CN103965822A - Epoxy modified moisture curing polyurethane hot melt adhesive for compounding fabrics - Google Patents
Epoxy modified moisture curing polyurethane hot melt adhesive for compounding fabrics Download PDFInfo
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- CN103965822A CN103965822A CN201410193048.9A CN201410193048A CN103965822A CN 103965822 A CN103965822 A CN 103965822A CN 201410193048 A CN201410193048 A CN 201410193048A CN 103965822 A CN103965822 A CN 103965822A
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Abstract
The invention discloses an epoxy modified moisture curing polyurethane hot melt adhesive for compounding fabrics. The epoxy modified moisture curing polyurethane hot melt adhesive for compounding the fabrics is characterized by comprising the following components according to the mass content: 46 parts of polyether polyol, 22 parts of polyester polyol, 0.5 part of epoxy resin, 0.4 part of an antioxidant, 16 to 18 parts of tackifying resin, 13 to 14 parts of 4, 4'-diphenylmethane diisocyanate (MDI), 0.1 part of a catalyst, 0 to 0.5 part of a chain extender and 0 to 1.5 parts of a silane coupling agent. The preparation of the epoxy modified moisture curing polyurethane hot melt adhesive comprises the following steps of: (1) selecting raw materials; (2) mixing polyol with the antioxidant, and dehydrating for 0.5 hour; (3) increasing the tackifying resin and dehydrating for 1.5 hours; (4) adding MDI and the catalyst at the temperature of 87 DEG C and reacting for 70 minutes at the temperature of 85 to 90 DEG C; (5) adding 1,4-butanediol, and reacting for 50 minutes; (6) adding the silane coupling agent at the temperature of 70 to 80 DEG C, and reacting for 1 hour; (7) under the protection of nitrogen, discharging and carrying out sealed package. The epoxy modified moisture curing polyurethane hot melt adhesive for compounding the fabrics disclosed by the invention has the advantages of high peel intensity, good initial adhesion, short opening time, good hydrolysis resistance performance, environmental protection and the like.
Description
Technical field
The present invention relates to that a kind of fabric is compound uses epoxide modified moisture-curable polyurethane hot melt adhesive.
Background technology
Moisture-curable polyurethane hot melt adhesive (hereinafter to be referred as PUR) is the polyurethane adhesive of a class containing end-NCO group.When use, heating and melting applying glue, produces after preliminary bonding force until the cooling physical solidification of glue-line, and the end NCO in glue-line reacts with the active hydrogen compounds on airborne moisture or adherend surface again, produces chemically crosslinked and solidifies.Moisture-curable polyurethane hot melt adhesive not only has the quick cemented in place of traditional thermoplasticity hot melt adhesive, higher initial adhesive strength advantage is provided, and also further curing cross-linked, can be significantly improved bonding force, the cohesive strength etc. of glue-line.Therefore, moisture-curable polyurethane hot melt adhesive be widely used in that textiles is compound, rubber, plastics, metal and automobile making, textile industry, shoe industry, adhesive bookbinding, timber industry and furniture industry, electron trade etc. bonding.It is compound that moisture-curable polyurethane hot melt adhesive prepared by the present invention is mainly used in fabric.Fabric is compound to be had and just glues preferably and whole stripping strength, good anti-hydrolytic performance and flexibility with PUR requirement.
PUR has two kinds of full polyether-type performed polymer class and whole polyester type performed polymer classes.The polyurethane hot melt adhesive of full polyether-type has that melt viscosity is low, melt viscosity good stability, water-tolerant, low cost and other advantages, but just sticky and eventually sticky intensity is lower; And the polyurethane hot melt adhesive of whole polyester has well just sticky and whole stripping strength, but anti-hydrolytic performance is poor, snappiness is poor; Particularly also a difficult problem to sticky the bonding of fabric of difficulty.In order to overcome the above problems, advantage of the present invention is, adopt the polyol blend raw material of polyether glycol and polyester polyol to have the advantage of polyether-type moisture-curable polyurethane hot melt adhesive and polyester type moisture curing reactive polyurethane hot melt concurrently, the tackifying resin adding is to glue at the beginning of acrylic resin can play increase, epoxy resin can improve the stripping strength of sizing agent, and add silane coupling agent to carry out modification, the sticky fabric of difficulty is had to good wettability, be conducive to difficulty to glue the bonding of fabric, also there is good flexibility.
Summary of the invention
One of object of the present invention is to provide in order to solve above-mentioned technical problem that a kind of fabric is compound uses epoxide modified moisture-curable polyurethane hot melt adhesive.
Two of object of the present invention is to provide the preparation method of the above-mentioned epoxide modified moisture-curable polyurethane hot melt adhesive of the compound use of a kind of fabric.
A preparation method for the epoxide modified moisture-curable polyurethane hot melt adhesive of the compound use of fabric, is characterized in that comprising the steps:
(1) polyether glycol, polyester polyol, epoxy resin, oxidation inhibitor are uniformly mixed, are heated to 120 DEG C of left and right, the 0.5h that dewaters under absolute pressure is less than 100Pa, described epoxy resin is selected from bisphenol A type epoxy resin;
(2) in the product of step (1), add tackifying resin, continue to be warming up to 135-140 DEG C, under absolute pressure is less than 100Pa, dehydration 1.5h;
(3) product of step (2) is cooled to 87 DEG C, adds MDI and catalyzer, stir, be less than under 100KPa, temperature of reaction 85-90 DEG C condition and react 70min in absolute pressure;
(4) in the product of step (3), add chainextender, be less than continuation reaction 50min at 100Pa, temperature of reaction 85-90 DEG C in absolute pressure;
(5) product of step (4) is cooled to 70-80 DEG C, add silane coupling agent, be less than at 100Pa, temperature of reaction 70-80 DEG C and continue reaction 1 hour in absolute pressure, be then warming up to 85-100 DEG C, quickly discharging being packaged in aluminium foil bag under nitrogen protection;
(6) product of step (5) is placed in to the baking oven slaking 4h of 80-85 DEG C, obtains object product;
Taking 100 parts of products as benchmark, described each constituent mass content is respectively: 46 parts of polyether glycols, 22 parts of polyester polyols, 0.5 part of epoxy resin, 0.4 part, oxidation inhibitor, tackifying resin 15-18 part, (MDI) 13-14 part, 0.1 part of catalyzer, 0.5 part of chainextender, silane coupling agent 0-1.5 part;
Described MDI is 4,4 '-diphenylmethanediisocyanate.
The bisphenol A type epoxy resin of the preferred epoxy equivalent (weight) 210～240g/mol of described epoxy resin, addition is gross weight 0.5%.
Described polyester polyol, for poly-hexanodioic acid BDO esterdiol and polyneopentyl glycol adipate glycol, calculates in mass ratio, poly-hexanodioic acid BDO esterdiol: polyneopentyl glycol adipate glycol is 1:1.。
Described catalyzer is stannous octoate.
Described chainextender is BDO, and its mass content is 0.5%.
Described silane coupling agent is selected from γ-methacryloxypropyl trimethoxy silane, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane and γ-aminopropyl triethoxysilane, and its mass content is 0-1.5%.
Beneficial effect of the present invention
Moisture-curable polyurethane hot melt adhesive prepared by the present invention adopts the polyol blend raw material of polyether glycol and polyester polyol, the moisture-curable polyurethane hot melt adhesive that makes like this present invention prepare has the advantage of polyether-type moisture-curable polyurethane hot melt adhesive and polyester type moisture curing reactive polyurethane hot melt concurrently: melt viscosity good stability, water-tolerant, cost is low, just sticky and eventually sticky intensity is good, snappiness is better, the tackifying resin adding is that acrylic resin can play increase sticky intensity at first bonding end, add epoxy resin can significantly improve the stripping strength of sizing agent, add silane coupling agent to carry out modification, the sticky fabric of difficulty is had to good wettability, be conducive to difficulty to glue the bonding of fabric, also there is good flexibility.Moisture-curable polyurethane hot melt adhesive prepared by the present invention, be applied to textiles compound in, be 5 g/m in grammes per square metre
2time stripping strength better, through 5 times washing after do not come unglued, concrete outcome, in table 1, has met the performance requriements of difficult sticky fabric to PUR glue well.
Embodiment
Below by embodiment, the present invention is further set forth, but do not limit the present invention.。
The raw material information relating in various embodiments of the present invention is as follows:
4,4 '-diphenylmethanediisocyanate (MDI): water white solid, pure MDI;
Tackifying resin BR-113: white powder, i.e. acrylic resin;
Polyether glycol: colourless viscous liquid, polyoxypropyleneglycol, is called for short PPG, molecular weight 4000;
Polyester polyol 3000H: white solid, poly-hexanodioic acid-1,6-hexylene glycol esterdiol, molecular weight 3000;
Polyester polyol 2000N: colourless viscous liquid, polyneopentyl glycol adipate glycol, molecular weight 2000;
Epoxy resin: colourless viscous liquid, epoxy equivalent (weight) 210～240g/mol;
Antioxidant 1010: four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, i.e. antioxidant 1010, white crystalline powder, fusing point: 110.0-125.0 DEG C, transmittance: 425nm >=90%, 500nm >=95%;
The positive octadecanol ester of antioxidant 1076: β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid, white powder or particle, fusing point 50-55 DEG C, ash content <0.10%, volatile matter <0.50%, transmittance: 425nm >=96%, 500nm >=98%; Content is greater than 98%;
The sub-tin of octoate catalyst: pale yellow oily liquid body, dissolve in polyalcohols and most of organic solvent, be insoluble to alcohol and water, sub-tin content (accounting for total tin amount) is more than 96%, tin content: 28% ± 0.5%, and viscosity (20 DEG C) :≤500mPa.s, density (25 DEG C): (1.25 ± 0.02) g/cm3, specific refractory power (20 DEG C): 1.495 ± 0.005, zero pour :-25 DEG C, flash-point: 142 DEG C;
Silane coupling agent: trade mark Z-6030, Chinese name γ-methacryloxypropyl trimethoxy silane, this product is colourless to light yellow transparent liquid, fusing point is-48 DEG C, 190 DEG C of boiling points, density p 201.045g/cm
3, refractive index n
d 201.431.Be dissolved in organic solvent, alcohol, benzene, toluene etc., water insoluble, in the sour water that is 4-5 in pH value, be hydrolyzed into silanol.
embodiment 1
A kind of textiles is compound with moisture-curable polyurethane hot melt adhesive, get by weight percentage following composition: 46 parts of polyether glycols, 22 parts of polyester polyols (comprise poly-hexanodioic acid-1,11 parts of 6 11 parts of hexylene glycol esterdiols and polyneopentyl glycol adipate glycol), 0.4 part, oxidation inhibitor, 16 parts of tackifying resins, 4,14.0 parts of 4 '-diphenylmethanediisocyanates (MDI), 0.1 part of catalyzer (comprising 0.05 part of stannous octoate and DMDEE0.05 part), 1.5 parts of silane coupling agents.
Preparation process is as follows:
(1) polyether glycol, polyester polyol, oxidation inhibitor are uniformly mixed, are heated to 120 DEG C of left and right, under absolute pressure is less than 100Pa, dehydration 0.5h;
(2) add tackifying resin, continue to be warming up to 135-140 DEG C, under absolute pressure is less than 100Pa, dehydration 1.5h;
(3) be cooled to 87 DEG C, add 4,4 '-diphenylmethanediisocyanate (MDI), catalyzer, stir, and is less than at 100Pa, 85-90 DEG C and reacts 2h in absolute pressure;
(4) be cooled to 70-80 DEG C, add silane coupling agent, be less than at 100Pa, temperature of reaction 70-80 DEG C and continue to react 1 hour in absolute pressure;
(5) keep drop temperature at 85-100 DEG C, quickly discharging being packaged in aluminium foil bag under nitrogen protection;
(6) package after in the baking oven of 80-85 DEG C slaking 4h, obtain product A.
embodiment 2
A kind of textiles is compound with moisture-curable polyurethane hot melt adhesive, get by weight percentage following composition: 46 parts of polyether glycols, 22 parts of polyester polyols (comprising poly-hexanodioic acid-1,11 parts of 6 11 parts of hexylene glycol esterdiols and polyneopentyl glycol adipate glycol), 0.4 part, oxidation inhibitor, 18 parts of tackifying resins, 4,13 parts of 4 '-diphenylmethanediisocyanates (MDI), 0.1 part of catalyzer (comprising 0.05 part of stannous octoate and DMDEE0.05 part), 0.5 part of chainextender BDO.
Its preparation process is as follows.
(1) polyether glycol, polyester polyol, oxidation inhibitor are uniformly mixed, are heated to 120 DEG C of left and right, under absolute pressure is less than 100Pa, dehydration 0.5h;
(2) add tackifying resin, continue to be warming up to 135-140 DEG C, under absolute pressure is less than 100Pa, dehydration 1.5h;
(3) be cooled to 87 DEG C, add 4,4 '-diphenylmethanediisocyanate (MDI), catalyzer, stir, and is less than at 100Pa, 85-90 DEG C and reacts 70min in absolute pressure;
(4) add chainextender, be less than continuation reaction 50min at 100Pa, temperature of reaction 85-90 DEG C in absolute pressure;
(5) keep drop temperature at 85-100 DEG C, quickly discharging being packaged in aluminium foil bag under nitrogen protection;
(6) package after in the baking oven of 80-85 DEG C slaking 4h, obtain product B.
embodiment 3
A kind of textiles is compound with moisture-curable polyurethane hot melt adhesive, get by weight percentage following composition: 46 parts of polyether glycols, 22 parts of polyester polyols (comprise poly-hexanodioic acid-1,11 parts of 6 11 parts of hexylene glycol esterdiols and polyneopentyl glycol adipate glycol), 0.4 part, oxidation inhibitor, 17 parts of tackifying resins, 4,14 parts of 4 '-diphenylmethanediisocyanates (MDI), 0.1 part of catalyzer (comprising 0.5 part of stannous octoate and DMDEE0.5 part).
Its preparation process is as follows:
(1) polyether glycol, polyester polyol, oxidation inhibitor are uniformly mixed, are heated to 120 DEG C of left and right, under absolute pressure is less than 100Pa, dehydration 0.5h;
(2) add tackifying resin, continue to be warming up to 135-140 DEG C, under absolute pressure is less than 100Pa, dehydration 1.5h;
(3) be cooled to 87 DEG C, add 4,4 '-diphenylmethanediisocyanate (MDI), catalyzer, stir, and is less than at 100Pa, 85-90 DEG C and reacts 2h in absolute pressure;
(4) keep drop temperature at 85-100 DEG C, quickly discharging being packaged in aluminium foil bag under nitrogen protection;
(5) package after in the baking oven of 80-85 DEG C slaking 4h, obtain products C.
application Example
The textiles of the above embodiments gained compound with the technical parameter of moisture-curable polyurethane hot melt adhesive in table 1, the compound application in fabric is compound with moisture-curable polyurethane hot melt adhesive of textiles, its application method comprises the steps:
Respectively compound the fabric of above-described embodiment gained heating at the temperature of 120 DEG C with moisture-curable polyurethane hot melt adhesive product then coated on TUP air-permeable envelope with the cylinder in 0.2 μ m aperture, then with 20% polyester fabric (difficult sticky fabric) carries out compound, then by the cloth after compound with carrying out hot pressure (70 DEG C of fusing conditions, 1.5kgf/cm under pressing machine
2pressure, 8s), be placed in 20 DEG C, the constant-temperature constant-humidity environment of humidity 70% and place 48h.Then cloth is cut into the cloth of wide 5cm, long 10cm, detect its grammes per square metre (quality of the contained glue of unit surface cloth), test its stripping strength, through washing (30 DEG C of washing 40min 5 times, dry 30 minutes for 40 DEG C, this is one-period, and each washing all adds washing powder 10g) after test again its stripping strength, concrete outcome is in table 1.
Table 1 fabric compound performance perameter and application test result with moisture-curable polyurethane hot melt adhesive
Note: 30 DEG C of washing 40min (each washing all adds washing powder), dry 30min for 40 DEG C, and this process is once complete water washing process.
Be product A, B, the C that the present invention manufactures from table 1 data, and the performance comparison of external product D, E, be 5 g/m in grammes per square metre
2time stripping strength better, through 5 times washing after do not come unglued, stripping strength is good compared with external product, has well met the performance requriements of difficult sticky fabric to PUR glue.
Above said content is only the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (6)
1. a preparation method for the epoxide modified moisture-curable polyurethane hot melt adhesive of the compound use of fabric, is characterized in that comprising the steps:
(1) polyether glycol, polyester polyol, epoxy resin, oxidation inhibitor are uniformly mixed, are heated to 120 DEG C of left and right, the 0.5h that dewaters under absolute pressure is less than 100Pa, described epoxy resin is selected from bisphenol A type epoxy resin;
(2) in the product of step (1), add tackifying resin, continue to be warming up to 135-140 DEG C, under absolute pressure is less than 100Pa, dehydration 1.5h;
(3) product of step (2) is cooled to 87 DEG C, adds MDI and catalyzer, stir, be less than under 100KPa, temperature of reaction 85-90 DEG C condition and react 70min in absolute pressure;
(4) in the product of step (3), add chainextender, be less than continuation reaction 50min at 100Pa, temperature of reaction 85-90 DEG C in absolute pressure;
(5) product of step (4) is cooled to 70-80 DEG C, add silane coupling agent, be less than at 100Pa, temperature of reaction 70-80 DEG C and continue reaction 1 hour in absolute pressure, be then warming up to 85-100 DEG C, quickly discharging being packaged in aluminium foil bag under nitrogen protection;
(6) product of step (5) is placed in to the baking oven slaking 4h of 80-85 DEG C, obtains object product;
Taking 100 parts of products as benchmark, described each constituent mass content is respectively: 46 parts of polyether glycols, 22 parts of polyester polyols, 0.5 part of epoxy resin, 0.4 part, oxidation inhibitor, tackifying resin 15-18 part, (MDI) 13-14 part, 0.1 part of catalyzer, 0.5 part of chainextender, silane coupling agent 0-1.5 part;
Described MDI is 4,4 '-diphenylmethanediisocyanate.
2. a kind of fabric as claimed in claim 1 is compound uses epoxide modified moisture-curable polyurethane hot melt adhesive, it is characterized in that, and the bisphenol A type epoxy resin of the preferred epoxy equivalent (weight) 210～240g/mol of described epoxy resin, addition is gross weight 0.5%.
3. a kind of fabric as claimed in claim 1 is compound uses epoxide modified moisture-curable polyurethane hot melt adhesive, it is characterized in that, described polyester polyol is poly-hexanodioic acid 1,4-butanediol ester glycol and polyneopentyl glycol adipate glycol, calculate in mass ratio, poly-hexanodioic acid BDO esterdiol: polyneopentyl glycol adipate glycol is 1:1.
4. a kind of fabric as claimed in claim 1 is compound uses epoxide modified moisture-curable polyurethane hot melt adhesive, it is characterized in that described catalyzer is stannous octoate.
5. a kind of fabric as claimed in claim 1 is compound uses epoxide modified moisture-curable polyurethane hot melt adhesive, it is characterized in that described chainextender is BDO, and its mass content is 0.5%.
6. a kind of fabric as claimed in claim 1 is compound uses epoxide modified moisture-curable polyurethane hot melt adhesive, it is characterized in that described silane coupling agent is selected from γ-methacryloxypropyl trimethoxy silane, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane and γ-aminopropyl triethoxysilane, its mass content is 0-1.5%.
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| CN104610902A (en) * | 2015-02-12 | 2015-05-13 | 厦门誉匠复合材料有限公司 | Rapidly post-cured polyurethane hot melt adhesive and preparation method thereof |
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| CN107090268A (en) * | 2017-06-09 | 2017-08-25 | 南通恒华粘合材料科技有限公司 | Fabric is compound with high moisture-inhibiting monocomponent polyurethane hot melt adhesive and preparation method thereof |
| CN110218546A (en) * | 2019-06-20 | 2019-09-10 | 佛山南宝高盛高新材料有限公司 | A kind of Halogen is from flame retardant polyurethane hot melt adhesive and preparation method thereof |
| CN110845983A (en) * | 2019-12-19 | 2020-02-28 | 万果新材料科技(上海)有限公司 | Epoxy modified polyurethane hot melt adhesive and preparation method thereof |
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| CN110218546A (en) * | 2019-06-20 | 2019-09-10 | 佛山南宝高盛高新材料有限公司 | A kind of Halogen is from flame retardant polyurethane hot melt adhesive and preparation method thereof |
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| CN110845983A (en) * | 2019-12-19 | 2020-02-28 | 万果新材料科技(上海)有限公司 | Epoxy modified polyurethane hot melt adhesive and preparation method thereof |
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Application publication date: 20140806 |