CN103088672A - Photochromic silica gel printing paste and its application in silica gel printing - Google Patents

Photochromic silica gel printing paste and its application in silica gel printing Download PDF

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Publication number
CN103088672A
CN103088672A CN2011103425476A CN201110342547A CN103088672A CN 103088672 A CN103088672 A CN 103088672A CN 2011103425476 A CN2011103425476 A CN 2011103425476A CN 201110342547 A CN201110342547 A CN 201110342547A CN 103088672 A CN103088672 A CN 103088672A
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China
Prior art keywords
silica gel
photochromic
printing paste
gel printing
preparation
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CN2011103425476A
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Chinese (zh)
Inventor
边俊民
孟继本
王霁华
韩健
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TIANJIN FORESEEN TECHNOLOGY CO LTD
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TIANJIN FORESEEN TECHNOLOGY CO LTD
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Abstract

The invention provides a photochromic silica gel printing paste and its application in silica gel printing. The photochromic silica gel printing paste comprises the following components by weight: 70-90 parts of a silica gel paste, 0-1 part of an ordinary pigment, 0-5 parts of a color fixing agent, and 0.5-5 parts of microencapsulated photochromic powder. The microencapsulated photochromic powder is a photochromic material encapsulated melamine resin microcapsule prepared from a photochromic material and melamine resin. The invention also provides a preparation method of the photochromic silica gel printing paste and application in silica gel printing. The photochromic silica gel printing paste provided in the invention has the advantages that preparation of the printing paste adopts a microencapsulation treatment method, so that the color fastness to washing and water penetration resistance of the color-changing material are improved, and the obtained fabric has more excellent performance, thus being in favor of people's wear health. The invention also provides a silica gel printing process suitable for the photochromic silica gel printing paste so as to facilitate popularization and application of the printing paste.

Description

A kind of photochromic silica gel printing paste and the application in the silica gel stamp thereof
Technical field
The invention belongs to the cloth print technology field, be specifically related to a kind of photochromic silica gel printing paste and printing technology thereof
Background technology
The main component of silica gel printing paste is stamp silica gel, and this kind printing paste combines the advantages such as the feel of elasticity, thermosetting silica gel of environmental protection, the rubber cement of water slurry and light, is subject to people's favor at Printing Industry.
The photochromic material that developed recently gets up enjoys people to favor with its photochromic characteristic, and this kind material has the effect of experiencing the sunlight turn colors, can be under the irradiation of sunlight, and the various colors of conversion present a kind of visual novel sense and impulsive force.Adopt clothes that this kind material makes also and novelty functional because of it be subject to youthfully liking.Mainly at the new photochromic compound of exploitation and in how applying it to garment industry, explore a kind of printing technology of suitable photochromic material about the study hotspot of off-color material, will cater to market demand, photochromic material is applied.
Chinese patent 200710068399.7 has been announced a kind of preparation technology of photochromic printing coated fabric, mainly carry out stamp and do top finish with Curtains Fabrics for umbrella cover is thick, its printing paste includes only three kinds of compositions: photochromic agent, synthetic thickening agent, adhesive, this kind printing paste is identical with the auxiliary element of traditional printing paste, can not well adapt to the characteristics of photochromic agent, the color fastness to washing of the fabric of preparing, water permeability resistance all can not be effectively guaranteed.
Summary of the invention
The technical scheme that the present invention will solve is to provide photochromic silica gel printing paste and the application in printing technology thereof that the indices such as a kind of color fastness to washing, water permeability resistance are excellent, be fit to the silica gel stamp
Concrete technical scheme is as follows:
A kind of photochromic silica gel printing paste is characterized in that: the component that comprises following weight portion:
Figure BSA00000604105200011
The preparation method of described microencapsulation light-induced variable toner is:
1) core preparation: the ratio according to percentage by weight 0.5-3% in the organic solvent adds photochromic material, is heated to 60-90 ℃, and stirring and dissolving is cooled to room temperature, gets core solution;
2) add appropriate emulsifier solution in core solution, emulsify at a high speed obtains the emulsification core solution of oil droplet size 1-10 μ m;
3) add suitable quantity of water in the emulsification core solution that obtains in the step 2, stir, slowly splashing into the wall material under rapid stirring is the melamine resin prepolymer, dropwise, rapid stirring, oil bath is warming up to 50-70 ℃, reaction 1-2h, continue to be warmed up to 70-90 ℃, rapid stirring reacts 2-3h, obtains encapsulating the melamine resin microcapsule slurry of photochromic material;
4) slurries that step 3 obtained are cooled to room temperature, with 5%NaOH aqueous solution regulation system pH value to 8.0-9.0;
5) the slurries spray drying that step 4 is obtained, obtaining solid product is microencapsulation light-induced variable toner.
Further, the organic solvent addition is: 30-65g, the emulsifying agent addition is: 90-130g, wall material: 30-65g, water: 200-1000mL.
The organic solvent that the core preparation of above-mentioned steps 1 is selected is any in dioctyl phthalate, n-hexane, cyclohexane, tetrachloro-ethylene, carbon tetrachloride.
Described emulsifying agent is selected any in SDS (lauryl sodium sulfate), neopelex, styrene-maleic anhydride copolymer.
The preparation method of above-mentioned a kind of photochromic silica gel printing paste is characterized in that: comprise the following steps:
1) described microencapsulation light-induced variable toner, common pigments are added respectively in proportion in the silica gel slurry, fully stir, until watch color even under all band spectrum;
2) use step 1 gained solution to carry out the experiment of small size stamp, evenly judge with color: if evenly, carry out step 3, continue to stir otherwise return to step 1;
3) solution that step 2 is obtained uses 100 order silk screen filter;
4) add color-fixing agent, and fully stir.
The application of a kind of photochromic silica gel printing paste in the silica gel printing technology that above-mentioned steps obtains.
Silica gel slurry used in the present invention, melamine resin prepolymer, color-fixing agent etc. all can be buied by market.
The main body of photochromic material of the present invention is photochromic compound, mainly selects following large class:
(1) naphtho-spirooxazine
R 1=H, CH 3, OCH 3, halogen
R 2=C 1-C 6Alkyl, C 1-C 6Alkyl heterocycle
R 3=azacyclo-, C 1-C 6Alkyl diamine
R 4=C 1-C 6Alkoxyl
At Chinese patent: ZL97120274.5 photochromic spiro-compound and preparation method thereof;
ZL200410072348.8 6 '-heterocycle substituted spirooxazine photochromic compound and preparation method thereof;
201110058243.7 record in detail in the preparation method of substituted spirooxazine photochromic compound.
(2) quino spirooxazine
Figure BSA00000604105200032
R 1=H, CH 3, OCH 3, halogen
R 2=C 1-C 6Alkyl, C 1-C 6Alkyl heterocycle
R 3=azacyclo-, C 1-C 6Alkyl diamine
Be documented in 201110058251.1 quino spirooxazine photochromic compounds and preparation method thereof
(3) benzo spirooxazine
Figure BSA00000604105200041
R 1=H, CH 3, OCH 3, halogen
R 2=C 1-C 6Alkyl, C 1-C 6Alkyl heterocycle
R 3=azacyclo-, C 1-C 6Alkyl diamine
(4) two aromatic heterocyclic ethylene compounds
Figure BSA00000604105200042
X=Y=S X=S Y=N
R 1=R 2=R 3=CH 3 R 1=R 2=R 3=CH 3
R 1=R 3=CH 3 R 1=R 2=CH 3
R 1=H R 2=H
R 2=R 1=CH 3,R 3=H R 2=R 1=CH 3,R 3=H
Figure BSA00000604105200051
X=Y=S X=S Y=N
R 1=R 2=R 3=CH 3 R 1=R 2=R 3=CH 3
R 1=R 3=CH 3 R 1=R 3=CH 3
R 1=H R 2=H
Figure BSA00000604105200052
X=Y=S X=S Y=N
R=CH 3 R=CH 3
X=Y=S X=S Y=N
R=CH 3 R=CH 3
Figure BSA00000604105200061
X=Y=S X=N Y=S
R 1=R 2=R 3=CH 3 R 1=R 2=R 3=CH 3
R 4=H R 4=OCH 3
R 1=R 2=CH 3 R 1=R 2=CH 3
R 3=CN,CHO R 3=CN,CHO
R 4=H R 4=OCH 3
R 1=CH 3,R 2=H,R 3=CN,CHO,R 4=OCH 3
Figure BSA00000604105200062
X=Y=S X=N Y=S
R 1=R 2=R 3=CH 3 R 1=R 2=R 3=CH 3
R 4=H R 4=OCH 3
R 3=R 1=CH 3 R 2=R 4=H
R 1=CH 3,R 2=R 4=H R 1=R 2=CH 3 R 3=CN,CHO
R 3=CN,CHO R 4=OCH 3
R 1=CH 3, R 2=H
R 3=CN,CHO R 4=OCH 3
(5) aryl replaces the aphthopyrans class
Figure BSA00000604105200071
R 1=2-C 1-C 8Alkoxyl R 2=4-C 1-C 8Alkoxyl
R 1=2-halogen R 2=4-C 1-C 8Alkoxyl or C 1-C 8Alkyl
R 1=H R 2=SCH 3
R 1=2-C 1-C 8Alkoxyl R 2=4-C 1-C 8Alkyl
R 1=2-aryl oxide R 2=4-aryl oxide
R 1=H R 2=4-C 1-C 8Alkoxyl
R 1=H R 2=4-halogen
R 1=H R 2=4-CF 3
Figure BSA00000604105200081
R 1=R 2=H
At 200510013276.4 photochromic compound of naphtho-pyrans and goods thereof; 200410072350.5 be documented in 2,2-diaryl naphthopyran compounds and preparation method thereof.
(6) spiro-pyrans compounds
R 1=H, halogen, C 1-C 6Alkyl, C 1-C 6Alkoxyl
R 2=C 1-C 8Alkyl, C 1-C 8The alkoxy aromatic heterocycle
Patents: ZL97120274.5 photochromic spiro-compound and preparation method thereof
Figure BSA00000604105200083
R 1=H, halogen, C 1-C 6Alkyl, C 1-C 6Alkoxyl
R 2=C 1-C 8Alkyl, C 1-C 8The alkoxy aromatic heterocycle
Advantage and beneficial effect that the present invention has are: the main component of a kind of photochromic silica gel printing paste of the present invention is photochromic compound, adopted the processing method of microencapsulation, homogeneous grain diameter, painted good, the color fastness to washing of the off-color material that makes and water permeability resistance etc. are improved, the fabric property that obtains is more excellent, and useful people wear health; The present invention also provides the application of this kind printing paste in the silica gel stamp, is convenient to applying of this kind printing paste.
The specific embodiment
Embodiment 1
Consisting of of the photochromic silica gel printing paste of the present embodiment 1:
Described photochromic compound is selected the quino spirooxazine photochromic compound.
The preparation method of above-mentioned a kind of photochromic silica gel printing paste is characterized in that: comprise the following steps:
1) described microencapsulation light-induced variable toner, common pigments are added respectively in proportion in the silica gel slurry, fully stir, until watch color even under all band spectrum;
2) use step 1 gained solution to carry out the experiment of small size stamp, evenly judge with color: if evenly, carry out step 3, continue to stir otherwise return to step 1;
3) solution that step 2 is obtained uses 100 order silk screen filter;
4) add color-fixing agent, and fully stir.
Use the printing paste of the present embodiment preparation to carry out the PRINTED FABRIC foundation that the silica gel stamp makes
The GB18401-2003 National Fundamental Safety Technical Standard For Textiles, assay is as follows:
Figure BSA00000604105200092
Figure BSA00000604105200101
Embodiment 2
Consisting of of the photochromic silica gel printing paste of the present embodiment 2:
Figure BSA00000604105200102
Described photochromic compound is selected substituted spirooxazine photochromic compound.
The preparation method of above-mentioned a kind of photochromic silica gel printing paste is characterized in that: comprise the following steps:
1) described microencapsulation light-induced variable toner, common pigments are added respectively in proportion in the silica gel slurry, fully stir, until watch color even under all band spectrum;
2) use step 1 gained solution to carry out the experiment of small size stamp, evenly judge with color: if evenly, carry out step 3, continue to stir otherwise return to step 1;
3) solution that step 2 is obtained uses 100 order silk screen filter;
4) add color-fixing agent, and fully stir.
Embodiment 3
Consisting of of the photochromic silica gel printing paste of the present embodiment 3:
Silica gel slurry 80kg
Color-fixing agent 0.5kg
Microencapsulation light-induced variable toner 2kg
Described photochromic compound is selected the spiro-pyrans compounds.
The preparation method of above-mentioned a kind of photochromic silica gel printing paste is characterized in that: comprise the following steps:
1) described microencapsulation light-induced variable toner, common pigments are added respectively in proportion in the silica gel slurry, fully stir, until watch color even under all band spectrum;
2) use step 1 gained solution to carry out the experiment of small size stamp, evenly judge with color: if evenly, carry out step 3, continue to stir otherwise return to step 1;
3) solution that step 2 is obtained uses 100 order silk screen filter;
4) add color-fixing agent, and fully stir.
Embodiment 4
In above-mentioned three embodiment, the preparation method of microencapsulation light-induced variable toner is:
1) core preparation: according to the 0.6g photochromic material, be heated to 70 ℃ in the dioctyl phthalate 30g, stirring and dissolving is cooled to room temperature, gets core solution;
2) add 5% emulsifier solution 100g in core solution, what the present embodiment was selected is styrene-maleic anhydride copolymer, and emulsify at a high speed obtains the emulsification core solution of oil droplet size 1-10 μ m;
3) add entry 800ml in the emulsification core solution that obtains in the step 2, stir, slowly splashing into the wall material under rapid stirring is melamine resin prepolymer 45g, dropwise, rapid stirring, oil bath is warming up to 70 ℃, reaction 1h, continue to be warmed up to 90 ℃, rapid stirring reacts 2h, obtains encapsulating the melamine resin microcapsule slurry of photochromic material;
4) slurries that step 3 obtained are cooled to room temperature, with 5%NaOH aqueous solution regulation system pH value to 8.8;
5) the slurries spray drying that step 4 is obtained, obtaining solid product is microencapsulation light-induced variable toner.

Claims (5)

1. photochromic silica gel printing paste is characterized in that: the component that comprises following weight portion:
Figure FSA00000604105100011
2. a kind of photochromic silica gel printing paste according to claim 1, it is characterized in that: the preparation method of described microencapsulation light-induced variable toner is:
1) core preparation: the ratio according to percentage by weight 0.5-3% in the organic solvent adds photochromic material, is heated to 60-90 ℃, and stirring and dissolving is cooled to room temperature, gets core solution;
2) add appropriate emulsifier solution in core solution, emulsify at a high speed obtains the emulsification core solution of oil droplet size 1-10 μ m;
3) add suitable quantity of water in the emulsification core solution that obtains in the step 2, stir, slowly splashing into the wall material under rapid stirring is the melamine resin prepolymer, dropwise, rapid stirring, oil bath is warming up to 50-70 ℃, reaction 1-2h, continue to be warmed up to 70-90 ℃, rapid stirring reacts 2-3h, obtains encapsulating the melamine resin microcapsule slurry of photochromic material;
4) slurries that step 3 obtained are cooled to room temperature, with 5%NaOH aqueous solution regulation system pH value to 8.0-9.0;
5) the slurries spray drying that step 4 is obtained, obtaining solid product is microencapsulation light-induced variable toner.
3. the preparation method of a kind of photochromic silica gel printing paste according to claim 2, it is characterized in that: in the preparation method of described microencapsulation light-induced variable toner, organic solvent in step 1 is selected any in dioctyl phthalate, n-hexane, cyclohexane, tetrachloro-ethylene, carbon tetrachloride, and described emulsifying agent is selected any in SDS (lauryl sodium sulfate), neopelex, styrene-maleic anhydride copolymer.
4. the preparation method of a kind of photochromic silica gel printing paste according to claim 1 is characterized in that: comprise the following steps:
1) described microencapsulation light-induced variable toner, common pigments are added respectively in proportion in the silica gel slurry, fully stir, until watch color even under all band spectrum;
2) use step 1 gained solution to carry out the experiment of small size stamp, evenly judge with color: if evenly, carry out step 3, continue to stir otherwise return to step 1;
3) solution that step 2 is obtained uses 100 order silk screen filter;
4) add color-fixing agent, and fully stir.
5. the application of a kind of photochromic silica gel printing paste according to claim 1 in the silica gel stamp.
CN2011103425476A 2011-11-03 2011-11-03 Photochromic silica gel printing paste and its application in silica gel printing Pending CN103088672A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104490021A (en) * 2015-01-08 2015-04-08 深圳市博恩实业有限公司 Intelligent color changing bracelet
CN107059441A (en) * 2017-06-13 2017-08-18 安踏(中国)有限公司 A kind of PM2.5 early warning mark and its application
CN111393895A (en) * 2020-04-13 2020-07-10 探路者控股集团股份有限公司 Long-acting optical variable powder and preparation method and application thereof

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CN101225296A (en) * 2008-02-01 2008-07-23 北京服装学院 Method for preparing photochromic micro-encapsulation
JP2009149774A (en) * 2007-12-20 2009-07-09 Sakata Corp Ink composition for inkjet printing and method for inkjet printing

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
CN101058946A (en) * 2007-04-29 2007-10-24 浙江理工大学 Process of preparing photochromic printing coated fabric
JP2009149774A (en) * 2007-12-20 2009-07-09 Sakata Corp Ink composition for inkjet printing and method for inkjet printing
CN101225296A (en) * 2008-02-01 2008-07-23 北京服装学院 Method for preparing photochromic micro-encapsulation

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104490021A (en) * 2015-01-08 2015-04-08 深圳市博恩实业有限公司 Intelligent color changing bracelet
CN107059441A (en) * 2017-06-13 2017-08-18 安踏(中国)有限公司 A kind of PM2.5 early warning mark and its application
CN111393895A (en) * 2020-04-13 2020-07-10 探路者控股集团股份有限公司 Long-acting optical variable powder and preparation method and application thereof

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Application publication date: 20130508