CN104927745B - Adhesive for reflecting elastic fabrics and preparing method thereof - Google Patents
Adhesive for reflecting elastic fabrics and preparing method thereof Download PDFInfo
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- CN104927745B CN104927745B CN201510357292.9A CN201510357292A CN104927745B CN 104927745 B CN104927745 B CN 104927745B CN 201510357292 A CN201510357292 A CN 201510357292A CN 104927745 B CN104927745 B CN 104927745B
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Abstract
The invention provides adhesive for reflecting elastic fabrics and a preparing method thereof. The adhesive comprises polyester polyol 4000 in molecular weight, polyester polyol 2000 in molecular weight, elastic rubber, long-chain hydroxyl acrylate, diisocyanate, small molecule diols, organic solvent, silane coupler and initiator. By effectively improving elasticity, adhesion, water resistance and wear resistance of the adhesive, the use of the adhesive in the reflecting elastic fabrics effectively improve the performances of the reflecting elastic fabrics, such as washability, dry cleaning fastness and wear resistance.
Description
Technical field
The invention belongs to reflective fabric preparing technical field, and in particular to reflective stretch fabric adhesive and preparation method thereof.
Background technology
Reflective fabric also referred to as reflects cloth, regression reflective fabric, and it is glass microballoon to be put on fabric, is existed using light
The optical principle returned after refraction reflection in glass microballoon, makes reflected light penetrate light direction by people and mostly returns light source direction,
It is widely used in traffic safety equipment, reflective clothes, all kinds of business wears, work clothes, fashionable dress, shoes and hats, gloves, knapsack, personal protection
Articles for use, outdoor goods etc., can also be fabricated to all kinds of reflective articles, ornaments.This reflector is micro- with the glass of high index of refraction
Pearl retroreflecting principle, is made by the advanced technologies of focusing post processing.It can postback distant place direct light line reflection at light, no
There is good reflex reflection optical property by daytime or night, especially evening, the high energy as daytime can be played
Degree of opinion.Therefore reflective fabric has extensively been accepted and received by the social economic value of its excellent optical characteristics and brilliance.
As the demand of reflective fabric increasingly increases, in order to adapt to the needs in market, various reflective fabrics are occurred in that, such as reflective bullet
Power cloth, but existing reflective stretch fabric is poor because adhesive has an elastic effect, and viscosity is not enough, and abrasion resistant effect is bad so that production
Obtain reflective stretch fabric and equally there is also water-fastness, resistance to dry-cleaning or wearability etc. that needs can not be met.
The content of the invention
For above-mentioned the deficiencies in the prior art, the present invention is intended to provide a kind of reflective stretch fabric adhesive and its preparation side
Method, by the elasticity, viscosity, resistance to water and the anti-wear performance that are effectively improved adhesive, is used on reflective stretch fabric, effectively
Improve performance of the reflective stretch fabric at the aspect such as water-fastness, resistance to dry-cleaning, wear-resisting.
To realize goal of the invention, the technical scheme that the present invention takes is：Reflective stretch fabric adhesive, by weight
Meter, including following component：
Preferably, the PEPA of the molecular weight 4000 is selected from polyadipate-BDO esterdiol, gathers oneself
Diacid neopentyl glycol esterdiol, polyadipate neopentyl glycol-BDO esterdiol or polyadipate -2- methyl propanediols -
Any one in BDO esterdiol.
Preferably, the PEPA of the molecular weight 2000 is selected from polyadipate -2- methyl propanediol esterdiols, gathers
Any one in NGA neopentyl glycol adipate glycol or polyadipate -2- methyl propanediol neopentyl glycol esterdiols.
Preferably, any one of the elastic caoutchouc in butadiene-styrene rubber, nitrile rubber, butyl rubber.
Preferably, the long chain allcyl acrylate is the acrylic acid hydroxyl ester or the propylene of pentaerythrite three of caprolactone grafting
Acid esters.
Preferably, the diisocyanate is selected from methyl diphenylene diisocyanate, hexamethylene diisocyanate, first
In phenylene diisocyanate it is arbitrary one or two.
Preferably, the small molecule glycol is selected from neopentyl glycol, 4- ethoxy oxygen ethyl -1- hydroxyethylbenzene diether, Isosorbide-5-Nitrae
Any one in butanediol, 2- methyl -2,4-PD or two kinds.
Preferably, any one of the organic solvent in ethyl acetate, toluene, butanone, dimethylformamide
Or two kinds.
Preferably, described organic solvent is the mixture of ethyl acetate and toluene, butanone or dimethylformamide, two
The weight ratio for planting component is 1:1～3:1.
Preferably, the silane coupler is selected from γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-aminopropyl
It is any one in triethoxysilane, B- (3,4 epoxycyclohexyl) ethyl trimethoxy silane, phenylamino propyl trimethoxy silicane
Kind.
Preferably, the initiator is azodiisobutyronitrile or dibenzoyl peroxide, from parts by weight 0.01～
0.1 part of initiator, monomer conversion is good, and initiator parts by weight react less incomplete；Can cause more than initiator parts by weight
The waste of initiator, cost increases.
The invention further relates to the preparation method of above-mentioned reflective stretch fabric adhesive, takes following technical scheme：
A kind of preparation method of reflective stretch fabric adhesive, comprises the steps：
(1) organic solvent of the same weight portion of 3～10 parts of use of elastic caoutchouc weight portion prepares the rubber that mass concentration is 50%
Sol solution, is warming up to 75 DEG C～80 DEG C by 3～10 parts of long chain allcyl acrylate weight portion and initiator weight portion 0.01～0.1
Part is added dropwise to into rubber solutions, is reacted more than 4 hours, obtains rubber polymer solution；
(2) by 20～40 parts of the PEPA weight portion and the PEPA weight of molecular weight 2000 of molecular weight 4000
3～10 parts of part is put in reactor, and 1～2 hour is vacuumized at a temperature of 110～120 DEG C, adds when being cooled to 70～90 DEG C
Enter rubber polymer solution, after being sufficiently mixed uniformly, add 15～20 parts of organic solvent weight portion and diisocyanate weight
1～3 part of part of amount, reacts 0.5～1 hour in 75～80 DEG C；
(3) again toward the reactor in step (2) plus 0.3～1 part of small molecule glycol weight portion and organic solvent weight portion
15～20 parts, react 2～3 hours, add 7～10 parts of 2～5 parts of diisocyanate weight portion and organic solvent weight portion, in
40～50 DEG C add 0.5～5 part of silane coupler weight portion, discharging to obtain the polyurethane adhesive host.
Beneficial effects of the present invention are embodied in：
1. the PEPA of molecular weight 4000 and molecular weight 2000 is used in combination so that PEPA has high resistance to
Mill oil resistance, high intensity, initial bonding strength are strong, intermolecular cohesive energy is big, good crystallinity the features such as；
2. preparation technology adopts performed polymer synthetic method, by the way that acrylate monomers and elastic caoutchouc are introduced into polymeric acceptor
System effectively improves elasticity, viscosity, resistance to water, the wearability of polyurethane system；
3. preparation technology is because using reaction step by step, avoiding causing the danger of blast because discharging amount of heat；
4. preparation technology is using control reaction time step by step, preferably controls the weatherability of polyurethane system and attached
The property is good.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
A kind of reflective stretch fabric adhesive, including the component preparation of following weight proportion：20 parts of polyadipate-Isosorbide-5-Nitrae-fourths
Glycol esterdiol, 3 parts of polyadipate -2- methyl propanediol esterdiols, 3 parts of butadiene-styrene rubber, the acrylic acid hydroxyl of 3 parts of caprolactone grafting
Ester, 3 parts of methyl diphenylene diisocyanates, 0.3 part of neopentyl glycol, 40 parts of toluene, 0.5 part of γ-glycidyl ether oxygen propyl three
Methoxy silane, 0.01 azodiisobutyronitrile.
(1) butadiene-styrene rubber for weighing above-mentioned weight ratio prepares the rubber solutions that mass concentration is 50% with 3 parts of toluene, heats up
The acrylic acid hydroxyl ester and azodiisobutyronitrile being grafted to 75 DEG C～80 DEG C caprolactones by above-mentioned parts by weight is added dropwise to rubber
In solution, react 5 hours, obtain rubber polymer solution；
(2) by above-mentioned 20 parts of polyadipates-BDO esterdiol and 3 parts of polyadipate -2- methyl propanediols esters two
Alcohol is put in reactor, is vacuumized at a temperature of 110 DEG C 2 hours, and when being cooled to 85 DEG C rubber polymer solution is added, and waits to fill
Divide after being well mixed, add 15 parts of toluene and 1 part of methyl diphenylene diisocyanate, react 0.5 hour in 75 DEG C；
(3) again toward the reactor in step (2) plus 0.3 part of neopentyl glycol and 15 parts of toluene, react 2 hours, add 2
Part methyl diphenylene diisocyanate and 7 parts of toluene, in 40 DEG C 0.5 part of γ-glycidyl ether oxygen propyl trimethoxy silicon is added
Alkane, discharging obtains the polyurethane adhesive host.
Embodiment 2
A kind of reflective stretch fabric adhesive, including the component preparation of following weight proportion：40 parts of polyadipates new penta 2
Alcohol esterdiol, 10 parts of polyneopentyl glycol adipate glycol, 10 parts of nitrile rubbers, 10 parts of pentaerythritol triacrylates, 8 part six
Methylene diisocyanate, 1 part of 2- methyl -2,4- pentanediols, 30 parts of ethyl acetate, 30 parts of dimethylformamides, 5 parts of phenylaminos third
Base trimethoxy silane, 0.1 part of dibenzoyl peroxide.
(1) 10 parts of nitrile rubber weight portions, 5 parts of ethyl acetate are weighed and 5 parts of dimethylformamides preparation mass concentrations is
50% rubber solutions, are warming up to 75 DEG C～80 DEG C by 10 parts of pentaerythritol triacrylates and 0.1 part of dibenzoyl peroxide
It is added dropwise to into rubber solutions, reacts 6 hours, obtains rubber polymer solution；
(2) 40 parts of polyneopentyl glycol adipate glycol and 10 parts of polyneopentyl glycol adipate glycol are put into into reaction
In kettle, 1 hour is vacuumized at a temperature of 115 DEG C, when being cooled to 70 DEG C rubber polymer solution is added, wait to be sufficiently mixed uniformly
After, 10 parts of ethyl acetate and 10 parts of dimethylformamides and 3 parts of hexamethylene diisocyanates are added, react 0.5 in 80 DEG C
Hour；
(3) again toward the reactor in step (2) plus 1 part of 2- methyl -2,4-PD and 10 parts of ethyl acetate and 10 parts
Dimethylformamide, reacts 2 hours, adds 5 parts of hexamethylene diisocyanates, 5 parts of ethyl acetate and 5 parts of dimethyl formyls
Amine, adds 5 parts of phenylamino propyl trimethoxy silicanes, discharging to obtain the polyurethane adhesive host in 40 DEG C.
Embodiment 3
A kind of reflective stretch fabric adhesive, including the component preparation of following weight proportion：30 parts of polyadipate -2- methyl
Propane diols-BDO esterdiol, 8 parts of polyadipate -2- methyl propanediol neopentyl glycol esterdiols, 6 parts of butyl rubbers, 5
The acrylic acid hydroxyl ester of part caprolactone grafting, 6 parts of toluene di-isocyanate(TDI)s, 0.8 part of 4- ethoxy oxygen ethyl -1- hydroxyethylbenzene two
Ether, 36 parts of ethyl acetate, 12 parts of butanone, 3 parts of B- (3,4 epoxycyclohexyl) ethyl trimethoxy silanes, 0.05 part of azo two is different
Butyronitrile.
(1) 6 parts of butyl rubber weight portions, 4.5 parts of ethyl acetate are weighed and 1.5 parts of butanone prepares mass concentration for 50%
Rubber solutions, be warming up to 78 DEG C by the acrylic acid hydroxyl esters of 5 parts of caprolactones grafting and 0.05 part of azodiisobutyronitrile be added dropwise to
In rubber solutions, react 4.5 hours, obtain rubber polymer solution；
(2) by 30 parts of polyadipate -2- methyl propanediols-BDO esterdiols and 8 parts of polyadipate -2- methyl-props
Glycol neopentyl glycol esterdiol is put in reactor, and 1 hour is vacuumized at a temperature of 120 DEG C, adds when being cooled to 70 DEG C
Rubber polymer solution, after being sufficiently mixed uniformly, adds 13.5 parts of ethyl acetate and 4.5 parts of butanone and 2 parts of toluene two different
Cyanate, reacts 0.5 hour in 80 DEG C；
(3) again toward the reactor in step (2) plus 0.8 part of 4- ethoxys oxygen ethyl -1- hydroxyethylbenzenes diether and 13.5
Part ethyl acetate and 4.5 parts of butanone, react 2 hours, add 2 parts of toluene di-isocyanate(TDI)s, 4.5 parts of ethyl acetate and 1.5 parts
Butanone, adds 3 parts of B- (3,4 epoxycyclohexyl) ethyl trimethoxy silanes, discharging to obtain the polyurethane adhesive in 40 DEG C
Host.
Claims (8)
1. reflective stretch fabric adhesive, it is characterised in that count by weight, including following component：
20～40 parts of the PEPA of molecular weight 4000
3～10 parts of the PEPA of molecular weight 2000
3～10 parts of elastic caoutchouc
3～10 parts of long chain allcyl acrylate
3～8 parts of diisocyanate
0.3～1 part of small molecule glycols
40～60 parts of organic solvent
0.5～5 part of silane coupler
0.01～0.1 part of initiator
The long chain allcyl acrylate is the acrylic acid hydroxyl ester or pentaerythritol triacrylate of caprolactone grafting；
The preparation method of described reflective stretch fabric adhesive, comprises the steps：
(1) the same weight portion of 3～10 parts of use of elastic caoutchouc weight portion organic solvent prepare mass concentration be 50% rubber it is molten
Liquid, is warming up to 75 DEG C～80 DEG C by 0.01～0.1 part of drop of 3～10 parts of long chain allcyl acrylate weight portion and initiator weight portion
Add into rubber solutions, react more than 4 hours, obtain rubber polymer solution；
(2) by 20～40 parts of the PEPA weight portion and the PEPA weight portion 3 of molecular weight 2000 of molecular weight 4000
～10 parts are put in reactor, and 1～2 hour is vacuumized at a temperature of 110～120 DEG C, are added when being cooled to 70～90 DEG C
Rubber polymer solution, after being sufficiently mixed uniformly, adds 15～20 parts of organic solvent weight portion and diisocyanate weight
1～3 part of part, reacts 0.5～1 hour in 75～80 DEG C；
(3) again toward the reactor in step (2) plus 0.3～1 part of small molecule glycol weight portion and organic solvent weight portion 15～
20 parts, react 2～3 hours, add 7～10 parts of 2～5 parts of diisocyanate weight portion and organic solvent weight portion, in 40～
50 DEG C of 0.5～5 part of silane couplers of addition, discharging.
2. reflective stretch fabric adhesive according to claim 1, it is characterised in that the polyester of the molecular weight 4000 is more
First alcohol is selected from polyadipate-BDO esterdiol, polyneopentyl glycol adipate glycol, polyadipate neopentyl glycol -1,
Any one in 4- butyl glycol ester diols or polyadipate -2- methyl propanediols-BDO esterdiol.
3. reflective stretch fabric adhesive according to claim 1, it is characterised in that the polyester of the molecular weight 2000 is more
First alcohol is selected from polyadipate -2- methyl propanediol esterdiols, polyneopentyl glycol adipate glycol or polyadipate -2- methyl-props
Any one in glycol neopentyl glycol esterdiol.
4. reflective stretch fabric adhesive according to claim 1, it is characterised in that the elastic caoutchouc is selected from butylbenzene rubber
Any one in glue, nitrile rubber, butyl rubber.
5. reflective stretch fabric adhesive according to claim 1, it is characterised in that the diisocyanate is selected from hexichol
In dicyclohexylmethane diisocyanate, hexamethylene diisocyanate, toluene di-isocyanate(TDI) it is arbitrary one or two.
6. reflective stretch fabric adhesive according to claim 1, it is characterised in that the small molecule glycol is selected from new penta
Glycol, 4- ethoxy oxygen ethyl -1- hydroxyethylbenzene diether, Isosorbide-5-Nitrae butanediol, 2- methyl -2, in 4- pentanediols any one or
Two kinds.
7. reflective stretch fabric adhesive according to claim 1, it is characterised in that the organic solvent is selected from acetic acid second
Any one in ester, toluene, butanone, dimethylformamide or two kinds.
8. reflective stretch fabric adhesive according to claim 1, it is characterised in that the silane coupler is selected from γ-contracting
Water glycerine ether oxygen propyl trimethoxy silicane, gamma-aminopropyl-triethoxy-silane, β-(3,4 epoxycyclohexyl) ethyl trimethoxy
Any one in base silane, phenylamino propyl trimethoxy silicane；The initiator is azodiisobutyronitrile or diphenyl peroxide
Formyl.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510357292.9A CN104927745B (en) | 2015-06-24 | 2015-06-24 | Adhesive for reflecting elastic fabrics and preparing method thereof |
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| CN201510357292.9A CN104927745B (en) | 2015-06-24 | 2015-06-24 | Adhesive for reflecting elastic fabrics and preparing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106479425A (en) * | 2016-08-26 | 2017-03-08 | 杭州星华反光材料股份有限公司 | A kind of adhesive of resistance to industrial washing and preparation method and application |
| CN109206569B (en) * | 2017-07-03 | 2021-01-19 | 比亚迪股份有限公司 | Waterborne polyurethane, waterborne polyurethane adhesive and preparation method thereof |
| CN109294204A (en) * | 2018-09-03 | 2019-02-01 | 安徽新恒辉反光材料有限公司 | A kind of elastic reflecting material and its preparation process |
| CN110093135A (en) * | 2019-05-14 | 2019-08-06 | 永隆高新科技(青岛)有限公司 | A kind of density board polyurethane adhesive suitable for ultralow temperature |
| CN110408330B (en) * | 2019-06-28 | 2021-11-26 | 江西盛富莱光学科技股份有限公司 | Adhesive for all-weather road beads |
| CN115612083A (en) * | 2022-02-22 | 2023-01-17 | 浙江星华反光材料有限公司 | Silane modified polyester prepolymer and preparation method thereof |
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| JP3964648B2 (en) * | 2001-10-30 | 2007-08-22 | オート化学工業株式会社 | One-part moisture-curing polyurethane adhesive and flooring adhesive method using the same |
| CN103396753B (en) * | 2013-08-15 | 2015-02-25 | 西安大天新材料有限公司 | Preparation method of hot-melt polyurethane resin for bonding material |
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Address after: 310000, Hangzhou District, Zhejiang City, Yuhang Province town of Cao Bridge Village, Lantau Peak Applicant after: HANGZHOU CHINASTARS REFLECTIVE MATERIAL Co.,Ltd. Address before: 310000, Hangzhou District, Zhejiang City, Yuhang Province town of Cao Bridge Village, Lantau Peak Applicant before: HANGZHOU CHINASTARS REFLECTIVE MATERIALS CO.,LTD. |
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Address after: 311100 Fenghuang Mountain, Caoqiao Village, Jingshan Town, Yuhang District, Hangzhou City, Zhejiang Province Patentee after: Zhejiang Xinghua New Materials Group Co.,Ltd. Address before: 310000 Fenghuang mountain, Caoqiao village, Jingshan Town, Yuhang District, Hangzhou City, Zhejiang Province Patentee before: HANGZHOU CHINASTARS REFLECTIVE MATERIAL Co.,Ltd. |
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