CN105297487A - Washing resistant adhesive and preparation method thereof - Google Patents
Washing resistant adhesive and preparation method thereof Download PDFInfo
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- CN105297487A CN105297487A CN201510807807.0A CN201510807807A CN105297487A CN 105297487 A CN105297487 A CN 105297487A CN 201510807807 A CN201510807807 A CN 201510807807A CN 105297487 A CN105297487 A CN 105297487A
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Abstract
The invention discloses a washing resistant adhesive and a preparation method thereof. The adhesive comprises the following raw materials in percentage by weight: 30.5 to 35% of polyester polyol, micromolecular polyol mixture composed of 1 to 3% of glycol and 1 to 35% of 1,4-butylene glycol, 4 to 14% of 4,4-diphenylmethane diisocyanate, 15 to 20% of 2,4-toluene diisocyanate, 20 to 45% of organic solvent namely dimethyl formamide, 0.1 to 0.3% of antioxidant (SP-10), 0.05 to 0.07% of catalyst (V-600), 3 to 5% of unsaturated polyester SK-310, and 0.5 to 1% of trimethylol propane; wherein the polyester polyol is a polyether-segmented-polyamide copolymer (PEBA) with a molecular weight of 2000, the micromolecular polyol mixture comprises glycol and 1,4-butylene glycol, and the organic solvent is dimethyl formamide. The adhesive has the characteristics of hydrolysis resistance, high peel strength, and good stability.
Description
Technical field
The invention belongs to textile auxiliary's technical field, be specifically related to a kind of water-fastness type adhesive and preparation method thereof.
Background technology
Clothes adhesion technique is a kind of gimmick conventional in clothes processing and fabricating, adhesive is occupied an leading position in the application of adhesion technique, present garment production producer adopts waterborne polyurethane resin to make adhesive usually, fabric and ventilated membrane are bonded together under uniform temperature, time, reach hydrolysis, object that peel strength is high.Polyurethane take water as the polymer of decentralized medium, have good film-forming property, excellent spring, wear-resisting, with the adhesive fastness of fabric the advantage such as high and environmental protection, be one of material of textile coating agent first-selection.But containing a large amount of hydrophilic radicals or hydrophilic segment on polyurethane segment, as the top finish of fabric, but experience repeatedly to decline the phenomenon even peeled off through often there will be peel strength after washing, does not reach certain water resistance.General employing external crosslinking method, as added the water-based polyurethane curing agent of end-blocking or aziridine type crosslinking agent to improve the resistance to water of coating, but there is short, the shortcoming such as poor storage performance, toxicity are larger in service life in the method gained polyaminoester emulsion, and could use after needing outside cross-linking agent and coating agent to allocate, complicated operation.In addition, there is certain limit in the life-span of most of MR adhesive, and some mechanically actuated performances are good, but water-fast degree significantly reduces.In order to improve better MR adhesive combination property, suitable modification need be carried out to it.This patent adds cross-linking monomer trimethylolpropane in production polyurethane resin process, and the rational formula of polyurethane polyol and isocyanates, improves hydrolysis and the peel strength of adhesive.
Summary of the invention
The object of the invention is the deficiency solving the existence of above-mentioned prior art, provides a kind of water-fastness type adhesive and preparation method thereof.
In order to solve technique scheme, the present invention adopts following technical scheme:
A kind of water-fastness type adhesive, its composition of raw materials comprises mixed polyester polyalcohol, small molecule polyol mixture, 4, 4 methyl diphenylene diisocyanates, 2, 4 toluene di-isocyanate(TDI)s, organic solvent dimethyl formamide, antioxidant (SP-10), catalyst, unsaturated polyester (UP), its raw material also comprises trimethylolpropane, described polyester polyol to be molecular weight be 2000 polyether-block-polyamide copolymer (PEBA), described small molecule polyol mixture is ethylene glycol and 1, 4 butanediols, described organic solvent is dimethyl formamide, with the total weight of adhesive, the mass content of above-mentioned each component is as follows:
Polyester polyol 30.5-35%;
Small molecule polyol mixture ethylene glycol: 1-3%1.4 butanediol 1-35%;
4,4 methyl diphenylene diisocyanate 4-14%;
2,4 toluene di-isocyanate(TDI) 15-20%;
Trimethylolpropane 0.5-1%;
Organic solvent dimethyl formamide 20-45%;
Antioxidant (SP-10) 0.1-0.3%;
Catalyst V-6000.05-0.07%;
Unsaturated polyester (UP) SK-3103-5%.
Described adhesive is obtained by following technique synthesis:
(1) polyester polyol of 80% organic solvent dimethyl formamide of formula ratio and formula ratio, small molecule polyol mixture, antioxidant (SP-10) are dropped into stirring at normal temperature in reactor and mix, stir 30 minutes to 60 minutes;
(2) equivalent divides equally 4, the 4 ditolylmethane vulcabond that three times times add formula ratio, puts in reactor every half an hour, and after adding the catalyst V-600 of formula ratio, reaction temperature controls at 70-80 DEG C, and the reaction time controls at 2h-4h;
(3) add formula ratio 2,4 toluene di-isocyanate(TDI) and trimethylolpropanes are started through step (2);
(4) start sampling and testing when viscosity in reactor arrives 30,000 CPS/25 DEG C later, after sampling viscosity reaches 8-12 ten thousand CPS/25 DEG C, add remainder 20% organic solvent of formula ratio and the unsaturated polyester (UP) of formula ratio;
(5) repetition measurement viscosity qualified stable after cooling, discharging when temperature reaches 40 DEG C-60 DEG C.
Water-fastness type adhesive of one disclosed by the invention and preparation method thereof, by the improvement of filling a prescription to resin raw material, the trimethylolpropane particularly introduced, has beneficial effect:
1, by 4,4 ditolylmethane vulcabond every half an hour equivalent divide equally three times and time add in reactor, adopt successive reaction condensation method, be convenient to control, make reaction more abundant, avoid producing too much impurity.
2, polyurethane is in film forming procedure, and hydrophilic segment is assembled gradually and formed hydrophilic microcell, and hydrone is easily adsorbed by the hydrophilic radical on strand and enters the hydrophilic microcell of glued membrane, thus causes that polyurethane laminate water imbibition is strong, resistance to water is low.The introducing of trimethylolpropane can improve the resistance to water of polyurethane laminate preferably, polyurethane laminate dissolves completely in water, along with the increase of trimethylolpropane consumption, glued membrane crosslinking degree increases, molecular hydrophobicity increases, hydrone is difficult to enter polyurethane laminate inside, and thus glued membrane water absorption rate reduces, and resistance to water improves.
3, along with the increase of cross-linking monomer TMP consumption, in polyurethane molecular, crosslinking degree increases, and the TENSILE STRENGTH of glued membrane increases gradually, and elongation at break reduces gradually, and the elasticity of polyurethane is good, improves its peel strength.
Detailed description of the invention
In conjunction with following for specific embodiments of the invention, the present invention is made further instructions:
According to the composition of raw materials of the water-fastness type adhesive of the present embodiment be:
Polyester polyol 30.5-35%, small molecule polyol mixture (ethylene glycol 1-3%, 1.4 butanediol 1-35%), 4,4 methyl diphenylene diisocyanate 4-14%, 2,4 toluene di-isocyanate(TDI) 15-20%, trimethylolpropane 0.5-1%, organic solvent dimethyl formamide 20-45%, antioxidant (SP-10) 0.1-0.3%, catalyst V-6000.05-0.07%, unsaturated polyester (UP) SK-3103-5%;
Embodiment one
Table 1 is this adhesive parameters test result
| Trimethylolpropane formula ratio used (%) | Particle diameter (nm) | Percentage of water loss (%) | Glued membrane water absorption rate (%) | Elongation at break (%) | TENSILE STRENGTH (MPa) | Resistance to hydrostatic pressure (mm) |
| 0.5 | 50 | 69 | 49 | 510 | 11.6 | 192 |
As can be seen from Table 1, by 16 parts of organic solvent dimethyl formamides and 30.5 parts of polyester polyol, 1 part of ethylene glycol, 1 part of 1.4 butanediol, 0.1 part of antioxidant (SP-10) is dropped in reactor, stir 30 minutes at normal temperatures, make it mix, add 2 part 4, 4 ditolylmethane vulcabond, 2 part 4 is added again every half an hour, 4 ditolylmethane vulcabond are put in reactor, 2 part 4 is added again after 0.5 hour, 4 ditolylmethane vulcabond and 0.05 part of rear reaction temperature of catalyst V-600 control at 70 DEG C, abundant reaction 2 hours, then 15 part 2 is added, 4 toluene di-isocyanate(TDI)s and 0.5 part of trimethylolpropane, after adding trimethylolpropane, cross-linked structure is formed with polyisocyanate reactant, the particle diameter of polyaminoester emulsion reaches 50nm, in the film forming procedure of emulsion, the percentage of water loss of glued membrane is 69%, water absorption rate is 49%, elongation at break is 510%, TENSILE STRENGTH reaches 11.6MPa, start sampling and testing when viscosity in reactor arrives 30,000 CPS/25 DEG C later, after sampling viscosity reaches 80,000 CPS/25 DEG C, add remaining 2 parts of organic solvents and 3 parts of unsaturated polyester (UP)s, repetition measurement viscosity qualified stable after obtain water-fastness type adhesive disclosed in this invention when cooling to 40 DEG C, its resistance to hydrostatic pressure is 192mm.
Embodiment two
Table 2 is this adhesive parameters test result
| Trimethylolpropane formula ratio used (%) | Particle diameter (nm) | Percentage of water loss (%) | Glued membrane water absorption rate (%) | Elongation at break (%) | TENSILE STRENGTH (MPa) | Resistance to hydrostatic pressure (mm) |
| 0.7 | 55 | 86 | 34 | 470 | 12.8 | 239 |
As can be seen from Table 2, by 24 parts of organic solvent dimethyl formamides and 35 parts of polyester polyol, 2 parts of ethylene glycol, 10 part of 1.4 butanediol, 0.1 part of antioxidant (SP-10) is dropped in reactor, stir 45 minutes at normal temperatures, make it mix, add 2 part 4, 4 ditolylmethane vulcabond, 2 part 4 is added again every half an hour, 4 ditolylmethane vulcabond are put in reactor, 2 part 4 is added again after 0.5 hour, 4 ditolylmethane vulcabond and 0.06 part of rear reaction temperature of catalyst V-600 control at 70 DEG C, abundant reaction 2 hours, then 15 part 2 is added, 4 toluene di-isocyanate(TDI)s and 0.7 part of trimethylolpropane, after adding trimethylolpropane, cross-linked structure is formed with polyisocyanate reactant, the particle diameter of polyaminoester emulsion reaches 55nm, in the film forming procedure of emulsion, the percentage of water loss of glued membrane is 86%, water absorption rate is 34%, elongation at break is 470%, TENSILE STRENGTH reaches 12.8MPa, start sampling and testing when viscosity in reactor arrives 30,000 CPS/25 DEG C later, after sampling viscosity reaches 80,000 CPS/25 DEG C, add remaining 6 parts of organic solvents and 3 parts of unsaturated polyester (UP)s, repetition measurement viscosity qualified stable after obtain water-fastness type adhesive disclosed in this invention when cooling to 40 DEG C, its resistance to hydrostatic pressure is 239mm.
Embodiment three
Table 3 is this adhesive parameters test result
| Trimethylolpropane formula ratio used (%) | Particle diameter (nm) | Percentage of water loss (%) | Glued membrane water absorption rate (%) | Elongation at break (%) | TENSILE STRENGTH (MPa) | Resistance to hydrostatic pressure (mm) |
| 1.0 | 60 | 74 | 45 | 400 | 13.4 | 210 |
As can be seen from Table 3, by 24 parts of organic solvent dimethyl formamides and 35 parts of polyester polyol, 2.5 parts of ethylene glycol, 12 part of 1.4 butanediol, 0.3 part of antioxidant (SP-10) is dropped in reactor, stir 60 minutes at normal temperatures, make it mix, add 2 part 4, 4 ditolylmethane vulcabond, 2 part 4 is added again every half an hour, 4 ditolylmethane vulcabond are put in reactor, 2 part 4 is added again after 0.5 hour, 4 ditolylmethane vulcabond and 0.06 part of rear reaction temperature of catalyst V-600 control at 75 DEG C, abundant reaction 2 hours, then 15 part 2 is added, 4 toluene di-isocyanate(TDI)s and 1 part of trimethylolpropane, after adding trimethylolpropane, cross-linked structure is formed with polyisocyanate reactant, the particle diameter of polyaminoester emulsion reaches 60nm, in the film forming procedure of emulsion, the percentage of water loss of glued membrane is 74%, water absorption rate is 45%, elongation at break is 400%, TENSILE STRENGTH reaches 13.4MPa, start sampling and testing when viscosity in reactor arrives 30,000 CPS/25 DEG C later, after sampling viscosity reaches 100,000 CPS/25 DEG C, add remaining 2 parts of organic solvents and 5 parts of unsaturated polyester (UP)s, repetition measurement viscosity qualified stable after obtain water-fastness type adhesive disclosed in this invention when cooling to 40 DEG C, its resistance to hydrostatic pressure is 210mm.
Comparative example one
Table 4 is contrast adhesive parameters test result
| Trimethylolpropane formula ratio used (%) | Particle diameter (nm) | Percentage of water loss (%) | Glued membrane water absorption rate (%) | Elongation at break (%) | TENSILE STRENGTH (MPa) | Resistance to hydrostatic pressure (mm) |
| 0 | 40 | 50 | 76 | 580 | 10.9 | 172 |
As can be seen from Table 4, by 16 parts of organic solvent dimethyl formamides and 30.5 parts of polyester polyol, 1 part of ethylene glycol, 1 part of 1.4 butanediol, 0.1 part of antioxidant (SP-10) is dropped in reactor, stir 30 minutes at normal temperatures, make it mix, add 2 part 4, 4 ditolylmethane vulcabond, 2 part 4 is added again every half an hour, 4 ditolylmethane vulcabond are put in reactor, 2 part 4 is added again after 0.5 hour, 4 ditolylmethane vulcabond and 0.05 part of rear reaction temperature of catalyst V-600 control at 70 DEG C, abundant reaction 2 hours, then 15 part 2 is added, 4 toluene di-isocyanate(TDI)s, the particle diameter of polyaminoester emulsion reaches 40nm, in the film forming procedure of emulsion, the percentage of water loss of glued membrane is 50%, water absorption rate is 76%, elongation at break is 580%, TENSILE STRENGTH reaches 10.9MPa, start sampling and testing when viscosity in reactor arrives 30,000 CPS/25 DEG C later, after sampling viscosity reaches 80,000 CPS/25 DEG C, add remaining 2 parts of organic solvents and 3 parts of unsaturated polyester (UP)s, repetition measurement viscosity qualified stable after obtain water-fastness type adhesive disclosed in this invention when cooling to 40 DEG C, its resistance to hydrostatic pressure is 172mm.
Comparative example two
Table 5 is contrast adhesive parameters test result
| Trimethylolpropane formula ratio used (%) | Particle diameter (nm) | Percentage of water loss (%) | Glued membrane water absorption rate (%) | Elongation at break (%) | TENSILE STRENGTH (MPa) | Resistance to hydrostatic pressure (mm) |
| 1.3 | 86 | 53 | 40 | 320 | 14.5 | 220 |
As can be seen from Table 5, by 24 parts of organic solvent dimethyl formamides and 35 parts of polyester polyol, 2 parts of ethylene glycol, 10 part of 1.4 butanediol, 0.1 part of antioxidant (SP-10) is dropped in reactor, stir 45 minutes at normal temperatures, make it mix, add 2 part 4, 4 ditolylmethane vulcabond, 2 part 4 is added again every half an hour, 4 ditolylmethane vulcabond are put in reactor, 2 part 4 is added again after 0.5 hour, 4 ditolylmethane vulcabond and 0.06 part of rear reaction temperature of catalyst V-600 control at 70 DEG C, abundant reaction 2 hours, then 15 part 2 is added, 4 toluene di-isocyanate(TDI)s and 1.3 parts of trimethylolpropanes, after adding trimethylolpropane, cross-linked structure is formed with polyisocyanate reactant, the particle diameter of polyaminoester emulsion reaches 86nm, in the film forming procedure of emulsion, the percentage of water loss of glued membrane is 53%, water absorption rate is 40%, elongation at break is 320%, TENSILE STRENGTH reaches 14.5MPa, start sampling and testing when viscosity in reactor arrives 30,000 CPS/25 DEG C later, after sampling viscosity reaches 80,000 CPS/25 DEG C, add remaining 6 parts of organic solvents and 3 parts of unsaturated polyester (UP)s, repetition measurement viscosity qualified stable after obtain water-fastness type adhesive disclosed in this invention when cooling to 40 DEG C, its resistance to hydrostatic pressure is 220mm.
Table 6 is this adhesive and the contrast list contrasting adhesive parameters
Can obtain upper table 6 by embodiment and comparative example, along with the increase of trimethylolpropane consumption, stability of emulsion is deteriorated, and particle diameter becomes large, and film forming speed is slow, and glued membrane water absorption rate diminishes, and the TENSILE STRENGTH of glued membrane increases gradually, and elongation at break reduces gradually.When not adding trimethylolpropane, obtained polyurethane molecular is linear molecule, and its TENSILE STRENGTH is little, elongation at break is large.When cross-linking monomer TMP consumption is less than 0.7%, along with the increase of trimethylolpropane consumption, in polyurethane molecular, crosslinking degree increases, the little and distribution relative narrower of particle diameter, and show as stability better, the TENSILE STRENGTH of glued membrane increases gradually, and elongation at break declines gradually; When 1.3%, the cross-linked structure of polyurethane system increases, crosslinking degree increases, and emulsion is unstable, causes the dispersive property of emulsion to be deteriorated, particle diameter increases, domain size distribution broadens, and polyurethane molecular quality becomes large, shows as that TENSILE STRENGTH sharply increases, elongation at break sharply reduces, lose the due elasticity of polyurethane, be unfavorable for the application of polyurethane on fabric coating.And when selecting the trimethylolpropane of 0.7%, polyaminoester emulsion particle diameter is little, stability is better, and film forming speed is fast, and elastic polyurethane is better, and water-fastness, peel strength improves further.
The above, be only preferred embodiment of the present invention, not does any pro forma restriction to the present invention; The those of ordinary skill of all industry all can implement the present invention described in by specification swimmingly; But all those skilled in the art are not departing within the scope of technical solution of the present invention, disclosed above technology contents can be utilized and make a little change, modify with differentiation equivalent variations, be Equivalent embodiments of the present invention; Meanwhile, all according to substantial technological of the present invention to the change of any equivalent variations that above embodiment is done, modify and differentiation etc., within the protection domain all still belonging to technical scheme of the present invention.
Claims (2)
1. a water-fastness type adhesive, it is characterized in that, its composition of raw materials comprises mixed polyester polyalcohol, small molecule polyol mixture, 4, 4 methyl diphenylene diisocyanates, 2, 4 toluene di-isocyanate(TDI)s, organic solvent, antioxidant (SP-10), catalyst, unsaturated polyester (UP), its raw material also comprises trimethylolpropane, described polyester polyol to be molecular weight be 2000 polyether-block-polyamide copolymer (PEBA), described small molecule polyol mixture is ethylene glycol and 1, 4 butanediols, described organic solvent is dimethyl formamide, with the total weight of adhesive, the mass content of above-mentioned each component is as follows:
Polyester polyol 30.5-35%;
Small molecule polyol mixture ethylene glycol: 1-3%1.4 butanediol 1-3.5%;
4,4 methyl diphenylene diisocyanate 4-14%;
2,4 toluene di-isocyanate(TDI) 15-20%;
Trimethylolpropane 0.5-1%;
Organic solvent dimethyl formamide 20-45%;
Antioxidant (SP-10) 0.1-0.3%;
Catalyst V-6000.05-0.07%;
Unsaturated polyester (UP) SK-3103-5%.
2. the preparation method of a kind of water-fastness type adhesive according to claim 1, is characterized in that, comprise the following steps:
1) polyester polyol of 80% organic solvent dimethyl formamide of formula ratio and formula ratio, small molecule polyol mixture, antioxidant (SP-10) are dropped into stirring at normal temperature in reactor and mix, stir 30 minutes to 60 minutes;
(2) equivalent divides equally 4, the 4 ditolylmethane vulcabond that three times times add formula ratio, puts in reactor every half an hour, and after adding the catalyst V-600 of formula ratio, reaction temperature controls at 70-80 DEG C, and the reaction time controls at 2h-4h;
(3) add formula ratio 2,4 toluene di-isocyanate(TDI) and trimethylolpropanes are started through step (2);
(4) start sampling and testing when viscosity in reactor arrives 30,000 CPS/25 DEG C later, after sampling viscosity reaches 8-12 ten thousand CPS/25 DEG C, add remainder 20% organic solvent of formula ratio and the unsaturated polyester (UP) of formula ratio;
(5) repetition measurement viscosity qualified stable after cooling, discharging when temperature reaches 40 DEG C-60 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105821681A (en) * | 2016-05-12 | 2016-08-03 | 东莞市联洲知识产权运营管理有限公司 | Preparation method of low-cost environment-friendly fabric adhesive |
| CN106590504A (en) * | 2016-11-18 | 2017-04-26 | 浙江工业大学之江学院 | Washable and durable polyurethane adhesive composition and preparation method thereof |
| CN114525692A (en) * | 2020-11-23 | 2022-05-24 | 财团法人纺织产业综合研究所 | Humidity sensitive ink |
| CN115746763A (en) * | 2022-12-06 | 2023-03-07 | 深圳市东升塑胶制品有限公司 | Modified epoxy adhesive, preparation method thereof, prepreg and flexible copper clad laminate |
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| CN115746763A (en) * | 2022-12-06 | 2023-03-07 | 深圳市东升塑胶制品有限公司 | Modified epoxy adhesive, preparation method thereof, prepreg and flexible copper clad laminate |
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Application publication date: 20160203 |