CN105368372A - PE composite-suitable adhesive for solventless two-component polyurethane and preparation method for adhesive - Google Patents
PE composite-suitable adhesive for solventless two-component polyurethane and preparation method for adhesive Download PDFInfo
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Abstract
The present invention discloses a PE composite-suitable adhesive for solventless two-component polyurethane and a preparation method for the adhesive. The adhesive comprises a component A that is obtained by reaction on isocyanate and polyester polyol and terminated by the isocyanate, and a component B consisting of polyester polyol, wherein the functional group molar ratio of the component A and the component B is (1.4-1.7):1. The preparation method comprises: uniformly mixing 100 parts of polyisocyanate with 30-50 parts of polyester diol or 10-30 parts of castor oil, preserving the temperature at 50-60 DEG C for 2-3 hours, and raising the temperature to 80-90 DEG C and preserving the temperature to react for 3-4 hours to generate an adhesive component A terminated by isocyanato; and directly using polyester diol as the component B, or using vacuum dewatered castor oil as the component B, or using uniformly mixed 60-80 parts of polyester diol and 20-40 parts of polyester diolscastor oil after vacuum dewater as the component B. The problems, a thin PE composite is used in a flexible package inner layer and the friction coefficient of the heat sealing layer increases and it is difficult to open, are solved. The adhesive is environmental-friendly, free of solvent emission, and is suitable for compounding of various structures, particularly for compounding f thin PE as inner layers, so that the higher peeling strength can be achieved, and the effect on the friction coefficient of the heat sealing layer is relatively less.
Description
Technical field
The present invention relates to polyurethane binder that one is applicable to composite soft packaging (food, medicine, beverage and makeup), particularly relate to a kind of solvent-free dual-component polyurethane tackiness agent being applicable to thin PE compound and preparation method thereof.
Background technology
In recent years, there is explosive growth in solvent-free composite machine domestic installation quantity, its lower tooling cost is undoubtedly the maximum impetus of this phenomenon.
At present, process flexible packing material with the frictional coefficient paying close attention to all very much packaging material hot sealing layer using flexible packing material.Frictional coefficient is the index measuring wrapping material sliding properties, and thin-film material surface is smooth and have suitable frictional coefficient for extremely important film packaging technique, and the wrapping material product producing different purposes has different requirements to frictional coefficient.Frictional force in actual packaging process is usually drawing force and resistance, therefore effectively must control the size of frictional coefficient, makes it in suitable scope.If frictional coefficient is excessive, if composite membrane frictional coefficient is more than 0.3, so package film there will be and draws motionless situation on some horizontal boards, if the frictional coefficient of bag product is more than 0.25, the sack that specification is less just easily occurs the phenomenon that opening is bad; Frictional coefficient neither be the smaller the better, as automatic packaging coiled material, when internal layer frictional coefficient is too small, fold material instability when likely causing bag shaping and produce misalignment, outer layer friction coefficient is too little may can cause again tractor skidding to cause electric eye tracking and cut-out location to be forbidden.Refer now to, the frictional coefficient between 0.1-0.2 seems to become industry standard sanctified by usage.
In prior art, many compound producers select different modes to change this realistic situation, such as ripening at low temperature, reduce machine speed etc., but these methods are not the key solving problems, also there are some mistaken ideas in some understanding.Solvent-free glue containing polyethers can absorb slipping agent, and curing temperature is high can accelerate slipping agent to film internal migration, thus causes the rising of heat cover frictional coefficient, the theoretical foundation of this seemingly " ripening at low temperature ".But should be noted that: it is its person's character that the glue containing polyethers absorbs slipping agent, can't change along with the change of temperature, the speed of its migration only can be accelerated or reduce to temperature.Certainly, effectively can to improve the problem of frictional coefficient as added appropriate mineral-type opening agent by changing the blown film formula of heat-sealable material itself, reason is that the opening agent of mineral-type can make heat cover and printed layers surface keep suitable distance, decrease because winding tension is excessive, under film interlayer pressure excess force that, slipping agent can be pressed into hot sealing layer and printed layers is inner, causes frictional coefficient to rise.
Summary of the invention
The object of this invention is to provide a kind of stripping strength high, for less solvent-free dual-component polyurethane tackiness agent being applicable to thin PE compound of frictional coefficient impact and preparation method thereof of hot sealing layer.
The object of the invention is to be achieved through the following technical solutions:
The solvent-free two-component polyurethane adhesive being applicable to thin PE compound of the present invention, comprise and to be reacted by isocyanic ester and polyester polyol and by isocyanate-terminated component A and the B component that is made up of polyester polyol, functional group's mol ratio of described component A and B component is 1.4-1.7:1.
The preparation method being applicable to the solvent-free two-component polyurethane adhesive of thin PE compound above-mentioned in the present invention, described component A is synthesized by the following method:
Mixed with the polyester diol of 30-50 part or the Viscotrol C of 10-30 part by the polyisocyanates of 100 parts, 50-60 DEG C of insulation 2-3 hour, is warming up to 80-90 DEG C of insulation reaction 3-4 hour, generates by the adhesive A component of isocyano end-blocking;
Described B component is synthesized by one or more methods following:
Directly using polyester diol as B component, using after Viscotrol C vacuum hydro-extraction as B component, the polyester diol of 60-80 part mixed final vacuum with the Viscotrol C of 20-40 part dewater as B component.
As seen from the above technical solution provided by the invention, what the embodiment of the present invention provided solvent-free dual-component polyurethane tackiness agent being applicable to thin PE compound and preparation method thereof, solve and occur that hot sealing layer frictional coefficient increases at the thin PE of soft packaging internal layer (thickness≤35um) compound tense, the not easily problem of opening, environmental friendliness, solvent-free discharge, be applicable to the compound of various structures, be particularly useful for the compound of thin PE (thickness≤35) as inner layer material, higher stripping strength can not only be reached, frictional coefficient impact for hot sealing layer is less, only increase about 0.05 than former film frictional coefficient.
Embodiment
To be described in further detail the embodiment of the present invention below.
The solvent-free two-component polyurethane adhesive being applicable to thin PE compound of the present invention, its preferably embodiment be:
Comprise and to be reacted by isocyanic ester and polyester polyol and by isocyanate-terminated component A and the B component that is made up of polyester polyol, functional group's mol ratio of described component A and B component is 1.4-1.7:1.
Described isocyanic ester comprises one or more mixture following:
The diphenylmethanediisocyanate of 2,4-liquid diphenylmethanediisocyanates, 4,4-solid-state diphenylmethanediisocyanates, isoflurane chalcone diisocyanate, Carbodiimide-Modified;
Described polyester polyol comprises a kind of in the vegetable oil polyol of 500-600 molecular weight and the polyester diol of 500-1000 molecular weight or both mixtures.
The above-mentioned preparation method being applicable to the solvent-free two-component polyurethane adhesive of thin PE compound of the present invention, its preferably embodiment be:
Described component A is synthesized by the following method:
Mixed with the polyester diol of 30-50 part or the Viscotrol C of 10-30 part by the polyisocyanates of 100 parts, 50-60 DEG C of insulation 2-3 hour, is warming up to 80-90 DEG C of insulation reaction 3-4 hour, generates by the adhesive A component of isocyano end-blocking;
Described B component is synthesized by any one or more method following:
Directly using polyester diol as B component, using after Viscotrol C vacuum hydro-extraction as B component, the polyester diol of 60-80 part mixed final vacuum with the Viscotrol C of 20-40 part dewater as B component.
The polyester diol of described 500-1000 molecular weight is synthesized by any one or more method following:
By the hexanodioic acid of 45 parts, the glycol ether of the 3-methyl pentanediol of 8 parts and 47 parts joins in polyester still, stir, continue to add the triphenyl phosphite of 0.5 part as oxidation inhibitor, the tetra-n-butyl titanate of 0.05 part is as catalyzer, after the process of esterifying polycondensation, obtain hydroxyl value between 210-220mgKOH/g, molecular weight is the polyester diol of 500;
By the hexanodioic acid of 46 parts, the glycol ether of the 2-methyl propanediol of 16 parts and 38 parts joins in polyester still, stir, continue to add the triphenyl phosphite of 0.5 part as oxidation inhibitor, the tetra-n-butyl titanate of 0.05 part is as catalyzer, after the process of esterifying polycondensation, obtain hydroxyl value between 210-220mgKOH/g, molecular weight is the polyester diol of 500;
By the hexanodioic acid of 26 parts, the isophthalic anhydride of 29 parts, 1 of the glycol ether of 13 parts and 32 parts, 2-propylene glycol joins in polyester still, stirs, and continues to add the triphenyl phosphite of 0.5 part as oxidation inhibitor, the tetra-n-butyl titanate of 0.03 part is as catalyzer, after the process of esterifying polycondensation, obtain hydroxyl value between 110-120mgKOH/g, molecular weight is the polyester diol of 1000.
Of the present inventionly be applicable to solvent-free two-component polyurethane adhesive of thin PE compound and preparation method thereof, solve and occur that hot sealing layer frictional coefficient increases at the thin PE of soft packaging internal layer (thickness≤35um) compound tense, the not easily problem of opening.
The solvent-free two-component polyurethane adhesive of the present invention's synthesis, environmental friendliness, solvent-free discharge, be applicable to the compound of various structures, be particularly useful for the compound of thin PE (thickness≤35) as inner layer material, can not only reach higher stripping strength, the frictional coefficient impact for hot sealing layer is less, only increases about 0.05 than former film frictional coefficient.
Specific embodiment:
Embodiment 1:
The synthetic method of component A:
By 100 parts 2,4-diphenylmethanediisocyanate mixes with the Viscotrol C of 20 parts with the polyester diol of 30 parts, first at 50-60 DEG C of insulation 2-3 hour, after be warming up to 80-90 DEG C of insulation reaction 3-4 hour, sampling detects the content of NCO in synthetics, when NCO massfraction is at 16-17%, prove that product is qualified, as component A after blowing packaging.
The preparation of polyester diol:
By the hexanodioic acid of 45 parts, the glycol ether of the 3-methyl pentanediol of 8 parts and 47 parts joins in polyester still, stir, continue to add the triphenyl phosphite of 0.5 part as oxidation inhibitor, the tetra-n-butyl titanate of 0.05 part is as catalyzer, after the process of esterifying polycondensation, obtain hydroxyl value between 210-220mgKOH/g, molecular weight is about the polyester diol of 500.
The synthetic method of B component:
Viscotrol C is dewatered, as B component after packing.
Above A/B component is pressed NCO/OH=1.5:1 compound on solvent-free composite machine, and spread, at about 1.3g/m2, carries out compound to PET12/PE30, and outward appearance is good, and 40 DEG C of slakings are after 24 hours, and T-shaped stripping strength can reach 4.5N/15mm.
The former film frictional coefficient of PE is 0.1, and compound after heat sealing frictional coefficient is 0.12.
Embodiment 2:
The synthetic method of component A:
By 100 parts 2,4-diphenylmethanediisocyanate mixes with the Viscotrol C of 30 parts, first at 50-60 DEG C of insulation 2-3 hour, after be warming up to 80-90 DEG C of insulation reaction 3-4 hour, sampling detects the content of NCO in synthetics, when NCO massfraction is at 16-17%, prove that product is qualified, as component A after blowing packaging.
The synthetic method of B component:
By the hexanodioic acid of 46 parts, the glycol ether of the 2-methyl propanediol of 16 parts and 38 parts joins in polyester still, stir, continue to add the triphenyl phosphite of 0.5 part as oxidation inhibitor, the tetra-n-butyl titanate of 0.05 part, as catalyzer, after the process of esterifying polycondensation, obtains hydroxyl value between 210-220mgKOH/g, molecular weight is about the polyester diol of 500, as B component after blowing.
Above A/B component is pressed NCO/OH=1.6:1 compound on solvent-free composite machine, and spread is at 1.3g/m
2left and right, carries out compound to PET12/PE20, and outward appearance is good, and 40 DEG C of slakings are after 24 hours, and T-shaped stripping strength can reach 4.5N/15mm.
The former film frictional coefficient of PE is 0.1, and compound after heat sealing frictional coefficient is 0.11.
Embodiment 3:
The synthetic method of component A:
By 100 parts 4,4-diphenylmethanediisocyanate mixes with the Viscotrol C of 30 parts, first at 50-60 DEG C of insulation 2-3 hour, after be warming up to 80-90 DEG C of insulation reaction 3-4 hour, sampling detects the content of NCO in synthetics, when NCO massfraction is at 16-17%, prove that product is qualified, as component A after blowing packaging.
The synthetic method of B component:
The polyester diol of 60 parts and the Viscotrol C of 40 parts are mixed final vacuum dewater, blowing is as B component.
The preparation of polyester diol:
By the hexanodioic acid of 26 parts, the isophthalic anhydride of 29 parts, 1 of the glycol ether of 13 parts and 32 parts, 2-propylene glycol joins in polyester still, stirs, and continues to add the triphenyl phosphite of 0.5 part as oxidation inhibitor, the tetra-n-butyl titanate of 0.03 part is as catalyzer, after the process of esterifying polycondensation, obtain hydroxyl value between 110-120mgKOH/g, molecular weight is about the polyester diol of 1000.
Above A/B component is pressed NCO/OH=1.5:1 compound on solvent-free composite machine, and spread is at 1.3g/m
2left and right, carries out compound to PET12/PE20, and outward appearance is good, and 40 DEG C of slakings are after 24 hours, and T-shaped stripping strength can reach 4.5N/15mm.
The former film frictional coefficient of PE is 0.1, and compound after heat sealing frictional coefficient is 0.13.
Embodiment 4:
The synthetic method of component A:
The polyester diol of the carbodiimide modified diphenylmethane diisocyanate of 100 parts with 50 parts is mixed, first at 50-60 DEG C of insulation 2-3 hour, after be warming up to 80-90 DEG C of insulation reaction 3-4 hour, sampling detects the content of NCO in synthetics, when NCO massfraction is at 16-17%, proof product is qualified, as component A after blowing packaging.
The preparation of polyester diol:
By the hexanodioic acid of 26 parts, the isophthalic anhydride of 29 parts, 1 of the glycol ether of 13 parts and 32 parts, 2-propylene glycol joins in polyester still, stirs, and continues to add the triphenyl phosphite of 0.5 part as oxidation inhibitor, the tetra-n-butyl titanate of 0.03 part is as catalyzer, after the process of esterifying polycondensation, obtain hydroxyl value between 110-120mgKOH/g, molecular weight is about the polyester diol of 1000.
The synthetic method of B component:
Viscotrol C is dewatered, as B component after packing.
Above A/B component is pressed NCO/OH=1.6:1 compound on solvent-free composite machine, and spread is at 1.3g/m
2left and right, carries out compound to PET12/PE35, and outward appearance is good, and 40 DEG C of slakings are after 24 hours, and T-shaped stripping strength can reach 4.5N/15mm.
The former film frictional coefficient of PE is 0.1, and compound after heat sealing frictional coefficient is 0.1.
Embodiment 5:
The synthetic method of component A:
Many methyl polyphenyl polyisocyanate of 100 parts is mixed with the polyester diol of 40 parts, first at 50-60 DEG C of insulation 2-3 hour, after be warming up to 80-90 DEG C of insulation reaction 3-4 hour, sampling detects the content of NCO in synthetics, when NCO massfraction is at 16-17%, proof product is qualified, as component A after blowing packaging.
The preparation of polyester diol:
By the hexanodioic acid of 46 parts, the glycol ether of the 2-methyl propanediol of 16 parts and 38 parts joins in polyester still, stir, continue to add the triphenyl phosphite of 0.5 part as oxidation inhibitor, the tetra-n-butyl titanate of 0.05 part is as catalyzer, after the process of esterifying polycondensation, obtain hydroxyl value between 210-220mgKOH/g, molecular weight is about the polyester diol of 500.
The synthetic method of B component:
By the hexanodioic acid of 45 parts, the glycol ether of the 3-methyl pentanediol of 8 parts and 47 parts joins in polyester still, stir, continue to add the triphenyl phosphite of 0.5 part as oxidation inhibitor, the tetra-n-butyl titanate of 0.05 part, as catalyzer, after the process of esterifying polycondensation, obtains hydroxyl value between 210-220mgKOH/g, molecular weight is about the polyester diol of 500, as B component after blowing.
Above A/B component is pressed NCO/OH=1.5:1 compound on solvent-free composite machine, and spread is at 1.3g/m
2left and right, carries out compound to PET12/PE35, and outward appearance is good, and 40 DEG C of slakings are after 24 hours, and T-shaped stripping strength can reach 4.5N/15mm.
The former film frictional coefficient of PE is 0.1, and compound after heat sealing frictional coefficient is 0.12.
Embodiment 6:
The synthetic method of component A:
By 100 parts 2,4-diphenylmethanediisocyanate mixes with the Viscotrol C of 30 parts with the polyester diol of 40 parts, first at 50-60 DEG C of insulation 2-3 hour, after be warming up to 80-90 DEG C of insulation reaction 3-4 hour, sampling detects the content of NCO in synthetics, when NCO massfraction is at 16-17%, prove that product is qualified, as component A after blowing packaging.
The preparation of polyester diol:
By the hexanodioic acid of 26 parts, the isophthalic anhydride of 29 parts, 1 of the glycol ether of 13 parts and 32 parts, 2-propylene glycol joins in polyester still, stirs, and continues to add the triphenyl phosphite of 0.5 part as oxidation inhibitor, the tetra-n-butyl titanate of 0.03 part is as catalyzer, after the process of esterifying polycondensation, obtain hydroxyl value between 110-120mgKOH/g, molecular weight is about the polyester diol of 1000.
The synthetic method of B component:
By the hexanodioic acid of 45 parts, the glycol ether of the 3-methyl pentanediol of 8 parts and 47 parts joins in polyester still, stir, continue to add the triphenyl phosphite of 0.5 part as oxidation inhibitor, the tetra-n-butyl titanate of 0.05 part, as catalyzer, after the process of esterifying polycondensation, obtains hydroxyl value between 210-220mgKOH/g, molecular weight is about the polyester diol of 500, as B component after blowing.
Above A/B component is pressed NCO/OH=1.5:1 compound on solvent-free composite machine, and spread is at 1.3g/m
2left and right, carries out compound to PET12/PE30, and outward appearance is good, and 40 DEG C of slakings are after 24 hours, and T-shaped stripping strength can reach 4.5N/15mm.
The former film frictional coefficient of PE is 0.1, and compound after heat sealing frictional coefficient is 0.12.
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (4)
1. one kind is applicable to the solvent-free two-component polyurethane adhesive of thin PE compound, it is characterized in that, comprise and to be reacted by isocyanic ester and polyester polyol and by isocyanate-terminated component A and the B component that is made up of polyester polyol, functional group's mol ratio of described component A and B component is 1.4-1.7:1.
2. the solvent-free two-component polyurethane adhesive being applicable to thin PE compound according to claim 1, is characterized in that, described isocyanic ester comprises one or more mixture following:
The diphenylmethanediisocyanate of 2,4-liquid diphenylmethanediisocyanates, 4,4-solid-state diphenylmethanediisocyanates, isoflurane chalcone diisocyanate, Carbodiimide-Modified;
Described polyester polyol comprises a kind of in the vegetable oil polyol of 500-600 molecular weight and the polyester diol of 500-1000 molecular weight or both mixtures.
3. the preparation method being applicable to the solvent-free two-component polyurethane adhesive of thin PE compound described in claim 1 or 2, it is characterized in that, described component A is synthesized by the following method:
Mixed with the polyester diol of 30-50 part or the Viscotrol C of 10-30 part by the polyisocyanates of 100 parts, 50-60 DEG C of insulation 2-3 hour, is warming up to 80-90 DEG C of insulation reaction 3-4 hour, generates by the adhesive A component of isocyano end-blocking;
Described B component is synthesized by any one or more method following:
Directly using polyester diol as B component, using after Viscotrol C vacuum hydro-extraction as B component, the polyester diol of 60-80 part mixed final vacuum with the Viscotrol C of 20-40 part dewater as B component.
4. the preparation method being applicable to the solvent-free two-component polyurethane adhesive of thin PE compound according to claim 3, is characterized in that, the polyester diol of described 500-1000 molecular weight is synthesized by any one or more method following:
By the hexanodioic acid of 45 parts, the glycol ether of the 3-methyl pentanediol of 8 parts and 47 parts joins in polyester still, stir, continue to add the triphenyl phosphite of 0.5 part as oxidation inhibitor, the tetra-n-butyl titanate of 0.05 part is as catalyzer, after the process of esterifying polycondensation, obtain hydroxyl value between 210-220mgKOH/g, molecular weight is the polyester diol of 500;
By the hexanodioic acid of 46 parts, the glycol ether of the 2-methyl propanediol of 16 parts and 38 parts joins in polyester still, stir, continue to add the triphenyl phosphite of 0.5 part as oxidation inhibitor, the tetra-n-butyl titanate of 0.05 part is as catalyzer, after the process of esterifying polycondensation, obtain hydroxyl value between 210-220mgKOH/g, molecular weight is the polyester diol of 500;
By the hexanodioic acid of 26 parts, the isophthalic anhydride of 29 parts, 1 of the glycol ether of 13 parts and 32 parts, 2-propylene glycol joins in polyester still, stirs, and continues to add the triphenyl phosphite of 0.5 part as oxidation inhibitor, the tetra-n-butyl titanate of 0.03 part is as catalyzer, after the process of esterifying polycondensation, obtain hydroxyl value between 110-120mgKOH/g, molecular weight is the polyester diol of 1000.
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| CN201510881504.3A CN105368372A (en) | 2015-12-03 | 2015-12-03 | PE composite-suitable adhesive for solventless two-component polyurethane and preparation method for adhesive |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106520054A (en) * | 2016-11-16 | 2017-03-22 | 北京高盟新材料股份有限公司 | Low-friction-coefficient and solvent-free type polyurethane adhesive and preparation method thereof |
| CN108659770A (en) * | 2018-04-10 | 2018-10-16 | 广东华粘新材料研究有限公司 | A kind of bi-component solvent-free reaction type polyurethane hot melt adhesive and its application method applied to Soft Roll industry |
| CN110092893A (en) * | 2019-05-22 | 2019-08-06 | 无锡风鹏新材料科技有限公司 | A kind of room temperature liquid polyesters and preparation method thereof |
| CN110734732A (en) * | 2019-11-07 | 2020-01-31 | 北京京都大成新材料科技有限公司 | Solvent-free bi-component polyurethane laminating adhesive and preparation method thereof |
| CN113667444A (en) * | 2021-09-26 | 2021-11-19 | 湖北回天新材料(宜城)有限公司 | Solvent-free bi-component polyurethane adhesive and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101880516A (en) * | 2010-07-05 | 2010-11-10 | 广东多正化工科技有限公司 | Low free MDI monomer bicomponent solvent-free |
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- 2015-12-03 CN CN201510881504.3A patent/CN105368372A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101880516A (en) * | 2010-07-05 | 2010-11-10 | 广东多正化工科技有限公司 | Low free MDI monomer bicomponent solvent-free |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106520054A (en) * | 2016-11-16 | 2017-03-22 | 北京高盟新材料股份有限公司 | Low-friction-coefficient and solvent-free type polyurethane adhesive and preparation method thereof |
| CN108659770A (en) * | 2018-04-10 | 2018-10-16 | 广东华粘新材料研究有限公司 | A kind of bi-component solvent-free reaction type polyurethane hot melt adhesive and its application method applied to Soft Roll industry |
| CN110092893A (en) * | 2019-05-22 | 2019-08-06 | 无锡风鹏新材料科技有限公司 | A kind of room temperature liquid polyesters and preparation method thereof |
| CN110734732A (en) * | 2019-11-07 | 2020-01-31 | 北京京都大成新材料科技有限公司 | Solvent-free bi-component polyurethane laminating adhesive and preparation method thereof |
| CN113667444A (en) * | 2021-09-26 | 2021-11-19 | 湖北回天新材料(宜城)有限公司 | Solvent-free bi-component polyurethane adhesive and preparation method and application thereof |
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