CN107337758A - A kind of water-fastness environmental-friendly stiffening agent and preparation method thereof - Google Patents

A kind of water-fastness environmental-friendly stiffening agent and preparation method thereof Download PDF

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Publication number
CN107337758A
CN107337758A CN201611034525.2A CN201611034525A CN107337758A CN 107337758 A CN107337758 A CN 107337758A CN 201611034525 A CN201611034525 A CN 201611034525A CN 107337758 A CN107337758 A CN 107337758A
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China
Prior art keywords
stiffening agent
water
water resistance
reactor
mix monomer
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CN201611034525.2A
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Chinese (zh)
Inventor
谭阁
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Transfar Forland Fine Chemicals Foshan Co Ltd
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Transfar Forland Fine Chemicals Foshan Co Ltd
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Priority to CN201611034525.2A priority Critical patent/CN107337758A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F218/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid
    • C08F218/02Esters of monocarboxylic acids
    • C08F218/04Vinyl esters
    • C08F218/08Vinyl acetate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/12Polymerisation in non-solvents
    • C08F2/16Aqueous medium
    • C08F2/22Emulsion polymerisation
    • C08F2/24Emulsion polymerisation with the aid of emulsifying agents
    • C08F2/30Emulsion polymerisation with the aid of emulsifying agents non-ionic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/327Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
    • D06M15/333Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof of vinyl acetate; Polyvinylalcohol

Abstract

The invention discloses a kind of water resistance environmental-friendly stiffening agent, it is characterised in that:The water resistance environmental-friendly stiffening agent includes mix monomer, water-soluble, film-forming colloid, emulsifying agent, initiator and deionized water, said components:40 60 parts of mix monomer, 15 parts of water-soluble, film-forming colloid, 15 parts of emulsifying agent, 0.5 1 parts of initiator, 25 40 parts of deionized water.The water resistance environmental-friendly stiffening agent of the present invention both meets environmental requirement, but also with excellent wash durability.

Description

A kind of water-fastness environmental-friendly stiffening agent and preparation method thereof
Technical field
The present invention relates to the processing aid in a kind of textile printing and dyeing, specifically a kind of water resistance environmental-friendly stiffening agent and its system Preparation Method.
Background technology
At present, when the processing of the fabrics such as cloth, wall paper, suitcase cloth is played in such as casement, directly, fabric needs to have after machining There is certain stiffness.Especially warp knit type fabric, the stiffness after the processing of its fabric have strict requirements.Stiffening agent is should With quite varied textile auxiliary, it makes fabric have stiffening characteristic by assigning fabric elasticity and sense of fullness.Pass The stiffening agent of system mainly has four kinds of polyacrylate, Lauxite, polyvinyl acetate and vinegar propylene copolymer, but above-mentioned stiffening agent It is respectively provided with itself unsurmountable technological deficiency.The stiffening effect of polyacrylate is good, but its durability extreme difference on fabric, And have it is heated it is tacky, be cooled the defects of becoming fragile;Lauxite is stiffening to work well, but its content of formaldehyde after processing is high, with The continuous reinforcement of people's environmental consciousness and the progressively constraint of related environmental regulation, it can not meet that increasingly strict fabric adds Work demand;Polyvinyl acetate is the most long hard finishing auxiliary agent of application time, its biggest advantage is that formaldehyde is free of, but its is hard Very property is poor, and has the shortcomings that water resistance, weatherability difference;The stiffening effect of vinegar propylene copolymer is good and is free of formaldehyde, so it should With also more and more extensive, but its wash durability extreme difference after being arranged to fabric, it is mainly shown as fabric hard finishing Moisture regain softens afterwards, and hardness declines obvious after washing.
Based on drawbacks described above, the various modes for once occurring stiffening agent in yarn fabric processing aid industry are improved.Such as in public affairs The number of opening is in CN1524911A Chinese patent literature, is disclosed a kind of more for timber, paper, fiberboard, foamed plastics etc. The synthesis of the polyvinyl acetate emulsion of the bonding of Porous materials and preparation method.Be primary raw material with vinegar third, compound nertralizer, Emulsion is aggregated into the presence of the materials such as initiator, surfactant.But above-mentioned emulsion has the shortcomings that solid content is relatively low, and should Emulsion is directed to the adhesive property of material, thus cannot be used for the hard finishing of fabric.
And in Publication No. CN102433750B Chinese patent literature, then disclose one kind and be applied to fabric hard finishing Environmental-friendly stiffening agent and preparation method, with vinyl acetate, acrylate etc. for primary raw material, aggregated into the presence of initiator Emulsion.The solid content of the emulsion can reach 50% or so, and it is preferable that effect is endured with all one's will in textile finishing.But its wash durability still compared with Difference, the situation that moisture regain softens equally occurs after fabric hard finishing, its hardness declines fairly obvious after especially washing.
Therefore, how to develop it is a kind of there is excellent wash durability, may conform to the cloth hard finishing agent of ecological requirements again is One of significant technology issues of yarn fabric processing aid industry at present.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide one kind both to meet environmental requirement, but also with excellent The water resistance environmental-friendly stiffening agent of wash durability.
Another object of the present invention is to provide, a kind of technique is simple, reaction stability is strong prepares above-mentioned water resistance environmental protection The method of stiffening agent.
What the goal of the invention of the present invention was realized in:A kind of water resistance environmental-friendly stiffening agent, it is characterised in that:It is described water-fast Property environmental-friendly stiffening agent includes mix monomer, water-soluble, film-forming colloid, emulsifying agent, initiator and deionized water, and said components press matter Measuring number is respectively:Mix monomer 40-60 parts, water-soluble, film-forming colloid 1-5 parts, emulsifying agent 1-5 parts, initiator 0.5-1 parts, Deionized water 25-40 parts.
Furtherly, mix monomer includes vinyl acetate, acrylate and function monomer, and three kinds of component contents press quality hundred It is respectively vinyl acetate 80-90%, acrylate 5-10%, function monomer 5-10% to divide than calculating.
Furtherly, acrylate is methyl acrylate or butyl acrylate.
Furtherly, function monomer is diisooctyl maleate or dibutyl maleate.
Furtherly, water-soluble, film-forming colloid is polyvinyl alcohol 1788 and one kind in polyvinyl alcohol 1799 or arbitrarily to compare Example mixing.
Furtherly, emulsifying agent be AEO, isomeric alcohol polyethenoxy ether, castor oil polyoxyethylene ether, One kind in alkyl polyoxyethylene ether is mixed with arbitrary proportion.
Furtherly, initiator is potassium peroxydisulfate, sodium peroxydisulfate, one kind in ammonium persulfate or mixed with arbitrary proportion.
The present invention also provides a kind of method for preparing above-mentioned water resistance environmental-friendly stiffening agent, as follows the step of this method:
a:Corresponding raw material for standby is weighed according to said ratio;
b:Vinyl acetate, acrylate and function monomer are added in the container with agitating device, at normal temperatures and pressures It is standby to be stirred until homogeneous into mix monomer;
c:Under normal temperature and pressure, water-soluble, film-forming colloid and deionized water quality are added in the reactor with agitating device The 60-80% of total amount, is then stirred until homogeneous;
d:Toward adding emulsifying agent in mixture obtained by step c in the state of the lasting stirring, and temperature of reactor is lifted To 40-60 DEG C, then toward being passed through nitrogen in reactor;
e:Temperature of reactor is maintained 40-60 DEG C, adds and draws in being incubated after 1-2 hours toward mixture obtained by Step d Mix monomer obtained by agent and b step to be sent out, and continues stirring until it uniformly, mix monomer addition is the 10-15% of its gross mass, Initiator addition is the 10-15% of its gross mass;
f:Temperature of reactor is promoted to 70-80 DEG C and is incubated, while remaining mix monomer and initiator is added dropwise, during dropwise addition Between 3-6 hours;
g:After f steps are added dropwise to complete, temperature of reactor is promoted to 85-95 DEG C, and isothermal reaction 20-40 minutes, then Temperature of reactor is down to 65-75 DEG C, then balance deionized water, water resistance environmental protection can be obtained firmly by being finally stirred until homogeneous discharging Very agent.
The present invention is improved to the fabric stiffening agent of prior art, and its advantage is as follows:
1st, in water resistance environmental-friendly stiffening agent of the invention, mix monomer, water-soluble, film-forming colloid and emulsifying agent are employed Combined type reaction system.First, water-soluble, film-forming colloid can form the extremely strong colloid film of cohesive in reaction system, and this is thin Surface tension when film can pass through infiltration is adhered to the fiber surface of fabric, so as to improve stiffening agent when arranging and fiber it is viscous Conjunction ability, the wash durability of stiffening agent greatly improved.Meanwhile there is collaboration breast between water-soluble, film-forming colloid and emulsifying agent Change effect, the dispersive property of emulsification system can be improved in the reaction.Secondly, mix monomer employs vinyl acetate, acrylate With the compound system of function monomer.Vinyl acetate has good bond properties, and belongs to lower-cost in reaction system Hard monomer.Acrylate then has excellent compatibility and copolyreaction, and reactant can be greatly improved by matching with vinyl acetate The water-wash resistance of system, and can effectively improve the defects of vinyl acetate weatherability is poor.In addition, above-mentioned combined type reaction system is being entered Row does not produce formaldehyde or containing formaldehyde gas after arranging, stiffening agent is met the requirement of environmental protection processing.
2nd, in water resistance environmental-friendly stiffening agent of the invention, function monomer uses diisooctyl maleate or maleic two Dibutyl phthalate.Diisooctyl maleate itself has extremely strong surface-active and more active hydrogen group, and it is except can be big , can be using active hydrogen group as base between width reduction mix monomer, water-soluble, film-forming colloid and emulsifying agent outside two-phase surface tension Point forms IPN cross-linked network molecular structure, so as to improve the dispersive property of stiffening agent and wash durability.And maleic two Dibutyl phthalate in addition to equally there is more active hydrogen group and good dispersive property, its also have excellent wetting capacity and Greasy property, cladding ability and uniformity of the stiffening agent on fabric fibre can be improved.
3rd, in water resistance environmental-friendly stiffening agent of the invention, employ AEO, isomeric alcohol polyethenoxy ether, The compound emulsion system of castor oil polyoxyethylene ether, alkyl polyoxyethylene ether.Pass through said components emulsifying capacity and surface-active Combination, make in the deep fibrous that stiffening agent fully can infiltrate into fabric during arrangement, so as to improve the reaction of stiffening agent Uniformity.
4th, water resistance environmental-friendly stiffening agent of the invention is prepared using secondary mixing titration, and reaction environment is in all the time Less than 100 DEG C.Water-soluble, film-forming colloid and emulsifying agent first first carries out film formation reaction, and adds a certain amount of mix monomer and draw Send out agent and carry out an emulsion reaction, then remaining mix monomer and initiator are added in chemical reaction system in a manner of titrating. This method can effectively ensure that mix monomer carries out sufficiently emulsifying film formation reaction in the presence of initiator, and pass through mix monomer In function monomer constantly trigger be copolymerized into chain reaction, make stiffening agent formed the preferable space interpenetrating network of compliance, from And effectively increase the water resistance, chemical proofing and weatherability of stiffening agent.Further, since reaction environment temperature is relatively low, It can avoid the phenomenon of accessory substance or side reaction occur because reaction speed is too fast in whole course of reaction, it is whole so as to improve Prepare the stability of reaction.
Embodiment
The water resistance environmental-friendly stiffening agent of the present invention includes mix monomer, water-soluble, film-forming colloid, emulsifying agent, initiator and gone Ionized water, said components are respectively by mass fraction:Mix monomer 40-60 parts, water-soluble, film-forming colloid 1-5 parts, emulsifying agent 1-5 parts, initiator 0.5-1 parts, deionized water 25-40 parts.Formed using water-soluble, film-forming colloid in reaction system with compared with The colloid film of strong adhesive capacity, improve the wash durability of stiffening agent.And pass through vinyl acetate, acrylate and function list Body forms mix monomer, improves copolyreaction, water-wash resistance and the weatherability of reaction system.Meanwhile stiffening agent of the invention It is formaldehydeless during arrangement to wait disengaging for pernicious gas, the residual of harmful substance will not be also produced after the completion of arrangement, is made hard Very agent meets the requirement of environmental protection processing.
In the water resistance environmental-friendly stiffening agent of the present invention, mix monomer includes vinyl acetate, acrylate and function monomer, and three Kind component content calculates respectively vinyl acetate 80-90%, acrylate 5-10%, function monomer 5-10% by mass percentage. Vinyl acetate has good bond properties, and belongs to lower-cost hard monomer in reaction system, therefore can be used as stiffening The main component of agent, to reduce the processing cost of stiffening agent.Acrylate then has excellent compatibility and copolyreaction, its Reactive group can form the strand of shielding ester group polarity after being copolymerized with vinyl acetate, thus improve reaction system Water-wash resistance, and can effectively improve the defects of vinyl acetate weatherability is poor.In addition, acrylate itself have it is stronger resistance to Oil and heat resistance, it can strengthen the weatherability and solvent resistance of stiffening agent after reaction system is added.
In the water resistance environmental-friendly stiffening agent of the present invention, acrylate can use methyl acrylate or butyl acrylate.Propylene Sour methyl esters and butyl acrylate are the intermediate monomer of organic synthesis, are respectively provided with activated double bonds in both, thus it is in reactant There is excellent copolyreaction performance in system.It is active double meanwhile the Chain Flexibility of methyl acrylate and butyl acrylate is stronger Key can assign the higher bond properties of reaction system and strand deformability after participating in reaction, so as to improve reaction system Water-wash resistance.
In the water resistance environmental-friendly stiffening agent of the present invention, function monomer can use diisooctyl maleate or maleic two Dibutyl phthalate.First, said components are respectively provided with extremely strong surface-active, can reduce mix monomer, water-soluble, film-forming colloid and breast Two-phase surface tension between agent, to improve the dispersive property of stiffening agent.Secondly, said components contain more active hydrogen group, And form IPN cross-linked network molecular structure using it as connection basic point in reaction system.The molecular structure can effectively improve molecule The stability of interchain group connection, so as to improve the wash durability of stiffening agent.
In the water resistance environmental-friendly stiffening agent of the present invention, water-soluble, film-forming colloid is polyvinyl alcohol 1788 and polyvinyl alcohol 1799 In one kind or mixed with arbitrary proportion.Said components have outstanding film forming ability and bond properties, and have after film forming good Good solvent resistance and rub resistance.Polyvinyl alcohol 1788 itself has stronger emulsifying capacity, and can be risen in emulsification system Stabilization, so as to improve the stability of stiffening agent emulsification system;And polyvinyl alcohol 1799 then has good heat resistance, and Play collaboration emulsification in emulsification system, so as to improve the emulsifying capacity of stiffening agent.
In the water resistance environmental-friendly stiffening agent of the present invention, emulsifying agent is using AEO, isomery alcohol polyoxyethylene One kind in ether, castor oil polyoxyethylene ether, alkyl polyoxyethylene ether is mixed with arbitrary proportion.Said components are respectively provided with stronger Emulsifying capacity and surface-active, stiffening agent is infiltrated into when arranging inside the deep fibrous of fabric, and improve stiffening agent The stability of dispersed phase.Meanwhile said components can avoid stiffening agent drop from occurring coacervation during arrangement, so as to improve Uniformity of the stiffening agent when arranging.
In the water resistance environmental-friendly stiffening agent of the present invention, initiator can be used in potassium peroxydisulfate, sodium peroxydisulfate, ammonium persulfate One kind is mixed with arbitrary proportion.Free radical is readily decomposed to after said components are heated, and free radical can be in reaction system The reaction such as free radical grafting, copolymerization, crosslinking is produced with activated double bonds, and because the free radical after decomposition of initiator has itself It is more highly polar, it can effectively strengthen the stability of chemical reaction.
The preparation method of water resistance environmental-friendly stiffening agent of the present invention comprises the following steps:
a:Corresponding raw material for standby is weighed according to said ratio;
b:Vinyl acetate, acrylate and function monomer are added in the container with agitating device, at normal temperatures and pressures It is standby to be stirred until homogeneous into mix monomer;
c:Under normal temperature and pressure, water-soluble, film-forming colloid and deionized water quality are added in the reactor with agitating device The 60-80% of total amount, is then stirred until homogeneous;
d:Toward adding emulsifying agent in mixture obtained by step c in the state of the lasting stirring, and temperature of reactor is lifted To 40-60 DEG C, then toward being passed through nitrogen in reactor;
e:Temperature of reactor is maintained 40-60 DEG C, adds and draws in being incubated after 1-2 hours toward mixture obtained by Step d Mix monomer obtained by agent and b step to be sent out, and continues stirring until it uniformly, mix monomer addition is the 10-15% of its gross mass, Initiator addition is the 10-15% of its gross mass;
f:Temperature of reactor is promoted to 70-80 DEG C and is incubated, while remaining mix monomer and initiator is added dropwise, during dropwise addition Between 3-6 hours;
g:After f steps are added dropwise to complete, temperature of reactor is promoted to 85-95 DEG C, and isothermal reaction 20-40 minutes, then Temperature of reactor is down to 65-75 DEG C, then balance deionized water, water resistance environmental protection can be obtained firmly by being finally stirred until homogeneous discharging Very agent.
By carrying out bending property test (testing standard to the water resistance environmental-friendly stiffening agent of the present invention:GB/T 18318), Bending length of the yarn fabric of the water resistance environmental-friendly stiffening agent arrangement of the present invention after arrangement is used as 7.3-8.2cm;Washing 3 times Bending length is 6.6-7.8cm afterwards;Bending length is 6.1-7.6cm after washing 5 times;Bending length is 5.9- after washing 8 times 7.5cm。
It is described in detail with reference to a pair of each embodiments of table, but does not therefore limit the invention to the implementation In the range of example:
Embodiment 1
The water resistance environmental-friendly stiffening agent of the present invention includes mix monomer, polyvinyl alcohol 1788, AEO, mistake Potassium sulfate and deionized water, said components are respectively by mass fraction:40 parts of mix monomer, 1,788 1 parts of polyvinyl alcohol, fat 1 part of fat alcohol APEO, 0.5 part of potassium peroxydisulfate, 25 parts of deionized water.
Mix monomer includes vinyl acetate, methyl acrylate, diisooctyl maleate, and three kinds of component contents press quality It is respectively vinyl acetate 90%, methyl acrylate or butyl acrylate 5%, diisooctyl maleate 5% that percentage, which is calculated,.
The preparation method of water resistance environmental-friendly stiffening agent of the present invention comprises the following steps:
a:Corresponding raw material for standby is weighed according to said ratio;
b:Vinyl acetate, acrylate and function monomer are added in the container with agitating device, at normal temperatures and pressures It is standby to be stirred until homogeneous into mix monomer;
c:Under normal temperature and pressure, water-soluble, film-forming colloid and deionized water quality are added in the reactor with agitating device The 60% of total amount, is then stirred until homogeneous;
d:Toward adding emulsifying agent in mixture obtained by step c in the state of the lasting stirring, and temperature of reactor is lifted To 40 DEG C, then toward being passed through nitrogen in reactor;
e:Temperature of reactor is maintained 40 DEG C, after insulation 1 hour toward addition initiator in mixture obtained by Step d and Mix monomer obtained by b step, and continue stirring until it uniformly, mix monomer addition is the 10% of its gross mass, and initiator adds Enter 10% that amount is its gross mass;
f:Temperature of reactor is promoted to 70 DEG C and is incubated, while remaining mix monomer and initiator, time for adding 3 is added dropwise Hour;
g:After f steps are added dropwise to complete, temperature of reactor is promoted to 85 DEG C, and isothermal reaction 20 minutes, then reaction Device temperature is down to 65 DEG C, then balance deionized water, and water resistance environmental-friendly stiffening agent can be obtained by being finally stirred until homogeneous discharging.
By carrying out bending property test (testing standard to the water resistance environmental-friendly stiffening agent of the present invention:GB/T 18318), Bending length of the yarn fabric of the water resistance environmental-friendly stiffening agent arrangement of the present invention after arrangement is used as 7.3cm;Wash 3 palintropes Qu Changdu is 6.6cm;Bending length is 6.1cm after washing 5 times;Bending length is 5.9cm after washing 8 times.
Embodiment 2
The water resistance environmental-friendly stiffening agent of the present invention includes mix monomer, polyvinyl alcohol 1788, polyvinyl alcohol 1799, fatty alcohol APEO, isomeric alcohol polyethenoxy ether, castor oil polyoxyethylene ether, alkyl polyoxyethylene ether, potassium peroxydisulfate, persulfuric acid Sodium, ammonium persulfate and deionized water, said components are respectively by mass fraction:60 parts of mix monomer, polyvinyl alcohol 1,788 3 Part, 1,799 2 parts of polyvinyl alcohol, 2 parts of AEO, 1 part of isomeric alcohol polyethenoxy ether, castor oil polyoxyethylene ether 1 Part, 1 part of alkyl polyoxyethylene ether, 0.3 part of potassium peroxydisulfate, 0.3 part of sodium peroxydisulfate, 0.4 part of ammonium persulfate, 40 parts of deionized water.
Mix monomer includes vinyl acetate, butyl acrylate, dibutyl maleate, and three kinds of component contents press quality hundred It is respectively vinyl acetate 80%, butyl acrylate 10%, dibutyl maleate 10% to divide than calculating.
The preparation method of water resistance environmental-friendly stiffening agent of the present invention comprises the following steps:
a:Corresponding raw material for standby is weighed according to said ratio;
b:Vinyl acetate, acrylate and function monomer are added in the container with agitating device, at normal temperatures and pressures It is standby to be stirred until homogeneous into mix monomer;
c:Under normal temperature and pressure, water-soluble, film-forming colloid and deionized water quality are added in the reactor with agitating device The 80% of total amount, is then stirred until homogeneous;
d:Toward adding emulsifying agent in mixture obtained by step c in the state of the lasting stirring, and temperature of reactor is lifted To 60 DEG C, then toward being passed through nitrogen in reactor;
e:Temperature of reactor is maintained 60 DEG C, after insulation 2 hours toward addition initiator in mixture obtained by Step d and Mix monomer obtained by b step, and continue stirring until it uniformly, mix monomer addition is the 15% of its gross mass, and initiator adds Enter 15% that amount is its gross mass;
f:Temperature of reactor is promoted to 80 DEG C and is incubated, while remaining mix monomer and initiator, time for adding 6 is added dropwise Hour;
g:After f steps are added dropwise to complete, temperature of reactor is promoted to 95 DEG C, and isothermal reaction 40 minutes, then reaction Device temperature is down to 75 DEG C, then balance deionized water, and water resistance environmental-friendly stiffening agent can be obtained by being finally stirred until homogeneous discharging.
By carrying out bending property test (testing standard to the water resistance environmental-friendly stiffening agent of the present invention:GB/T 18318), Bending length of the yarn fabric of the water resistance environmental-friendly stiffening agent arrangement of the present invention after arrangement is used as 8.2cm;Wash 3 palintropes Qu Changdu is 7.8cm;Bending length is 7.6cm after washing 5 times;Bending length is 7.5cm after washing 8 times.
Embodiment 3
The water resistance environmental-friendly stiffening agent of the present invention includes mix monomer, polyvinyl alcohol 1799, isomeric alcohol polyethenoxy ether, castor Sesame oil APEO, sodium peroxydisulfate, ammonium persulfate and deionized water, said components are respectively by mass fraction:Mixing is single 43 parts of body, 1,799 2 parts of polyvinyl alcohol, 1 part of isomeric alcohol polyethenoxy ether, 1 part of castor oil polyoxyethylene ether, sodium peroxydisulfate 0.4 Part, 0.3 part of ammonium persulfate, 28 parts of deionized water.
Mix monomer includes vinyl acetate, butyl acrylate, dibutyl maleate, and three kinds of component contents press quality hundred It is respectively vinyl acetate 86%, butyl acrylate 7%, dibutyl maleate 7% to divide than calculating.
The preparation method of water resistance environmental-friendly stiffening agent of the present invention comprises the following steps:
a:Corresponding raw material for standby is weighed according to said ratio;
b:Vinyl acetate, acrylate and function monomer are added in the container with agitating device, at normal temperatures and pressures It is standby to be stirred until homogeneous into mix monomer;
c:Under normal temperature and pressure, water-soluble, film-forming colloid and deionized water quality are added in the reactor with agitating device The 65% of total amount, is then stirred until homogeneous;
d:Toward adding emulsifying agent in mixture obtained by step c in the state of the lasting stirring, and temperature of reactor is lifted To 45 DEG C, then toward being passed through nitrogen in reactor;
e:Temperature of reactor is maintained 44 DEG C, toward adding initiator in mixture obtained by Step d after insulation 1.5 hours And mix monomer obtained by b step, and continuing stirring until it uniformly, mix monomer addition is the 12% of its gross mass, initiator Addition is the 12% of its gross mass;
f:Temperature of reactor is promoted to 73 DEG C and is incubated, while remaining mix monomer and initiator, time for adding is added dropwise 3.5 hour;
g:After f steps are added dropwise to complete, temperature of reactor is promoted to 88 DEG C, and isothermal reaction 25 minutes, then reaction Device temperature is down to 68 DEG C, then balance deionized water, and water resistance environmental-friendly stiffening agent can be obtained by being finally stirred until homogeneous discharging.
By carrying out bending property test (testing standard to the water resistance environmental-friendly stiffening agent of the present invention:GB/T 18318), Bending length of the yarn fabric of the water resistance environmental-friendly stiffening agent arrangement of the present invention after arrangement is used as 7.6cm;Wash 3 palintropes Qu Changdu is 7.0cm;Bending length is 6.6cm after washing 5 times;Bending length is 6.5cm after washing 8 times.
Embodiment 4
The water resistance environmental-friendly stiffening agent of the present invention includes mix monomer, polyvinyl alcohol 1788, polyvinyl alcohol 1799, fatty alcohol APEO, isomeric alcohol polyethenoxy ether, alkyl polyoxyethylene ether, potassium peroxydisulfate, sodium peroxydisulfate and deionized water, above-mentioned group Divide by mass fraction and be respectively:50 parts of mix monomer, 1,788 1 parts of polyvinyl alcohol, 1,799 2 parts of polyvinyl alcohol, poly alkyl alcohol 1 part of oxygen vinethene, 1 part of isomeric alcohol polyethenoxy ether, 1 part of alkyl polyoxyethylene ether, 0.4 part of potassium peroxydisulfate, sodium peroxydisulfate 0.4 Part, 33 parts of deionized water.
Mix monomer includes vinyl acetate, methyl acrylate, diisooctyl maleate, and three kinds of component contents press quality It is respectively vinyl acetate 84%, methyl acrylate 8%, diisooctyl maleate 8% that percentage, which is calculated,.
The preparation method of water resistance environmental-friendly stiffening agent of the present invention comprises the following steps:
a:Corresponding raw material for standby is weighed according to said ratio;
b:Vinyl acetate, acrylate and function monomer are added in the container with agitating device, at normal temperatures and pressures It is standby to be stirred until homogeneous into mix monomer;
c:Under normal temperature and pressure, water-soluble, film-forming colloid and deionized water quality are added in the reactor with agitating device The 70% of total amount, is then stirred until homogeneous;
d:Toward adding emulsifying agent in mixture obtained by step c in the state of the lasting stirring, and temperature of reactor is lifted To 50 DEG C, then toward being passed through nitrogen in reactor;
e:Temperature of reactor is maintained 50 DEG C, toward adding initiator in mixture obtained by Step d after insulation 1.5 hours And mix monomer obtained by b step, and continuing stirring until it uniformly, mix monomer addition is the 13% of its gross mass, initiator Addition is the 13% of its gross mass;
f:Temperature of reactor is promoted to 76 DEG C and is incubated, while remaining mix monomer and initiator, time for adding is added dropwise 4.5 hour;
g:After f steps are added dropwise to complete, temperature of reactor is promoted to 91 DEG C, and isothermal reaction 30 minutes, then reaction Device temperature is down to 71 DEG C, then balance deionized water, and water resistance environmental-friendly stiffening agent can be obtained by being finally stirred until homogeneous discharging.
By carrying out bending property test (testing standard to the water resistance environmental-friendly stiffening agent of the present invention:GB/T 18318), Bending length of the yarn fabric of the water resistance environmental-friendly stiffening agent arrangement of the present invention after arrangement is used as 7.8cm;Wash 3 palintropes Qu Changdu is 7.3cm;Bending length is 7.1cm after washing 5 times;Bending length is 6.9cm after washing 8 times.
Embodiment 5
The water resistance environmental-friendly stiffening agent of the present invention includes mix monomer, polyvinyl alcohol 1788, polyvinyl alcohol 1799, fatty alcohol APEO, isomeric alcohol polyethenoxy ether, castor oil polyoxyethylene ether, alkyl polyoxyethylene ether, potassium peroxydisulfate, persulfuric acid Sodium, ammonium persulfate and deionized water, said components are respectively by mass fraction:57 parts of mix monomer, polyvinyl alcohol 1,788 2 Part, 1,799 2 parts of polyvinyl alcohol, 1 part of AEO, 1 part of isomeric alcohol polyethenoxy ether, castor oil polyoxyethylene ether 1 Part, 1 part of alkyl polyoxyethylene ether, 0.3 part of potassium peroxydisulfate, 0.3 part of sodium peroxydisulfate, 0.3 part of ammonium persulfate, 38 parts of deionized water.
Mix monomer includes vinyl acetate, butyl acrylate, dibutyl maleate, and three kinds of component contents press quality hundred It is respectively vinyl acetate 82%, butyl acrylate 9%, dibutyl maleate 9% to divide than calculating.
The preparation method of water resistance environmental-friendly stiffening agent of the present invention comprises the following steps:
a:Corresponding raw material for standby is weighed according to said ratio;
b:Vinyl acetate, acrylate and function monomer are added in the container with agitating device, at normal temperatures and pressures It is standby to be stirred until homogeneous into mix monomer;
c:Under normal temperature and pressure, water-soluble, film-forming colloid and deionized water quality are added in the reactor with agitating device The 75% of total amount, is then stirred until homogeneous;
d:Toward adding emulsifying agent in mixture obtained by step c in the state of the lasting stirring, and temperature of reactor is lifted To 55 DEG C, then toward being passed through nitrogen in reactor;
e:Temperature of reactor is maintained 56 DEG C, after insulation 2 hours toward addition initiator in mixture obtained by Step d and Mix monomer obtained by b step, and continue stirring until it uniformly, mix monomer addition is the 14% of its gross mass, and initiator adds Enter 14% that amount is its gross mass;
f:Temperature of reactor is promoted to 78 DEG C and is incubated, while remaining mix monomer and initiator, time for adding is added dropwise 5.5 hour;
g:After f steps are added dropwise to complete, temperature of reactor is promoted to 94 DEG C, and isothermal reaction 35 minutes, then reaction Device temperature is down to 73 DEG C, then balance deionized water, and water resistance environmental-friendly stiffening agent can be obtained by being finally stirred until homogeneous discharging.
By carrying out bending property test (testing standard to the water resistance environmental-friendly stiffening agent of the present invention:GB/T 18318), Bending length of the yarn fabric of the water resistance environmental-friendly stiffening agent arrangement of the present invention after arrangement is used as 7.9cm;Wash 3 palintropes Qu Changdu is 7.6cm;Bending length is 7.4cm after washing 5 times;Bending length is 7.3cm after washing 8 times.
Table one (content is mass fraction in table)

Claims (8)

  1. A kind of 1. water resistance environmental-friendly stiffening agent, it is characterised in that:The water resistance environmental-friendly stiffening agent includes mix monomer, water solubility Film-forming colloids, emulsifying agent, initiator and deionized water, said components are respectively by mass fraction:Mix monomer 40-60 parts, Water-soluble, film-forming colloid 1-5 parts, emulsifying agent 1-5 parts, initiator 0.5-1 parts, deionized water 25-40 parts.
  2. 2. water resistance environmental-friendly stiffening agent according to claim 1, it is characterised in that:The mix monomer include vinyl acetate, Acrylate and function monomer, three kinds of component contents calculate respectively vinyl acetate 80-90%, acrylate 5- by mass percentage 10%th, function monomer 5-10%.
  3. 3. water resistance environmental-friendly stiffening agent according to claim 2, it is characterised in that:The acrylate be methyl acrylate or Butyl acrylate.
  4. 4. water resistance environmental-friendly stiffening agent according to claim 2, it is characterised in that:The function monomer is maleic acid two Different monooctyl ester or dibutyl maleate.
  5. 5. water resistance environmental-friendly stiffening agent according to claim 1, it is characterised in that:The water-soluble, film-forming colloid is polyethylene Alcohol 1788 and one kind in polyvinyl alcohol 1799 are mixed with arbitrary proportion.
  6. 6. water resistance environmental-friendly stiffening agent according to claim 1, it is characterised in that:The emulsifying agent is aliphatic alcohol polyethenoxy One kind in ether, isomeric alcohol polyethenoxy ether, castor oil polyoxyethylene ether, alkyl polyoxyethylene ether is mixed with arbitrary proportion.
  7. 7. water resistance environmental-friendly stiffening agent according to claim 1, it is characterised in that:The initiator is potassium peroxydisulfate, over cure One kind in sour sodium, ammonium persulfate is mixed with arbitrary proportion.
  8. A kind of 8. preparation method of the environmental-friendly stiffening agent of water resistance according to claim 1, it is characterised in that:The preparation method The step of it is as follows:
    a:Corresponding raw material for standby is weighed according to said ratio;
    b:Vinyl acetate, acrylate and function monomer are added in the container with agitating device, is stirred at normal temperatures and pressures To uniformly standby into mix monomer;
    c:Under normal temperature and pressure, water-soluble, film-forming colloid and deionized water quality total amount are added in the reactor with agitating device 60-80%, be then stirred until homogeneous;
    d:Toward adding emulsifying agent in mixture obtained by step c in the state of the lasting stirring, and temperature of reactor is promoted to 40- 60 DEG C, then toward being passed through nitrogen in reactor;
    e:Temperature of reactor is maintained 40-60 DEG C, initiator is added in being incubated after 1-2 hours toward mixture obtained by Step d And mix monomer obtained by b step, and continuing stirring until it uniformly, mix monomer addition is the 10-15% of its gross mass, is triggered Agent addition is the 10-15% of its gross mass;
    f:Temperature of reactor is promoted to 70-80 DEG C and is incubated, while remaining mix monomer and initiator, time for adding 3- is added dropwise 6 hours;
    g:After f steps are added dropwise to complete, temperature of reactor is promoted to 85-95 DEG C, and isothermal reaction 20-40 minutes, then anti- Device temperature is answered to be down to 65-75 DEG C, then balance deionized water, being finally stirred until homogeneous discharging, can to obtain water resistance environmental protection stiffening Agent.
CN201611034525.2A 2016-11-23 2016-11-23 A kind of water-fastness environmental-friendly stiffening agent and preparation method thereof Pending CN107337758A (en)

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CN108130736A (en) * 2017-12-11 2018-06-08 江苏新瑞贝科技股份有限公司 A kind of preparation method of environment-friendlytype type fabric deflection reinforcing agent
CN109897139A (en) * 2017-12-11 2019-06-18 江苏新瑞贝科技股份有限公司 A kind of fabric stiffening agent and preparation method thereof
CN110029498A (en) * 2019-03-11 2019-07-19 常州市雄泰纺织品有限公司 A kind of weaving stiffening agent and preparation method thereof
CN110284329A (en) * 2019-05-30 2019-09-27 嘉兴亚展纺织品有限公司 A kind of preparation method of the environmental-friendly stiffening agent with thick and solid feel
CN113832726A (en) * 2021-08-20 2021-12-24 广东传化富联精细化工有限公司 Environment-friendly fabric stiffening finishing agent and preparation method thereof

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CN108130736A (en) * 2017-12-11 2018-06-08 江苏新瑞贝科技股份有限公司 A kind of preparation method of environment-friendlytype type fabric deflection reinforcing agent
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CN110029498A (en) * 2019-03-11 2019-07-19 常州市雄泰纺织品有限公司 A kind of weaving stiffening agent and preparation method thereof
CN110284329A (en) * 2019-05-30 2019-09-27 嘉兴亚展纺织品有限公司 A kind of preparation method of the environmental-friendly stiffening agent with thick and solid feel
CN113832726A (en) * 2021-08-20 2021-12-24 广东传化富联精细化工有限公司 Environment-friendly fabric stiffening finishing agent and preparation method thereof

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