CN101265670A - Formaldehyde-free self-crosslinked nanometer emulsion coating dye printing cementing substance and method for making same - Google Patents
Formaldehyde-free self-crosslinked nanometer emulsion coating dye printing cementing substance and method for making same Download PDFInfo
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Abstract
A formaldehyde-free self-crosslinking nanometer emulsion coating printing and dyeing adhesive and a preparation method thereof. According to the technical proposal provided by the invention, the formaldehyde-free self-crosslinking nanometer emulsion coating printing and dyeing adhesive contains: crosslinking monomer 1-20, hard monomer 1-20, hydrophilic monomer 0-5, initiator 0.01-0.5, and surfactant 2-5; the mass part is taken as the unit. The crosslinking monomer can be one of or a combination of hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxybutyl acrylate, hydroxyhexyl acrylate, methyl methacrylate, glycol methacrylate, and propylene glycol monomethacrylate. When the formaldehyde-free self-crosslinking nanometer emulsion coating printing and dyeing adhesive is used in fabric coating printing or dyeing, no mesh blocking or roll coating happens; the printing and dyeing pattern has bright color, and clear figure and pattern; the fabric feels soft; and the color fastness is excellent.
Description
Technical field
The present invention relates to the preparation method of textile coating printing and dyeing usefulness adhesive in the textile and dyeing industry, more particularly relate to the preparation method of the emulsion binding agent of the formaldehydeless release that is used for coating dye printing processing.
Background technology
The dyeing of textiles and stamp are the important process technologies of giving functions such as textiles color, decorative pattern and fiber protection, so printing technology always is the emphasis of textile science field and textile industry circle research and development.Traditional dyeing and stamp utilize various types of dyestuffs that fiber or fabric are carried out painted processing mostly.For many years scientific research and industrial practice show that there are following three aspect deficiencies at least in dye printing and dyeing technology: (1) does not utilize the discharging of dyestuff to run off in a large number increases the use amount of dyestuff, improves cost of material; (2) utilization rate of dyestuff is not high causes cleaning process water consumption, power consumption to increase; (3) waste water after the processing, organic dyestuff still has remaining, and long-term discharging accumulation will inevitably cause environmental pollution.
Dyeing is general to be dissolved or dispersed in organic dyestuff in the water earlier, adopts means such as dipping or rolling to make dyestuff with fiber-reactive or in its surface absorption and fixing then, makes the color of textiles acquisition requirement again through operations such as washing processing.Dye printing adopts the mixed system (print paste) that cylinder, screen cloth or other method (as shifting etc.) will contain the dye well auxiliary agent optionally to be coated on fabric face, forms designed pattern or decorative pattern through serial post processing.No matter dye or stamp, all have certain dye-uptake, therefore always some can not utilize and along with dyeing waste water is discharged, cause serious environmental to pollute the dyestuff that is added.Especially in recent years adopt chemically-reactive dyes in a large number, fabric face has more unreacted dyestuff residual, and therefore dyeing or stamp clean water consumption later increases greatly, through estimating about 200L water/kg fabric, calculate by weight, the water yield that the fabrics printing and dyeing process is consumed is 200 times of output!
The exploitation and the extensive use of all drawbacks of dye printing and dyeing technology, the progress of pigment synthetic technology and polymer builder/additive have promoted the coating dye printing technology rapid development.Compare with traditional dyeing and finishing technology, coating dye printing possesses some significant advantages, and is complete as chromatogram, and it is extensive to adapt to kinds of fibers, and technology simple (need not wash) is saved resource, and environmental pollution is little etc., develops into main printing and dyeing processing method gradually.According to statistics, the whole world has the dyeing that surpasses 60% textiles to handle employing coating dye printing technology with stamp to finish.Coating dye printing is that with the difference of dye printing and dyeing maximum both used colouring agents are different, and coating dye printing uses pigment to be colouring agent.Do not have affinity between pigment and the fiber, chemical reaction can not take place, therefore only depend on pigment self to fix, must add adhesive and combine with fiber to help pigment at textile surface.In present textile coating dyeing and printing process, adhesive is the unique auxiliary agent that makes pigment combine with fiber, plays a part very important.But the adding of most adhesives brings new problem for coating dye printing technology, concludes and gets up to mainly contain following three major types:
(1) formaldehyde discharges problem.
(2) contradiction of the feel of coating dye printing goods and COLOR FASTNESS.
(3) network blocking in the coating dye printing process, roll banding problem.
The formaldehyde of textiles discharges multiple factor, and cross-linking monomers such as the N hydroxymethyl acrylamide of crosslinking binder produce formaldehyde in mechanism be one of major reason.Formaldehyde discharges the pollution of environment and the harm of health be can not be ignored, and therefore seeking effective substitute becomes the instant research topic in this field.In the coating dye printing process, adhesive forms epithelium at fabric face, pigment is adhered to and is bonded to fiber surface by physics or chemical action, makes color or pattern that fabric shows to be needed.Obviously, the flexibility of textile touch and adhesive epithelium, adhesiveness etc. have much relations, and the character of epithelium is determined by the factors such as kind, character, membrance casting condition and addition of adhesive fully.At present synthetic adhesive generally makes the feel variation of fabric, needs to add softener and puts in order, makes process complications and effect limited.Therefore, solve the contradiction between coating dye printing fabric feeling and the COLOR FASTNESS, become one of the researcher of paint dyeing and printing adhesive agent and problem that industrial quarters is paid close attention to most.In addition, produce network blocking, roll banding problem in the coating dye printing process, main cause also is the adding of adhesive.Because factors such as the stability of the kind of soft monomer and each latex particle different with the high polymer glass transition temperature of content inequality, various copolymerization sequential structures and minimum film formation temperature be different in the high polymer component that adhesive comprised, cause partly breakdown of emulsion film forming (technological requirement is to realize adhesive function at the follow-up stage of curing breakdown of emulsion) of in process adhesive agent emulsion, thereby produce the phenomenon of network blocking, roll banding.
Summary of the invention
In order to solve the problems referred to above that the coating dye printing technology exists, the present invention will provide a kind of formaldehyde-free self-crosslinked nanometer emulsion coating dye printing cementing substance and preparation method thereof.
One of the problem to be solved in the present invention is to select to provide the self-crosslinking function monomer of a class novel formaldehyde-free paint dyeing and printing adhesive agent.
Two of the problem to be solved in the present invention provides the preparation method of the novel formaldehyde-free paint dyeing and printing adhesive agent of using above-mentioned crosslinked functional monomer.
According to technical scheme provided by the invention, described formaldehyde-free self-crosslinked nanometer emulsion coating dye printing cementing substance comprises: cross-linking monomer 1～20; Hard monomer 1～20; Hydrophilic monomer 0～5; Initator 0.01～0.5; Surfactant 2～5, unit are parts by mass.
Described cross-linking monomer is one or more the combination in hydroxy-ethyl acrylate, hydroxypropyl acrylate, acrylic acid hydroxy butyl ester, the own ester of acrylic acid hydroxyl, hydroxy methyl methacrylate, hydroxyethyl methylacrylate, the hydroxy propyl methacrylate.
Described hard monomer is acrylic or methacrylic acid or the mixture of the two, and a kind of in methyl methacrylate, styrene or the acrylonitrile.
Also comprise soft monomer 20～80 in described dyeing and printing adhesive agent, unit is a parts by mass.
Described soft monomer is one or more the combination in butyl acrylate, ethyl acrylate, 2-EHA, hydroxy-ethyl acrylate, hydroxypropyl acrylate, acrylic acid hydroxy butyl ester, the own ester of acrylic acid hydroxyl.
Described hydrophilic monomer is an acrylamide; Described initator is ammonium persulfate or potassium peroxydisulfate; Described surfactant is the combination of lauryl sodium sulfate, neopelex, octylphenol polyethylene glycol ether.
In each compositing monomer of described copolymer adhesive, what described soft monomer can be part or all of is substituted by described crosslinked functional monomer.Meaning is that one or more the combination in hydroxy-ethyl acrylate, hydroxypropyl acrylate, acrylic acid hydroxy butyl ester, the own ester of acrylic acid hydroxyl both can be used as crosslinked function monomer, also can be used as soft monomer.
The preparation method of described formaldehyde-free self-crosslinked nanometer emulsion coating dye printing cementing substance is:
With the soft monomer of 1/8～1/3 in the said components, 1/8～1/3 hard monomer, 1/8～1/3 initator and whole emulsifying agent and deionized water adding reactor, stir pre-emulsification 15in～30min down at 20～50 ℃, be warming up to 75～90 ℃ again; Drip remaining soft monomer, hard monomer, initator and crosslinked functional monomer behind the initiated polymerization, dropwise the back and be incubated 90～150min down, be cooled to room temperature again at 75～90 ℃.
Described cross-linking monomer is one or more the combination in hydroxy-ethyl acrylate, hydroxypropyl acrylate, acrylic acid hydroxy butyl ester, the own ester of acrylic acid hydroxyl, hydroxy methyl methacrylate, hydroxyethyl methylacrylate, the hydroxy propyl methacrylate;
Described hard monomer is acrylic or methacrylic acid or the mixture of the two, and a kind of in methyl methacrylate, styrene or the acrylonitrile;
Described hydrophilic monomer is an acrylamide;
Described initator is ammonium persulfate or potassium peroxydisulfate; Described surfactant is the combination of lauryl sodium sulfate, neopelex, octylphenol polyethylene glycol ether.
Also comprise soft monomer 20～80 in described dyeing and printing adhesive agent, unit is a parts by mass;
Described soft monomer is one or more the combination in butyl acrylate, ethyl acrylate, 2-EHA, hydroxy-ethyl acrylate, hydroxypropyl acrylate, acrylic acid hydroxy butyl ester, the own ester of acrylic acid hydroxyl.
Every performance of the product of the present invention that makes by said method can adopt following method to detect.
(1) emulsion solid content is measured
Measuring cup is dried to constant weight under 100 ℃～105 ℃, accurately sample (the m about weighing 2g
1) in measuring cup, place 100 ℃～105 ℃ Constant Temp. Ovens to dry to constant weight, be transferred in the drier behind the cooling 30min accurately weighing (m then
2), then solid content can be calculated as follows:
Solid content (%)=m
2/ m
1* 100%
(2) emulsion viscosity is measured
Adopt the viscosity of the DV-III ULTRA type rotary viscosity design determining adhesive agent emulsion of U.S. Brookfield company.
(3) emulsion particle diameter and particle size distribution measuring
Adopt the Nano-ZS90 type Zeta potential of Britain Malvern instrument company and particle diameter and the particle diameter distribution that particle size analyzer is measured adhesive agent emulsion.
(4) stability of emulsion is measured
Adopting 80-1 type centrifuge is with the centrifugal 30min of sample under the 4000rpm at rotating speed.Get the adhesive agent emulsion of 1ml after centrifugal with pipette again, dilution back 722 grating spectrophotometers, the absorbance A of mensuration dilution
30Use the same method and measure the not absorbance A of centrifugal sample
0The ratio of the absorbance before the absorbance after emulsion is centrifugal and the centrifugal treating is referred to as than absorbance R
30, as the index of the centrifugal sedimentation stability of weighing emulsion:
(5) adhesive is used for the COLOR FASTNESS test of COAT PRINTING
The adhesive that synthesized with the prescription modulation mill base of other composition according to routine, is carried out manual platen stamp to cotton or wash/cotton (80/20) fabric then, behind the stamp according to the brushing fastness of GB/T420-1990 test PRINTED FABRIC; Crock fastness according to GB/T3920-1997 test PRINTED FABRIC; Color fastness to washing according to the GB/T3921.3-1997 test fabric.
(6) adhesive feel test
With adhesive that the present invention synthesized with other composition according to conventional formulation modulation mill base, then cotton or wash/cotton (80/20) fabric is carried out manual platen stamp, adopt the feel of the fabric that the comparison of hand palpating manipulation printed.
(7) adhesive formaldehyde test
At first with adhesive that the present invention synthesized by following PROCESS FOR TREATMENT fabric: adhesive 300g/L, two soak two rolls pure cotton fabric → greater than 100 ℃ of oven dry → bake 2min greater than 150 ℃.Then according to contained formaldehyde on the GB/T2912.1-1998 test fabric.
Advantage of the present invention is: adopt end to contain the acrylic ester monomer of hydroxyl as crosslinked functional monomer, wherein the monomer of long alkyl chain can partly replace soft monomer as (methyl) hydroxy-ethyl acrylate, (methyl) acrylic acid hydroxy butyl ester and the own ester of (methyl) acrylic acid hydroxyl etc.; The monomer of short alkyl chain is mainly acrylic acid hydroxyl methyl esters or hydroxy methyl methacrylate and can partly replaces hard monomer.Because the hydroxy acrylate of long-chain both can be used as crosslinked function monomer and also can be used as soft monomer, therefore, the present invention can improve the dyeing colour fastness to greatest extent on the basis that does not influence the coating dye printing fabric feeling.Secondly, all cross-linking monomers of the present invention do not contain compositions such as n-methylolacrylamide, and release formaldehyde not is outstanding environment-friendly products fully.
The specific embodiment
Embodiment 1
Adhesive agent emulsion polymerization formula (each composition of reaction system accounts for the percentage of monomer gross mass):
Hydroxy-ethyl acrylate and hydroxy propyl methacrylate 1～20
Ethyl acrylate and 2-EHA 20～80
Methacrylic acid 1～10
Methyl methacrylate 1～10
Styrene 0～5
Acrylamide 0～5
Ammonium persulfate 0.01～0.5
Lauryl sodium sulfate and octylphenol polyethylene glycol ether 2～5
Deionized water is an amount of
Synthesis technique:
Soft monomer, hard monomer, initator and whole emulsifying agent and the deionized water of 1/8～1/3 in the above-mentioned reactant prescription are added reactor, stir pre-emulsification 15min～30min down, be warming up to 75 ℃～90 ℃ at 20 ℃～50 ℃; Drip remaining soft monomer, hard monomer, initator and crosslinked functional monomer behind the initiated polymerization, dropwise the back and be incubated 90min～180min down, be cooled to room temperature at 75 ℃～90 ℃.Add proper ammonia and regulate the pH value, discharging, filter adhesive agent emulsion.
Embodiment 2
Adhesive agent emulsion polymerization formula (each composition of reaction system accounts for the percentage of monomer gross mass):
Hydroxyethyl methylacrylate and hydroxypropyl acrylate 1～20
Ethyl acrylate and butyl acrylate 20～80
Acrylic acid 1～10
Methyl methacrylate 1～10
Acrylonitrile 0～5
Acrylamide 0～5
Potassium peroxydisulfate 0.01～0.5
Neopelex and octylphenol polyethylene glycol ether 2～5
Deionized water is an amount of
Synthesis technique:
Soft monomer, hard monomer, initator and whole emulsifying agent and the deionized water of 1/8～1/3 in the above-mentioned reactant prescription are added reactor, stir pre-emulsification 15min～30min down, be warming up to 75 ℃～90 ℃ at 20 ℃～50 ℃; Drip remaining soft monomer, hard monomer, initator and crosslinked functional monomer behind the initiated polymerization, dropwise the back and be incubated 90min～180min down, be cooled to room temperature at 75 ℃～90 ℃.Add proper ammonia and regulate the pH value, discharging, filter adhesive agent emulsion.
Embodiment 3
Adhesive agent emulsion polymerization formula (each composition of reaction system accounts for the percentage of monomer gross mass):
Hydroxyethyl methylacrylate and acrylic acid hydroxy butyl ester 1～20
Butyl acrylate and 2-EHA 20～80
Acrylic acid and methacrylic acid 1～10
Methyl methacrylate 1～5
Styrene 0～5
Acrylamide 0～5
Ammonium persulfate 0.01～0.5
Lauryl sodium sulfate and octylphenol polyethylene glycol ether 2～5
Deionized water is an amount of
Synthesis technique:
Soft monomer, hard monomer, initator and whole emulsifying agent and the deionized water of 1/8～1/3 in the above-mentioned reactant prescription are added reactor, stir pre-emulsification 15min～30min down, be warming up to 75 ℃～90 ℃ at 20 ℃～50 ℃; Drip remaining soft monomer, hard monomer, initator and crosslinked functional monomer behind the initiated polymerization, dropwise the back and be incubated 90min～180min down, be cooled to room temperature at 75 ℃～90 ℃.Add proper ammonia and regulate the pH value, discharging, filter adhesive agent emulsion.
Embodiment 4
Adhesive agent emulsion polymerization formula (each composition of reaction system accounts for the percentage of monomer gross mass):
Hydroxy methyl methacrylate and acrylic acid hydroxy butyl ester 1～20
Butyl acrylate and 2-EHA 20～80
Acrylic acid and methacrylic acid 1～10
Methyl methacrylate 1～5
Acrylonitrile 0～5
Acrylamide 0～5
Ammonium persulfate 0.01～0.5
Neopelex and octylphenol polyethylene glycol ether 1～5
Deionized water is an amount of
Synthesis technique:
Soft monomer, hard monomer, initator and whole emulsifying agent and the deionized water of 1/8～1/3 in the above-mentioned reactant prescription are added reactor, stir pre-emulsification 15min～30min down, be warming up to 75 ℃～90 ℃ at 20 ℃～50 ℃; Drip remaining soft monomer, hard monomer, initator and crosslinked functional monomer behind the initiated polymerization, dropwise the back and be incubated 90min～180min down, be cooled to room temperature at 75 ℃～90 ℃.Add proper ammonia and regulate the pH value, discharging, filter adhesive agent emulsion.COAT PRINTING experiment and detection
Adopt coating series printing adhesive of the present invention (JNHA-1) that fabric is carried out COAT PRINTING test, the print paste prescription following (unit: g):
Pigment yellow 310
Adhesive of the present invention (solid content about 30%) 30
Synthetic thickening agent+water 60
Printing technology adopts the conventional method of the manual platen stamp in laboratory, and fabric COLOR FASTNESS and content of formaldehyde test result behind the stamp are as shown in table 1.
Table 1JNHA-1 particle diameter and every application performance detect data
Claims (9)
1, formaldehyde-free self-crosslinked nanometer emulsion coating dye printing cementing substance is characterized in that this dyeing and printing adhesive agent comprises: cross-linking monomer 1～20; Hard monomer 1～20; Hydrophilic monomer 0～5; Initator 0.01～0.5; Surfactant 2～5, unit are parts by mass.
2, formaldehyde-free self-crosslinked nanometer emulsion coating dye printing cementing substance according to claim 1, it is characterized in that described cross-linking monomer is one or more the combination in hydroxy-ethyl acrylate, hydroxypropyl acrylate, acrylic acid hydroxy butyl ester, the own ester of acrylic acid hydroxyl, hydroxy methyl methacrylate, hydroxyethyl methylacrylate, the hydroxy propyl methacrylate.
3, formaldehyde-free self-crosslinked nanometer emulsion coating dye printing cementing substance according to claim 1 is characterized in that, described hard monomer is acrylic or methacrylic acid or the mixture of the two, and a kind of in methyl methacrylate, styrene or the acrylonitrile.
4, formaldehyde-free self-crosslinked nanometer emulsion coating dye printing cementing substance according to claim 1 is characterized in that, also comprises soft monomer 20～80 in described dyeing and printing adhesive agent, and unit is a parts by mass.
5, formaldehyde-free self-crosslinked nanometer emulsion coating dye printing cementing substance according to claim 4, it is characterized in that described soft monomer is one or more the combination in butyl acrylate, ethyl acrylate, 2-EHA, hydroxy-ethyl acrylate, hydroxypropyl acrylate, acrylic acid hydroxy butyl ester, the own ester of acrylic acid hydroxyl.
6, formaldehyde-free self-crosslinked nanometer emulsion coating dye printing cementing substance according to claim 1 is characterized in that, described hydrophilic monomer is an acrylamide; Described initator is ammonium persulfate or potassium peroxydisulfate; Described surfactant is the combination of lauryl sodium sulfate, neopelex, octylphenol polyethylene glycol ether.
7,, it is characterized in that the preparation process of described adhesive is according to the preparation method of claim 1,2,3 and 4 described formaldehyde-free self-crosslinked nanometer emulsion coating dye printing cementing substances:
With the soft monomer of 1/8～1/3 in the said components, 1/8～1/3 hard monomer, 1/8～1/3 initator and whole emulsifying agent and deionized water adding reactor, stir pre-emulsification 15min～30min down at 20～50 ℃, be warming up to 75～90 ℃ again; Drip remaining soft monomer, hard monomer, initator and crosslinked functional monomer behind the initiated polymerization, dropwise the back and be incubated 90～150min down, be cooled to room temperature again at 75～90 ℃.
8, the preparation method of formaldehyde-free self-crosslinked nanometer emulsion coating dye printing cementing substance according to claim 7, it is characterized in that described cross-linking monomer is one or more the combination in hydroxy-ethyl acrylate, hydroxypropyl acrylate, acrylic acid hydroxy butyl ester, the own ester of acrylic acid hydroxyl, hydroxy methyl methacrylate, hydroxyethyl methylacrylate, the hydroxy propyl methacrylate; Described hard monomer is acrylic or methacrylic acid or the mixture of the two, and a kind of in methyl methacrylate, styrene or the acrylonitrile; Described hydrophilic monomer is an acrylamide;
Described initator is ammonium persulfate or potassium peroxydisulfate; Described surfactant is the combination of lauryl sodium sulfate, neopelex, octylphenol polyethylene glycol ether.
9, the preparation method of formaldehyde-free self-crosslinked nanometer emulsion coating dye printing cementing substance according to claim 7 is characterized in that, also comprises soft monomer 20～80 in described dyeing and printing adhesive agent, and unit is a parts by mass;
Described soft monomer is one or more the combination in butyl acrylate, ethyl acrylate, 2-EHA, hydroxy-ethyl acrylate, hydroxypropyl acrylate, acrylic acid hydroxy butyl ester, the own ester of acrylic acid hydroxyl.
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|---|---|---|---|
| CNA2008100255217A CN101265670A (en) | 2008-04-29 | 2008-04-29 | Formaldehyde-free self-crosslinked nanometer emulsion coating dye printing cementing substance and method for making same |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100255217A CN101265670A (en) | 2008-04-29 | 2008-04-29 | Formaldehyde-free self-crosslinked nanometer emulsion coating dye printing cementing substance and method for making same |
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| CN101928367A (en) * | 2010-08-24 | 2010-12-29 | 华南理工大学 | Environmentally-friendly acrylic ester coating printing adhesive emulsion and preparation method |
| CN101928367B (en) * | 2010-08-24 | 2012-06-20 | 华南理工大学 | Environmentally-friendly acrylic ester coating printing adhesive emulsion and preparation method |
| CN102532399A (en) * | 2011-12-10 | 2012-07-04 | 江阴市尼美达助剂有限公司 | Acrylic acid textile size and preparation method thereof |
| CN102952230B (en) * | 2012-10-11 | 2014-09-17 | 宿迁市神龙家纺有限公司 | Preparation method of low-temperature adhering agent for pigment printing |
| CN102952230A (en) * | 2012-10-11 | 2013-03-06 | 宿迁市神龙家纺有限公司 | Preparation method of low-temperature adhering agent for pigment printing |
| CN102899928A (en) * | 2012-11-01 | 2013-01-30 | 三门峡市八四八化工厂 | Novel environment-friendly bonding agent for pigment printing |
| CN103526584A (en) * | 2013-10-23 | 2014-01-22 | 合肥聚合辐化技术有限公司 | Corrosion-resistance pigment printing adhesive and preparation method thereof |
| CN103936941A (en) * | 2014-04-30 | 2014-07-23 | 江南大学 | Amphiphilic core-shell emulsion adhesive for pigment printing of textile and preparation method thereof |
| CN104278564A (en) * | 2014-09-26 | 2015-01-14 | 无锡市东北塘宏良染色厂 | Dyeing agent and method for dyeing nylon fabric by using dyeing agent |
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| CN107604698A (en) * | 2017-09-26 | 2018-01-19 | 安踏（中国）有限公司 | A kind of manufacture craft of concentrator, fabric and fabric |
| CN109320665A (en) * | 2018-10-08 | 2019-02-12 | 浙江科峰新材料有限公司 | A kind of preparation method of research of silicone modified coating printing adhesive |
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