8~1 in mass ratio；10 mixing, obtain ethyl orthosilicate mixture.The Ethanol-Acetic Acid mixture is by second
1:1 is mixed alcohol by volume with acetic acid, obtains Ethanol-Acetic Acid mixture.The silane coupling agent is silane resin acceptor kh-550, silicon
Any one in alkane coupling agent KH-560 or Silane coupling reagent KH-570.The organic solvent is cyclohexanone, dimethylbenzene or toluene
In any one.The emulsifier is emulsifier op-10, any one in emulsifier AEO-7 or emulsifier 1303.Example 1
Epoxidized soybean oil is mixed with hydrogen peroxide 8:1 in mass ratio, and is added into the mixture of epoxidized soybean oil and hydrogen peroxide
The acetic acid that 0.3 times of Quaity of Epoxidized Soybean Oil is 85 DEG C in temperature, under conditions of revolving speed is 400r/min, is stirred to react 40min
Afterwards, pretreatment epoxidized soybean oil is obtained, pretreatment epoxidized soybean oil is mixed with nickel 50:1 in mass ratio, and big to pretreatment epoxy
Hydrogen is passed through with the rate of 8mL/min in the mixture of soya-bean oil and nickel, is 70 DEG C in temperature, revolving speed is the condition of 400r/min
Under, after being stirred to react 2h, obtain modified epoxy soybean oil；According to parts by weight, it successively weighs: 205 parts of toluene, 165 parts of TEPM, 42
Toluene and TEPM are mixed in four-hole boiling flask by part styrene and 4 parts of initiators, and styrene is added into four-hole boiling flask and draws
Agent is sent out, nitrogen is passed through into four-hole boiling flask with the rate of 12mL/min, is 90 DEG C in temperature, revolving speed is the condition of 400r/min
Under, after being stirred to react 4h, modified phenylethylene mixture is obtained, modified phenylethylene mixture is mixed with petroleum ether 1:3 in mass ratio,
It is 60 DEG C in temperature, under conditions of revolving speed is 400r/min, after being stirred 40min, filtering obtains modified phenylethylene；Carbon is received
Mitron and dehydrated alcohol 1:100 in mass ratio are mixed in three-necked flask, the ultrasonic disperse 2h under conditions of frequency is 55kHz
Afterwards, the pH to 10 of material in three-necked flask is adjusted with the potassium hydroxide solution that mass fraction is 17%, and is 88 DEG C in temperature, is turned
Under conditions of speed is 400r/min, after being stirred to react 8h, the pH of material in three-necked flask is adjusted with the hydrochloric acid that mass fraction is 12%
It to neutrality, filters, must pre-process carbon nanotube blank, will pre-process after carbon nanotube blank is washed with water 6 times, and be in temperature
After being dried in vacuo 4h under conditions of 70 DEG C, pretreatment carbon nanotube is obtained, the second that carbon nanotube will be pre-processed and mass fraction is 60%
Alcohol solution 1:250 in mass ratio mixing must pre-process carbon nanometer under conditions of frequency is 55kHz after ultrasonic disperse 70min
The ammonium hydroxide 35:1 in mass ratio for pre-processing carbon nanotube mixture and mass fraction is 24% is mixed in flask by pipe mixture,
And pretreatment carbon nanotube mixture matter is added dropwise into flask with the rate of 18mL/min under frequency is the ultrasound condition of 55kHz
The ethyl orthosilicate mixture of 0.2 times of amount after being added dropwise, is 45 DEG C in temperature, under conditions of revolving speed is 400r/min, stirs
After mixing 18h, pre- modified carbon nano-tube mixture is obtained, pre- modified carbon nano-tube mixture and Ethanol-Acetic Acid mixture are pressed into matter
Amount is mixed in reaction kettle than 120:1, and the silane of 0.08 times of pre- modified carbon nano-tube mixture quality is added into reaction kettle
Coupling agent is 45 DEG C in temperature, after revolving speed is stirred 6h under conditions of being 400r/min, filters, obtain modified carbon nano tube pipe
Material after modified carbon nano tube blank is washed with water 8 times, after being dried in vacuo 3h under conditions of being 70 DEG C in temperature, obtains carbon modified
Nanotube；Modified carbon nano-tube is mixed with modified epoxy soybean oil 8:1 in mass ratio, and to modified carbon nano-tube and is modified ring
Be added in the mixture of oxygen soybean oil 6 times of modified carbon nano-tube quality organic solvent and 0.2 times of modified carbon nano-tube quality
Dicyclohexyl diimine is 80 DEG C in temperature, and under conditions of revolving speed is 400r/min, after being stirred to react 3h, filtering must be added
Agent；Acrylic acid is mixed with methyl methacrylate 3:1 in mass ratio, and to the mixture of acrylic acid and methyl methacrylate
The middle hydroxyethyl methacrylate for being added 0.6 times of acrylic acid quality, the butyl acrylate that 0.4 times of acrylic acid quality, acrylic acid matter
8 times of water and 0.2 times of acrylic acid quality of emulsifier are measured, is 60 DEG C in temperature, revolving speed stirs mixed under conditions of being 400r/min
After closing 90min, mixing blank is obtained, blank will be mixed and mixed with modified phenylethylene 10:3 in mass ratio, and to mixing blank and changed
Property styrene mixture in be added and mix 0.3 times of blank quality of additive, be 45 DEG C in temperature, revolving speed is 450r/min's
Under the conditions of be stirred 30min after, obtain blank, water mixed with initiator 40:1 in mass ratio, be 40 DEG C in temperature, revolving speed is
Under conditions of 400r/min, after being stirred 40min, bottom liquid is obtained, blank is mixed with bottom liquid 8:3 in mass ratio, is in temperature
85 DEG C, under conditions of revolving speed is 400r/min, after being stirred to react 3h, cotton fabric stiffening agent blank is obtained, is 10% with mass fraction
Sodium hydroxide solution adjust cotton fabric stiffening agent blank pH to 7, obtain cotton fabric stiffening agent.The TEPM is methyl-prop
Alkene acryloxypropylethoxysilane triethoxysilane.The initiator is potassium peroxydisulfate.The ethyl orthosilicate mixture is by positive silicic acid
Ethyl ester and ethyl alcohol in mass ratio 1；10 mixing, obtain ethyl orthosilicate mixture.The Ethanol-Acetic Acid mixture is by ethyl alcohol and acetic acid
1:1 is mixed by volume, obtains Ethanol-Acetic Acid mixture.The silane coupling agent is silane resin acceptor kh-550.It is described organic molten
Agent is dimethylbenzene.The emulsifier is emulsifier op-10.Example 2
Epoxidized soybean oil is mixed with hydrogen peroxide 8:1 in mass ratio, and is added into the mixture of epoxidized soybean oil and hydrogen peroxide
The acetic acid that 0.3 times of Quaity of Epoxidized Soybean Oil is 85 DEG C in temperature, under conditions of revolving speed is 400r/min, is stirred to react 40min
Afterwards, pretreatment epoxidized soybean oil is obtained, pretreatment epoxidized soybean oil is mixed with nickel 50:1 in mass ratio, and big to pretreatment epoxy
Hydrogen is passed through with the rate of 8mL/min in the mixture of soya-bean oil and nickel, is 70 DEG C in temperature, revolving speed is the condition of 400r/min
Under, after being stirred to react 2h, obtain modified epoxy soybean oil；Carbon nanotube and dehydrated alcohol 1:100 in mass ratio are mixed in three mouthfuls
In flask, under conditions of frequency is 55kHz after ultrasonic disperse 2h, three are adjusted with the potassium hydroxide solution that mass fraction is 17%
The pH to 10 of material in mouth flask, and be 88 DEG C in temperature, under conditions of revolving speed is 400r/min, after being stirred to react 8h, use matter
The pH of material in the hydrochloric acid adjusting three-necked flask that score is 12% is measured to neutrality, suction filtration must pre-process carbon nanotube blank, will be pre-
Processing carbon nanotube blank be washed with water 6 times after, and in temperature be 70 DEG C under conditions of be dried in vacuo 4h after, carbon must be pre-processed and received
The ethanol water 1:250 in mass ratio for pre-processing carbon nanotube with mass fraction is 60% is mixed, is in frequency by mitron
Under conditions of 55kHz after ultrasonic disperse 70min, obtain pretreatment carbon nanotube mixture, will pretreatment carbon nanotube mixture with
Mass fraction be 24% ammonium hydroxide 35:1 in mass ratio be mixed in flask, and in frequency be 55kHz ultrasound condition under with
The ethyl orthosilicate mixture of 0.2 times of carbon nanotube mixture quality of pretreatment, drop are added dropwise into flask for the rate of 18mL/min
After adding, it is 45 DEG C in temperature, under conditions of revolving speed is 400r/min, after being stirred 18h, it is mixed obtains pre- modified carbon nano-tube
Object is closed, pre- modified carbon nano-tube mixture and Ethanol-Acetic Acid mixture 120:1 in mass ratio are mixed in reaction kettle, and to
The silane coupling agent of 0.08 times of pre- modified carbon nano-tube mixture quality is added in reaction kettle, is 45 DEG C in temperature, revolving speed is
After being stirred 6h under conditions of 400r/min, filters, obtain modified carbon nano tube blank, modified carbon nano tube blank is washed with water
After washing 8 times, after being dried in vacuo 3h under conditions of being 70 DEG C in temperature, modified carbon nano-tube is obtained；By modified carbon nano-tube and modification
Epoxidized soybean oil 8:1 in mass ratio mixing, and be added and be modified into the mixture of modified carbon nano-tube and modified epoxy soybean oil
The organic solvent and 0.2 times of modified carbon nano-tube quality of dicyclohexyl diimine that 6 times of carbon nanotube mass, in temperature be 80
DEG C, under conditions of revolving speed is 400r/min, after being stirred to react 3h, filtering obtains additive；By acrylic acid and methyl methacrylate
3:1 in mass ratio is mixed, and the methyl of 0.6 times of acrylic acid quality is added into the mixture of acrylic acid and methyl methacrylate
Hydroxy-ethyl acrylate, the butyl acrylate that 0.4 times of acrylic acid quality, the water that 8 times of acrylic acid quality and 0.2 times of acrylic acid quality
Emulsifier is 60 DEG C in temperature, after revolving speed is stirred 90min under conditions of being 400r/min, obtains mixing blank, will mix base
Material is mixed with styrene 10:3 in mass ratio, and mixes blank quality 0.3 with addition in the mixture of styrene to mixing blank
Times additive, in temperature be 45 DEG C, revolving speed be 450r/min under conditions of be stirred 30min after, obtain blank, by water with draw
Agent 40:1 in mass ratio mixing is sent out, is 40 DEG C in temperature, under conditions of revolving speed is 400r/min, after being stirred 40min, obtains bottom
Liquid mixes blank with bottom liquid 8:3 in mass ratio, is 85 DEG C in temperature, under conditions of revolving speed is 400r/min, is stirred to react 3h
Afterwards, cotton fabric stiffening agent blank is obtained, adjusts cotton fabric stiffening agent blank with the sodium hydroxide solution that mass fraction is 10%
PH to 7 obtains cotton fabric stiffening agent.The initiator is potassium peroxydisulfate.The ethyl orthosilicate mixture is by positive silicic acid second
Ester and ethyl alcohol in mass ratio 1；10 mixing, obtain ethyl orthosilicate mixture.The Ethanol-Acetic Acid mixture presses ethyl alcohol and acetic acid
Volume ratio 1:1 mixing, obtains Ethanol-Acetic Acid mixture.The silane coupling agent is silane resin acceptor kh-550.The organic solvent
For dimethylbenzene.The emulsifier is emulsifier op-10.Example 3
Epoxidized soybean oil is mixed with hydrogen peroxide 8:1 in mass ratio, and is added into the mixture of epoxidized soybean oil and hydrogen peroxide
The acetic acid that 0.3 times of Quaity of Epoxidized Soybean Oil is 85 DEG C in temperature, under conditions of revolving speed is 400r/min, is stirred to react 40min
Afterwards, pretreatment epoxidized soybean oil is obtained, pretreatment epoxidized soybean oil is mixed with nickel 50:1 in mass ratio, and big to pretreatment epoxy
Hydrogen is passed through with the rate of 8mL/min in the mixture of soya-bean oil and nickel, is 70 DEG C in temperature, revolving speed is the condition of 400r/min
Under, after being stirred to react 2h, obtain modified epoxy soybean oil；According to parts by weight, it successively weighs: 205 parts of toluene, 165 parts of TEPM, 42
Toluene and TEPM are mixed in four-hole boiling flask by part styrene and 4 parts of initiators, and styrene is added into four-hole boiling flask and draws
Agent is sent out, nitrogen is passed through into four-hole boiling flask with the rate of 12mL/min, is 90 DEG C in temperature, revolving speed is the condition of 400r/min
Under, after being stirred to react 4h, modified phenylethylene mixture is obtained, modified phenylethylene mixture is mixed with petroleum ether 1:3 in mass ratio,
It is 60 DEG C in temperature, under conditions of revolving speed is 400r/min, after being stirred 40min, filtering obtains modified phenylethylene；Carbon is received
Mitron is mixed with modified epoxy soybean oil 8:1 in mass ratio, and is added into the mixture of carbon nanotube and modified epoxy soybean oil
Enter 6 times of carbon nanotube mass of organic solvent and 0.2 times of carbon nanotube mass of dicyclohexyl diimine, in temperature be 80 DEG C,
Under conditions of revolving speed is 400r/min, after being stirred to react 3h, filtering obtains additive；Acrylic acid and methyl methacrylate are pressed
Mass ratio 3:1 is mixed, and the methyl-prop of 0.6 times of acrylic acid quality is added into the mixture of acrylic acid and methyl methacrylate
Olefin(e) acid hydroxyl ethyl ester, the butyl acrylate that 0.4 times of acrylic acid quality, the water and 0.2 times of acrylic acid quality of cream that 8 times of acrylic acid quality
Agent is 60 DEG C in temperature, after revolving speed is stirred 90min under conditions of being 400r/min, obtains mixing blank, will mix blank
It is mixed with modified phenylethylene 10:3 in mass ratio, and mixes blank matter with addition in the mixture of modified phenylethylene to mixing blank
The additive of 0.3 times of amount is 45 DEG C in temperature, after revolving speed is stirred 30min under conditions of being 450r/min, obtains blank, will
Water is mixed with initiator 40:1 in mass ratio, is 40 DEG C in temperature, under conditions of revolving speed is 400r/min, is stirred 40min
Afterwards, bottom liquid is obtained, blank is mixed with bottom liquid 8:3 in mass ratio, is 85 DEG C in temperature, under conditions of revolving speed is 400r/min, stirs
After mixing reaction 3h, cotton fabric stiffening agent blank is obtained, cotton fabric is adjusted with the sodium hydroxide solution that mass fraction is 10% and is used and endured with all one's will
The pH to 7 of agent blank, obtains cotton fabric stiffening agent.The TEPM is methacryloxypropyl.It is described
Initiator is potassium peroxydisulfate.The organic solvent is dimethylbenzene.The emulsifier is emulsifier op-10.
Example 4
According to parts by weight, successively weigh: 205 parts of toluene, 165 parts of TEPM, 42 parts of styrene and 4 parts of initiators, by toluene with
TEPM is mixed in four-hole boiling flask, and styrene and initiator are added into four-hole boiling flask, with the rate of 12mL/min to four mouthfuls
It is passed through nitrogen in flask, is 90 DEG C in temperature, under conditions of revolving speed is 400r/min, after being stirred to react 4h, obtains modified phenylethylene
Mixture mixes modified phenylethylene mixture with petroleum ether 1:3 in mass ratio, in temperature be 60 DEG C, revolving speed 400r/min
Under conditions of, after being stirred 40min, filtering obtains modified phenylethylene；By carbon nanotube and dehydrated alcohol 1:100 in mass ratio
It is mixed in three-necked flask, under conditions of frequency is 55kHz after ultrasonic disperse 2h, the potassium hydroxide for being 17% with mass fraction
Solution adjusts the pH to 10 of material in three-necked flask, and is 88 DEG C in temperature, under conditions of revolving speed is 400r/min, is stirred to react
After 8h, the pH for adjusting material in three-necked flask with the hydrochloric acid that mass fraction is 12% filters to neutrality, obtains pretreatment carbon nanotube
Blank, will pretreatment carbon nanotube blank be washed with water 6 times after, and in temperature be 70 DEG C under conditions of be dried in vacuo 4h after, obtain
Carbon nanotube is pre-processed, the ethanol water 1:250 in mass ratio for pre-processing carbon nanotube with mass fraction is 60% is mixed,
Under conditions of frequency is 55kHz after ultrasonic disperse 70min, pretreatment carbon nanotube mixture is obtained, carbon nanotube will be pre-processed
The ammonium hydroxide 35:1 in mass ratio that mixture and mass fraction are 24% is mixed in flask, and in the ultrasound condition that frequency is 55kHz
Under be added dropwise with the rate of 18mL/min into flask pretreatment 0.2 times of carbon nanotube mixture quality ethyl orthosilicate mixing
Object after being added dropwise, is 45 DEG C in temperature, under conditions of revolving speed is 400r/min, after being stirred 18h, obtains pre- carbon modified and receive
Pre- modified carbon nano-tube mixture and Ethanol-Acetic Acid mixture 120:1 in mass ratio are mixed in reaction kettle by nanotube mixture
In, and the silane coupling agent of 0.08 times of pre- modified carbon nano-tube mixture quality is added into reaction kettle, it is 45 DEG C in temperature, turns
After speed is stirred 6h under conditions of being 400r/min, filters, obtain modified carbon nano tube blank, modified carbon nano tube blank is used
After water washing 8 times, after being dried in vacuo 3h under conditions of being 70 DEG C in temperature, modified carbon nano-tube is obtained to get additive；By propylene
Acid is mixed with methyl methacrylate 3:1 in mass ratio, and is added third into the mixture of acrylic acid and methyl methacrylate
The hydroxyethyl methacrylate that 0.6 times of olefin(e) acid quality, the butyl acrylate that 0.4 times of acrylic acid quality, the water that 8 times of acrylic acid quality
With 0.2 times of emulsifier of acrylic acid quality, in temperature be 60 DEG C, revolving speed be 400r/min under conditions of be stirred 90min after,
Blank must be mixed, mixing blank is mixed with modified phenylethylene 10:3 in mass ratio, and to mixing blank and modified phenylethylene
The additive of 0.3 times of blank quality of mixing is added in mixture, is 45 DEG C in temperature, revolving speed stirs under conditions of being 450r/min
After mixing 30min, blank is obtained, water is mixed with initiator 40:1 in mass ratio, is 40 DEG C in temperature, revolving speed is 400r/min's
Under the conditions of, after being stirred 40min, bottom liquid is obtained, blank is mixed with bottom liquid 8:3 in mass ratio, is 85 DEG C in temperature, revolving speed is
Under conditions of 400r/min, after being stirred to react 3h, cotton fabric stiffening agent blank is obtained, the sodium hydroxide for being 10% with mass fraction
Solution adjusts the pH to 7 of cotton fabric stiffening agent blank, obtains cotton fabric stiffening agent.The TEPM is methacryloxy third
Ethyl triethoxy silicane alkane.The initiator is potassium peroxydisulfate.The ethyl orthosilicate mixture is by ethyl orthosilicate and ethyl alcohol
In mass ratio 1；10 mixing, obtain ethyl orthosilicate mixture.The Ethanol-Acetic Acid mixture is by ethyl alcohol and acetic acid by volume 1:
1 mixing, obtains Ethanol-Acetic Acid mixture.The silane coupling agent is silane resin acceptor kh-550.The organic solvent is diformazan
Benzene.The emulsifier is emulsifier op-10.
Comparative example: the cotton fabric stiffening agent of Science and Technology Ltd. of Jiangyin City production.
By example 1 to the resulting cotton fabric stiffening agent of example 4 and comparative example product, performance detection is carried out, it is specific to detect
Method is as follows:
Bending length: its bending length is tested according to GB/T18318.
Water-wash resistance: the cotton after example 1 to 4 resulting cotton fabric stiffening agent of example and comparative example product treatment is knitted
Object after washing 5 times, tests bending length in the water that temperature is 25 DEG C.
Specific testing result is as shown in table 1:
Table 1 cotton fabric stiffening agent performance test results
By 1 testing result of table it is found that the cotton fabric of technical solution of the present invention preparation stiffening agent has excellent stiffening effect, and
With preferable waterproofness, stiffening effect is lasting.
Claims (9)
1. a kind of preparation method of cotton fabric stiffening agent, which is characterized in that specific preparation step are as follows:
(1) according to parts by weight, it successively weighs: 200~205 parts of toluene, 160~165 parts of TEPM, 40~42 parts of styrene and 2
Toluene is mixed with TEPM, and styrene and initiator is added by~4 parts of initiators, under nitrogen atmosphere, after being stirred to react, is obtained
Modified phenylethylene mixture mixes modified phenylethylene mixture with petroleum ether 1:2~1:3 in mass ratio, and filtering obtains modified benzene
Ethylene；
(2) carbon nanotube is mixed with dehydrated alcohol 1:80~1:100 in mass ratio, after ultrasonic disperse, adjusts pH to 8~10,
It is stirred to react, and adjusts pH to neutrality, filter washing, drying obtains pretreatment carbon nanotube, will pretreatment carbon nanotube and ethyl alcohol
Aqueous solution 1:200~1:250 in mass ratio mixing, ultrasonic disperse obtain pretreatment carbon nanotube mixture, will pre-process carbon nanometer
Pipe mixture is mixed with ammonium hydroxide 20:1~35:1 in mass ratio, and pretreatment carbon nanotube mixture matter is added dropwise under ultrasound condition
The ethyl orthosilicate mixture of 0.1~0.2 times of amount, after being stirred, obtains pre- modified carbon nano-tube mixture, pre- carbon modified is received
Nanotube mixture is mixed with Ethanol-Acetic Acid mixture 100:1~120:1 in mass ratio, and pre- modified carbon nano-tube mixing is added
The silane coupling agent that 0.05~0.08 times of amount of substance after being stirred, is filtered, is washed, dry, obtains modified carbon nano-tube；
(3) modified carbon nano-tube is mixed with modified epoxy soybean oil 5:1~8:1 in mass ratio, and modified carbon nano-tube is added
The organic solvent and 0.1~0.2 times of modified carbon nano-tube quality of dicyclohexyl diimine that 5~6 times of quality, after being stirred to react,
Filtering, obtains additive；
(4) acrylic acid is mixed with methyl methacrylate 2:1~3:1 in mass ratio, and acrylic acid quality 0.3~0.6 is added
Times hydroxyethyl methacrylate, the butyl acrylate that 0.2~0.4 times of acrylic acid quality, the water that 5~8 times of acrylic acid quality and
The emulsifier that 0.1~0.2 times of acrylic acid quality after being stirred, obtains mixing blank, and mixing blank and modified phenylethylene are pressed matter
Amount is mixed than 10:2~10:3, and the additive of 0.2~0.3 times of blank quality of mixing is added, and is stirred, is obtained blank, by water
It is mixed with initiator 30:1~40:1 in mass ratio, obtains bottom liquid, blank is mixed with bottom liquid 8:3 in mass ratio, after being stirred to react,
PH to 6~7 is adjusted, cotton fabric stiffening agent is obtained.
2. a kind of preparation method of cotton fabric stiffening agent according to claim 1, it is characterised in that: step (1) is described
TEPM is methacryloxypropyl.
3. a kind of preparation method of cotton fabric stiffening agent according to claim 1, it is characterised in that: the initiator is
Any one in potassium peroxydisulfate, sodium peroxydisulfate or azodiisobutyronitrile.
4. a kind of preparation method of cotton fabric stiffening agent according to claim 1, it is characterised in that: step (2) is described
Ethyl orthosilicate mixture is by ethyl orthosilicate and ethyl alcohol 1:8~1 in mass ratio；10 mixing, obtain ethyl orthosilicate mixture.
5. a kind of preparation method of cotton fabric stiffening agent according to claim 1, it is characterised in that: step (2) is described
By ethyl alcohol, 1:1 is mixed Ethanol-Acetic Acid mixture by volume with acetic acid, obtains Ethanol-Acetic Acid mixture.
6. a kind of preparation method of cotton fabric stiffening agent according to claim 1, it is characterised in that: step (2) is described
Silane coupling agent is silane resin acceptor kh-550, any one in silane coupling agent KH-560 or Silane coupling reagent KH-570.
7. a kind of preparation method of cotton fabric stiffening agent according to claim 1, it is characterised in that: step (3) is described
Organic solvent is cyclohexanone, any one in dimethylbenzene or toluene.
8. a kind of preparation method of cotton fabric stiffening agent according to claim 1, it is characterised in that: step (4) is described
Emulsifier is emulsifier op-10, any one in emulsifier AEO-7 or emulsifier 1303.
9. a kind of preparation method of cotton fabric stiffening agent according to claim 1, it is characterised in that: step (3) is described
Modified epoxy soybean oil is to mix epoxidized soybean oil with hydrogen peroxide 5:1~8:1 in mass ratio, and Quaity of Epoxidized Soybean Oil is added
0.2~0.3 times of acetic acid after being stirred to react, obtains pretreatment epoxidized soybean oil, in mass ratio with nickel by pretreatment epoxidized soybean oil
30:1~50:1 mixing, and under atmosphere of hydrogen, it is stirred to react, obtains modified epoxy soybean oil.
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| CN112981645A (en) * | 2021-02-07 | 2021-06-18 | 康宝莱(宁波)织造有限公司 | Environment-friendly wool knot colored point fancy yarn and preparation method thereof |
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