CN105418887B - A kind of anionic polyurethane color fixing agent, preparation method and application for acid dyes - Google Patents
A kind of anionic polyurethane color fixing agent, preparation method and application for acid dyes Download PDFInfo
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- CN105418887B CN105418887B CN201510928891.1A CN201510928891A CN105418887B CN 105418887 B CN105418887 B CN 105418887B CN 201510928891 A CN201510928891 A CN 201510928891A CN 105418887 B CN105418887 B CN 105418887B
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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
- C08G18/28—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
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4244—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups
- C08G18/4258—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups derived from polycarboxylic acids containing at least one ether group and polyols
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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
- C08G18/4833—Polyethers containing oxyethylene units
- C08G18/4837—Polyethers containing oxyethylene units and other oxyalkylene units
- C08G18/4845—Polyethers containing oxyethylene units and other oxyalkylene units containing oxypropylene or higher oxyalkylene end groups
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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
- C08G18/50—Polyethers having heteroatoms other than oxygen
- C08G18/5072—Polyethers having heteroatoms other than oxygen containing sulfur
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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
- D06P1/39—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 acid dyes
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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
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/001—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated using acid dyes
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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
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/02—Material containing basic nitrogen
- D06P3/04—Material containing basic nitrogen containing amide groups
- D06P3/06—Material containing basic nitrogen containing amide groups using acid dyes
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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
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/02—Material containing basic nitrogen
- D06P3/04—Material containing basic nitrogen containing amide groups
- D06P3/24—Polyamides; Polyurethanes
- D06P3/241—Polyamides; Polyurethanes using acid dyes
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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
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
- D06P5/04—After-treatment with organic compounds
- D06P5/08—After-treatment with organic compounds macromolecular
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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
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/22—Effecting variation of dye affinity on textile material by chemical means that react with the fibre
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Polyurethanes Or Polyureas (AREA)
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Abstract
The invention discloses a kind of anionic polyurethane color fixing agent, preparation method and applications for acid dyes.Isoflurane chalcone diisocyanate is added in into polyether Glycols and containing being reacted in sulfonic chain extender, it adds hyperbranched hydroxyl telechelic polyester and carries out cross-linking reaction, and remaining isocyanate group is closed with methyl ethyl ketoxime, prepare the anionic polyurethane color fixing agent for acid dyes.Present invention process is simple, and gained color fixing agent is free of formaldehyde, and contaminating acid dyes polyamide fibre or real silk fabric has good colour fixation.
Description
Technical field
The present invention relates to textile auxiliary synthesis technical fields, and in particular to a kind of poly- ammonia of anionic for acid dyes
Ester color fixing agent, preparation method and application.
Background technology
Polyamide fibre has excellent wearability, excellent mechanical strength and unique wearability；Silk has soft, smooth
Feel, there is good moisture absorption, permeability, and with skin-protection and health-care effect；It is widely used in garment material field.Brocade
Synthetic fibre, silk are dyed usually using acid dyes, and dyestuff relies primarily on Van der Waals force and hydrogen bond action fixation on the fabric.By
In acid dyes be anionic dyes, good water solubility, and Van der Waals force and hydrogen bond and insecure, polyamide fibre, silk after dyeing
Fabric color fastness to washing, colour fastness to rubbing, colour fastness to perspiration are poor.Therefore, polyamide fibre, silk also need after acid dyeing
Fixation treatment is carried out to improve fabric items color fastness.
There is Form aldehyde release in traditional dicyandiamide resin and general anionic fixative, be unfavorable for green ring
It protects；And though Cationic fixing agents are there is no Form aldehyde release problem, such color fixing agent has shadow to coloured light, the chlorine resistance of fabric
It rings, and compatibility is also poor.
Invention content
The present invention for existing product insufficient existing for technical aspect, provide it is a kind of without formaldehyde, compatibility is good, forms a film
Property good and film excellent water resistance anionic polyurethane color fixing agent, preparation method and the application for acid dyes.
In order to achieve the above objectives, technical solution provided by the invention is a kind of anionic polyurethane for acid dyes
The preparation method of color fixing agent, includes the following steps：
It will be through the dried polypropylene glycol of vacuum dehydration, sulfonate type chain extender α, ω-polypropylene glycol-diamines-sulphur
Propyl sodium salt and catalyst dibutyltin dilaurylate, which are added to the reaction equipped with blender, thermometer, condensation reflux unit, to be held
In device, stirring is opened, under conditions of temperature is 50~55 DEG C and nitrogen protection, isoflurane chalcone diisocyanate is slowly added dropwise
Into reaction vessel, it is warming up to 80~85 DEG C after being added dropwise, reacts 3~4 hours, when-NCO content no longer reduces, cooling
To 70~75 DEG C, the superbrnaching end-hydroxy polyester Boltorn H20 that addition N-Methyl pyrrolidone dissolves, react 1~2 hour
After be cooled to 55~60 DEG C, with methyl ethyl ketoxime end capping reaction 0.5~1 hour, be cooled to room temperature, add in deionized water and be vigorously stirred
Emulsification 0.5~1 hour obtains the anionic polyurethane color fixing agent that solid content is 40%~50%, structural formula such as I institute of formula
Show：
Wherein, R isR1ForR2ForR3For17 ＞ a ＞, 0,34 ＞ b ＞, 12,7 ＞ c ＞, 4,17 ＞ d ＞ 0；For Boltorn H20；
Wherein, it is polypropylene glycol by reactant, α, ω-polypropylene glycol-diamines-sulfopropyl sodium salt, two isocyanide of isophorone
Acid esters and hyper-branched polyester Boltorn H20 meters, the sulfonic acid type chain extender α, ω-polypropylene glycol-diamines-sulfopropyl sodium salt
Dosage is the 6%~8% of reactant gross mass；The dosage of the catalyst dibutyltin dilaurylate is reactant gross mass
0.05%~0.1%；The isoflurane chalcone diisocyanate:Polypropylene glycol and α, ω-polypropylene glycol-diamines-sulfopropyl sodium salt
The ratio between total amount of substance is 1.4~1.5:1；The dosage of the hyper-branched polyester Boltorn H20 is reactant gross mass
1%~2%.
In one embodiment：The average molecular weight of the polypropylene glycol is one kind in 800,1000,2000.
In one embodiment：Superbrnaching end-hydroxy polyester Boltorn H20, the molecular weight 1747g/mol, it is theoretical
Hydroxyl value is 16, and structural formula is as shown in formula II：
Technical solution provided by the invention further includes：
According to the preparation-obtained anionic polyurethane color fixing agent for acid dyes of above-mentioned preparation method in acid
Application in property dyes polyamide fibre or real silk fabric fixing finish.
Technical solution provided by the invention further includes：
A kind of anionic polyurethane color fixing agent for acid dyes, it is characterised in that：The poly- ammonia of the anionic
Ester color fixing agent structure is as shown in formula I：
Wherein, R isR1ForR2ForR3For17 ＞ a ＞, 0,34 ＞ b ＞, 12,7 ＞ c ＞, 4,17 ＞ d ＞ 0；For Boltorn H20, concrete structure formula is as shown in formula II：
Raw material according to the present invention and equipment, unless otherwise stated, can be from buying on the market；It is according to the present invention
Method is this field routine techniques unless otherwise stated.
The principle of the present invention is：With α, ω-polypropylene glycol-diamines-sulfopropyl sodium salt makees hydrophilic chain extender, the sulfonic acid of side chain
Base can provide color fixing agent excellent water dispersible, and have stronger repulsion to acid dyes；Using superbrnaching end-hydroxy polyester as
Crosslinking agent can effectively improve the film forming of color fixing agent and the water resistance of film；In the case where high temperature bakes, the isocyanate group of deblocking and work
Property group reaction, increase the film forming of color fixing agent；There is a large amount of carbamate groups in fixation agent molecule, easily with brocade
Amide groups on synthetic fibre, cocoon fiber forms hydrogen bond, and fixation agent molecule has stronger affinity to polyamide fibre, cocoon fiber.Poly- ammonia
Ester fixing agent wraps form one layer of film with good water resistance in fiber surface, reduce connecing for dyestuff and water on fiber
It touches；Meanwhile negatively charged film has repulsion to the acid dyes on fiber, makes dyestuff that can not be precipitated, so as to improve color fastness.
Due to the utilization of above technical scheme, the invention has the advantages that：
1. a kind of anionic polyurethane color fixing agent for acid dyes prepared by the present invention is free of formaldehyde.
2. the present invention is with α, ω-polypropylene glycol-diamines-sulfopropyl sodium salt makees hydrophilic chain extender, and the sulfonic group of side chain can carry
There is stronger repulsion for the water dispersible that color fixing agent is excellent, and to acid dyes；Using superbrnaching end-hydroxy polyester as crosslinking agent,
The film forming of color fixing agent and the water resistance of film can be effectively improved；In the case where high temperature bakes, the isocyanate group and active group of deblocking
Reaction increases the film forming of color fixing agent；There is a large amount of carbamate groups in fixation agent molecule, easily with polyamide fibre, silk
Amide groups on fiber forms hydrogen bond, and fixation agent molecule has stronger affinity to fiber.The poly- ammonia of prepared anionic
Ester color fixing agent compatibility is good, good film-forming property, excellent water resistance, has good fixation to acid dyes dye polyamide fibre, real silk fabric
Effect.
3. present invention process is simple, it is suitble to industrialized production.
Description of the drawings
Fig. 1 is the infrared spectrum of cloudy subtype polyurethane color fixing agent synthesized in embodiment 1；
Fig. 2 is the infrared spectrum of cloudy subtype polyurethane color fixing agent synthesized in embodiment 2；
Fig. 3 is the infrared spectrum of cloudy subtype polyurethane color fixing agent synthesized in embodiment 3.
Specific embodiment
Technical solution of the present invention is further elaborated with reference to the accompanying drawings and examples.
Embodiment 1
It will be through the dried 80g polypropylene glycols 800 of vacuum dehydration, 8.2g sulfonate type chain extenders α, ω-poly- the third two
Alcohol-diamines-sulfopropyl sodium salt and 0.12g catalyst dibutyltin dilaurylates are added to equipped with blender, thermometer, are condensed back to
The reaction vessel of device is flowed, stirring is opened, is heated to 55 DEG C under nitrogen protection, 35.8g isoflurane chalcone diisocyanates are delayed
Slowly it is added dropwise in reaction vessel, is warming up to 85 DEG C after being added dropwise, react 3 hours, when-NCO content no longer reduces, be cooled to
75 DEG C, the 2.5g hyper-branched polyester Boltorn H20 dissolved with 15gN- methyl pyrrolidones are added in, reaction is cooled to after 1 hour
60 DEG C, in survey system-NCO content, with 5.08g methyl ethyl ketoximes end capping reaction 0.5 hour, be cooled to room temperature, add in 165g go from
Sub- water is vigorously stirred emulsification 0.5 hour, obtains the anionic polyurethane color fixing agent that solid content is about 48%.
Referring to attached drawing 1, it is the infrared spectrum of target product in the present embodiment.3352cm in figure-1Locate as N-H stretching vibrations
Peak, 2971cm-1And 2871cm-1Locate as-CH3With-CH2Stretching vibration peak, 1732cm-1Place can be classified as carbamate, substitution
Urea groups and C=O base stretching vibration peaks in ester group, 1651cm-1Locate as C=N stretching vibrations, 1541cm-1Place can be classified as carbamic acid
N-H deformation vibrations and C-N stretching vibration peaks, 1232cm in ester and substituted urea-1Locate to shake for the asymmetric stretch of carbamate groups
Dynamic peak, 1107cm-1Place has a wider absorption peak that can be classified as-SO3The overlap peak of Na and C-O-C, in 2270cm-1Neighbouring-NCO
Characteristic peak disappears.Show to have synthesized anionic polyurethane color fixing agent.
Among the present embodiment, the assay method of-NCO content is as follows：
Using di-n-butylamine method, with the di-n-butylamine of hydrochloric acid standard solution overtitration, make indicator, color with bromophenol blue
Yellow is become from blue and reaches titration end-point.Calculating formula is：
Wherein：The percentage composition of W-isocyanate groups, %；
V1The volume of the Hydrochloric Standard Titration of-blank test consumption, mL；
V2The volume of the Hydrochloric Standard Titration of-titration sample consumption, mL；
The concentration of c-Hydrochloric Standard Titration, mol/L；
M-sample mass, g.
In remaining embodiment of the present invention-the same the method for NCO content measure.
Embodiment 2
It will be through the dried 100g polypropylene glycols 1000 of vacuum dehydration, 11g α, ω-polypropylene glycol-diamines-sulfopropyl
Sodium salt and 0.12g catalyst dibutyltin dilaurylates, which are added to the reaction equipped with blender, thermometer, condensation reflux unit, to be held
Device opens stirring, is heated to 50 DEG C under nitrogen protection, 40g isoflurane chalcone diisocyanates are slowly added dropwise to reaction vessel
In, it is warming up to 85 DEG C after being added dropwise, reacts 2.5 hours, when-NCO content no longer reduces, be cooled to 70 DEG C, add in and use
The 2.3g hyper-branched polyester BoltornH20 of 20gN- methyl pyrrolidones dissolving, reaction are cooled to 58 DEG C after 2 hours, survey system
In-NCO content, with 6.7g methyl ethyl ketoximes end capping reaction 1 hour, room temperature is cooled to, 195g deionized waters is added in and is vigorously stirred breast
Change 1 hour, obtain the anionic polyurethane color fixing agent that solid content is about 45%.
Referring to attached drawing 2, it is the infrared spectrum of target product in the present embodiment.3354cm in figure-1Locate to stretch for N-H and shake
Dynamic peak, 2973cm-1And 2878cm-1Locate as-CH3With-CH2Stretching vibration peak, 1734cm-1Place can be classified as carbamate, take
For C=O base stretching vibration peaks in urea groups and ester group, 1655cm-1Locate as C=N stretching vibrations, 1539cm-1Place can be classified as amino first
N-H deformation vibrations and C-N stretching vibration peaks, 1236cm in acid esters and substituted urea-1Locate the asymmetric stretch for carbamate groups
Vibration peak, 1109cm-1Place has a wider absorption peak that can be classified as-SO3The overlap peak of Na and C-O-C, in 2270cm-1Neighbouring-
NCO characteristic peaks disappear.Show to have synthesized anionic polyurethane color fixing agent.
Embodiment 3
It will be through the dried 200g polypropylene glycols 1000 of vacuum dehydration, 16.5g α, ω-polypropylene glycol-diamines-sulphur third
Base sodium salt and 1.26g catalyst dibutyltin dilaurylates are added to the reaction equipped with blender, thermometer, condensation reflux unit
Container opens stirring, is heated to 50 DEG C under nitrogen protection, 40.4g isoflurane chalcone diisocyanates are slowly added dropwise to reaction
In container, it is warming up to 80 DEG C after being added dropwise, reacts 2 hours, when-NCO content no longer reduces, be cooled to 70 DEG C, add in and use
The 2.6g hyper-branched polyester H20 of 39gN- methyl pyrrolidones dissolving, reaction are cooled to 55 DEG C after 1 hour, and-NCO contains in survey system
Amount with 5.9g methyl ethyl ketoximes end capping reaction 0.5 hour, is cooled to room temperature, and adding in 310g deionized waters, to be vigorously stirred emulsification 1 small
When, obtain the anionic polyurethane color fixing agent that solid content is about 46%.
Referring to attached drawing 3, it is the infrared spectrum of target product in the present embodiment.3352cm in figure-1Locate to stretch for N-H and shake
Dynamic peak, 2968cm-1And 2869cm-1Locate as-CH3With-CH2Stretching vibration peak, 1732cm-1Place can be classified as carbamate, take
For C=O base stretching vibration peaks in urea groups and ester group, 1652cm-1Locate as C=N stretching vibrations, 1527cm-1Place can be classified as amino first
N-H deformation vibrations and C-N stretching vibration peaks, 1235cm in acid esters and substituted urea-1Locate the asymmetric stretch for carbamate groups
Vibration peak, 1112cm-1Place has a wider absorption peak that can be classified as-SO3The overlap peak of Na and C-O-C, in 2270cm-1Neighbouring-
NCO characteristic peaks disappear.Show to have synthesized anionic polyurethane color fixing agent.
Experimental example
A kind of anionic polyurethane color fixing agent for acid dyes prepared by Examples 1 to 3, by following finisher
Skill carries out acid dyeing polyamide fibre, real silk fabric fixing finish, and to the soaping fastness of fabric, friction jail after fixing finish
Degree, perspiration fastness are tested, and test result is as shown in table 1,2.
Fixing finish technique：
A concentration of 30g/L of fixing finish liquid (color fixing agent solid content is in terms of 45%), bath raio 30:1.
Dyeing nylon fabric pads that (80%) immersing and rolling, pick-up rate, which are about, → drying (100 DEG C, 3min) → bakes (170
DEG C 2min) → washing → dry
(80%) immersing and rolling, pick-up rate are about → drying (90 DEG C, 3min) → bakes (150 to dyeing of real silk textile pad
DEG C 2min) → washing → dry
Color fastness is tested：
By GB/T3921-2008《Textile color stability is tested：Soaping fastness》Method test fixing finish nylon fabric
Soaping fastness；
By GB/T3921-2008《Textile color stability is tested：Crock fastness》Method test fixing finish nylon fabric
Crock fastness；
By GB/T 3922-1995《Textile colour fastness to perspiration test method》Test the resistance to of fixing finish nylon fabric
PERSPIRATION COLOR FASTNESS；
By GB/T 250-2008《Textile color stability test evaluation discoloration gray scale》Rating.
The colour fixation of the nylon fabric after the arrangement of anionic polyurethane color fixing agent of table 1
The colour fixation of the real silk fabric after the arrangement of anionic polyurethane color fixing agent of table 2
The above, only present pre-ferred embodiments, therefore the range implemented of the present invention cannot be limited according to this, i.e., according to
The equivalent changes and modifications that the scope of the claims of the present invention and description are made all should still belong in the range of the present invention covers.
Claims (4)
1. a kind of preparation method of anionic polyurethane color fixing agent for acid dyes, it is characterised in that：Including walking as follows
Suddenly：
It will be through the dried polypropylene glycol of vacuum dehydration, sulfonate type chain extender α, ω-polypropylene glycol-diamines-sulfopropyl
Sodium salt and catalyst dibutyltin dilaurylate be added to equipped with blender, thermometer, condensation reflux unit reaction vessel in,
Stirring is opened, under conditions of temperature is 50~55 DEG C and nitrogen protection, isophorone diisocyanate is slowly added dropwise to anti-
It answers in container, is warming up to 80~85 DEG C after being added dropwise, react 3~4 hours, when-NCO content no longer reduces, be cooled to 70
~75 DEG C, the superbrnaching end-hydroxy polyester Boltorn H20 that addition N-Methyl pyrrolidone dissolves, reaction is dropped after 1~2 hour
Temperature, with methyl ethyl ketoxime end capping reaction 0.5~1 hour, is cooled to room temperature to 55~60 DEG C, adds in deionized water and is vigorously stirred emulsification
0.5~1 hour, the anionic polyurethane color fixing agent that solid content is 40%~50% is obtained, structural formula is as shown in formula I：
Formula I
Wherein, R is, R1For, R2For, R3For
Or；17 ＞ a ＞, 0,34 ＞ b ＞, 12,7 ＞ c ＞, 4,17 ＞ d ＞ 0；For Boltorn
H20；
Wherein, it is polypropylene glycol by reactant, α, ω-polypropylene glycol-diamines-sulfopropyl sodium salt, isophorone diisocyanate
It is counted with hyper-branched polyester Boltorn H20, the sulfonate type chain extender α, the use of ω-polypropylene glycol-diamines-sulfopropyl sodium salt
Measure 6%~8% for reactant gross mass；The dosage of the catalyst dibutyltin dilaurylate is reactant gross mass
0.05%~0.1%；The isophorone diisocyanate:Polypropylene glycol and α, ω-polypropylene glycol-diamines-sulfopropyl sodium salt are total
The ratio between the amount of substance be 1.4~1.5:1；The dosage of the hyper-branched polyester Boltorn H20 is the 1% of reactant gross mass
~2%.
2. a kind of preparation method of anionic polyurethane color fixing agent for acid dyes according to claim 1,
It is characterized in that：The superbrnaching end-hydroxy polyester Boltorn H20, molecular weight 1704g/mol, theoretical hydroxyl value are 16
A, structural formula is as shown in formula II：
Formula II.
3. the preparation-obtained anionic polyurethane for acid dyes of preparation method according to claim 1 or 2
Application of the color fixing agent in acid dyes contaminates polyamide fibre or real silk fabric fixing finish.
4. a kind of anionic polyurethane color fixing agent for acid dyes, it is characterised in that：The anionic polyurethane
Color fixing agent structure is as shown in formula I：
Formula I
Wherein, R is, R1For, R2For, R3ForOr；17 ＞ a ＞, 0,34 ＞ b ＞, 12,7 ＞ c ＞, 4,17 ＞ d ＞ 0；For Boltorn
H20, concrete structure formula is as shown in formula II：
Formula II.
Priority Applications (1)
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| CN106087485A (en) * | 2016-06-25 | 2016-11-09 | 仇颖超 | A kind of method that aqueous polyurethane grafted collagen peptide prepares color fixing agent |
| CN111826979A (en) * | 2020-08-04 | 2020-10-27 | 广东湛丰精细化工有限公司 | Environment-friendly acidic color fixing agent capable of being subjected to dyeing and fixing one-bath treatment, and preparation method and application thereof |
| CN113121790B (en) * | 2021-04-27 | 2022-04-15 | 苏州大学 | Wet rubbing fastness improver for acid dye and preparation method thereof |
| CN113512168B (en) * | 2021-04-30 | 2022-08-23 | 浙江理工大学桐乡研究院有限公司 | Dyeing-promoting anti-sticking agent for acid dye dyeing of polyamide-ammonia fabric and synthetic method thereof |
| CN115124690B (en) * | 2022-07-04 | 2024-01-26 | 上海应用技术大学 | Hyperbranched cationic waterborne polyurethane color fixing agent and preparation method thereof |
| CN116289259A (en) * | 2023-04-13 | 2023-06-23 | 达利(中国)有限公司 | Method for improving dyeing leveling property of PA 56/real silk mixed fabric |
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