CN105669942B - A kind of preparation method of polyurethane-modified pigment printing binding agent - Google Patents
A kind of preparation method of polyurethane-modified pigment printing binding agent Download PDFInfo
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- CN105669942B CN105669942B CN201610047858.2A CN201610047858A CN105669942B CN 105669942 B CN105669942 B CN 105669942B CN 201610047858 A CN201610047858 A CN 201610047858A CN 105669942 B CN105669942 B CN 105669942B
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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)
- Chemical Kinetics & Catalysis (AREA)
- 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)
- Adhesives Or Adhesive Processes (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a kind of preparation methods of polyurethane-modified pigment printing binding agent, belong to pigment printing binding agent and synthesize field, with isophorone diisocyanate according to molar ratio 1 after the polyether polyol dehydration by evaporation for being 1500 by molecular weight:1.5 being mixed, dropwise addition dibutyl tin laurate and acrylic acid temperature reaction, 2,2 dihydromethyl propionic acids of addition and styrene are down to room temperature after the reaction was continued, it is eventually adding triethylamine progress neutralization reaction and is eventually adding distillation water emulsification, polyurethane-modified pigment printing binding agent is made.The present invention is on the basis of existing technology, optimize reaction condition, and it is added to acrylic acid and styrene, polyurethane-modified quality can be improved, there is good hand feeling quality and water-fastness fastness to soaping after the modified coating printing adhesive application being prepared, high financial profit is conducive to industrialization promotion.
Description
Technical field：
The present invention relates to a kind of preparation methods of polyurethane-modified pigment printing binding agent, belong to pigment printing binding agent conjunction
At field.
Background technology：
It is domestic often higher to pigment printing binding agent quality requirement, it is desirable that adhesive has multi-functional and in a variety of conditions
Such as：It can be used under acid, alkali, high temperature, low temperature, this just considerably increases the difficulty of adhesive product quality control, excellent with foreign countries
Grade adhesive compare, state's inner binder unstable quality, be mainly manifested in molecular weight is small, emulsification system is poor, particle diameter distribution
The uneven, aspect such as level of residual monomers is high.In addition, for self-cross linking type adhesive there are the problem of be exactly formaldehyde release, be
The wearability and washability for improving adhesive add N hydroxymethyl acrylamide monomer in the synthesis of self-cross linking type adhesive,
To make adhesive self-crosslinking and adhesive are crosslinked with cellulose fibre.In the synthesis process due to N hydroxymethyl acrylamide
Polymer methylolation is made using formaldehyde method, therefore the adhesive of self-crosslinking component is made using it and contains a small amount of free first
Aldehyde can be more than largely release limit using the fabric surface free formaldehyde after its arrangement.Therefore, the use of such adhesive by
Certain restrictions is arrived.In addition it is exactly feel problem, yellowing phenomenon of the adhesive to printing large area flower-shape fabric in pigment printing
And all need to be further increased with the problems such as crock fastness of fiber, adhesion force difference.
People they in water or the adhesive of formation soluble in water aqueous polyurethane adhesive, also have person
Aqueous polyurethane is water-based polyurethane or aqueous polyurethane.It can be divided into according to the grain size of aqueous polyurethane or appearance：Grain size ＜
0.001 μm, the aqueous polyurethane of appearance transparent；Grain size is between 0.001~0.1 μm, the polyurethane point of translucent appearance
Dispersion liquid；0.1 μm of grain size ＞, the polyaminoester emulsion of appearance gonorrhoea.Traditionally polyurethane of the people by grain size more than 0.001 μm is called
Polyurethane dispersing liquid or polyaminoester emulsion.Aqueous polyurethane exists with polyaminoester emulsion mostly in practical applications, aqueous solution shape
There are less for formula.
Aqueous polyurethane has that smell is small, energy saving, operation is easy to process, non-ignitable, free from environmental pollution etc. excellent using water as medium
Point, is paid close attention to by more and more people.It is a few days ago domestic still with polyvinyl acetate vinyl lotion, poly- in aqueous binder
Based on the adhesives such as acrylic emulsion, aqueous three urea formaldehyde, aqueous polyurethane.Aqueous polyurethane has viscosity big, flexible
Property the excellent properties such as good, low temperature resistant, so aqueous polyurethane adhesive has larger development prospect.
Xi'an Polytechnic University's textile chemistry in 2013 and dye range specialine Gao Qiaoyan disclose one it is entitled《Polyurethane-modified painting
Expect the synthesis and application study of printing adhesive》Using isophorone diisocyanate and polyether polyol, 2,2- dihydroxymethyls
Propionic acid, epoxy resin, silane coupling agent, triethylamine are primary raw material, and polyurethane-modified coating is prepared using the method for self-emulsifying
Printing adhesive：65 DEG C of pre-polymerization temperature, time 120min, 75 DEG C of chain extension temperature, time 120min, R values are 2.5, DMPA dosages
Be 2.5% of free-NCO groups in prepolymerization system, degree of neutralization 100%, content of epoxy resin be prepolymerization system in dissociate-
The 4% of NCO group, silane coupling agent dosage are 3% of free-NCO groups in prepolymerization system, 80 DEG C of modification temperature, when modified
Between 60min, be made stablize, the polyurethane-modified pigment printing binding agent that has excellent performance.The document is the present invention closest to now
There is a technology, but the fastness to wet rubbing of product made of this method and to rinse color fastness not high, while complex process, it is not easy to work
Industryization is promoted.
Invention content：
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of systems of polyurethane-modified pigment printing binding agent
Preparation Method has relatively simple preparation process, and there is product good fastness to rubbing and color to wash jail after stamp processing
Degree, comfortable feel have higher economic benefit.
The present invention provides the following technical solutions：
A kind of preparation method of polyurethane-modified pigment printing binding agent, including following operating procedure：
The first step：In 110-115 DEG C of temperature, vacuum pressure it is 0.1MPA's by polyether polyol that molecular weight is 1500
Under the conditions of dehydration by evaporation 1h；
Second step：By polyether polyol and isophorone diisocyanate according to molar ratio 1:1.5 are slowly added in container,
It stirs and is warming up to dibutyl tin laurate and 0.05-0.1% volumes that 0.05-0.06% volumes are added dropwise after 55-60 DEG C
Acrylic acid, adjust temperature to 65-70 DEG C react 3h；
Third walks：It is warming up to the 2,2- dihydromethyl propionic acids and 0.01-0.02% mass of 80-85 DEG C of addition 1-2% mass
Styrene react 2h；
4th step：It is down to room temperature, is added and the triethylamine of the amount of substance such as 2,2- dihydromethyl propionic acids carries out neutralization reaction, soon
Speed stirring 1h；
5th step：Container is added in the distilled water of same volume, quickly stirs 1-2h, it is viscous that polyurethane-modified pigment printing is made
Mixture.
Preferably, it is in 110 DEG C of temperature, vacuum pressure by the polyether polyol that molecular weight is 1500 in the first step
Dehydration by evaporation 1h under the conditions of 0.1MPA；
Polyether polyol and isophorone diisocyanate are slowly added in container in the second step, stirs and rises
Temperature adjusts temperature to 65 DEG C to the acrylic acid for the dibutyl tin laurate and 0.05% volume that 0.05% volume is added dropwise after 60 DEG C
React 3h.
Preferably, 2, the 2- dihydromethyl propionic acids and 0.01% matter of 80 DEG C of 2% mass of addition are warming up in the third step
The styrene of amount reacts 2h.
Preferably, the acrylic acid is analytical reagents, acrylic acid active constituent content >=99.5%, ignition residue content
≤ 0.01%, level of inhibitor≤0.01.
Preferably, the styrene be analytical reagents, styrene active constituent content >=99%, polymer content≤
0.002%, combustion residue content≤0.05%, moisture≤0.1%, ether content≤0.02%.
Preferably, 2, the 2- dihydromethyl propionic acids are analytical reagents, 2,2- dihydromethyl propionic acid active constituent contents
>=99%, moisture≤0.1%, content of ashes≤0.03%, hydroxy radical content >=24%.
The raw material of composite adhesives, main functional property monomer, hard monomer and soft monomer.Wherein functional monomer such as 2,2-
The substance containing carboxyl such as dihydromethyl propionic acid, maleic acid, methacrylic acid, acrylic acid mainly rises from thickening power, crosslinking
Catalytic action improves stability of emulsion.Further include in self-cross linking type adhesive as：N hydroxymethyl acrylamide, acrylamide, ring
The cross-linkable monomers such as oxygen resin (E-44), silane coupling agent (KH-550)；Wherein rigid monomer have isocyanates, vinyl acetate,
Methyl methacrylate, styrene, acrylonitrile, vinyl chloride etc., main function are to provide wearability, structural strength, stiffness, resistance to
Chemicals and washability performance；Wherein soft monomer has polyethylene glycol, polypropylene glycol, polyglycerol, ethyl acrylate, fourth two
Alkene, butyl methacrylate, ethylene, n-butyl acrylate, ethyl propylene acid alcohol etc., main function are to confer to polymer to hard single
The adhesive force and shielding of body light fugitive group and certain flexibility；In addition to be also added in chemical synthesis initiator and
Emulsifier etc..
The present invention is added to acrylic acid on the basis of the process conditions of the prior art during prepolymerization reaction, and acrylic acid is
Simplest unsaturated carboxylic acid has the association response of double bond and carboxyl functional group, addition reaction, functional group reactions can occur
And ester exchange reaction, prepare polycyclic and heterocyclic compound, easily by hydrogen reduction be propionic acid, meet alkali can decompose formic acid and acetic acid,
During invention, a small amount of acrylic acid is added, touching for polyether polyol and isophorone diisocyanate group can be increased
Probability is hit, reaction rate is improved, reduces the reaction time.
The most important purposes of styrene is the monomer as synthetic rubber and plastics.Viscosity is one important use of adhesive
Performance indicator, the ion and antiparticle number on high-polymer molecular chain are more, and the viscosity of synthesized aqueous polyurethane emulsion is got over
Greatly, in addition, the viscosity of aqueous polyurethane is influenced not significantly by factors such as crosslinking agent, the molecular weight of polyurethane, solid contents.This
A small amount of styrene is added in invention in chain extending reaction, for keeping the good viscosity of aqueous polyurethane to play an important role.
Beneficial effects of the present invention：
1. process of the present invention adds a small amount of acrylic acid, polyether polyol and isophorone diisocyanate collection can be increased
The collision probability of group improves reaction rate, reduces the reaction time.
2. the present invention adds a small amount of styrene in chain extending reaction, for keeping the good viscosity of aqueous polyurethane to play weight
The effect wanted.
3. adhesive there is adhesion strength, adhesive to have centainly to coating after fabric surface film forming coating and fabric
Fastness, and film is smooth, thickness is uniform.
4. the modified coating printing adhesive that the present invention is prepared has good hand feeling quality and water-fastness resistance to soaps
Fastness has high economic benefit, is conducive to industrialization promotion.
Specific implementation mode：
The embodiment of the present invention is described in detail below, the present embodiment carries out under premised on inventive technique scheme
Implement, gives detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following realities
Apply example.The experimental program of actual conditions is not specified in embodiment, the condition usually according to normal condition or proposed by manufacturer
Implement.
Embodiment one
A kind of preparation method of polyurethane-modified pigment printing binding agent, including following operating procedure：
The first step：The condition for being 0.1MPA in 110 DEG C of temperature, vacuum pressure by the polyether polyol that molecular weight is 1500
Lower dehydration by evaporation 1h；
Second step：By polyether polyol and isophorone diisocyanate according to molar ratio 1:1.5 are slowly added in container,
The acrylic acid of dibutyl tin laurate and 0.05% volume that 0.05% volume is added dropwise after 55 DEG C is stirred and be warming up to, is adjusted
Temperature reacts 3h to 65 DEG C；
Third walks：The styrene for being warming up to 2,2- dihydromethyl propionic acids and 0.01% mass that 80 DEG C are added 1% mass is anti-
Answer 2h；
4th step：It is down to room temperature, is added and the triethylamine of the amount of substance such as 2,2- dihydromethyl propionic acids carries out neutralization reaction, soon
Speed stirring 1h；
5th step：Container is added in the distilled water of same volume, quickly stirs 1h, polyurethane-modified pigment printing bonding is made
Agent.
Embodiment two
A kind of preparation method of polyurethane-modified pigment printing binding agent, including following operating procedure：
The first step：The condition for being 0.1MPA in 115 DEG C of temperature, vacuum pressure by the polyether polyol that molecular weight is 1500
Lower dehydration by evaporation 1h；
Second step：By polyether polyol and isophorone diisocyanate according to molar ratio 1:1.5 are slowly added in container,
The acrylic acid of dibutyl tin laurate and 0.1% volume that 0.06% volume is added dropwise after 60 DEG C is stirred and be warming up to, is adjusted
Temperature reacts 3h to 70 DEG C；
Third walks：The styrene for being warming up to 2,2- dihydromethyl propionic acids and 0.02% mass that 85 DEG C are added 2% mass is anti-
Answer 2h；
4th step：It is down to room temperature, is added and the triethylamine of the amount of substance such as 2,2- dihydromethyl propionic acids carries out neutralization reaction, soon
Speed stirring 1h；
5th step：Container is added in the distilled water of same volume, quickly stirs 2h, polyurethane-modified pigment printing bonding is made
Agent.
Embodiment three
A kind of preparation method of polyurethane-modified pigment printing binding agent, including following operating procedure：
The first step：The condition for being 0.1MPA in 110 DEG C of temperature, vacuum pressure by the polyether polyol that molecular weight is 1500
Lower dehydration by evaporation 1h；
Second step：By polyether polyol and isophorone diisocyanate according to molar ratio 1:1.5 are slowly added in container,
The acrylic acid of dibutyl tin laurate and 0.1% volume that 0.05% volume is added dropwise after 60 DEG C is stirred and be warming up to, is adjusted
Temperature reacts 3h to 65 DEG C；
Third walks：The styrene for being warming up to 2,2- dihydromethyl propionic acids and 0.02% mass that 85 DEG C are added 1% mass is anti-
Answer 2h；
4th step：It is down to room temperature, is added and the triethylamine of the amount of substance such as 2,2- dihydromethyl propionic acids carries out neutralization reaction, soon
Speed stirring 1h；
5th step：Container is added in the distilled water of same volume, quickly stirs 1h, polyurethane-modified pigment printing bonding is made
Agent.
Example IV
A kind of preparation method of polyurethane-modified pigment printing binding agent, including following operating procedure：
The first step：The condition for being 0.1MPA in 115 DEG C of temperature, vacuum pressure by the polyether polyol that molecular weight is 1500
Lower dehydration by evaporation 1h；
Second step：By polyether polyol and isophorone diisocyanate according to molar ratio 1:1.5 are slowly added in container,
The acrylic acid of dibutyl tin laurate and 0.05% volume that 0.06% volume is added dropwise after 55 DEG C is stirred and be warming up to, is adjusted
Temperature reacts 3h to 70 DEG C；
Third walks：The styrene for being warming up to 2,2- dihydromethyl propionic acids and 0.01% mass that 80 DEG C are added 2% mass is anti-
Answer 2h；
4th step：It is down to room temperature, is added and the triethylamine of the amount of substance such as 2,2- dihydromethyl propionic acids carries out neutralization reaction, soon
Speed stirring 1h；
5th step：Container is added in the distilled water of same volume, quickly stirs 2h, polyurethane-modified pigment printing bonding is made
Agent.
Embodiment five
A kind of preparation method of polyurethane-modified pigment printing binding agent, including following operating procedure：
The first step：By polyether polyol that molecular weight is 1500 under the conditions of 110 DEG C of temperature, vacuum pressure are 0.1MPA
Dehydration by evaporation 1h；
Second step：By polyether polyol and isophorone diisocyanate according to molar ratio 1:1.5 are slowly added in container,
The acrylic acid of dibutyl tin laurate and 0.05% volume that 0.05% volume is added dropwise after 60 DEG C is stirred and be warming up to, is adjusted
Temperature reacts 3h to 65 DEG C；
Third walks：The styrene for being warming up to 2,2- dihydromethyl propionic acids and 0.01% mass that 80 DEG C are added 2% mass is anti-
Answer 2h；
4th step：It is down to room temperature, is added and the triethylamine of the amount of substance such as 2,2- dihydromethyl propionic acids carries out neutralization reaction, soon
Speed stirring 1h；
5th step：Container is added in the distilled water of same volume, quickly stirs 1h, polyurethane-modified pigment printing bonding is made
Agent.
Embodiment six
A kind of preparation method of polyurethane-modified pigment printing binding agent, including following operating procedure：
The first step：By polyether polyol that molecular weight is 1500 under the conditions of 110 DEG C of temperature, vacuum pressure are 0.1MPA
Dehydration by evaporation 1h；
Second step：By polyether polyol and isophorone diisocyanate according to molar ratio 1:1.5 are slowly added in container,
The acrylic acid of dibutyl tin laurate and 0.05% volume that 0.05% volume is added dropwise after 60 DEG C is stirred and be warming up to, is adjusted
Temperature reacts 3h to 65 DEG C；
Third walks：The styrene for being warming up to 2,2- dihydromethyl propionic acids and 0.01% mass that 85 DEG C are added 2% mass is anti-
Answer 2h；
4th step：It is down to room temperature, is added and the triethylamine of the amount of substance such as 2,2- dihydromethyl propionic acids carries out neutralization reaction, soon
Speed stirring 1h；
5th step：Container is added in the distilled water of same volume, quickly stirs 2h, polyurethane-modified pigment printing bonding is made
Agent.
Comparative example：
Using commercially available low-temperature adhesive.
The acrylic acid be analytical reagents, acrylic acid active constituent content >=99.5%, ignition residue content≤
0.01%, level of inhibitor≤0.01.
The styrene be analytical reagents, styrene active constituent content >=99%, polymer content≤0.002%,
Combustion residue content≤0.05%, moisture≤0.1%, ether content≤0.02%.
2, the 2- dihydromethyl propionic acids be analytical reagents, 2,2- dihydromethyl propionic acid active constituent content >=99%,
Moisture≤0.1%, content of ashes≤0.03%, hydroxy radical content >=24%.
Printing coating is applied to using the pigment printing binding agent that the embodiment of the present invention is prepared, to its Printing
It can carry out research comparison.The fabric is the pure cotton fabric obtained by desizing, boiling-off and bleaching.
Pigment printing technique：
Printing paste prescription：Material basket 2.5g, adhesive 5g, thickener 1.5g, water 41g are applied, 50g is amounted to.
Printing technology：Stamp → preliminary drying (70 DEG C × 5min) → it bakes (150 DEG C × 5min).
Performance test：
(1) colour fastness to rubbing is tested
With reference to GB/T 251-2008 regulations.Prepare each two pieces samples for being not less than 50mm × 200mm of longitude and latitude, is used for unlubricated friction
Rubbing fastness and fastness to wet rubbing test.
(2) scrubbing-resistant color fastness is tested
According to GB/T 420-90 standards.Prepare one piece of sample for being not less than 80mm × 250mm, is surveyed for scrubbing color fastness
Examination.
(3) K/S values measure
PRINTED FABRIC is taken, its K/S value is measured with Datacolor-SF600 color measurement and color match instrument, K/S values are bigger, indicate fabric
Color is deeper.
(4) hand feel performance is tested
It closes the fabric that mesh touches after arranging to grade using 5-10 people as a small group, is knitted stamp according to different feels
Object carries out hand feel evaluation, and specific assessment method is：Feel grading is carried out in terms of flexibility, smooth feeling two, is divided into 5 grades, 1 grade most
Difference, fabric feeling is harder, and sliding glutinous sense is poor.5 grades preferably, and fabrics feel soft, cunning are glutinous.
Specific grading is as shown in Table 1.
Table one：Feel is graded
| 5 grades | 4 grades | 3 grades | 2 grades | 2 grades |
| It is very good | Well | In | It is slightly worse | Difference |
Table two:The polyurethane-modified pigment printing effect of the embodiment of the present invention
Invention adhesives are 10% in additive amount, in the case where being substantially reduced additive amount compared with the prior art, after stamp
The resistance to dry fastness of fabric and fastness to wet rubbing all have higher level, and coloration is deep, and printing performance is superior.
(5) Fabric Style is tested
On KESFB2 auto testing instruments to stamp after Fabric Style test.Including compression performance, bending property and
Surface friction property is tested.
Table three：The compression performance of fabric after adhesive stamp of the embodiment of the present invention
Table four：The bending property of fabric after adhesive stamp of the embodiment of the present invention
Table five：The surface friction property of fabric after adhesive stamp of the embodiment of the present invention
Compression performance, bending property and surface friction property can indicate the flexibility of fabric, by above-mentioned three table it is found that
Cotton fabric compressibility after stamp becomes smaller, and bending property becomes smaller, and the frictional behaviour of fabric surface then increases, this master
If since the crosslinked action of adhesive makes the style of original cotton fabric change, because adhesive is crosslinked film forming on the fabric,
This layer of membranaceous material makes fabric bulkiness decline, and stiffness rises, and overcomes original fabric surface and have groove or bumps
Injustice increases the smooth feeling of fabric.In comparison, the adhesive described in the embodiment of the present invention each performance performance more
It is prominent.
The above content is only the better embodiment of the present invention, for those of ordinary skill in the art, according to the present invention
Thought, there will be changes in the specific implementation manner and application range, and the content of the present specification should not be construed as to this hair
Bright limitation.
Claims (6)
1. a kind of preparation method of polyurethane-modified pigment printing binding agent, which is characterized in that including following operating procedure：
The first step：By polyether polyol that molecular weight is 1500 under conditions of 110-115 DEG C of temperature, vacuum pressure are 0.1MPa
Dehydration by evaporation 1h；
Second step：By polyether polyol and isophorone diisocyanate according to molar ratio 1:1.5 are slowly added in container, stirring
And it is warming up to the third of dibutyl tin laurate and 0.05-0.1% volumes that 0.05-0.06% volumes are added dropwise after 55-60 DEG C
Olefin(e) acid adjusts temperature to 65-70 DEG C of reaction 3h；
Third walks：It is warming up to the benzene of the 2,2- dihydromethyl propionic acids and 0.01-0.02% mass of 80-85 DEG C of addition 1-2% mass
Ethylene reaction 2h；
4th step：It is down to room temperature, is added and the triethylamine of the amount of substance such as 2,2- dihydromethyl propionic acids carries out neutralization reaction, quickly stir
Mix 1h；
5th step：Container is added in the distilled water of same volume, quickly stirs 1-2h, polyurethane-modified pigment printing bonding is made
Agent.
2. a kind of preparation method of polyurethane-modified pigment printing binding agent according to claim 1, it is characterised in that：
By polyether polyol that molecular weight is 1500 in 110 DEG C of temperature, vacuum pressure it is 0.1MPa conditions in the first step
Lower dehydration by evaporation 1h；
Polyether polyol and isophorone diisocyanate are slowly added in container in the second step, stirs and is warming up to
The acrylic acid of the dibutyl tin laurate and 0.05% volume of 0.05% volume is added dropwise after 60 DEG C, adjusts temperature and is reacted to 65 DEG C
3h。
3. a kind of preparation method of polyurethane-modified pigment printing binding agent according to claim 1, it is characterised in that：Institute
State the styrene reaction 2h of 2,2- dihydromethyl propionic acids and 0.01% mass that 80 DEG C of 2% mass of addition are warming up in third step.
4. a kind of preparation method of polyurethane-modified pigment printing binding agent according to claim 1 or 2, feature exist
In：The acrylic acid is analytical reagents, acrylic acid active constituent content >=99.5%, ignition residue content≤0.01%, resistance
Poly- agent content≤0.01.
5. a kind of preparation method of polyurethane-modified pigment printing binding agent according to claim 1 or 3, feature exist
In：The styrene be analytical reagents, styrene active constituent content >=99%, polymer content≤0.002%, burning it is residual
Slag content≤0.05%, moisture≤0.1%, ether content≤0.02%.
6. a kind of preparation method of polyurethane-modified pigment printing binding agent according to claim 1, it is characterised in that：Institute
State 2,2- dihydromethyl propionic acids be analytical reagents, 2,2- dihydromethyl propionic acid active constituent content >=99%, moisture≤
0.1%, content of ashes≤0.03%, hydroxy radical content >=24%.
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| CN109610202A (en) * | 2018-10-29 | 2019-04-12 | 薛向东 | A kind of environment-protection coating printing adhesive and preparation method thereof |
| CN112709083A (en) * | 2021-02-08 | 2021-04-27 | 魔力薇薇(上海)服饰科技有限公司 | Modified water-soluble high-elasticity polyurethane printing coating material and preparation method and application thereof |
| CN117188187B (en) * | 2023-09-08 | 2024-03-19 | 广东彩格科技有限公司 | Polyurethane composite printing paint and production process thereof |
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| CN102432767A (en) * | 2011-08-12 | 2012-05-02 | 上海邦中高分子材料有限公司 | Adhesive resin for padding cloth of clothes |
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