CN108486925A - A kind of preparation method of synthetic leather dyeing dye dispersant - Google Patents
A kind of preparation method of synthetic leather dyeing dye dispersant Download PDFInfo
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- CN108486925A CN108486925A CN201810423547.0A CN201810423547A CN108486925A CN 108486925 A CN108486925 A CN 108486925A CN 201810423547 A CN201810423547 A CN 201810423547A CN 108486925 A CN108486925 A CN 108486925A
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- Prior art keywords
- cyclodextrin
- beta
- preparation
- microwave
- ultrasonic
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- 239000002270 dispersing agent Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000004043 dyeing Methods 0.000 title claims abstract description 19
- 239000002649 leather substitute Substances 0.000 title claims abstract description 18
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 56
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims abstract description 49
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims abstract description 49
- 239000001116 FEMA 4028 Substances 0.000 claims abstract description 41
- 229960004853 betadex Drugs 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 230000004048 modification Effects 0.000 claims abstract description 14
- 238000012986 modification Methods 0.000 claims abstract description 14
- 239000000049 pigment Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims description 28
- 239000002245 particle Substances 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 20
- 238000010992 reflux Methods 0.000 claims description 20
- 238000000605 extraction Methods 0.000 claims description 18
- 239000006210 lotion Substances 0.000 claims description 18
- 239000003595 mist Substances 0.000 claims description 18
- 230000002195 synergetic effect Effects 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 17
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical class O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 229920000805 Polyaspartic acid Polymers 0.000 claims description 12
- 229910052782 aluminium Inorganic materials 0.000 claims description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 12
- 239000004411 aluminium Substances 0.000 claims description 12
- 239000007921 spray Substances 0.000 claims description 12
- 239000000839 emulsion Substances 0.000 claims description 11
- 229920001296 polysiloxane Polymers 0.000 claims description 11
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000000084 colloidal system Substances 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 7
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 229960000541 cetyl alcohol Drugs 0.000 claims description 5
- 108010064470 polyaspartate Proteins 0.000 claims description 5
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
- 235000019394 potassium persulphate Nutrition 0.000 claims description 5
- ODHCTXKNWHHXJC-VKHMYHEASA-N 5-oxo-L-proline Chemical compound OC(=O)[C@@H]1CCC(=O)N1 ODHCTXKNWHHXJC-VKHMYHEASA-N 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 238000007385 chemical modification Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 229940084106 spermaceti Drugs 0.000 claims description 3
- 239000012177 spermaceti Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 2
- 239000000975 dye Substances 0.000 abstract description 40
- 238000003860 storage Methods 0.000 abstract description 5
- 238000004040 coloring Methods 0.000 abstract description 4
- 239000008187 granular material Substances 0.000 abstract description 3
- 238000004062 sedimentation Methods 0.000 abstract description 3
- 229940097362 cyclodextrins Drugs 0.000 description 7
- 125000005395 methacrylic acid group Chemical class 0.000 description 7
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 229910052700 potassium Inorganic materials 0.000 description 6
- 239000011591 potassium Substances 0.000 description 6
- 239000010985 leather Substances 0.000 description 5
- 239000004925 Acrylic resin Substances 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- WCOATMADISNSBV-UHFFFAOYSA-K diacetyloxyalumanyl acetate Chemical compound [Al+3].CC([O-])=O.CC([O-])=O.CC([O-])=O WCOATMADISNSBV-UHFFFAOYSA-K 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000191 poly(N-vinyl pyrrolidone) Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000012905 visible particle Substances 0.000 description 1
Classifications
-
- 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
- D06P1/46—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 natural macromolecular substances or derivatives thereof
- D06P1/48—Derivatives of carbohydrates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0009—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Glucans, e.g. polydextrose, alternan, glycogen; (alpha-1,4)(alpha-1,6)-D-Glucans; (alpha-1,3)(alpha-1,4)-D-Glucans, e.g. isolichenan or nigeran; (alpha-1,4)-D-Glucans; (alpha-1,3)-D-Glucans, e.g. pseudonigeran; Derivatives thereof
- C08B37/0012—Cyclodextrin [CD], e.g. cycle with 6 units (alpha), with 7 units (beta) and with 8 units (gamma), large-ring cyclodextrin or cycloamylose with 9 units or more; Derivatives thereof
-
- 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
- D06P1/5278—Polyamides; Polyimides; Polylactames; Polyalkyleneimines
-
- 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
- D06P1/5292—Macromolecular compounds obtained otherwise than by reactions involving only unsaturated carbon-to-carbon bonds containing Si-atoms
-
- 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
- D06P1/673—Inorganic compounds
- D06P1/67333—Salts or hydroxides
- D06P1/6735—Salts or hydroxides of alkaline or alkaline-earth metals with anions different from those provided for in D06P1/67341
- D06P1/67358—Halides or oxyhalides
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Colloid Chemistry (AREA)
- Coloring (AREA)
Abstract
The invention discloses a kind of preparation methods of synthetic leather dyeing dye dispersant, are related to dyeing assistant technical field, include the following steps：(1) the ultrasonic microwave collaboration processing of beta cyclodextrin, the modification of (2) beta cyclodextrin, the preparation of (3) pigment dispersing agent.The made dispersant of the present invention can promote dyestuff evenly dispersed in water soluble dyestuffs, improve suspensibility, enhance low tempertaure storage stability and high-temperature storage stability, prevent water soluble dyestuffs from occurring the phenomenon that dyestuff sedimentation and dye granule increase during storage, to ensure uniform coloring when water soluble dyestuffs application.
Description
Technical field：
The present invention relates to dyeing assistant technical fields, and in particular to a kind of preparation side of synthetic leather dyeing dye dispersant
Method.
Background technology：
Synthetic leather is the plastic products simulated the Nomenclature Composition and Structure of Complexes of natural leather and can be used as its substitute material.Usually with warp
The non-woven fabrics of dipping is lamina reticularis, and microporous polyurethane layer is made as grain layer.Its positive and negative is all quite similar with leather, and
With certain gas permeability, than common artificial leather closer to natural leather.It is widely used in and makes shoes, boots, luggage and ball etc..
In order to assign synthesis leather goods abundant color effect, need to dye synthetic leather using dye liquor.And dye liquor
Important composition ingredient be dyestuff.But dyestuff has that dyestuff sedimentation and dye granule increase after being configured to dye liquor, shadow
Store quality is rung, and then influences coloring when dye liquor is applied to synthetic leather dyeing, especially reduces dye uniformity.In order to
Solve the problems, such as this, it usually needs addition dye dispersant is to promote evenly dispersed in dye liquor of dyestuff and ensure stably dispersing
Property.
Invention content：
Technical problem to be solved by the present invention lies in provide conjunction a kind of easy to operate and that dyeing quality can be effectively ensured
The preparation method of finished leather dyeing dye dispersant.
The technical problems to be solved by the invention are realized using technical solution below：
A kind of preparation method of synthetic leather dyeing dye dispersant, includes the following steps：
(1) the ultrasonic-microwave collaboration processing of beta-cyclodextrin：Beta-cyclodextrin is added to the water, being uniformly dispersed, it is super to be placed on
In sound wave-microwave synergistic extraction instrument, and supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz, microwave work(are set
Rate 700W, return stirring close Ultrasonic-microwave synergistic extraction instrument after handling 5-10min, and interval 15-30min continues reflux and stirs
Processing 5-10min is mixed, lotion is made through being concentrated under reduced pressure in gained mixture, and lotion is sent into freeze-drying after cooled to room temperature
In machine, particle is made through pulverizer in dry obtained solid；
(2) modification of beta-cyclodextrin：It cooperateing with treated through ultrasonic-microwave, beta-cyclodextrin adds water stirring to be made admittedly to contain
The colloid for measuring 30-40%, the mixing added dissolved with N,N-DMAA, methacrylic acid and potassium peroxydisulfate are water-soluble
Liquid is then heated to reflux state insulated and stirred, gained mixture is sent into spray dryer after polymerisation, dry
Micro mist is made to get modified cyclodextrin through micronizer in gained particle；
(3) preparation of pigment dispersing agent：Silicone emulsion is first added into made modified cyclodextrin, and is heated to 70-80 DEG C
Insulated and stirred 5-10min adds white aluminium polychloride and poly-aspartic-acid, continues to be heated to 100-110 DEG C of heat preservation to stir
5-10min is mixed to get dye dispersant.
The mass ratio of beta-cyclodextrin and water is 1 in the step (1):5-10.
Beta-cyclodextrin, N in the step (2), N- dimethacrylamide, methacrylic acid and potassium peroxydisulfate mass ratio
It is 50:10:5-10:0.1-0.5.
The mass ratio of modified cyclodextrin, silicone emulsion, white aluminium polychloride, poly-aspartic-acid in the step (3)
It is 50:1-10:1-10:0.5-5.
The cetanol passes through chemical modification, and modification procedure is：It is after cetanol and L-Glutimic acid are mixed plus anhydrous
Ethyl alcohol dissolves, then the concentrated sulfuric acid is added dropwise and adjusts solution ph to 4-5, and is heated to reflux state insulated and stirred, stops after reaction
It only heating, ethyl alcohol is recycled through being concentrated under reduced pressure, condensate residue is dissolved in water completely, and gained mixed liquor is sent into spray dryer,
Micro mist is made to get modified cetanol through micronizer in dry gained particle.
The cetanol, L-Glutimic acid mass ratio be 10:5-10.
The beneficial effects of the invention are as follows：
(1) present invention is handled by ultrasonic-microwave collaboration to destroy the crystalline texture of beta-cyclodextrin, and it is hydrophilic to improve its
Property, to solve the technical issues of beta-cyclodextrin easily crystallizes to be insoluble in water in water；
(2) present invention further increases the water solubility of beta-cyclodextrin by the modification, keeps made modified cyclodextrin easy
Water is dissolved in prepare major ingredient as dispersant；The modification utilizes N, N- dimethacrylamide aggregated anti-with methacrylic acid
Water soluble acrylic resin should be generated, and the acrylic resin generated forms modified ring through esterification with beta-cyclodextrin and pastes
Essence, so as to improve the water solubility of beta-cyclodextrin；
(3) present invention keeps made modified cetanol soluble easily in water by the chemical modification to cetanol, while utilizing spermaceti
The emulsifiability that alcohol itself has further promotes made dispersant in water evenly dispersed；
(4) the made dispersant of the present invention can promote dyestuff evenly dispersed in water soluble dyestuffs, improve suspensibility, and enhancing is low
Warm bin stability and high-temperature storage stability prevent water soluble dyestuffs from occurring dyestuff sedimentation and dye granule increase during storage
The phenomenon that, to ensure uniform coloring when water soluble dyestuffs application.
Specific implementation mode：
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention be easy to understand, tie below
Specific embodiment is closed, the present invention is further explained.
Embodiment 1
(1) the ultrasonic-microwave collaboration processing of beta-cyclodextrin：50g beta-cyclodextrins are added in 300g water, after being uniformly dispersed
Be placed in Ultrasonic-microwave synergistic extraction instrument, and be arranged supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz,
Microwave power 700W, return stirring close Ultrasonic-microwave synergistic extraction instrument after handling 10min, and interval 15min continues reflux and stirs
Processing 10min is mixed, lotion is made through being concentrated under reduced pressure in gained mixture, and lotion is sent into freeze drier after cooled to room temperature
In, particle is made through pulverizer in dry obtained solid；
(2) modification of beta-cyclodextrin：By 50g, through ultrasonic-microwave collaboration, treated that beta-cyclodextrin adds that water stirring is made
The colloid of solid content 30-40% is added dissolved with 10g N,N-DMAAs, 10g methacrylic acids and 0.5g over cures
The mixed aqueous solution of sour potassium is then heated to reflux state insulated and stirred, is sent into gained mixture after polymerisation and sprays
In mist drying machine, micro mist is made to get modified cyclodextrin through micronizer in dry gained particle；
(3) preparation of pigment dispersing agent：2.5g silicone emulsions are first added into made 50g modified cyclodextrins, and are heated to
70-80 DEG C of insulated and stirred 10min, adds 2.5g whites aluminium polychloride and 0.5g poly-aspartic-acids, continues to be heated to
100-110 DEG C of insulated and stirred 10min is to get dye dispersant.
Embodiment 2
(1) the ultrasonic-microwave collaboration processing of beta-cyclodextrin：50g beta-cyclodextrins are added in 300g water, after being uniformly dispersed
Be placed in Ultrasonic-microwave synergistic extraction instrument, and be arranged supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz,
Microwave power 700W, return stirring close Ultrasonic-microwave synergistic extraction instrument after handling 10min, and interval 15min continues reflux and stirs
Processing 10min is mixed, lotion is made through being concentrated under reduced pressure in gained mixture, and lotion is sent into freeze drier after cooled to room temperature
In, particle is made through pulverizer in dry obtained solid；
(2) modification of beta-cyclodextrin：By 50g, through ultrasonic-microwave collaboration, treated that beta-cyclodextrin adds that water stirring is made
The colloid of solid content 30-40% is added dissolved with 10g N,N-DMAAs, 10g methacrylic acids and 0.5g over cures
The mixed aqueous solution of sour potassium is then heated to reflux state insulated and stirred, is sent into gained mixture after polymerisation and sprays
In mist drying machine, micro mist is made to get modified cyclodextrin through micronizer in dry gained particle；
(3) preparation of pigment dispersing agent：3g silicone emulsions are first added into made 50g modified cyclodextrins, and are heated to 70-
80 DEG C of insulated and stirred 10min, add 2g whites aluminium polychloride and 0.5g poly-aspartic-acids, continue to be heated to 100-110
DEG C insulated and stirred 10min is to get dye dispersant.
Embodiment 3
(1) the ultrasonic-microwave collaboration processing of beta-cyclodextrin：50g beta-cyclodextrins are added in 300g water, after being uniformly dispersed
Be placed in Ultrasonic-microwave synergistic extraction instrument, and be arranged supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz,
Microwave power 700W, return stirring close Ultrasonic-microwave synergistic extraction instrument after handling 10min, and interval 15min continues reflux and stirs
Processing 10min is mixed, lotion is made through being concentrated under reduced pressure in gained mixture, and lotion is sent into freeze drier after cooled to room temperature
In, particle is made through pulverizer in dry obtained solid；
(2) modification of beta-cyclodextrin：By 50g, through ultrasonic-microwave collaboration, treated that beta-cyclodextrin adds that water stirring is made
The colloid of solid content 30-40% is added dissolved with 10g N,N-DMAAs, 10g methacrylic acids and 0.5g over cures
The mixed aqueous solution of sour potassium is then heated to reflux state insulated and stirred, is sent into gained mixture after polymerisation and sprays
In mist drying machine, micro mist is made to get modified cyclodextrin through micronizer in dry gained particle；
(3) preparation of pigment dispersing agent：3g silicone emulsions are first added into made 50g modified cyclodextrins, and are heated to 70-
80 DEG C of insulated and stirred 10min, add 2g whites aluminium polychloride and 0.5g poly-aspartic-acids, continue to be heated to 100-110
DEG C insulated and stirred 10min is to get dye dispersant.
The preparation of modified cetanol：After 10g cetanols and 10g L-Glutimic acids are mixed plus absolute ethyl alcohol dissolves, then drips
Enriching sulfuric acid regulation solution pH value is heated to reflux state insulated and stirred to 4-5, stops heating after reaction, through decompression
Concentration and recovery ethyl alcohol, condensate residue are dissolved in water completely, and gained mixed liquor is sent into spray dryer, dry gained particle warp
Micro mist is made to get modified cetanol in micronizer.
Reference examples 1
(1) the ultrasonic-microwave collaboration processing of beta-cyclodextrin：50g beta-cyclodextrins are added in 300g water, after being uniformly dispersed
Be placed in Ultrasonic-microwave synergistic extraction instrument, and be arranged supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz,
Microwave power 700W, return stirring close Ultrasonic-microwave synergistic extraction instrument after handling 10min, and interval 15min continues reflux and stirs
Processing 10min is mixed, lotion is made through being concentrated under reduced pressure in gained mixture, and lotion is sent into freeze drier after cooled to room temperature
In, particle is made through pulverizer in dry obtained solid；
(2) modification of beta-cyclodextrin：By 50g, through ultrasonic-microwave collaboration, treated that beta-cyclodextrin adds that water stirring is made
The colloid of solid content 30-40% is added dissolved with 10g N,N-DMAAs, 10g methacrylic acids and 0.5g over cures
The mixed aqueous solution of sour potassium is then heated to reflux state insulated and stirred, is sent into gained mixture after polymerisation and sprays
In mist drying machine, micro mist is made to get modified cyclodextrin through micronizer in dry gained particle；
(3) preparation of pigment dispersing agent：3g silicone emulsions are first added into made 50g modified cyclodextrins, and are heated to 70-
80 DEG C of insulated and stirred 10min add 2g white aluminium polychlorides, continue to be heated to 100-110 DEG C of insulated and stirred 10min, i.e.,
Obtain dye dispersant.
Reference examples 2
(1) the ultrasonic-microwave collaboration processing of beta-cyclodextrin：50g beta-cyclodextrins are added in 300g water, after being uniformly dispersed
Be placed in Ultrasonic-microwave synergistic extraction instrument, and be arranged supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz,
Microwave power 700W, return stirring close Ultrasonic-microwave synergistic extraction instrument after handling 10min, and interval 15min continues reflux and stirs
Processing 10min is mixed, lotion is made through being concentrated under reduced pressure in gained mixture, and lotion is sent into freeze drier after cooled to room temperature
In, particle is made through pulverizer in dry obtained solid；
(2) modification of beta-cyclodextrin：By 50g, through ultrasonic-microwave collaboration, treated that beta-cyclodextrin adds that water stirring is made
The colloid of solid content 30-40% is added dissolved with 10g N,N-DMAAs, 10g methacrylic acids and 0.5g over cures
The mixed aqueous solution of sour potassium is then heated to reflux state insulated and stirred, is sent into gained mixture after polymerisation and sprays
In mist drying machine, micro mist is made to get modified cyclodextrin through micronizer in dry gained particle；
(3) preparation of pigment dispersing agent：3g silicone emulsions are first added into made 50g modified cyclodextrins, and are heated to 70-
80 DEG C of insulated and stirred 10min, add 0.5g poly-aspartic-acids, continue to be heated to 100-110 DEG C of insulated and stirred 10min, i.e.,
Obtain dye dispersant.
Reference examples 3
(1) the ultrasonic-microwave collaboration processing of beta-cyclodextrin：50g beta-cyclodextrins are added in 300g water, after being uniformly dispersed
Be placed in Ultrasonic-microwave synergistic extraction instrument, and be arranged supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz,
Microwave power 700W, return stirring close Ultrasonic-microwave synergistic extraction instrument after handling 10min, and interval 15min continues reflux and stirs
Processing 10min is mixed, lotion is made through being concentrated under reduced pressure in gained mixture, and lotion is sent into freeze drier after cooled to room temperature
In, particle is made through pulverizer in dry obtained solid；
(2) modification of beta-cyclodextrin：By 50g, through ultrasonic-microwave collaboration, treated that beta-cyclodextrin adds that water stirring is made
The colloid of solid content 30-40% is added dissolved with 10g N,N-DMAAs, 10g methacrylic acids and 0.5g over cures
The mixed aqueous solution of sour potassium is then heated to reflux state insulated and stirred, is sent into gained mixture after polymerisation and sprays
In mist drying machine, micro mist is made to get modified cyclodextrin through micronizer in dry gained particle；
(3) preparation of pigment dispersing agent：Made 50g modified cyclodextrins are heated to 70-80 DEG C of insulated and stirred 10min, then
2g whites aluminium polychloride and 0.5g poly-aspartic-acids is added, continue to be heated to 100-110 DEG C of insulated and stirred 10min to get
Dye dispersant.
Reference examples 4
(1) modification of beta-cyclodextrin：Add water stirring that the colloid of solid content 30-40% is made 50g beta-cyclodextrins, adds
Dissolved with 10g N,N-DMAAs, the mixed aqueous solution of 10g methacrylic acids and 0.5g potassium peroxydisulfates, it is then heated to
Gained mixture is sent into spray dryer after polymerisation by reflux state insulated and stirred, and dry gained particle is through super
Micro mist is made to get modified cyclodextrin in atomizer；
(2) preparation of pigment dispersing agent：3g silicone emulsions are first added into made 50g modified cyclodextrins, and are heated to 70-
80 DEG C of insulated and stirred 10min, add 2g whites aluminium polychloride and 0.5g poly-aspartic-acids, continue to be heated to 100-110
DEG C insulated and stirred 10min is to get dye dispersant.
Reference examples 5
(1) the ultrasonic-microwave collaboration processing of beta-cyclodextrin：50g beta-cyclodextrins are added in 300g water, after being uniformly dispersed
Be placed in Ultrasonic-microwave synergistic extraction instrument, and be arranged supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz,
Microwave power 700W, return stirring close Ultrasonic-microwave synergistic extraction instrument after handling 10min, and interval 15min continues reflux and stirs
Processing 10min is mixed, lotion is made through being concentrated under reduced pressure in gained mixture, and lotion is sent into freeze drier after cooled to room temperature
In, particle is made through pulverizer in dry obtained solid；
(2) preparation of pigment dispersing agent：It is first cooperateed with during treated through ultrasonic-microwave to made 50g and 3g emulsifications is added
Silicone oil, and it is heated to 70-80 DEG C of insulated and stirred 10min, 2g whites aluminium polychloride and 0.5g poly-aspartic-acids are added, after
It is continuous to be heated to 100-110 DEG C of insulated and stirred 10min to get dye dispersant.
Embodiment 4
Based on embodiment 2, setting does not add the reference examples 1 of poly-aspartic-acid, does not add white aluminium polychloride
Reference examples 2, do not add silicone emulsion reference examples 3, to beta-cyclodextrin carry out ultrasonic-microwave collaboration processing reference examples
4, the reference examples 5 of processing are not modified to beta-cyclodextrin.
Be utilized respectively embodiment 1-3, reference examples 1-5 prepares dye dispersant, and be added to synthesis by percentage shown in table 1
It removes from office in dye liquor.Made synthetic leather dye liquor is used to, with the dyeing of batch equivalent synthetic leather, measure dye liquor by identical dyeing
Coloring after storing situation and storing 6 months, as shown in table 2.
The preparation of 1 synthetic leather dye liquor of table
| Raw material | Mass percent/% |
| 1:The 2 red G of type premetallized dye | 2 |
| Pigment dispersing agent | 1.5 |
| Peregal O-25 | 1 |
| The double dodecyl dimethyl ammoniums of chlorination | 0.5 |
| Aluminum triacetate | 0.25 |
| Water | It is added to 100% |
Dispersibility：Top grade-is in misty automatic dispersion in water, and no visible particle sinks；Good grade-can divide automatically in water
It dissipates, has particles sink, could disperse after being vigorously shaken；Bad grade-cannot disperse automatically in water, sinking is in granular form, through strong
It could disperse after strong shake.
DEcmc values are smaller, indicate that level-dyeing property is better.
The performance of the 2 made dye dispersant of the present invention of table
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (6)
1. a kind of preparation method of synthetic leather dyeing dye dispersant, which is characterized in that include the following steps：
(1) the ultrasonic-microwave collaboration processing of beta-cyclodextrin：Beta-cyclodextrin is added to the water, is uniformly dispersed and is placed on ultrasonic wave-
In microwave synergistic extraction instrument, and supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz, microwave power are set
700W, return stirring close Ultrasonic-microwave synergistic extraction instrument after handling 5-10min, and interval 15-30min continues return stirring
5-10min is handled, lotion is made through being concentrated under reduced pressure in gained mixture, and lotion is sent into freeze drier after cooled to room temperature
In, particle is made through pulverizer in dry obtained solid；
(2) modification of beta-cyclodextrin：To cooperate with treated through ultrasonic-microwave, beta-cyclodextrin adds that solid content is made in water stirring
The colloid of 30-40% adds the mixed aqueous solution dissolved with N,N-DMAA, methacrylic acid and potassium peroxydisulfate,
It is then heated to reflux state insulated and stirred, gained mixture is sent into spray dryer after polymerisation, dry institute
It obtains particle and micro mist is made to get modified cyclodextrin through micronizer；
(3) preparation of pigment dispersing agent：Silicone emulsion is first added into made modified cyclodextrin, and is heated to 70-80 DEG C of heat preservation
5-10min is stirred, white aluminium polychloride and poly-aspartic-acid is added, continues to be heated to 100-110 DEG C of insulated and stirred 5-
10min is to get dye dispersant.
2. the preparation method of synthetic leather dyeing dye dispersant according to claim 1, it is characterised in that：The step
(1) mass ratio of beta-cyclodextrin and water is 1 in:5-10.
3. the preparation method of synthetic leather dyeing dye dispersant according to claim 1, it is characterised in that：The step
(2) mass ratio of beta-cyclodextrin, N in, N- dimethacrylamide, methacrylic acid and potassium peroxydisulfate are 50:10:5-10:
0.1-0.5。
4. the preparation method of synthetic leather dyeing dye dispersant according to claim 1, it is characterised in that：The step
(3) modified cyclodextrin in, silicone emulsion, white aluminium polychloride, poly-aspartic-acid mass ratio be 50:1-10:1-10:
0.5-5。
5. the preparation method of synthetic leather dyeing dye dispersant according to claim 1, it is characterised in that：The spermaceti
Alcohol passes through chemical modification, and modification procedure is：After cetanol and L-Glutimic acid are mixed plus absolute ethyl alcohol dissolves, then is added dropwise dense
Sulfuric acid regulation solution pH value is heated to reflux state insulated and stirred to 4-5, stops heating after reaction, through being concentrated under reduced pressure
Ethyl alcohol is recycled, condensate residue is dissolved in water completely, and gained mixed liquor is sent into spray dryer, and dry gained particle is through ultra micro
Micro mist is made to get modified cetanol in pulverizer.
6. the preparation method of synthetic leather dyeing dye dispersant according to claim 5, it is characterised in that：The spermaceti
Alcohol, L-Glutimic acid mass ratio be 10:5-10.
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| CN103357346A (en) * | 2013-06-27 | 2013-10-23 | 京东方科技集团股份有限公司 | Pigment dispersing agent, pigment dispersion liquid, colorized photoresist, and preparation and application thereof |
| CN106977955A (en) * | 2017-04-25 | 2017-07-25 | 江西展邦科技有限公司 | A kind of aqueous velvet auxiliary agent suitable for synthetic leather |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103357346A (en) * | 2013-06-27 | 2013-10-23 | 京东方科技集团股份有限公司 | Pigment dispersing agent, pigment dispersion liquid, colorized photoresist, and preparation and application thereof |
| CN106977955A (en) * | 2017-04-25 | 2017-07-25 | 江西展邦科技有限公司 | A kind of aqueous velvet auxiliary agent suitable for synthetic leather |
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