CN102477272A - Environment-friendly waterborne boiling-resistant adhesive and preparation method thereof - Google Patents
Environment-friendly waterborne boiling-resistant adhesive and preparation method thereof Download PDFInfo
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- CN102477272A CN102477272A CN2010105578397A CN201010557839A CN102477272A CN 102477272 A CN102477272 A CN 102477272A CN 2010105578397 A CN2010105578397 A CN 2010105578397A CN 201010557839 A CN201010557839 A CN 201010557839A CN 102477272 A CN102477272 A CN 102477272A
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Abstract
The invention relates to an environment-friendly waterborne boiling-resistant adhesive which comprises three components of colorless phenolic resin, polyester resin, and nanometer titanium dioxide with a weight ratio of 100:100-200:1-2. The preparation method of the adhesive comprises the following steps of: colorless phenolic resin preparation, polyester resin preparation, and nanometer titanium dioxide preparation; during application, the colorless phenolic resin, polyester resin, and nanometer titanium dioxide responsive to visible light are mixed according to a weight ratio of 100:100-200:1-2, and the mixture is dispersed by ultrasonic wave for 0.5 h. The adhesive prepared by the method of the invention belongs to a new material in the field of environmental protection, is nontoxic and harmless, and is widely applicable to the field of packaging of food and medicine.
Description
Technical field
The present invention relates to a kind of sizing agent and method of manufacture thereof, belong to the Process Technology of Polymer technical field, particularly a kind of environment-friendly type water boiling resistance sizing agent and method of manufacture thereof.
Background technology
At present the kind of domestic water based polyurethane also seldom, Application Areas also is confined to the hide finishes aspect.In the laminated film field, the domestic solvent borne polyurethane sizing agent that still uses in a large number, because difficult solvent recovery, so solvent has caused severe contamination all by directly discharging to environment.Selling on the home market from external laminated film use adhesive for polyurethane.
Conventional solvent type sizing agent is long a kind of sizing agent of food product pack sector application time, mainly comprises rubber, thermoplastic resin solution and heat-curable urethane sizing agent.Wherein rubber and thermoplastic resin solution's softening temperature is lower, can not satisfy High Temperature Sterilization, sterilization and the processing request of food packing composite film structure, generally can only be used for the bonding common wrapping material that need not carry out high-temperature sterilization.The heat-curable urethane tackiness agent then can overcome the defective of the former two's non-refractory.The glutinous agent of two-component polyurethane adhesive after the modification and be that main many sizing agents all can satisfy the requirement of anti-cooking food packing bag high-temperature boiling resistant disinfectant with urethane; Make adhesive for polyurethane aspect food product pack, occupy the status that becomes more and more important, especially the type of anti-boiling food product pack sizing agent is main with adhesive for polyurethane especially.Though domestic research to the type polyurethane of anti-boiling sizing agent begins already, the product that quality reaches a standard is also seldom compared the big gap of also existence with advanced country, main at present or dependence on import.And solvent-based adhesive includes a large amount of flammable solvents, to human body, all can work the mischief to environment, though at present always for improving this problem effort, as use the less methods such as solvent of hazardness as far as possible, this harm still exists.If want the harm of avoiding solvent that environment is brought when using solvent-based adhesive, then need expensive solvent recuperation or catalyticcombustion equipment.
Summary of the invention
To the deficiency of above prior art, the present invention provides a kind of environment-friendly type water boiling resistance sizing agent and method of manufacture thereof.
A kind of environment-friendly type water boiling resistance sizing agent is made up of multicolored resol, vibrin, nano titanium oxide three components, and its weight ratio is 100: 100-200: 1-2.
A kind of preparation method of environment-friendly type water boiling resistance sizing agent, it comprises and is prepared as follows step:
1) preparation of multicolored resol
In reaction kettle; Add entry 100 weight parts, start and stir, add phenol 40 weight parts; The adding weight percent is 40% sodium hydroxide solution 6.2-9.0 weight part, and adding Z 150PH 7-10 weight part, adding weight percent are 37% formaldehyde solution 88-100 weight part; Temperature is risen to 90-95 ℃, insulation 40-50min:
Be cooled to 80-85 ℃, add the phenol of 5 weight parts again, keep 80-85 ℃, reach required value until viscosity; Use tartrate to be acidified to the PU value and be 4-6, be cooled to 35-45 ℃, discharging gets multicolored transparent resol:
The said Z 150PH polymerization degree is 3000, and alcoholysis degree is 99%;
2) preparation of vibrin
In reaction kettle, polyethylene terephthalate 100 weight parts that adding is reclaimed, heating and melting adds terepthaloyl moietie 10-20 weight part in fused solution, stirring reaction 2h in the time of 190-230 ℃, cooling back discharging gets vibrin:
3) preparation of nano titanium oxide
In reaction kettle, add deionized water 100 weight parts, start and stir; Add technical grade titanium sulfate 5-8 weight part,, slowly drip unsaturated carbonate hydrogen ammonium solution fully until deposition with sulfuric acid adjust pH 1-4; Ageing 8-12h under the room temperature is dried to constant weight under 75-85 ℃ with microwave again, again roasting sample 2h under 300 ℃ of nitrogen atmospheres; Cooling discharging gets visible light-responded nano titanium oxide:
During use, with colorless phenolic resin, vibrin and visible light-responded nano titanium oxide by weight 100: 100-200: after the 1-2 blend, 0.5h gets final product with ultrasonic dispersing.
Environment-friendly type water boiling resistance sizing agent of the present invention and method of manufacture thereof, what it prepared sizing agent belongs to environmental protection field novel material, nontoxic, can be widely used in food, the pharmaceutical packing field.
Embodiment
Below, with embodiment the present invention is made more detailed description.These embodiment only are the descriptions to best mode for carrying out the invention, scope of the present invention are not had any restriction.
Embodiment 1
1) preparation of colorless phenolic resin
In reaction kettle; Add entry 100 weight parts, start and stir, add phenol 40 weight parts; The adding weight percent is 40% sodium hydroxide solution 6.2 weight parts, and adding Z 150PH 7.5 weight parts, adding weight percent are 37% formaldehyde solution 88 weight parts; Temperature is risen to 90 ℃, insulation 50min; Be cooled to 80 ℃, add the phenol of 5 weight parts again, keep 80 ℃, reach 2571mPa.s until viscosity; Using tartrate to be acidified to pH value is 4, is cooled to 35 ℃, and discharging gets multicolored transparent resol;
The said Z 150PH polymerization degree is 3000, and alcoholysis degree is 99%: the colorless phenolic resin viscosity of present invention is 2571mPa.s, and the content of free aldehyde weight percent is 0.18%.
2) preparation of vibrin
In reaction kettle, polyethylene terephthalate 100 weight parts that adding is reclaimed, heating and melting adds terepthaloyl moietie 10 weight parts in fused solution, stirring reaction 2h in the time of 190-200 ℃, cooling back discharging gets vibrin;
3) preparation of nano titanium oxide
In reaction kettle, add deionized water 100 weight parts, start and stir; Add technical grade titanium sulfate 5 weight parts,, slowly drip unsaturated carbonate hydrogen ammonium solution fully until deposition with sulfuric acid adjust pH 1; Ageing 8h under the room temperature is dried to constant weight under 75 ℃ with microwave again, again roasting sample 2h under 300 ℃ of nitrogen atmospheres; Cooling discharging gets visible light-responded nano titanium oxide; This nano titanium oxide particle diameter is 10-50nm, and in UV, visible light diffuse-reflectance absorption spectrum, the absorbing wavelength scope has been extended to 450-550nm.
During use, after blend in 100: 100: 1.5,0.5h gets final product with ultrasonic dispersing with colorless phenolic resin, vibrin and visible light-responded nano titanium oxide.
Embodiment 2:
1) preparation of colorless phenolic resin
In reaction kettle; Add entry 100 weight parts, start and stir, add phenol 40 weight parts; The adding weight percent is 40% sodium hydroxide solution 9.0 weight parts, and adding Z 150PH 10 weight parts, adding weight percent are 37% formaldehyde solution 100 weight parts; Temperature is risen to 95 ℃, insulation 40min; Be cooled to 85 ℃, add the phenol of 5 weight parts again, keep 85 ℃, when viscosity reaches 4985mPa.s; Using tartrate to be acidified to the PU value is 6, is cooled to 45 ℃, and discharging gets water white resol;
The said Z 150PH polymerization degree is 3000, and alcoholysis degree is 99%.
2) preparation of vibrin
In reaction kettle, polyethylene terephthalate 100 weight parts that adding is reclaimed, heating and melting adds terepthaloyl moietie 20 weight parts in fused solution, stirring reaction 2h in the time of 230 ℃, cooling back discharging gets vibrin.
3) preparation of nano titanium oxide
In reaction kettle, add deionized water 100 weight parts, start and stir; Add technical grade titanium sulfate 8 weight parts,, slowly drip unsaturated carbonate hydrogen ammonium solution fully until deposition with sulfuric acid adjust pH 4; Ageing 12h under the room temperature is dried to constant weight under 85 ℃ with microwave again, again roasting sample 2h under 300 ℃ of nitrogen atmospheres; Cooling discharging gets visible light-responded nano titanium oxide; This nano titanium oxide, particle diameter are 20-50nm, and in UV, visible light diffuse-reflectance absorption spectrum, the absorbing wavelength scope has been extended to the 450-650nm visible region.
During use, after blend in 100: 200: 2,0.5h gets final product with ultrasonic dispersing with multicolored resol, vibrin and visible light-responded nano titanium oxide.
Claims (2)
1. an environment-friendly type water boiling resistance sizing agent is made up of multicolored resol, vibrin, nano titanium oxide three components, and its weight ratio is 100: 100-200: 1-2.
2. the preparation method of environment-friendly type water boiling resistance sizing agent according to claim 1, it comprises and is prepared as follows step:
1) preparation of multicolored resol
In reaction kettle; Add entry 100 weight parts, start and stir, add phenol 40 weight parts; The adding weight percent is 40% sodium hydroxide solution 6.2-9.0 weight part, and adding Z 150PH 7-10 weight part, adding weight percent are 37% formaldehyde solution 88-100 weight part; Temperature is risen to 90-95 ℃, insulation 40-50min:
Be cooled to 80-85 ℃, add the phenol of 5 weight parts again, keep 80-85 ℃, reach required value until viscosity; Use tartrate to be acidified to the PU value and be 4-6, be cooled to 35-45 ℃, discharging gets multicolored transparent resol:
The said Z 150PH polymerization degree is 3000, and alcoholysis degree is 99%;
2) preparation of vibrin
In reaction kettle, polyethylene terephthalate 100 weight parts that adding is reclaimed, heating and melting adds terepthaloyl moietie 10-20 weight part in fused solution, stirring reaction 2h in the time of 190-230 ℃, cooling back discharging gets vibrin:
3) preparation of nano titanium oxide
In reaction kettle, add deionized water 100 weight parts, start and stir; Add technical grade titanium sulfate 5-8 weight part,, slowly drip unsaturated carbonate hydrogen ammonium solution fully until deposition with sulfuric acid adjust pH 1-4; Ageing 8-12h under the room temperature is dried to constant weight under 75-85 ℃ with microwave again, again roasting sample 2h under 300 ℃ of nitrogen atmospheres; Cooling discharging gets visible light-responded nano titanium oxide:
During use, with colorless phenolic resin, vibrin and visible light-responded nano titanium oxide by weight 100: 100-200: after the 1-2 blend, 0.5h gets final product with ultrasonic dispersing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105578397A CN102477272A (en) | 2010-11-23 | 2010-11-23 | Environment-friendly waterborne boiling-resistant adhesive and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105578397A CN102477272A (en) | 2010-11-23 | 2010-11-23 | Environment-friendly waterborne boiling-resistant adhesive and preparation method thereof |
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| CN102477272A true CN102477272A (en) | 2012-05-30 |
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| CN2010105578397A Pending CN102477272A (en) | 2010-11-23 | 2010-11-23 | Environment-friendly waterborne boiling-resistant adhesive and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343521A (en) * | 2008-08-15 | 2009-01-14 | 济南大学 | Preparation method for functional single-sided laminated sheet glue |
| CN101679048A (en) * | 2007-05-31 | 2010-03-24 | 赢创德固赛有限责任公司 | Tackiness agent and sealant systems |
| US20100137485A1 (en) * | 2007-05-22 | 2010-06-03 | Evonik Degussa Gmbh | Adhesives |
-
2010
- 2010-11-23 CN CN2010105578397A patent/CN102477272A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100137485A1 (en) * | 2007-05-22 | 2010-06-03 | Evonik Degussa Gmbh | Adhesives |
| CN101679048A (en) * | 2007-05-31 | 2010-03-24 | 赢创德固赛有限责任公司 | Tackiness agent and sealant systems |
| CN101343521A (en) * | 2008-08-15 | 2009-01-14 | 济南大学 | Preparation method for functional single-sided laminated sheet glue |
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Application publication date: 20120530 |