CN101220563A - Environment protection type pigment resin printing adhesive agent capable of self crosslinking at low-temperature, and preparation thereof - Google Patents
Environment protection type pigment resin printing adhesive agent capable of self crosslinking at low-temperature, and preparation thereof Download PDFInfo
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Abstract
The invention belongs to the water-base adhesive technical field, in particular to an environment-protecting pigment printing binder which auto-crosslinks in the low temperature and a preparation method thereof which includes a polymeric monomer is added into the water solution of the composite emulsifier and the sodium bicarbonate, and the mixture is stirred so as to obtain the pre-emulsion; the pre-emulsion is added into a reaction vessel in lots, a polymerization is initiated, and a styrene-acrylic emulsion base which crosslinks in the low temperature is obtained; the pH value is adjusted, a crosslinking agent is added and the needed binder is obtained. The pigment printing binder obtained by the preparation of the method does not comprise formalin, alkyl phenol polyoxyethylene ether and other harmful substances. The finished textile printing obtained by using the binder has the advantages of soft hand feeling, brilliant color, wear resistant, and high soaping fastness, etc.; the textile printing used for the cotton cloth, polyester-cotton can get better effect. The mixture of the binder and the synthetic thickener can modulate the proper textile printing pulp, and is applicable to plate printing and net-tube printing.
Description
Technical field
The invention belongs to the aqueous binder technical field, but be specifically related to pigment printing binding agent of a kind of environment-friendly type crosslinked at low temperature and preparation method thereof.
Technical background
COAT PRINTING is meant uses macromolecular compound (adhesive) to form film on fabric, and pigment is anchored at printing method on the fabric.In recent years, development along with synthetic fiber industry, great variety has taken place in people's clothes clothing, from originally based on the fiber textile of natural fabric become with various synthetic fiber and with the blended fabric of natural fabric be the multicomponent fibre textiles of representative, the textiles that has even be made into by the fiber that reaches more than four kinds.Therefore, originally those printing technologies based on affinity between dyestuff and the fiber can not satisfy the particularly needs of stamp of coloration of textile materials of all shapes and colors.Because coating itself does not have affinity to fiber, only by means of the help of adhesive mechanically attached to the painted formation pattern of fiber surface, thereby do not exist with dye printing and like that often need two or more dyestuffs of different nature that BLENDED FABRIC is carried out stamp and fixation.Therefore, the superiority of COAT PRINTING seems more outstanding.In addition, the technology of COAT PRINTING is simple, chromatogram is complete, colorant match is easy, generally need not washing after the fixation, therefore has characteristics energy-conservation, water saving, makes that also COAT PRINTING grows a lot.The share that COAT PRINTING is occupied in stamp market, the world increases year by year, and especially in the U.S., because the production of a large amount of polyester/cotton BLENDED FABRIC, the COAT PRINTING proportion is up to 80%.China recent years, because of technology tends to factors such as oversimplifying, cut down the consumption of energy, the ratio of COAT PRINTING is also in rising trend, has also accounted for about 50% of total stamp amount so far.Along with improving constantly of living standards of the people, the consumer is not only more and more higher to the requirement of garment material, and to indoor textile decoration with the requirement of cloth also progressively to middle and high shelves development, in order to adapt to different consumer demands, COAT PRINTING will be further developed.
Though COAT PRINTING has been saved washing, waste water is significantly reduced, but all auxiliary agents are stayed on the fabric, when PRINTED FABRIC is dried and is baked, part volatile materials can be discharged with the waste gas form, another part remains on the fabric, if wherein contain noxious material, taking in the wearing process afterwards also can produce harm to people's health.All paint-printing colour size can be brought in the waste water when on the other hand, washing PRINTING BLANKET and mill base bucket.Hence one can see that, and the COAT PRINTING development always can interrelate with environmental problem, and its prescription, application process and production technology general are constantly developed towards the direction of environmental protection.As the topmost factor-printing adhesive that influences the stamp product quality, development from now on must also be in the feel that guarantees the stamp product, on the basis of COLOR FASTNESS and vividness, carries out towards environmentally friendly direction.In addition, the adhesive of using belongs to the high temperature modification auto crosslinking binder more at present, for energy savings, also should strengthen the low temperature printing adhesive of development of new, simultaneously, new adhesive should be biodegradable, and adhesive should have good filming performance, characteristics such as film forming is strong and soft, fastness is good, new adhesive also should reduce needed additive in the printing paste, improves family's washing durability.Therefore, but research and development is nontoxic, formaldehydeless or the adhesive of the environment-friendly type crosslinked at low temperature of low formaldehyde not only has great importance, and meets the needs of future development.
Recently, the someone has reported and has used polyurethane-acrylic ester emulsion to prepare environment-protection coating printing adhesive (Chinese patent, publication number CN1936172A) as base-material, but this method preparation technology more complicated, and cost is higher, is unfavorable for large-scale production.
Summary of the invention
But the object of the present invention is to provide that a kind of technology is simple, with low cost, the pigment printing binding agent of the environment-friendly type low-temperature self-crosslinking that is easy to suitability for industrialized production and preparation method thereof.
The pigment printing binding agent preparation method that the present invention proposes, concrete steps are as follows:
(1) pre-emulsification
With compound emulsifying agent, sodium bicarbonate is dissolved in the deionized water, adds polymerization single polymerization monomer, stirs, and obtains pre-emulsion;
(2) preparation seed emulsion
In reactor, add 1/4～1/3 above-mentioned pre-emulsion, be warming up to 70 ℃～80 ℃; Add the initiator solution initiated polymerization, reacted 30-45 minute;
(3) temperature rose to 80 ℃～90 ℃, slowly drips the residue pre-emulsion, added a collection of initiator solution therebetween every 15～20 minutes;
(4) dropwise, continue reaction 1～2 hour.Reduce to room temperature then, add ammoniacal liquor and transfer pH to 7.2～7.8, add crosslinking agent again, the addition of crosslinking agent is 8%～12% of a polymerization system quality, and discharging promptly gets target product.
Among the present invention, described polymerization single polymerization monomer comprises main monomer, auxiliary monomer and crosslinkable monomers.Wherein, main monomer is butyl acrylate, styrene or methyl methacrylate; Auxiliary monomer is acrylic or methacrylic acid etc.; The crosslinkable functional monomer is diacetone acrylamide or AAEM; Wherein the main monomer mass ratio is 90%～98%, and the auxiliary monomer mass ratio is 1%～5%, and the function monomer mass ratio is 1%～5%, and three's total amount satisfies 100%; The weight ratio of butyl acrylate, styrene and methyl methacrylate is (4-30) in the main monomer: (1-3): (0.1～1).
Among the present invention, described compound emulsifying agent is the compound system that anion emulsifier and nonionic emulsifier mix by a certain percentage.Wherein, anion emulsifier is lauryl sodium sulfate or neopelex; Nonionic emulsifier is natural fatty alcohol polyoxyethylene ether (FAEO), APG (APG), peregal, Qu Latong (TX) series, sapn (span) series, and tween (Tween) series.The mass ratio of anion emulsifier and nonionic emulsifier can be 1: 1～and 1: 3.
Among the present invention, described initator is ammonium persulfate aqueous solution or persulfate aqueous solution, and weight concentration is 0.2%-0.6%, adds about 1/4 in step (2), adds remaining about 3/4 in step (3).
Among the present invention, described crosslinking agent is polynary hydrazide compound, specifically can be in adipic dihydrazide, carbonic acid two hydrazides, malonic acid two hydrazides, succinic acid hydrazide ii and glutaric acid two hydrazides one or more.
The pigment printing binding agent of the present invention's preparation, its constituent and proportioning are: polymer content is 30%～45%, and emulsifier content is 2%～6%, and content of crosslinking agent is 1%～5%, and total solid content is 35%～55%.
The product physical and chemical parameter of the present invention's preparation is as follows:
Solid content (%) 35%～55%
The light blue milky white system of outward appearance
Viscosity (MPas) 300～3000
Soft tack-free
Free formaldehyde (ppm)＜5ppm
Crock fastness/level does 4～5
Wet 3～4.
The present invention prepared a kind of complete formaldehydeless release, do not contain alkylphenol polyoxyethylene (APEO) but environment-friendly type low-temperature self-crosslinking pigment printing binding agent.Technology of the present invention is simple, uses general emulsion polymerisation device to produce, and cost is also comparatively cheap, is easy to carry out suitability for industrialized production.
The specific embodiment
By following examples synthetic method of the present invention is further elaborated, but and does not mean that restriction synthetic method of the present invention.
Embodiment 1
(1). pre-emulsification
With 2g lauryl sodium sulfate (SDS), 4g peregal 0-20,0.5g sodium bicarbonate are dissolved in the 60g deionized water, add 13.8g styrene, 4g methyl methacrylate, 20g butyl acrylate, 1.2g acrylic acid and 1.2g diacetone acrylamide mix monomer stir pre-emulsification, and be standby.
(2). the seed emulsion preparation
Adding 1/4 is warming up to 75 ℃ and is added 1/4 ammonium persulfate solution initiated polymerizations by the pre-emulsion that step (1) obtains in reactor, reacts 30 minutes.
(3). temperature rose to 85 ℃, slowly splashes into residue 3/4 pre-emulsion, wherein added a collection of ammonium persulfate aqueous solution every 20 minutes.
(4). dropwise, continue reaction 1 hour.Reduce to room temperature, filter the back and add about ammoniacal liquor accent pH to 7.5, add 10g crosslinking agent glutaric acid two hydrazides again, discharging promptly gets target product.
The pigment printing binding agent viscosity that above formulation obtains is lower, and stability is moderate, and flexibility is moderate behind the stamp, and is tack-free, and wear-resisting rubbing fastness is outstanding.
Embodiment 2
(1). pre-emulsification
With 3g neopelex (SDBS), 3g APG-12 (APG-12), 0.5g sodium bicarbonate is dissolved in the 60g deionized water, add 6.9g styrene, the 2g methyl methacrylate, 26.9g butyl acrylate, 2.0g acrylic acid and 1.5g diacetone acrylamide mix monomer stir pre-emulsification, and be standby.
(2). the seed emulsion preparation
In reactor, add 1/4 above pre-emulsion, be warming up to 78 ℃ and add the ammonium persulfate solution initiated polymerization, reacted 40 minutes.
(3). temperature rose to 87 ℃, slowly splashes into residue 3/4 pre-emulsion, wherein added a collection of ammonium persulfate aqueous solution every 18 minutes.
(4). dropwise, continue reaction 1.5 hours.Reduce to room temperature, filter the back and add about ammoniacal liquor accent pH to 7.2, add 12g crosslinking agent carbonic acid two hydrazides again, discharging promptly gets product.
The wear-resisting wiping of epithelium and the flexibility that obtain behind the paint adhesive stamp that is obtained by above formulation are all better, the adhesion strength height.
Embodiment 3
(1). pre-emulsification
With 2.7g neopelex (SDBS), 4g APG-12 (APG-12), 0.5g sodium bicarbonate is dissolved in the 60g deionized water, add 2.0g styrene, the 1g methyl methacrylate, the 35g butyl acrylate, 5g acrylic acid and 3.0g AAEM mix monomer stir pre-emulsification, and be standby.
(2). the seed emulsion preparation
In reactor, add 1/4 above pre-emulsion, be warming up to 75 ℃ and add the potassium persulfate solution initiated polymerization, reacted 40 minutes.
(3). temperature rose to 90 ℃, slowly splashes into residue 3/4 pre-emulsion, wherein added a collection of ammonium persulfate aqueous solution every 15 minutes.
(4). dropwise, continue reaction 1.5 hours.Reduce to room temperature, filter the back and add about ammoniacal liquor accent pH to 7.8, add 15g crosslinking agent malonic acid two hydrazides again, discharging promptly gets product.
The product viscosity height that above formulation obtains, emulsion particle are very fine and smooth, good stability.The more soft adhesion strength of epithelium is good behind the stamp.
Embodiment 4
(1). pre-emulsification
With 2.4g lauryl sodium sulfate SDS, 3.6g peregal 0S-15,0.5g sodium bicarbonate are dissolved in the 60g deionized water, add 4g styrene, the 33.8g butyl acrylate, and 0.7g acrylic acid and 1.5g diacetone acrylamide mix monomer stir pre-emulsification, and be standby.
(2). the seed emulsion preparation
In reactor, add 1/4 above pre-emulsion, be warming up to 75 ℃ and add the ammonium persulfate solution initiated polymerization, reacted 45 minutes.
(3). temperature rose to 85 ℃, slowly splashes into residue 3/4 pre-emulsion, wherein added a collection of ammonium persulfate aqueous solution every 20 minutes.
(4). dropwise, continue reaction 1 hour.Reduce to room temperature, filter the back and add about ammoniacal liquor accent pH to 7.8, add 13g crosslinking agent adipic dihydrazide again, discharging promptly gets product.
The pigment printing binding agent viscosity that above formulation obtains is lower, and wear-resisting wiping intensity is moderate.The super softness of epithelium behind the stamp, adhesion strength is also very outstanding.
Claims (3)
1. but the preparation method of the pigment printing binding agent of an environment-friendly type low-temperature self-crosslinking is characterized in that concrete steps are as follows:
(1) pre-emulsification
With compound emulsifying agent, sodium bicarbonate is dissolved in the deionized water, adds polymerization single polymerization monomer, stirs, and obtains pre-emulsion;
(2) preparation seed emulsion
In reactor, add 1/4～1/3 above-mentioned pre-emulsion, be warming up to 70 ℃～80 ℃; Add the initiator solution initiated polymerization, reacted 30-45 minute;
(3) temperature rose to 80 ℃～90 ℃, slowly drips the residue pre-emulsion, added a collection of initiator solution therebetween every 15～20 minutes;
(4) dropwise, continue reaction 1～2 hour, reduce to room temperature then, add ammoniacal liquor and transfer pH to 7.2～7.8, add crosslinking agent again, the addition of crosslinking agent is 8%～12% of a polymerization system quality, and discharging promptly gets target product;
Described compound emulsifying agent is the compound system that anion emulsifier and nonionic emulsifier mix; Wherein, anion emulsifier is lauryl sodium sulfate or neopelex; Nonionic emulsifier is natural fatty alcohol polyoxyethylene ether, APG, peregal, Qu Latong series, sapn series or tween series, and the mass ratio of anion emulsifier and nonionic emulsifier is 1: 1～1: 3;
Described polymerization single polymerization monomer comprises main monomer, auxiliary monomer and crosslinkable monomers; Wherein, main monomer is butyl acrylate, styrene or methyl methacrylate; Auxiliary monomer is acrylic or methacrylic acid; The crosslinkable functional monomer is diacetone acrylamide or AAEM; Wherein the main monomer mass ratio is 90%～98%, and the auxiliary monomer mass ratio is 1%～5%, and the function monomer mass ratio is 1%～5%;
Described crosslinking agent for in adipic dihydrazide, carbonic acid two hydrazides, malonic acid two hydrazides, succinic acid hydrazide ii and glutaric acid two hydrazides one or more;
2. but the preparation method of environment-friendly type low-temperature self-crosslinking pigment printing binding agent according to claim 1 is characterized in that described initator is ammonium persulfate aqueous solution or persulfate aqueous solution, and weight concentration is 0.2%-0.6%.
3. but environment-friendly type low-temperature self-crosslinking pigment printing binding agent of method preparation according to claim 1, it is characterized in that wherein polymer content is 30%～45%, emulsifier content is 2%～6%, content of crosslinking agent is 1%～5%, and total solid content is 35%～55%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2007101707950A CN101220563B (en) | 2007-11-22 | 2007-11-22 | Environment protection type pigment resin printing adhesive agent capable of self crosslinking at low-temperature, and preparation thereof |
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| CN2007101707950A CN101220563B (en) | 2007-11-22 | 2007-11-22 | Environment protection type pigment resin printing adhesive agent capable of self crosslinking at low-temperature, and preparation thereof |
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| CN101220563B CN101220563B (en) | 2010-12-15 |
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