CN103881630A - Composite transfer adhesive for high-brightness reflective fabric and preparation method thereof - Google Patents
Composite transfer adhesive for high-brightness reflective fabric and preparation method thereof Download PDFInfo
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- CN103881630A CN103881630A CN201410069828.2A CN201410069828A CN103881630A CN 103881630 A CN103881630 A CN 103881630A CN 201410069828 A CN201410069828 A CN 201410069828A CN 103881630 A CN103881630 A CN 103881630A
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Abstract
The invention discloses a composite transfer adhesive for a high-brightness reflective fabric. The composite transfer adhesive is prepared from raw materials comprising the following components in parts by weight: 50-70 parts of acrylate soft monomer, 10-40 parts of acrylate hard monomer, 3-12 parts of acrylate functional monomer, 0.2-1 part of initiator and 180-190 parts of solvent. The invention also discloses a preparation method of the composite transfer adhesive. The composite transfer adhesive has the beneficial effects that only low-toxicity ethyl acetate is adopted to serve as a solvent; the composite transfer adhesive for the high-brightness reflective fabric is synthesized by adopting a graft copolymerization method, so that high initial stickness is kept, and the holding power is greatly improved; the rubbing resistance and washing resistance applied to the high-brightness reflective fabric are far higher than those of random copolymer. A method for adding the initiators in batches is adopted, and the influence on the product performance in a traditional dripping mode due to the inconsistent dripping speed is avoided.
Description
Technical field
The present invention relates to a kind of highlighted reflective fabric with shifting composite adhesive and preparation method thereof.
Background technology
Highlighted reflective fabric can be widely used in the fields such as public security, fire-fighting, traffic, railway, environmental sanitation, colliery and personal security's protective articles, is normally made up of high refractive index glass micro pearl, tackiness agent and base material three parts.Wherein tackiness agent is the key basic material of light reflecting material, is the tackiness agent of glass microballon and base material, requires to have good film-forming properties, flexibility, wash durability and wear resisting property.
At present, the tackiness agent of two kinds of systems is mainly used in reflective fabric market, and one is polyacrylic ester system tackiness agent, and another is polyurethane system tackiness agent.But, highlighted reflective fabric is by its service requirements, esters of acrylic acid tackiness agent can meet its service requirements completely, can, at highlighted T/C cloth, on highlighted chemical fibre, use, also can on general bright cloth, use, polyurethane-modified polyacrylate product or polyurethane tackifier are multiplex on silver lustre series product, because its price is high, goods are harder, and its market share is well below highlighted reflective fabric.
Chinese patent 201010603660.0 discloses a kind of acrylate adhesive for reflective cloth and preparation method, adopt situ aggregation method to synthesize a kind of epoxide modified palyacrylate binder, the solution the inside placement that specifically esters of acrylic acid function monomer is dissolved in to epoxy compounds is no less than 48 hours, then after all monomers being mixed, adopt the mode dripping to synthesize a kind of acrylate adhesive for reflective cloth, this method relates to the solvent that the toxicity such as toluene, dimethylbenzene is higher.
Chinese patent CN201310079173.2 discloses a kind of general brightness reflective fabric tackiness agent, the polyacrylate resin and the Tg that by Tg are the high glass-transition temperature of 5～20 ℃ are the polyacrylate resin of the lower glass transition temperatures of～30 ℃ to～50 ℃, carry out physical mixed form according to certain ratio.The method of this employing physical blending operates cumbersome, first will synthesize the polyacrylate resin of different Tg, may be because the performance difference of the inconsistent blend of different batches monomer conversion when blend.
Summary of the invention
The object of the invention is to overcome the shortcoming of prior art, provide a kind of and not only kept good tack, hold highlighted reflective fabric that viscosity also increases substantially with shifting composite adhesive and preparation method thereof.
Object of the present invention is achieved through the following technical solutions: a kind of highlighted reflective fabric is with shifting composite adhesive, and it is prepared by the raw material that comprises following component, and the weight ratio of each component is:
Esters of acrylic acid soft monomer: 50～70,
Esters of acrylic acid hard monomer: 10～40,
Esters of acrylic acid function monomer: 3～12,
Initiator: 0.2～1,
Solvent: 180～190.
Described esters of acrylic acid soft monomer comprises: any one in ethyl acrylate, butyl acrylate, ethyl propenoate or multiple.
Described esters of acrylic acid hard monomer comprises: any one in methyl acrylate, methyl methacrylate, β-dimethyl-aminoethylmethacrylate, n-BMA, vinyl-acetic ester, vinylbenzene or multiple.
Described esters of acrylic acid function monomer comprises: any one in vinylformic acid, Hydroxyethyl acrylate, Propylene glycol monoacrylate, 2-hydroxyethyl methacrylate, methacrylic acid-2-hydroxypropyl acrylate, maleic acid or multiple.
Described initiator is: Diisopropyl azodicarboxylate.
Described solvent is: ethyl acetate.
The described preparation method who shifts composite adhesive for highlighted reflective fabric, it comprises the following steps:
S1, monomer by above-mentioned monomer second-order transition temperature below 0 ℃ are all put in reactor, add the solvent that accounts for solvent total amount 40%～60% in reactor;
S2, above-mentioned initiator is dissolved in the solvent that accounts for solvent total amount 5%～10% and is mixed with initiator solution, it is divided into 10 parts, add 1 part in reactor;
S3, be warmed up to 76～82 ℃, occur starting timing while backflow until feed liquid, add 1 part of initiator solution after 1 hour, while adding initiator solution to the 3rd time, by glass temperature, the monomer more than 0 ℃ all joins in reactor simultaneously; And continuation added 1 part of initiator solution after 1 hour;
S4, add after initiator solution for the last time, be incubated 2 hours;
S5, add remaining solvent, be stirred to 30～40 ℃, discharging obtains highlighted reflective fabric with shifting composite gum.
The present invention has the following advantages:
The present invention adopts the method for graft copolymerization to synthesize a kind of highlighted reflective fabric with shifting composite adhesive, first make esters of acrylic acid soft monomer copolymerization in the little ethyl acetate of toxicity that homopolymer second-order transition temperature is lower, then in this system, add the acrylic ester monomer that homopolymer second-order transition temperature is higher to carry out radical polymerization, this method can be introduced the hard segment of high glass transition temperature on the molecular backbone chain of low Tg, the tackiness agent random copolymers identical with proportioning of preparation compared the initial cohesiveness that has not only kept good, and greatly improve cohesive strength.
And the present invention only adopts ethyl acetate that toxicity is less as solvent; The present invention adopts the highlighted reflective fabric of the synthetic one of the method for graft copolymerization with shifting composite adhesive, has not only kept good tack, holds viscosity and also increases substantially; Be applied to resistance toly on highlighted reflective fabric rub, wash durability is better than random copolymers far away; The present invention adopts the method that adds in batches initiator, has avoided traditional dropping mode because of the inconsistent impact on product performance of rate of addition.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, and protection scope of the present invention is not limited to the following stated:
embodiment 1:
A kind of highlighted reflective fabric is with shifting composite adhesive, and it is prepared by the raw material that comprises following component, and the weight ratio of each component is:
Esters of acrylic acid soft monomer: 60,
Esters of acrylic acid hard monomer: 32,
Esters of acrylic acid function monomer: 8,
Initiator: 1,
Solvent: 186,
Described esters of acrylic acid soft monomer is: butyl acrylate, ethyl acrylate and ethyl propenoate, and said components weight ratio can be arbitrary value, the weight ratio adopting in this enforcement is: butyl acrylate: 20, ethyl acrylate: 35, ethyl propenoate: 5
Described esters of acrylic acid hard monomer is: methyl methacrylate and vinyl-acetic ester, and said components weight ratio can be arbitrary value, and the weight ratio adopting in this enforcement is: methyl methacrylate: 20, vinyl-acetic ester: 12,
Described esters of acrylic acid function monomer is vinylformic acid,
Described initiator is Diisopropyl azodicarboxylate,
Described solvent is ethyl acetate.
The described preparation method who shifts composite adhesive for highlighted reflective fabric, it comprises the following steps:
S1, monomer by above-mentioned monomer second-order transition temperature below 0 ℃, i.e. butyl acrylate, ethyl acrylate, ethyl propenoate, all puts in reactor, adds the solvent that accounts for solvent total amount 50% in reactor;
S2, by above-mentioned initiator, i.e. Diisopropyl azodicarboxylate, is dissolved in the solvent that accounts for solvent total amount 8% and is mixed with initiator solution, and it is divided into 10 parts, adds 1 part in reactor;
S3, be warmed up to 79 ℃, in the time that appearring in feed liquid, backflow starts timing, after 1 hour, add 1 part of initiator solution, while adding initiator solution to the 3rd time, the monomer more than 0 ℃ by glass temperature simultaneously, be methyl methacrylate, vinyl-acetic ester, vinylformic acid, all join in reactor; And continuation added 1 part of initiator solution after 1 hour;
S4, add after initiator solution for the last time, be incubated 2 hours;
S5, add remaining solvent, be stirred to 35 ℃, discharging obtains highlighted reflective fabric with shifting composite gum.
embodiment 2:
A kind of highlighted reflective fabric is with shifting composite adhesive, and it is prepared by the raw material that comprises following component, and the weight ratio of each component is:
Esters of acrylic acid soft monomer: 70,
Esters of acrylic acid hard monomer: 10,
Esters of acrylic acid function monomer: 12,
Initiator: 0.5,
Solvent: 190,
Described esters of acrylic acid soft monomer is: butyl acrylate, ethyl acrylate and ethyl propenoate, and said components weight ratio can be arbitrary value, the weight ratio adopting in this enforcement is: butyl acrylate: 25, ethyl acrylate: 35, ethyl propenoate: 10
Described esters of acrylic acid hard monomer is: methyl acrylate,
Described esters of acrylic acid function monomer is Hydroxyethyl acrylate, Propylene glycol monoacrylate, 2-hydroxyethyl methacrylate, methacrylic acid-2-hydroxypropyl acrylate and maleic acid, and said components weight ratio can be arbitrary value, the weight ratio adopting in this enforcement is: Hydroxyethyl acrylate: 3, Propylene glycol monoacrylate: 3,2-hydroxyethyl methacrylate: 2, methacrylic acid-2-hydroxypropyl acrylate 2, maleic acid: 2.
Described initiator is Diisopropyl azodicarboxylate,
Described solvent is ethyl acetate.
The described preparation method who shifts composite adhesive for highlighted reflective fabric, it comprises the following steps:
S1, monomer by above-mentioned monomer second-order transition temperature below 0 ℃, be butyl acrylate, ethyl acrylate, ethyl propenoate, Hydroxyethyl acrylate and Propylene glycol monoacrylate, all put in reactor, add the solvent that accounts for solvent total amount 60% in reactor;
S2, by above-mentioned initiator, i.e. Diisopropyl azodicarboxylate, is dissolved in the solvent that accounts for solvent total amount 10% and is mixed with initiator solution, and it is divided into 10 parts, adds 1 part in reactor;
S3, be warmed up to 82 ℃, in the time that appearring in feed liquid, backflow starts timing, after 1 hour, add 1 part of initiator solution, while adding initiator solution to the 3rd time, the monomer more than 0 ℃ by glass temperature simultaneously, be methyl acrylate, 2-hydroxyethyl methacrylate, methacrylic acid-2-hydroxypropyl acrylate and maleic acid, all join in reactor; And continuation added 1 part of initiator solution after 1 hour;
S4, add after initiator solution for the last time, be incubated 2 hours;
S5, add remaining solvent, be stirred to 40 ℃, discharging obtains highlighted reflective fabric with shifting composite gum.
embodiment 3:
A kind of highlighted reflective fabric is with shifting composite adhesive, and it is prepared by the raw material that comprises following component, and the weight ratio of each component is:
Esters of acrylic acid soft monomer: 50,
Esters of acrylic acid hard monomer: 40,
Esters of acrylic acid function monomer: 3,
Initiator: 0.2,
Solvent: 180,
Described esters of acrylic acid soft monomer is: butyl acrylate,
Described esters of acrylic acid hard monomer is: β-dimethyl-aminoethylmethacrylate, n-BMA and vinylbenzene, and said components weight ratio can be arbitrary value, the weight ratio adopting in this enforcement is: β-dimethyl-aminoethylmethacrylate: 20, n-BMA: 10, vinylbenzene: 10
Described esters of acrylic acid function monomer is vinylformic acid, Hydroxyethyl acrylate and Propylene glycol monoacrylate, and said components weight ratio can be arbitrary value, and the weight ratio adopting in this enforcement is: vinylformic acid: 1, Hydroxyethyl acrylate: 1 and Propylene glycol monoacrylate: 1.
Described initiator is Diisopropyl azodicarboxylate,
Described solvent is ethyl acetate.
The described preparation method who shifts composite adhesive for highlighted reflective fabric, it comprises the following steps:
S1, monomer by above-mentioned monomer second-order transition temperature below 0 ℃, i.e. butyl acrylate, Hydroxyethyl acrylate and Propylene glycol monoacrylate, all puts in reactor, adds the solvent that accounts for solvent total amount 40% in reactor;
S2, by above-mentioned initiator, i.e. Diisopropyl azodicarboxylate, is dissolved in the solvent that accounts for solvent total amount 5% and is mixed with initiator solution, and it is divided into 10 parts, adds 1 part in reactor;
S3, be warmed up to 76 ℃, in the time that appearring in feed liquid, backflow starts timing, after 1 hour, add 1 part of initiator solution, while adding initiator solution to the 3rd time, the monomer more than 0 ℃ by glass temperature simultaneously, be β-dimethyl-aminoethylmethacrylate, n-BMA, vinylbenzene and vinylformic acid, all join in reactor; And continuation added 1 part of initiator solution after 1 hour;
S4, add after initiator solution for the last time, be incubated 2 hours;
S5, add remaining solvent, be stirred to 30 ℃, discharging obtains highlighted reflective fabric with shifting composite gum.
Claims (7)
1. highlighted reflective fabric, with shifting a composite adhesive, it is characterized in that: it is prepared by the raw material that comprises following component, and the weight ratio of each component is:
Esters of acrylic acid soft monomer: 50～70,
Esters of acrylic acid hard monomer: 10～40,
Esters of acrylic acid function monomer: 3～12,
Initiator: 0.2～1,
Solvent: 180～190.
2. the highlighted reflective fabric of one according to claim 1, with shifting composite adhesive, is characterized in that: described esters of acrylic acid soft monomer comprises: any one in ethyl acrylate, butyl acrylate, ethyl propenoate or multiple.
3. the highlighted reflective fabric of one according to claim 1, with shifting composite adhesive, is characterized in that: described esters of acrylic acid hard monomer comprises: any one in methyl acrylate, methyl methacrylate, β-dimethyl-aminoethylmethacrylate, n-BMA, vinyl-acetic ester, vinylbenzene or multiple.
4. the highlighted reflective fabric of one according to claim 1, with shifting composite adhesive, is characterized in that: described esters of acrylic acid function monomer comprises: any one in vinylformic acid, Hydroxyethyl acrylate, Propylene glycol monoacrylate, 2-hydroxyethyl methacrylate, methacrylic acid-2-hydroxypropyl acrylate, maleic acid or multiple.
5. the highlighted reflective fabric of one according to claim 1, with shifting composite adhesive, is characterized in that: described initiator is Diisopropyl azodicarboxylate.
6. the highlighted reflective fabric of one according to claim 1, with shifting composite adhesive, is characterized in that: described solvent is ethyl acetate.
7. the preparation method who shifts composite adhesive for a kind of highlighted reflective fabric as described in any one in claim 1～6, is characterized in that: it comprises the following steps:
S1, monomer by above-mentioned monomer second-order transition temperature below 0 ℃ are all put in reactor, add the solvent that accounts for solvent total amount 40%～60% in reactor;
S2, above-mentioned initiator is dissolved in the solvent that accounts for solvent total amount 5%～10% and is mixed with initiator solution, it is divided into 10 parts, add 1 part in reactor;
S3, be warmed up to 76～82 ℃, occur starting timing while backflow until feed liquid, add 1 part of initiator solution after 1 hour, while adding initiator solution to the 3rd time, by glass temperature, the monomer more than 0 ℃ all joins in reactor simultaneously; And continuation added 1 part of initiator solution after 1 hour;
S4, add after initiator solution for the last time, be incubated 2 hours;
S5, add remaining solvent, be stirred to 30～40 ℃, discharging obtains highlighted reflective fabric with shifting composite gum.
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| CN201410069828.2A CN103881630B (en) | 2014-02-28 | 2014-02-28 | A kind of highlighted reflective fabric transfer composite adhesive and preparation method thereof |
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| CN201410069828.2A CN103881630B (en) | 2014-02-28 | 2014-02-28 | A kind of highlighted reflective fabric transfer composite adhesive and preparation method thereof |
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| CN103881630B CN103881630B (en) | 2016-06-08 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105419688A (en) * | 2015-12-02 | 2016-03-23 | 安徽金信地首饰有限公司 | Modified acrylate adhesive |
| CN105837737A (en) * | 2016-04-20 | 2016-08-10 | 成都艾迪生节能环保有限责任公司 | Special water-based acrylate adhesive for reflective fabric and production technology thereof |
| CN110791235A (en) * | 2019-11-14 | 2020-02-14 | 北京清鸿光科科技有限公司 | Intelligent watch sealant and preparation method thereof |
| CN113388347A (en) * | 2021-07-06 | 2021-09-14 | 长春工业大学 | Preparation method of high-adaptability solid adhesive |
| CN114196355A (en) * | 2021-12-30 | 2022-03-18 | 常州华日升反光材料有限公司 | Preparation method of bead-sinking adhesive for sedimentation type reflective film |
| CN114907795A (en) * | 2021-07-22 | 2022-08-16 | 杭州星华反光材料股份有限公司 | Composite adhesive for highlight chemical fiber material and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105419688A (en) * | 2015-12-02 | 2016-03-23 | 安徽金信地首饰有限公司 | Modified acrylate adhesive |
| CN105837737A (en) * | 2016-04-20 | 2016-08-10 | 成都艾迪生节能环保有限责任公司 | Special water-based acrylate adhesive for reflective fabric and production technology thereof |
| CN110791235A (en) * | 2019-11-14 | 2020-02-14 | 北京清鸿光科科技有限公司 | Intelligent watch sealant and preparation method thereof |
| CN113388347A (en) * | 2021-07-06 | 2021-09-14 | 长春工业大学 | Preparation method of high-adaptability solid adhesive |
| CN114907795A (en) * | 2021-07-22 | 2022-08-16 | 杭州星华反光材料股份有限公司 | Composite adhesive for highlight chemical fiber material and preparation method thereof |
| CN114907795B (en) * | 2021-07-22 | 2023-11-21 | 浙江星华新材料集团股份有限公司 | Composite adhesive for highlight chemical fiber material and preparation method thereof |
| CN114196355A (en) * | 2021-12-30 | 2022-03-18 | 常州华日升反光材料有限公司 | Preparation method of bead-sinking adhesive for sedimentation type reflective film |
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| CN103881630B (en) | 2016-06-08 |
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Effective date of registration: 20210413 Address after: Group 6 and 7, Zhongfeng village, Binlang Township, high tech Zone, Dazhou, Sichuan 610000 Patentee after: Cecep (Dazhou) new material Co.,Ltd. Address before: 610400 Sichuan Jintang Industrial Park, Zhao town, Jintang County, Chengdu City, Sichuan Province Patentee before: CHENGDU ZHONGJIENENG REFLECTIVE MATERIALS Co.,Ltd. |
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Denomination of invention: A transfer composite adhesive for high brightness reflective cloth and its preparation method Effective date of registration: 20221229 Granted publication date: 20160608 Pledgee: Dazhou Rural Commercial Bank Co.,Ltd. Dachuan Sub branch Pledgor: Cecep (Dazhou) new material Co.,Ltd. Registration number: Y2022510000335 |