CN103045152A - Reactive polyurethane hot-melt adhesive for fastening tape and preparation method thereof - Google Patents
Reactive polyurethane hot-melt adhesive for fastening tape and preparation method thereof Download PDFInfo
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- CN103045152A CN103045152A CN201310020819XA CN201310020819A CN103045152A CN 103045152 A CN103045152 A CN 103045152A CN 201310020819X A CN201310020819X A CN 201310020819XA CN 201310020819 A CN201310020819 A CN 201310020819A CN 103045152 A CN103045152 A CN 103045152A
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- melt adhesive
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Abstract
The invention relates to a reactive polyurethane hot-melt adhesive for a fastening tape and a preparation method thereof and particularly relates to the reactive polyurethane hot-melt adhesive for compounding the fastening tape, belonging to the field of polyurethane hot-melt adhesives. According to the preparation method of the reactive polyurethane hot-melt adhesive, amorphous polyester, crystalline polyester and tackifying resin are mixed, vacuumized and dehydrated, isocyanate is then added, and vacuum heating is carried out, thereby obtaining a product, i.e. the reactive polyurethane hot-melt adhesive for the fastening tape. According to the reactive polyurethane hot-melt adhesive and the preparation method of the reactive polyurethane hot-melt adhesive, the disadvantages in the prior art are overcome; and the reactive polyurethane hot-melt adhesive has high initial-stage strength and good soft handfeel, maintains an original transparent visual effect for adhering of transparent materials, and meanwhile, has an excellent adhering effect for polyamide (PA).
Description
Technical field
The present invention relates to a kind of magic tape with reaction type polyurethane hot-melt adhesive and preparation method thereof, particularly be used for the compound reactive polyurethane hot melt of magic tape, belong to the polyurethane hot melt field.
Background technology
Reactive polyurethane hot melt be for people known for a long time, it refers to the solvent-free Hotmelt Adhesive that contains isocyanate groups, at room temperature be solid-state, use after the melting at a certain temperature, in moisture, not only can cool off and solidify by physics, also can react and crosslinking curing by isocyanate groups and the aqueous vapor that exists.
Yet this reactive hot-melt has very large application limitation.The magic tape compounding technology can require certain early strength usually, and simultaneously the magic tape base material is polyamide (PA), at present known moisture-reactive polyurethane hot-melt glue be do not have resultful.
Summary of the invention
The purpose of this invention is to provide a kind of suitable reactive polyurethane hot melt, it overcomes existing technical disadvantages and has higher early strength, for polyamide (PA) excellent bond effect is arranged simultaneously.
According to technical scheme provided by the invention, the magic tape reaction type polyurethane hot-melt adhesive, formula rate is as follows by weight: 10 ~ 40 parts of isocyanic ester, 30 ~ 60 parts of amorphous polyesters, 30 ~ 60 parts of crystal type polyester, 5 ~ 15 parts of tackifying resins;
Amorphous polyester, crystal type polyester, tackifying resin mixing are vacuumized dehydration, add again the isocyanic ester heating under vacuum and namely get product magic tape reaction type polyurethane hot-melt adhesive.
Isocyanic ester is the isocyanic ester of two functionality preferably, particularly preferably be aromatic diisocyanate, concrete enforcement comprises: tolylene diisocyanate, methyl diphenylene diisocyanate and composition thereof, diphenyl diisocyanate refers to 4,4 '-2,4 '-and 2,2 '-methyl diphenylene diisocyanate and composition thereof, the methyl diphenylene diisocyanate of carbodiimide modified.Preferred one or both isocyanic ester, particularly preferred 4,4 ' methyl diphenylene diisocyanate (pure MDI).The component of isocyanic ester should be 10% ~ 40%(weight in the present embodiment), preferred 10% ~ 25%(weight).
Amorphous polyester refers to that diprotic acid and dibasic alcohol polycondensation form the polymkeric substance that end group is two OH groups.Its composition: acid is hexanodioic acid, sebacic acid, toxilic acid, fumaric acid, terephthalic acid, m-phthalic acid, one or more of phthalic acid, alcohol is 1,2-ethandiol, 1,3 butylene glycol, 1, the 4-butyleneglycol, 1,5-PD, glycol ether, one or more of neopentyl alcohol.Its molecular-weight average is 1000 ~ 8000, and is preferred 2000 ~ 8000, and particularly preferably 3000 ~ 6000(molecular-weight average is the number-average molecular weight that tests out by gel chromatograph).Above amorphous polyester can be buied from winning the wound Degussa, for example dynacoll 7130,7150,7210,7230,7250.Amorphous polyester is chosen as above one or more.
The consumption of amorphous polyester is 30% ~ 60%(weight according to the total amount of polyurethane hot melt), preferred 25% ~ 40%(weight).
The crystal type polyester refers to that diprotic acid and dibasic alcohol polycondensation form the polymkeric substance that end group is two OH groups.Its composition: acid is hexanodioic acid, sebacic acid, and suberic acid, dodecanedioic acid, one or more of tetradecane diacid, alcohol is 1,2-ethandiol, BDO, 1,6-hexylene glycol, 1,8-ethohexadiol, decamethylene-glycol, 1,12-dodecanediol, glycol ether, one or more of neopentyl alcohol.Its molecular-weight average is 1000 ~ 8000, and is preferred 2000 ~ 8000, and particularly preferably 3000 ~ 6000(molecular-weight average is the number-average molecular weight that tests out by gel chromatograph).Above crystal type polyester can be buied from winning the wound Degussa, for example dynacoll 7360,7381,7380.The crystal type polyester is chosen as above one or more.
The consumption of crystal type polyester is 30% ~ 60%(weight according to the total amount of polyurethane hot melt), preferred 15% ~ 30%(weight).
Tackifying resin refers to rosin and fat thereof, terpenes and phenolic modified resin thereof, hydrocarbon resin, a-vinyl toluene or its modified resin.The preferred a-vinyl toluene of this paper or its modified resin particularly preferably are a-vinyl toluene monomer resins.
The tackifying resin consumption is 5% ~ 15%(weight according to the total amount of polyurethane hot melt), preferred 5% ~ 12%(weight).
The described magic tape preparation method of reaction type polyurethane hot-melt adhesive, step is as follows by weight:
(1) mix: to get 30 ~ 60 parts of amorphous polyesters, 30 ~ 60 parts of crystal type polyester, 5 ~ 15 parts of tackifying resins, mix, vacuumize, vacuum tightness is-0.05 ~-0.09MPa, 45 ~ 50min dewaters under 110 ~ 120 ℃ temperature;
(2) preparation: get 10 ~ 40 parts of isocyanic ester and join in step (1) the gained mixture, be filled with nitrogen, under 110 ~ 120 ℃, vacuum tightness is-0.05 ~-0.09MPa reacts 45 ~ 50min, obtain hot melt adhesive, in its dry container of packing into, namely get product magic tape reaction type polyurethane hot-melt adhesive.
Described container prepares take aluminium, tin or its composite membrane as material.
The present invention has following advantage: the present invention has overcome existing technical disadvantages, has higher early strength, pleasant softness preferably keeps original transparent visual effect for the bonding of transparent material, for polyamide (PA) excellent bond effect is arranged simultaneously.
Embodiment
Hereinafter, utilize some exemplary example more detailed description the present invention.Below all the explanation, given amount is recently calculated according to weight.
Embodiment 1
The described magic tape preparation method of reaction type polyurethane hot-melt adhesive is characterized in that step is as follows by weight:
(1) mix: get 30 parts of amorphous polyesters, 30 parts of crystal type polyester, 5 parts of tackifying resins, mix, vacuumize, vacuum tightness is-0.05MPa that 50min dewaters under 110 ~ 120 ℃ temperature;
(2) preparation: get 10 parts of isocyanic ester and join in step (1) the gained mixture, be filled with nitrogen, under 110 ~ 120 ℃, vacuum tightness is-0.05MPa reacts 50min, obtain hot melt adhesive, in its dry container of packing into, namely get product magic tape reaction type polyurethane hot-melt adhesive.
Described isocyanic ester is the mixture of tolylene diisocyanate, methyl diphenylene diisocyanate.
Described diphenyl diisocyanate is 4,4 '-diphenyl methyl, two isocyanic acids.
Described amorphous polyester is that diprotic acid and dibasic alcohol polycondensation form, and end group is the polymkeric substance of two OH groups; Diprotic acid is specially hexanodioic acid; Dibasic alcohol is 1,2-ethandiol; The molecular-weight average of described amorphous polyester is 2000.
Described crystal type polyester is that the end group that diprotic acid and dibasic alcohol polycondensation form is the polymkeric substance of two OH groups; Described diprotic acid is hexanodioic acid, and dibasic alcohol is 1,2-ethandiol; The molecular-weight average of described crystal type polyester is 2000.
Described tackifying resin is rosin.
Detection method
Viscosity: with Brook field viscometer determining viscosity, rotor 27# to assigned temperature and preserved value 15 minutes, reads pipe heating 20 minutes that hot melt adhesive is housed displayed value and is viscosity.
Measure NCO%: with sample and known, excessive Di-n-Butyl Amine reacts in acetone, then returns with HCL and drips to determine NCO%.
Learn that product viscosity is 6000mpa.s (140 ℃) after detecting as stated above; NCO% 1.8%(weight).
Embodiment 2
The described magic tape preparation method of reaction type polyurethane hot-melt adhesive is characterized in that step is as follows by weight:
(1) mix: get 60 parts of amorphous polyesters, 60 parts of crystal type polyester, 15 parts of tackifying resins, mix, vacuumize, vacuum tightness is-0.09MPa that 45min dewaters under 110 ~ 120 ℃ temperature;
(2) preparation: get 40 parts of isocyanic ester and join in step (1) the gained mixture, be filled with nitrogen, under 110 ~ 120 ℃, vacuum tightness is-0.09MPa reacts 45min, obtain hot melt adhesive, in its dry container of packing into, namely get product magic tape reaction type polyurethane hot-melt adhesive.
Described isocyanic ester is the mixture of the methyl diphenylene diisocyanate of methyl diphenylene diisocyanate, carbodiimide modified.
Described diphenyl diisocyanate is 2,4 '-methyl diphenylene diisocyanate.
Described amorphous polyester is that diprotic acid and dibasic alcohol polycondensation form, and end group is the polymkeric substance of two OH groups; Diprotic acid is specially sebacic acid, toxilic acid, the mixture of fumaric acid; Dibasic alcohol is BDO, the mixture of 1,5-PD; The molecular-weight average of described amorphous polyester is 8000.
Described crystal type polyester is that the end group that diprotic acid and dibasic alcohol polycondensation form is the polymkeric substance of two OH groups; Described diprotic acid is dodecanedioic acid, and dibasic alcohol is 1,6-hexylene glycol, 1,8-ethohexadiol, decamethylene-glycol, mixture; The molecular-weight average of described crystal type polyester is 8000.
Described tackifying resin is rosin.
Measure to such an extent that viscosity is 8000mpa.s (140 ℃) by embodiment 1 described method; NCO% 1.5%(weight).
Embodiment 3
The described magic tape preparation method of reaction type polyurethane hot-melt adhesive is characterized in that step is as follows by weight:
(1) mix: get 40 parts of amorphous polyesters, 40 parts of crystal type polyester, 10 parts of tackifying resins, mix, vacuumize, vacuum tightness is-0.06MPa that 48min dewaters under 110 ~ 120 ℃ temperature;
(2) preparation: get 20 parts of isocyanic ester and join in step (1) the gained mixture, be filled with nitrogen, under 110 ~ 120 ℃, vacuum tightness is-0.06MPa reacts 48min, obtain hot melt adhesive, in its dry container of packing into, namely get product magic tape reaction type polyurethane hot-melt adhesive.
Described isocyanic ester is the mixture of tolylene diisocyanate, methyl diphenylene diisocyanate.
Described diphenyl diisocyanate is 2,2 '-methyl diphenylene diisocyanate.
Described amorphous polyester is that diprotic acid and dibasic alcohol polycondensation form, and end group is the polymkeric substance of two OH groups; Diprotic acid is specially m-phthalic acid; Dibasic alcohol is neopentyl alcohol; The molecular-weight average of described amorphous polyester is 8000.
Described crystal type polyester is that the end group that diprotic acid and dibasic alcohol polycondensation form is the polymkeric substance of two OH groups; Described diprotic acid is dodecanedioic acid, and tetradecane diacid, dibasic alcohol are 1,12-dodecanediol, glycol ether, neopentyl alcohol; The molecular-weight average of described crystal type polyester is 2000.
Described tackifying resin is the a-vinyl toluene.
Claims (8)
1. the magic tape reaction type polyurethane hot-melt adhesive is characterized in that formula rate is as follows by weight: 10 ~ 40 parts of isocyanic ester, 30 ~ 60 parts of amorphous polyesters, 30 ~ 60 parts of crystal type polyester, 5 ~ 15 parts of tackifying resins;
Amorphous polyester, crystal type polyester, tackifying resin mixing are vacuumized dehydration, add again the isocyanic ester heating under vacuum and namely get product magic tape reaction type polyurethane hot-melt adhesive.
2. magic tape reaction type polyurethane hot-melt adhesive as claimed in claim 1, it is characterized in that: described isocyanic ester is two functionality isocyanic ester, specifically comprises the mixture of one or more materials in the methyl diphenylene diisocyanate of tolylene diisocyanate, methyl diphenylene diisocyanate, carbodiimide modified; The parts by weight of isocyanic ester are 10 ~ 25 parts.
3. magic tape reaction type polyurethane hot-melt adhesive as claimed in claim 2, it is characterized in that: described diphenyl diisocyanate is 4,4 '-diphenyl methyl, two isocyanic acids, 2,4 '-methyl diphenylene diisocyanate or 2, the mixture of one or more materials in 2 '-methyl diphenylene diisocyanate.
4. magic tape reaction type polyurethane hot-melt adhesive as claimed in claim 1, it is characterized in that: described amorphous polyester is that diprotic acid and dibasic alcohol polycondensation form, and end group is the polymkeric substance of two OH groups; Diprotic acid is specially hexanodioic acid, sebacic acid, toxilic acid, fumaric acid, terephthalic acid, one or more in m-phthalic acid or the phthalic acid; Dibasic alcohol is 1,2-ethandiol, 1,3 butylene glycol, BDO, 1,5-PD, one or more of glycol ether or neopentyl alcohol;
The molecular-weight average of described amorphous polyester is 1000 ~ 8000, and parts by weight are 25 ~ 40.
5. magic tape reaction type polyurethane hot-melt adhesive as claimed in claim 1, it is characterized in that: described crystal type polyester is that the end group that diprotic acid and dibasic alcohol polycondensation form is the polymkeric substance of two OH groups; Described diprotic acid is hexanodioic acid, sebacic acid, and suberic acid, dodecanedioic acid, one or more of tetradecane diacid, dibasic alcohol are 1,2-ethandiol, BDO, 1,6-hexylene glycol, 1,8-ethohexadiol, decamethylene-glycol, 1,12-dodecanediol, glycol ether, one or more in the neopentyl alcohol;
The molecular-weight average of described crystal type polyester is 1000 ~ 8000, and weight part is 15 ~ 30 parts.
6. magic tape reaction type polyurethane hot-melt adhesive as claimed in claim 1, it is characterized in that: described tackifying resin is rosin and fat thereof, terpenes and phenolic modified resin thereof, hydrocarbon resin, the mixture of one or more materials in a-vinyl toluene or its modified resin.
7. the described magic tape of claim 1 is characterized in that step is as follows by weight with the preparation method of reaction type polyurethane hot-melt adhesive:
(1) mix: to get 30 ~ 60 parts of amorphous polyesters, 30 ~ 60 parts of crystal type polyester, 5 ~ 15 parts of tackifying resins, mix, vacuumize, vacuum tightness is-0.05 ~-0.09MPa, 45 ~ 50min dewaters under 110 ~ 120 ℃ temperature;
(2) preparation: get 10 ~ 40 parts of isocyanic ester and join in step (1) the gained mixture, be filled with nitrogen, under 110 ~ 120 ℃, vacuum tightness is-0.05 ~-0.09MPa reacts 45 ~ 50min, obtain hot melt adhesive, in its dry container of packing into, namely get product magic tape reaction type polyurethane hot-melt adhesive.
8. magic tape is with the preparation method of reaction type polyurethane hot-melt adhesive as claimed in claim 7, and it is characterized in that: described container prepares take aluminium, tin or its composite membrane as material.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104449533A (en) * | 2014-12-31 | 2015-03-25 | 广州市白云化工实业有限公司 | Reactive polyurethane hot melt adhesive for electronic appliance and preparing method thereof |
CN104497947A (en) * | 2014-09-26 | 2015-04-08 | 高鼎精细化工(昆山)有限公司 | Preparation method and use of moisture-curable polyurethane hot melt adhesive for special-shaped material coating |
CN111253900A (en) * | 2020-03-27 | 2020-06-09 | 重庆中科力泰高分子材料股份有限公司 | Moisture-cured polyurethane hot melt adhesive and preparation method thereof |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102585753A (en) * | 2012-01-16 | 2012-07-18 | 无锡市万力粘合材料有限公司 | Polyurethane hot-melt adhesive for bonding and preparation method thereof |
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- 2013-01-21 CN CN201310020819XA patent/CN103045152A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102585753A (en) * | 2012-01-16 | 2012-07-18 | 无锡市万力粘合材料有限公司 | Polyurethane hot-melt adhesive for bonding and preparation method thereof |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104497947A (en) * | 2014-09-26 | 2015-04-08 | 高鼎精细化工(昆山)有限公司 | Preparation method and use of moisture-curable polyurethane hot melt adhesive for special-shaped material coating |
CN104497947B (en) * | 2014-09-26 | 2017-01-11 | 高鼎精细化工(昆山)有限公司 | Preparation method and use of moisture-curable polyurethane hot melt adhesive for special-shaped material coating |
CN104449533A (en) * | 2014-12-31 | 2015-03-25 | 广州市白云化工实业有限公司 | Reactive polyurethane hot melt adhesive for electronic appliance and preparing method thereof |
CN111253900A (en) * | 2020-03-27 | 2020-06-09 | 重庆中科力泰高分子材料股份有限公司 | Moisture-cured polyurethane hot melt adhesive and preparation method thereof |
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Application publication date: 20130417 |