CN102634318A - Low-temperature-resisting solvent type polyurethane bonding agent and preparation method thereof - Google Patents
Low-temperature-resisting solvent type polyurethane bonding agent and preparation method thereof Download PDFInfo
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- CN102634318A CN102634318A CN2012101312567A CN201210131256A CN102634318A CN 102634318 A CN102634318 A CN 102634318A CN 2012101312567 A CN2012101312567 A CN 2012101312567A CN 201210131256 A CN201210131256 A CN 201210131256A CN 102634318 A CN102634318 A CN 102634318A
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Abstract
The invention relates to a low-temperature-resisting solvent type polyurethane bonding agent and a preparation method of the low-temperature-resisting solvent type polyurethane bonding agent. The bonding agent comprises the following raw materials: 2%- 10% of isocyanate, 25%-65% of a polyatomic alcohol compound, 0.1%-1% of a small molecule alcohol chain extender,0.01%-0.2% of an organotin catalyst,0.2%-0.5% of an assistant, 0.5%-2% of a coupling agent,0.03%-1% of a termination agent and 30%-70% of a solvent; and the polyatomic alcohol compound is the combination of 1-2 kinds of polyester polyol and 1-2 kinds of polyether glycol which are 1 to (0.05-0.5) according to weight percent. With the adoption of the low-temperature-resisting solvent type polyurethane bonding agent and the preparation method provided by the invention, the defect of contradiction between the bonding strength and low temperature resistance property of the existing polyurethane bonding agent is solved; when being used as a coating adhesive, the low-temperature-resisting solvent type polyurethane bonding agent has the advantages of low-temperature softness, high mechanical strength and the like.
Description
Technical field
the present invention relates to a kind of solvent borne polyurethane tackiness agent and preparation method thereof.
Background technology
polyurethane binder has good resistance to low temperature, water tolerance, oil-proofness and snappiness, has higher bonding strength simultaneously, is widely used in industries such as synthetic leather, laminated film, shoemaking.The performance of polyurethane binder depends on the polyvalent alcohol that it is used and the structure and the performance of isocyanic ester.Adopt the prepared polyurethane binder of polyether polyol to have lower second-order transition temperature, snappiness and anti-hydrolytic performance, but its physical strength is low; Adopt polyurethane binder of polyester polyol preparation to have higher physical strength and oil-proofness, but its anti-hydrolytic performance is poor, hardness is big under the low temperature, is difficult to satisfy market demands.Therefore, it is significant to prepare the high polyurethane binder of a kind of low temperature softness and physical strength.
Summary of the invention
technical problem to be solved by this invention is the deficiency that overcomes prior art, provides a kind of low temperature softness and physical strength high low temperature resistant solvent borne polyurethane tackiness agent.
the present invention also will provide a kind of preparation method of low temperature resistant solvent borne polyurethane tackiness agent simultaneously, and is good and physical strength is high by the low-temperature pliability of the low temperature resistant solvent borne polyurethane tackiness agent of its preparation.
For solving the problems of the technologies described above, a kind of technical scheme that the present invention takes is:
a kind of low temperature resistant solvent borne polyurethane tackiness agent; Percentage composition meter by weight; Its raw material is formed as follows: 2% ~ 10% isocyanic ester, 25% ~ 65% polyol compound, 0.1% ~ 1% small molecular alcohol chainextender, 0.01% ~ 0.2% organic tin catalyzer, 0.2% ~ 0.5% auxiliary agent, 0.5% ~ 2% coupling agent, 0.03% ~ 1% terminator and 30% ~ 70% solvent; Said polyol compound is that 1 ~ 2 kind of number-average molecular weight is that 1000 ~ 6000 polyester polyol and 1 ~ 2 kind of number-average molecular weight are the combination that constitutes of 1:0.05 ~ 0.5 by weight ratio of 1000 ~ 2000 polyether glycol; Wherein, Described polyether glycol is polyoxyethylene glycol, polypropylene oxide glycol or PTMG, and said polyester polyol is that hexanodioic acid obtains with one or both alcohol reactions that are selected from terepthaloyl moietie, glycol ether, butyleneglycol, NSC 6366, pinakon and the decanediol.
According to further embodiment of the present invention:
The ratio that the charging capacity of
isocyanic ester and polyol compound satisfies NCO and the mole number of hydroxyl is 0.90 ~ 0.99:1.
isocyanic ester can be for being selected from 4,4 '-'-diphenylmethane diisocyanate, 2; 4 '-'-diphenylmethane diisocyanate, 2,4 toluene diisocyanate; 2,6-tolylene diisocyanate, 1; The 5-naphthalene diisocyanate, an xylylene isocyanic ester and 1, one or both in the 3-dimethyl-isocyanic ester hexanaphthene.
small molecular alcohol chainextender can be for being selected from terepthaloyl moietie, 1; Ammediol, dihydroxymethyl ethane, 1,4-butyleneglycol, 2; 2-dimethyl propylene glycol, glycol ether, 1; 5-pentanediol, 3-methyl isophthalic acid, 5-pentanediol, 1, the combination of one or more in 6-pinakon, TriMethylolPropane(TMP), tetramethylolmethane and the sorbyl alcohol.
terminator can be terepthaloyl moietie, 1,2-Ucar 35 or 1,3 butylene glycol.
coupling agent is preferably and is selected from a kind of in silane coupling agent and the titanate coupling agent.
solvent is preferably and is selected from N, in dinethylformamide (DMF), toluene, ETHYLE ACETATE, butanone and the ethylene dichloride at least two kinds.
described auxiliary agent comprises inhibitor and stopper.In a concrete embodiment, auxiliary agent is made up of inhibitor 98wt% ~ 99wt% and stopper 1wt% ~ 2wt%.
according to the present invention, the commercially available acquisition of polyester polyol, or prepare by means commonly known in the art.Concrete polyester polyol has and for example gathers adipate glycol glycol ether esterdiol, gathers adipate glycol-1,4-butanediol ester glycol etc.Polyester polyol for example can prepare through method described below: adopt the high temperature nitrogen evaporation, in reaction kettle, drop into diprotic acid and the divalent alcohol that measures, feed the nitrogen excluding air.Under nitrogen protection, stir and be warming up to 140 ℃, progressively be warming up to 160 ℃ then, insulation 2hr.Then temperature is risen to 240 ℃, insulation and sampling analysis are until meeting the requirements of hydroxyl value and acid number, cooling discharge.
The another technical scheme that
the present invention takes is: a kind of preparation method of above-mentioned low temperature resistant solvent borne polyurethane tackiness agent, it is implemented as follows: in reaction kettle, add the polyol compound and small molecular alcohol chainextender, the solvent of 45% ~ 55% formula ratio, the auxiliary agent of formula ratio of formula ratio, 40 ~ 50 ℃ stir 30min ~ 60min down after the isocyanic ester of adding formula ratio; Add the organic tin catalyzer of formula ratio after stirring, be warming up to 80 ℃ ~ 90 ℃ and react, with the carrying out of reaction; Viscosity increases; When viscosity reaches prescribed value, drop into the terminator and the remaining solvent of formula ratio, termination reaction; Continue to stir until stable viscosity; The coupling agent that adds formula ratio continues to stir 30 ~ 60min, the discharging packing.
According to the present invention, the prescribed value of above-mentioned viscosity changes according to the difference of concrete application need
.Generally speaking, viscosity is controlled in 30,000 ~ 120, between 000cPs/25 ℃.
Because the enforcement of above technical scheme, the present invention compared with prior art has following advantage:
the present invention uses the pure composition that comes from different backgrounds and possess different abilities with the pure and mild specific polyether polyvalent alcohol of specific polyester polyols by the specified proportion combination, has solved conflicting deficiency between existing cohesive strength of existing polyurethane binder and the resistance to low temperature.Tackiness agent of the present invention uses as coating adhesive, has the low temperature softness, and the physical strength advantages of higher is suitable for and does fabric coating primer, the use of synthetic leather bonding coat.
The preparation method of
polyurethane adhesive of the present invention, technology is simple, and cost is low.
Embodiment
are done further detailed explanation below in conjunction with concrete embodiment to the present invention, but the invention is not restricted to following examples.
Embodiment 1
are following according to the composition of raw materials of the solvent borne polyurethane tackiness agent of present embodiment: 500 kg PTMGs 2000 (PTMG 2000, Mitsubishi Chemical); 1200kg gathers adipate glycol-1,4-butanediol ester glycol (number-average molecular weight 2000, self-control); 160.3kg 2,4 toluene diisocyanate and 2,6-tolylene diisocyanate (TDI-80/20); 7.6kg 1, the 4-butyleneglycol; 3.0kg oxidation inhibitor (BHT); 0.17 kg phosphoric acid; 3.1kg TriMethylolPropane(TMP); 3.0kg 1, the 2-Ucar 35; 0.6kg organotin catalysts (T-12); 5.0kg silane coupling agent (KH-560); 550kg toluene; 550kg ETHYLE ACETATE.
solvent borne polyurethane tackiness agent prepares through following steps: in reaction kettle, drop into the PTMG 2000 measure successively, gather adipate glycol-1; 4-butanediol ester glycol, TriMethylolPropane(TMP), 1; 4-butyleneglycol, phosphoric acid, antioxidant BHT and toluene; Add TDI-80/20 behind the stirring 40min down at 40 ~ 50 ℃, continue to add organotin catalysts T-12 behind the stirring 30min, be warming up to 90 ℃ and react.With the carrying out of reaction, viscosity increases, and when Gardner's bubble viscosity of system reaches T, drops into 1,3 butylene glycol and ETHYLE ACETATE termination reaction, continues to stir 1 hour until stable viscosity, adds silane coupling agent KH-560, continues to stir 40min, the discharging packing.
Embodiment 2
are following according to the composition of raw materials of the solvent borne polyurethane tackiness agent of present embodiment: 600 kg gather adipate glycol glycol ether esterdiol (number-average molecular weight 2000, Mitsubishi Chemical); 300kg polypropylene oxide glycol (number-average molecular weight 2000, high bridge petrochemical industry); 1000kg gathers adipate glycol-1,4-butanediol ester glycol (number-average molecular weight 2000, self-control); 265 kg 4,4 '-'-diphenylmethane diisocyanate (MDI); 5.2 kg 2,2-dimethyl--1,3 Ucar 35; 3.0kg oxidation inhibitor (BHT); 0.17 kg phosphoric acid; 5.0 kg TriMethylolPropane(TMP); 6.0kg terepthaloyl moietie; 0.2 kg catalyzer (T-9); 10.0kg titanate coupling agent (102); 1000kg toluene; The 4000kg butanone.
solvent borne polyurethane tackiness agent prepares through following steps: in reaction kettle, drop into gathering adipate glycol glycol ether ester, gathering adipate glycol-1 of measuring successively; 4-butanediol ester glycol, 2; 2-dimethyl--1,3 Ucar 35, TriMethylolPropane(TMP), phosphoric acid, antioxidant BHT and toluene stir 40min down at 40 ~ 50 ℃; Drop into MDI then, controlled temperature reacts at 75 ~ 80 ℃.Along with the carrying out of reaction, system viscosity increases, and divides three equivalent to add the dilution of 3000kg butanone.When Gardner's bubble viscosity of system reaches X, add terepthaloyl moietie and residue 1000kg butanone termination reaction, it is stable until system viscosity to continue stirring, adds titanate coupling agent 102, continues to stir 40min, and discharging is packed.
Embodiment 3
are following according to the composition of raw materials of the solvent borne polyurethane tackiness agent of present embodiment: 600 kg PTMGs 2000 (PTMG 2000, Mitsubishi Chemical); 1200 kg gather adipate glycol-1,4-butanediol ester glycol (number-average molecular weight 2000, self-control); 119.6 kg 2,4 toluene diisocyanate and 2,6-tolylene diisocyanate (TDI-80/20); 3.0 kg 1, the 4-butyleneglycol; 2.1 kg sorbyl alcohol; 3.0kg oxidation inhibitor (BHT); 0.15 kg phosphoric acid; 3.2 kg 1,3 butylene glycol; 0.3 kg organotin catalysts (T-12); 3.0kg silane coupling agent (KH-560); 400kg toluene; 500kg N, dinethylformamide.
solvent borne polyurethane tackiness agent prepares through following steps: in reaction kettle, drop into the PTMG 2000 measure successively, gather adipate glycol-1; 4-butanediol ester glycol, sorbyl alcohol, 1; 4-butyleneglycol, phosphoric acid, antioxidant BHT and toluene add TDI-80/20 behind the stirring 40min down at 40 ~ 50 ℃, stir 30min; Add organotin catalysts T-12, be warming up to 80 ℃ and react.With the carrying out of reaction, viscosity increases, when Gardner's bubble viscosity of system reaches V; Drop into 1,3 butylene glycol and N termination reaction, continue to stir 1 hour until stable viscosity; Add silane coupling agent KH-560, continue to stir 40min, the discharging packing.
become glue to above-mentioned prepared resin by following formulation for checking low temperature resistant solvent borne polyurethane tackiness agent of the present invention.
Resin 100
Solidifying agent 6.0
Promotor 2.0
Toluene 30
apply above-mentioned glue to base cloth woven cloth such as (taffeta/Nylon Taffeta/spring Asia) spinning, coating thickness is 0.5mm, under 150 ~ 160 ° of C, solidify 10min.
The test of wash durability and resistance to low temperature is carried out in
according to general testing method; The washing testing method is specially: adopt the washing machine washing; 45 ℃ of temperature, time 15min washes back 100 ℃ of oven dry; Whether with metal blunt scratch coating, observing has scratch and disbonding.The resistance to low temperature testing method is: sample is inserted in the cryostat, and the feel of test sample under each temperature is to confirm its minimum use temperature.Sample is hardening at low temperatures, when rubbing, has sound to send.Minimum temperature when test sample can keep soft feel and not rub sound.
test result shows, takes the wash durability of leather of the tackiness agent preparation of three embodiment to reach more than 5 times, under-15 ° of C ~-10 ° C, still has snappiness preferably.
More than the present invention has been done detailed description; Its purpose is to let the personage that is familiar with this art can understand content of the present invention and implements; Can not limit protection scope of the present invention with this; All equivalences of doing according to spirit of the present invention change or modify, and all should be encompassed in protection scope of the present invention
Claims (10)
1. low temperature resistant solvent borne polyurethane tackiness agent; It is characterized in that: percentage composition meter by weight; The raw material of said low temperature resistant solvent borne polyurethane tackiness agent is formed as follows: 2% ~ 10% isocyanic ester, 25% ~ 65% polyol compound, 0.1% ~ 1% small molecular alcohol chainextender, 0.01% ~ 0.2% organic tin catalyzer, 0.2% ~ 0.5% auxiliary agent, 0.5% ~ 2% coupling agent, 0.03% ~ 1% terminator and 30% ~ 70% solvent; Said polyol compound is that 1 ~ 2 kind of number-average molecular weight is that 1000 ~ 6000 polyester polyol and 1 ~ 2 kind of number-average molecular weight are the combination that constitutes of 1:0.05 ~ 0.5 by weight ratio of 1000 ~ 2000 polyether glycol; Wherein, Described polyether glycol is polyoxyethylene glycol, polypropylene oxide glycol or PTMG, and said polyester polyol is that hexanodioic acid obtains with one or both alcohol reactions that are selected from terepthaloyl moietie, glycol ether, butyleneglycol, NSC 6366, pinakon and the decanediol.
2. low temperature resistant solvent borne polyurethane tackiness agent according to claim 1 is characterized in that: the ratio that the charging capacity of said isocyanic ester and said polyol compound satisfies NCO and the mole number of hydroxyl is 0.90 ~ 0.99:1.
3. low temperature resistant solvent borne polyurethane tackiness agent according to claim 1 is characterized in that: described isocyanic ester is for being selected from 4,4 '-'-diphenylmethane diisocyanate, 2; 4 '-'-diphenylmethane diisocyanate, 2,4 toluene diisocyanate; 2,6-tolylene diisocyanate, 1; The 5-naphthalene diisocyanate, an xylylene isocyanic ester and 1, one or both in the 3-dimethyl-isocyanic ester hexanaphthene.
4. low temperature resistant solvent borne polyurethane tackiness agent according to claim 1 is characterized in that: said small molecular alcohol chainextender is for being selected from terepthaloyl moietie, 1, the 3-Ucar 35; Dihydroxymethyl ethane, 1; 4-butyleneglycol, 2,2-dimethyl propylene glycol, glycol ether, 1,5-pentanediol, 3-methyl isophthalic acid; 5-pentanediol, 1, the combination of one or more in 6-pinakon, TriMethylolPropane(TMP), tetramethylolmethane and the sorbyl alcohol.
5. low temperature resistant solvent borne polyurethane tackiness agent according to claim 1 is characterized in that: described terminator is a terepthaloyl moietie, 1,2-Ucar 35 or 1,3 butylene glycol.
6. low temperature resistant solvent borne polyurethane tackiness agent according to claim 1 is characterized in that: described coupling agent is to be selected from a kind of in silane coupling agent and the titanate coupling agent.
7. low temperature resistant solvent borne polyurethane tackiness agent according to claim 1 is characterized in that: said solvent is for being selected from N, in dinethylformamide, toluene, ETHYLE ACETATE, butanone and the ethylene dichloride at least two kinds.
8. low temperature resistant solvent borne polyurethane tackiness agent according to claim 1, it is characterized in that: described auxiliary agent comprises inhibitor and stopper.
9. low temperature resistant solvent borne polyurethane tackiness agent according to claim 8 is characterized in that: said auxiliary agent is made up of 98wt% ~ 99wt% and stopper 1wt% ~ 2wt%.
10. the preparation method of the described low temperature resistant solvent borne polyurethane tackiness agent of each claim in the claim 1 to 9, it is characterized in that: said method is implemented as follows: in reaction kettle, add the said polyol compound and small molecular alcohol chainextender, the solvent of 45% ~ 55% formula ratio, the auxiliary agent of formula ratio of formula ratio, at 40 ~ 50 ℃ of isocyanic ester of adding formula ratio behind stirring 30min ~ 60min down; Add the organic tin catalyzer of formula ratio after stirring, be warming up to 80 ℃ ~ 90 ℃ and react, with the carrying out of reaction; Viscosity increases; When viscosity reaches prescribed value, drop into the terminator and the remaining solvent of formula ratio, termination reaction; Continue to stir until stable viscosity; The coupling agent that adds formula ratio continues to stir 30 ~ 60min, the discharging packing.
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