CN105669942A - Polyurethane-modified pigment printing binding agent preparation method - Google Patents
Polyurethane-modified pigment printing binding agent preparation method Download PDFInfo
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- CN105669942A CN105669942A CN201610047858.2A CN201610047858A CN105669942A CN 105669942 A CN105669942 A CN 105669942A CN 201610047858 A CN201610047858 A CN 201610047858A CN 105669942 A CN105669942 A CN 105669942A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/0838—Manufacture of polymers in the presence of non-reactive compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/675—Low-molecular-weight compounds
- C08G18/6755—Unsaturated carboxylic acids
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/52—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
- D06P1/5264—Macromolecular compounds obtained otherwise than by reactions involving only unsaturated carbon-to-carbon bonds
- D06P1/5285—Polyurethanes; Polyurea; Polyguanides
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- Chemical & Material Sciences (AREA)
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- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Textile Engineering (AREA)
- Polyurethanes Or Polyureas (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a polyurethane-modified pigment printing binding agent preparation method and belongs to the field of pigment printing binding agent synthesis.The polyurethane-modified pigment printing binding agent preparation method includes the steps of subjecting polyether-type polyalcohol with the molecular weight being 1500 to dehydration by evaporation, mixing the dehydrated polyether-type polyalcohol with isophorone diisocyanate while stirring according to a molar ratio of 1:1.5, dropwise adding dibutyltin dilaurate and acrylic acid to perform temperature rise reaction, adding 2,2-dimethylol propionic acid and styrene to continue reacting prior to decreasing to the room temperature, adding triethylamine for neutral reaction and adding distilled water for emulsification so as to obtain a polyurethane-modified pigment printing binding agent.On the basis of the prior art, the polyurethane-modified pigment printing binding agent preparation method has the advantages that reaction conditions are optimized, and the acrylic acid and the styrene are added, so that polyurethane modification quality can be improved; the obtained polyurethane-modified pigment printing binding agent is excellent in hand feel quality, washable and good in soap fastness, thereby being high in economic benefit and beneficial to industrial popularization.
Description
Technical field:
The present invention relates to the preparation method of a kind of polyurethane-modified pigment printing binding agent, belong to pigment printing binding agent synthesis field.
Background technology:
Domestic often that pigment printing binding agent specification of quality is higher, require tackiness agent have multi-functional and multiple condition as: can use under acid, alkali, high temperature, low temperature, this just considerably increases the difficulty of adhesive product quality control, compared with external excellent level tackiness agent, state's inner binder quality is unstable, is mainly manifested in the aspects such as molecular weight is little, emulsification system is poor, particle dia distribution is uneven, level of residual monomers height. In addition, for the release that self-cross linking type tackiness agent Problems existing is exactly formaldehyde, wear resistance and washing fastness in order to improve tackiness agent add N hydroxymethyl acrylamide monomer in self-cross linking type tackiness agent synthesizes, thus tackiness agent self-crosslinking and tackiness agent and cellulosic fibre are cross-linked. Owing to N hydroxymethyl acrylamide adopts formaldehyde method to make polymkeric substance methylolation in building-up process, therefore adopt its tackiness agent making self-crosslinking component all containing a small amount of free formaldehyde, adopt the fabric face free formaldehyde major part after its arrangement can exceed release limit. Therefore, the use of this type of tackiness agent receives a definite limitation. In addition it is exactly tackiness agent to pigment printing being printed the feel problem of big area flower-shape fabric, yellowing phenomenon and all needs to be improved further with the problem such as the crock fastness of fiber, clinging power difference.
People are scattered in water urethane or are dissolved in water the tackiness agent formed aqueous polyurethane adhesive, and also someone claims aqueous polyurethane to be waterbased urethane or aqueous polyurethane. Particle diameter or outward appearance according to aqueous polyurethane can be divided into: particle diameter < 0.001 μm, the aqueous polyurethane of appearance transparent; Particle diameter is between 0.001～0.1 μm, the polyurethane dispersing liquid of translucent appearance; Particle diameter > 0.1 μm, the polyaminoester emulsion of outward appearance gonorrhoea. The urethane that particle diameter is greater than 0.001 μm by people traditionally is again polyurethane dispersing liquid or polyaminoester emulsion. Aqueous polyurethane exists mainly with polyaminoester emulsion greatly in actual applications, and aqueous solution form exists less.
Aqueous polyurethane is medium taking water, have smell little, energy-conservation, operate easy to process, do not fire, the advantage such as free from environmental pollution, the people got more and more pays close attention to.In aqueous binder, a few days ago domestic still based on tackiness agents such as polyethylene vinyl acetate between to for plastic class emulsion, polyacrylate emulsion, water-based three urea formaldehyde, aqueous polyurethanes. Aqueous polyurethane has the excellent properties such as viscosity is big, snappiness good, resistance to low temperature, so aqueous polyurethane adhesive has bigger development prospect.
Xi'an Polytechnic University's textile chemistries in 2013 and dye range specialine Gao Qiaoyan disclose one section " synthesis of polyurethane-modified pigment printing binding agent and applied research " by name and apply isophorone diisocyanate and polyether glycol, 2, 2-dimethylol propionic acid, epoxy resin, silane coupling agent, triethylamine is main raw material, the method of self-emulsifying is adopted to prepare polyurethane-modified pigment printing binding agent: pre-polymerization temperature 65 DEG C, time 120min, chain extension temperature 75 DEG C, time 120min, R value is 2.5, DMPA consumption is 2.5% of free-NCO groups in prepolymerization system, degree of neutralization is 100%, content of epoxy resin is 4% of free-NCO groups in prepolymerization system, silane coupling agent consumption is 3% of free-NCO groups in prepolymerization system, modification temperature 80 DEG C, modification time 60min, obtained stable, the polyurethane-modified pigment printing binding agent of excellent performance. the document be the present invention closest to prior art, but the fastness to wet rubbing of product made of the method and rinse that to wash colour fastness not high, complex process, is not easy to industrialization promotion simultaneously.
Summary of the invention:
It is an object of the invention to for the deficiencies in the prior art, the preparation method of a kind of polyurethane-modified pigment printing binding agent is provided, there is comparatively easy preparation technology, and the rear product of stamp process has good fastness to rubbing and look washes fastness, hand feel and drape, has higher economic benefit.
The present invention provides following technical scheme:
A preparation method for polyurethane-modified pigment printing binding agent, comprises following operation steps:
The first step: by molecular weight be 1500 polyether polyol temperature 110-115 DEG C, vacuum pressure be 0.1MPA when dehydration by evaporation 1h;
2nd step: polyether glycol and isophorone diisocyanate are slowly added in container according to mol ratio 1:1.5, stir and it is warming up to drip after 55-60 DEG C and add the dibutyl tin laurate of 0.05-0.06% volume and the vinylformic acid of 0.05-0.1% volume, regulate temperature to react 3h to 65-70 DEG C;
3rd step: be warmed up to 80-85 DEG C and add the 2,2-dimethylol propionic acid of 1-2% quality and the vinylbenzene reaction 2h of 0.01-0.02% quality;
4th step: be down to room temperature, adds the triethylamine with material amounts such as 2,2-dimethylol propionic acids and carries out neutralization reaction, stir 1h fast;
5th step: the distilled water of same volume is added container, stirs 1-2h fast, obtained polyurethane-modified pigment printing binding agent.
Preferably, by polyether polyol dehydration by evaporation 1h when temperature 110 DEG C, vacuum pressure are 0.1MPA that molecular weight is 1500 in the described the first step;
Polyether glycol and isophorone diisocyanate are slowly added in container by described 2nd step, stirs and drip add 0.05% dibutyl tin laurate of volume and the vinylformic acid of 0.05% volume after being warming up to 60 DEG C, regulate temperature to react 3h to 65 DEG C.
Preferably, described 3rd step is warmed up to 80 DEG C and adds the 2,2-dimethylol propionic acid of 2% quality and the vinylbenzene reaction 2h of 0.01% quality.
Preferably, described vinylformic acid is analytical reagent, vinylformic acid active constituent content >=99.5%, ignition residue content≤0.01%, level of inhibitor≤0.01.
Preferably, described vinylbenzene is analytical reagent, vinylbenzene active constituent content >=99%, polymer content≤0.002%, combustionresidue content≤0.05%, moisture content≤0.1%, ether content≤0.02%.
Preferably, described 2,2-dimethylol propionic acid is analytical reagent, 2,2-dimethylol propionic acid active constituent content >=99%, moisture content≤0.1%, ash oontent≤0.03%, hydroxy radical content >=24%.
The raw material of composite adhesives, mainly contains functional monomer, hard monomer and soft monomer. Wherein functional monomer is if 2,2-dimethylol propionic acid, toxilic acid, methacrylic acid, vinylformic acid etc. are containing the material of carboxyl, mainly rises from thickening power, crosslinked katalysis, improves stability of emulsion. Self-cross linking type tackiness agent also comprise such as cross-linkable monomers such as N hydroxymethyl acrylamide, acrylamide, epoxy resin (E-44), silane coupling agents (KH-550); Wherein rigid monomer has isocyanic ester, vinyl acetate between to for plastic, methyl methacrylate, vinylbenzene, vinyl cyanide, vinylchlorid etc., and main effect is to provide wear resistance, structural strength, stiffness, chemicals-resistant and washing fastness performance; Wherein soft monomer has polyoxyethylene glycol, polypropylene glycol, poly-glycerol, ethyl propenoate, divinyl, butyl methacrylate, ethene, n-butyl acrylate, ethyl propylene acid alcohol etc., and main effect gives polymkeric substance to the sticking power of hard monomer light fugitive group and shielding and certain flexibility; Chemical synthesis also to be added initiator and emulsifying agent etc. in addition.
The present invention with the addition of vinylformic acid on the processing condition basis of prior art in prepolymerization reaction process, vinylformic acid is the simplest unsaturated carboxylic acid, there is the association response of double bond and carboxyl functional group, addition reaction, functional group reactions and transesterification reaction, the many rings of preparation and heterogeneous ring compound can occur, be easily propionic acid by hydrogen reduction, meet alkali and can resolve into formic acid and acetic acid, in invention process, add a small amount of vinylformic acid, polyether glycol and the probability of collision of isophorone diisocyanate group can be increased, improve speed of reaction, reduce the reaction times.
The most important purposes of vinylbenzene is the monomer as synthetic rubber and plastics. Viscosity is tackiness agent important using property data, ion and antiparticle number on high-polymer molecular chain are more many, the viscosity of synthesized aqueous polyurethane emulsion is more big, and in addition, the viscosity of aqueous polyurethane affects not remarkable by factors such as the molecular weight of linking agent, urethane, solids contents. The present invention adds a small amount of vinylbenzene in chain extending reaction, plays important effect for keeping the viscosity that aqueous polyurethane is good.
The useful effect of the present invention:
1. process of the present invention adds a small amount of vinylformic acid, it is possible to increase the probability of collision of polyether glycol and isophorone diisocyanate group, it is to increase speed of reaction, reduces the reaction times.
2. the present invention adds a small amount of vinylbenzene in chain extending reaction, plays important effect for keeping the viscosity that aqueous polyurethane is good.
3. coating and fabric are had clinging power by tackiness agent, and coating is had certain fastness by tackiness agent after fabric face film forming, and film is smooth, thickness is even.
4. the modified paint printed adhesive agent that the present invention prepares has good hand feeling quality and water-fastness fastness to soaping, has extremely high economic benefit, is beneficial to industrialization promotion.
Embodiment:
Being described in detail by embodiments of the invention below, the present embodiment is implemented under premised on inventive technique scheme, gives detailed enforcement mode and concrete operating process, but protection scope of the present invention is not limited to following embodiment.The experimental program of unreceipted concrete condition in embodiment, the condition that conveniently condition or manufacturers advise usually is implemented.
Embodiment one
A preparation method for polyurethane-modified pigment printing binding agent, comprises following operation steps:
The first step: be polyether polyol dehydration by evaporation 1h when temperature 110 DEG C, vacuum pressure are 0.1MPA of 1500 by molecular weight;
2nd step: polyether glycol and isophorone diisocyanate are slowly added in container according to mol ratio 1:1.5, stir and drip add 0.05% dibutyl tin laurate of volume and the vinylformic acid of 0.05% volume after being warming up to 55 DEG C, regulate temperature to react 3h to 65 DEG C;
3rd step: be warmed up to 80 DEG C and add the 2,2-dimethylol propionic acid of 1% quality and the vinylbenzene reaction 2h of 0.01% quality;
4th step: be down to room temperature, adds the triethylamine with material amounts such as 2,2-dimethylol propionic acids and carries out neutralization reaction, stir 1h fast;
5th step: the distilled water of same volume is added container, stirs 1h fast, obtained polyurethane-modified pigment printing binding agent.
Embodiment two
A preparation method for polyurethane-modified pigment printing binding agent, comprises following operation steps:
The first step: be polyether polyol dehydration by evaporation 1h when temperature 115 DEG C, vacuum pressure are 0.1MPA of 1500 by molecular weight;
2nd step: polyether glycol and isophorone diisocyanate are slowly added in container according to mol ratio 1:1.5, stir and drip add 0.06% dibutyl tin laurate of volume and the vinylformic acid of 0.1% volume after being warming up to 60 DEG C, regulate temperature to react 3h to 70 DEG C;
3rd step: be warmed up to 85 DEG C and add the 2,2-dimethylol propionic acid of 2% quality and the vinylbenzene reaction 2h of 0.02% quality;
4th step: be down to room temperature, adds the triethylamine with material amounts such as 2,2-dimethylol propionic acids and carries out neutralization reaction, stir 1h fast;
5th step: the distilled water of same volume is added container, stirs 2h fast, obtained polyurethane-modified pigment printing binding agent.
Embodiment three
A preparation method for polyurethane-modified pigment printing binding agent, comprises following operation steps:
The first step: be polyether polyol dehydration by evaporation 1h when temperature 110 DEG C, vacuum pressure are 0.1MPA of 1500 by molecular weight;
2nd step: polyether glycol and isophorone diisocyanate are slowly added in container according to mol ratio 1:1.5, stir and drip add 0.05% dibutyl tin laurate of volume and the vinylformic acid of 0.1% volume after being warming up to 60 DEG C, regulate temperature to react 3h to 65 DEG C;
3rd step: be warmed up to 85 DEG C and add the 2,2-dimethylol propionic acid of 1% quality and the vinylbenzene reaction 2h of 0.02% quality;
4th step: be down to room temperature, adds the triethylamine with material amounts such as 2,2-dimethylol propionic acids and carries out neutralization reaction, stir 1h fast;
5th step: the distilled water of same volume is added container, stirs 1h fast, obtained polyurethane-modified pigment printing binding agent.
Embodiment four
A preparation method for polyurethane-modified pigment printing binding agent, comprises following operation steps:
The first step: be polyether polyol dehydration by evaporation 1h when temperature 115 DEG C, vacuum pressure are 0.1MPA of 1500 by molecular weight;
2nd step: polyether glycol and isophorone diisocyanate are slowly added in container according to mol ratio 1:1.5, stir and drip add 0.06% dibutyl tin laurate of volume and the vinylformic acid of 0.05% volume after being warming up to 55 DEG C, regulate temperature to react 3h to 70 DEG C;
3rd step: be warmed up to 80 DEG C and add the 2,2-dimethylol propionic acid of 2% quality and the vinylbenzene reaction 2h of 0.01% quality;
4th step: be down to room temperature, adds the triethylamine with material amounts such as 2,2-dimethylol propionic acids and carries out neutralization reaction, stir 1h fast;
5th step: the distilled water of same volume is added container, stirs 2h fast, obtained polyurethane-modified pigment printing binding agent.
Embodiment five
A preparation method for polyurethane-modified pigment printing binding agent, comprises following operation steps:
The first step: be polyether polyol dehydration by evaporation 1h when temperature 110 DEG C, vacuum pressure are 0.1MPA of 1500 by molecular weight;
2nd step: polyether glycol and isophorone diisocyanate are slowly added in container according to mol ratio 1:1.5, stir and drip add 0.05% dibutyl tin laurate of volume and the vinylformic acid of 0.05% volume after being warming up to 60 DEG C, regulate temperature to react 3h to 65 DEG C;
3rd step: be warmed up to 80 DEG C and add the 2,2-dimethylol propionic acid of 2% quality and the vinylbenzene reaction 2h of 0.01% quality;
4th step: be down to room temperature, adds the triethylamine with material amounts such as 2,2-dimethylol propionic acids and carries out neutralization reaction, stir 1h fast;
5th step: the distilled water of same volume is added container, stirs 1h fast, obtained polyurethane-modified pigment printing binding agent.
Embodiment six
A preparation method for polyurethane-modified pigment printing binding agent, comprises following operation steps:
The first step: be polyether polyol dehydration by evaporation 1h when temperature 110 DEG C, vacuum pressure are 0.1MPA of 1500 by molecular weight;
2nd step: polyether glycol and isophorone diisocyanate are slowly added in container according to mol ratio 1:1.5, stir and drip add 0.05% dibutyl tin laurate of volume and the vinylformic acid of 0.05% volume after being warming up to 60 DEG C, regulate temperature to react 3h to 65 DEG C;
3rd step: be warmed up to 85 DEG C and add the 2,2-dimethylol propionic acid of 2% quality and the vinylbenzene reaction 2h of 0.01% quality;
4th step: be down to room temperature, adds the triethylamine with material amounts such as 2,2-dimethylol propionic acids and carries out neutralization reaction, stir 1h fast;
5th step: the distilled water of same volume is added container, stirs 2h fast, obtained polyurethane-modified pigment printing binding agent.
Comparative example:
Adopt commercially available low-temperature adhesive.
Described vinylformic acid is analytical reagent, vinylformic acid active constituent content >=99.5%, ignition residue content≤0.01%, level of inhibitor≤0.01.
Described vinylbenzene is analytical reagent, vinylbenzene active constituent content >=99%, polymer content≤0.002%, combustionresidue content≤0.05%, moisture content≤0.1%, ether content≤0.02%.
Described 2,2-dimethylol propionic acid is analytical reagent, 2,2-dimethylol propionic acid active constituent content >=99%, moisture content≤0.1%, ash oontent≤0.03%, hydroxy radical content >=24%.
The pigment printing binding agent adopting the embodiment of the present invention to prepare is applied to printing coating, its Printing performance is carried out research and compares. Described fabric is the pure cotton fabric obtained through destarch, boiling-off and bleaching.
Pigment printing technique:
Printing paste prescription: coating blue 2.5g, tackiness agent 5g, thickening material 1.5g, water 41g, amount to 50g.
Printing technology: stamp → pre-baking (70 DEG C × 5min) → bake (150 DEG C × 5min).
Performance test:
(1) colour fastness to rubbing test
With reference to GB/T251-2008 regulation.Prepare each two pieces of samples being not less than 50mm × 200mm of longitude and latitude, test for dry fastness and fastness to wet rubbing.
(2) scrubbing-resistant color fastness test
According to GB/T420-90 standard. Prepare one piece of sample being not less than 80mm × 250mm, for scrubbing colour fastness test.
(3) K/S pH-value determination pH
Getting PRINTED FABRIC, measure its K/S value with Datacolor-SF600 color measurement and color match instrument, K/S value is more big, represents that fabric color is more dark.
(4) hand feel performance test
Close order and touch the fabric after arranging, taking 5-10 people as a small group, grade, according to different feels, PRINTED FABRIC being carried out hand feel evaluation, concrete assessment method is: carries out feel grading from flexibility, smooth feeling two aspect, is divided into 5 grades, 1 grade worst, and fabric feeling is relatively hard, and sliding glutinous sense is poor. 5 grades preferably, and fabrics feel soft, cunning are glutinous.
Concrete grading is as shown in Table 1.
Table one: feel is graded
| 5 grades | 4 grades | 3 grades | 2 grades | 2 grades |
| Very good | Well | In | Slightly poor | Difference |
Table two: the polyurethane-modified pigment printing effect of the embodiment of the present invention
Tackiness agent of the present invention is 10% at addition, and when relatively prior art obviously reduces addition, the resistance to dry fastness of the fabric after stamp and fastness to wet rubbing all have higher level, and colourity is dark, and printing performance is superior.
(5) Fabric Style test
On KESFB2 auto testing instrument to stamp after Fabric Style test. Comprise compression performance, bending property and surface friction property to test.
Table three: the compression performance of fabric after embodiment of the present invention tackiness agent stamp
Table four: the bending property of fabric after embodiment of the present invention tackiness agent stamp
Table five: the surface friction property of fabric after embodiment of the present invention tackiness agent stamp
Compression performance, bending property and surface friction property can represent the flexibility of fabric, from above-mentioned three tables, cotton fabric compressibility after stamp diminishes, bending property diminishes, the frictional behaviour of fabric face then increases, this is mainly owing to the crosslinked action of tackiness agent makes the style of original cotton fabric change, because tackiness agent is cross-linked into film on fabric, this layer of membranoid substance matter makes fabric fluffiness decline, stiffness rises, and overcome original fabric face and have groove or uneven, add the smooth feeling of fabric. Comparatively speaking, the tackiness agent described in the embodiment of the present invention is more given prominence in the performance of each performance.
Above content is only the better embodiment of the present invention, for the those of ordinary skill of this area, according to the thought of the present invention, all will change in specific embodiments and applications, and this description should not be construed as limitation of the present invention.
Claims (6)
1. the preparation method of a polyurethane-modified pigment printing binding agent, it is characterised in that, comprise following operation steps:
The first step: by molecular weight be 1500 polyether polyol temperature 110-115 DEG C, vacuum pressure be 0.1MPA when dehydration by evaporation 1h;
2nd step: polyether glycol and isophorone diisocyanate are slowly added in container according to mol ratio 1:1.5, stir and it is warming up to drip after 55-60 DEG C and add the dibutyl tin laurate of 0.05-0.06% volume and the vinylformic acid of 0.05-0.1% volume, regulate temperature to react 3h to 65-70 DEG C;
3rd step: be warmed up to 80-85 DEG C and add the 2,2-dimethylol propionic acid of 1-2% quality and the vinylbenzene reaction 2h of 0.01-0.02% quality;
4th step: be down to room temperature, adds the triethylamine with material amounts such as 2,2-dimethylol propionic acids and carries out neutralization reaction, stir 1h fast;
5th step: the distilled water of same volume is added container, stirs 1-2h fast, obtained polyurethane-modified pigment printing binding agent.
2. the preparation method of a kind of polyurethane-modified pigment printing binding agent according to claim 1, it is characterised in that:
Molecular weight is by the described the first step polyether polyol dehydration by evaporation 1h when temperature 110 DEG C, vacuum pressure are 0.1MPA of 1500;
Polyether glycol and isophorone diisocyanate are slowly added in container by described 2nd step, stirs and drip add 0.05% dibutyl tin laurate of volume and the vinylformic acid of 0.05% volume after being warming up to 60 DEG C, regulate temperature to react 3h to 65 DEG C.
3. the preparation method of a kind of polyurethane-modified pigment printing binding agent according to claim 1, it is characterised in that: described 3rd step is warmed up to 80 DEG C and adds the 2,2-dimethylol propionic acid of 2% quality and the vinylbenzene reaction 2h of 0.01% quality.
4. the preparation method of a kind of polyurethane-modified pigment printing binding agent according to claim 1 and 2, it is characterized in that: described vinylformic acid is analytical reagent, vinylformic acid active constituent content >=99.5%, ignition residue content≤0.01%, level of inhibitor≤0.01.
5. the preparation method of a kind of polyurethane-modified pigment printing binding agent according to claim 1 or 3, it is characterized in that: described vinylbenzene is analytical reagent, vinylbenzene active constituent content >=99%, polymer content≤0.002%, combustionresidue content≤0.05%, moisture content≤0.1%, ether content≤0.02%.
6. the preparation method of a kind of polyurethane-modified pigment printing binding agent according to claim 1, it is characterized in that: described 2,2-dimethylol propionic acid is analytical reagent, 2,2-dimethylol propionic acid active constituent content >=99%, moisture content≤0.1%, ash oontent≤0.03%, hydroxy radical content >=24%.
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