CN104610513A - Synthetic method for high-softening point modified rosin resin emulsion - Google Patents
Synthetic method for high-softening point modified rosin resin emulsion Download PDFInfo
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- CN104610513A CN104610513A CN201310549645.6A CN201310549645A CN104610513A CN 104610513 A CN104610513 A CN 104610513A CN 201310549645 A CN201310549645 A CN 201310549645A CN 104610513 A CN104610513 A CN 104610513A
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- rosin resin
- modified rosin
- point modified
- resin emulsion
- high softening
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Abstract
The invention discloses a synthetic method for a high-softening point modified rosin resin emulsion, which is characterized in that difficultly-fused high-softening point modified rosin resin emulsion is successfully conversed to liquid state high-softening point modified rosin resin emulsion, the emulsion does not contain a volatile organic solvent, and is conveniently added in an aqueous adhesive for usage, various performances of the adhesive can be increased, a problem that VOC tests for the routine aqueous adhesive volatile organic compounds can not reach a standard can be solved, and heat resistance of the aqueous adhesive can be greatly increased.
Description
Technical field
The present invention relates to the technical field of emulsion synthesize, be specifically related to a kind of synthetic method of high softening-point modified rosin resin emulsion.
Background technology
Common rosin is the mixture of a kind of complexity obtained from rosin, pine torch or tall oil, forms primarily of various diterpenoid resin acid, also containing a small amount of lipid acid and neutrals, is the transparent solid of micro-Huang to yellowish red color under normal temperature, softening temperature 70-90 DEG C.
High softening-point modified rosin resin is formed through reprocessing by common rosin, softening temperature 100-160 DEG C, as polymeric rosin resin, phenolic rosin resin, rosin glycerin ester resin etc., is commonly used for tackifying resin in tackiness agent, increase tack, improve bonding strength and thermotolerance.
High softening-point modified rosin resin is in solid-state at normal temperatures, and be applied in the past in tackiness agent and first will become liquid with organic solvent dissolution, conventional organic solvent is toluene, ethanol, solvent wet goods.Due to adding of these volatile organic solvents, bad impact will certainly be caused on human body and environment, and tackiness agent cannot be tested by volatile organic matter VOC.
Summary of the invention
For the problem that current adhesive industry prior art runs into, the invention provides a kind of synthetic method of high softening-point modified rosin resin emulsion.
Technical scheme of the present invention is as described below: a kind of synthetic method of high softening-point modified rosin resin emulsion, is characterized in that, its composition and weight percent are:
Add high softening-point modified rosin resin and acrylic ester monomer according to the above ratio in a kettle., be heated with stirring to 90-100 DEG C in molten state, then add emulsifying agent, stir.Then, add the deionized water of about 95 DEG C, constantly stir, maintain the temperature between 90-95 DEG C.Finally, add initiator solution, about 90 DEG C insulation reaction 5 hours, be cooled to less than 40 DEG C and filter and package, obtained high softening-point modified rosin resin emulsion.
Described high softening-point modified rosin resin is the one in polymeric rosin resin, phenolic rosin resin, rosin glycerin ester resin.
Described acrylic ester monomer be in vinylformic acid, butyl acrylate, ethyl propenoate, Isooctyl acrylate monomer, methacrylic acid any one or multiple.
Described emulsifying agent is the one in MS-1 emulsifying agent, homemade reactive emulsifier.
Described initiator is the one in ammonium persulphate, Potassium Persulphate, Sodium Persulfate.
Beneficial effect of the present invention is: the synthetic method that the invention discloses a kind of high softening-point modified rosin resin emulsion, it is characterized in that, the high softening-point modified rosin resin successful conversion that infusibility is melted is liquid high softening-point modified rosin resin emulsion, and make this emulsion not containing volatile organic solvent, conveniently be added in aqueous adhesive and use, improve the various performances of tackiness agent, solve standard aqueous tackiness agent volatile organic matter VOC and test problem not up to standard, significantly can improve the thermotolerance of aqueous adhesive simultaneously.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail:
Embodiment 1: polymeric rosin resin (softening temperature 115 DEG C) emulsion synthesize is tested
Being equipped with agitator, prolong, temperature take into account in four mouthfuls of containers of Dropping feeder, adds the polymeric rosin resin of 360g, 20g butyl acrylate and 5g vinylformic acid, after mixing, be heated to 95 DEG C, make polymeric rosin resin be dissolved as molten state completely.Add the MS-1 emulsifying agent of 120g, stir, holding temperature, between 90-100 DEG C, starts the deionized water 300g dripping about 95 DEG C heat, within about 1 hour, dropwises.First 2g Potassium Persulphate is dissolved in 60g deionized water, is then slowly added dropwise in above-mentioned emulsion, within about 0.5 hour, dropwises, remain on about 90 DEG C insulation reaction 5 hours.Be cooled to less than 40 DEG C, filter and package, obtained polymeric rosin resin emulsion.
Embodiment 2: rosin glycerin ester resin (softening temperature 105 DEG C) emulsion synthesize is tested
Being equipped with agitator, prolong, temperature take into account in four mouthfuls of containers of Dropping feeder, add the rosin glycerin ester resin of 400g, 20g Isooctyl acrylate monomer and 5g methacrylic acid, after mixing, be heated to 95 DEG C, make rosin glycerin ester resin be dissolved as molten state completely.Add the MS-1 emulsifying agent of 100g, stir, holding temperature, between 90-100 DEG C, starts the deionized water 320g dripping about 95 DEG C heat, within about 1 hour, dropwises.First 2g ammonium persulphate is dissolved in 60g deionized water, is then slowly added dropwise in above-mentioned emulsion, within about 0.5 hour, dropwises, remain on about 90 DEG C insulation reaction 5 hours.Be cooled to less than 40 DEG C, filter and package, obtained rosin glycerin ester resin emulsion.
Embodiment 3: phenolic rosin resin (softening temperature 146 DEG C) emulsion synthesize is tested
Being equipped with agitator, prolong, temperature take into account in four mouthfuls of containers of Dropping feeder, adds the phenolic rosin resin of 350g, 80g ethyl propenoate, after mixing, be heated to 95 DEG C, make phenolic rosin resin be dissolved as molten state completely.Add the homemade reactive emulsifier of 100g, stir, holding temperature, between 90-100 DEG C, starts the deionized water 300g dripping about 95 DEG C heat, within about 1 hour, dropwises.First 2g Sodium Persulfate is dissolved in 60g deionized water, is then slowly added dropwise in above-mentioned emulsion, within about 0.5 hour, dropwises, remain on about 90 DEG C insulation reaction 5 hours.Be cooled to less than 40 DEG C, filter and package, obtained phenolic rosin resin emulsion.
Embodiment 4: polymeric rosin resin (softening temperature 115 DEG C) emulsion synthesize is tested
Being equipped with agitator, prolong, temperature take into account in the reactor of Dropping feeder, add the polymeric rosin resin of 18kg, 1kg ethyl propenoate and 0.2kg methacrylic acid, after mixing, be heated to 95 DEG C, make polymeric rosin resin be dissolved as molten state completely.Add the homemade reactive emulsifier of 6kg, stir, holding temperature, between 90-100 DEG C, starts the deionized water 15kg dripping about 95 DEG C heat, within about 1 hour, dropwises.First 100g ammonium persulphate is dissolved in 3kg deionized water, is then slowly added dropwise in above-mentioned emulsion, within about 0.5 hour, dropwises, remain on about 90 DEG C insulation reaction 5 hours.Be cooled to less than 40 DEG C, filter and package, obtained polymeric rosin resin emulsion.
Embodiment 5: rosin glycerin ester resin (softening temperature 105 DEG C) emulsion synthesize is tested
Being equipped with agitator, prolong, temperature take into account in the reactor of Dropping feeder, add the rosin glycerin ester resin of 18kg, 1.5kg Isooctyl acrylate monomer and 0.3kg vinylformic acid, after mixing, be heated to 95 DEG C, make rosin glycerin ester resin be dissolved as molten state completely.Add the homemade reactive emulsifier of 6kg, stir, holding temperature, between 90-100 DEG C, starts the deionized water 15kg dripping about 95 DEG C heat, within about 1 hour, dropwises.First 100g ammonium persulphate is dissolved in 3kg deionized water, is then slowly added dropwise in above-mentioned emulsion, within about 0.5 hour, dropwises, remain on about 90 DEG C insulation reaction 5 hours.Be cooled to less than 40 DEG C, filter and package, obtained rosin glycerin ester resin emulsion.
Embodiment 6: phenolic rosin resin (softening temperature 146 DEG C) emulsion synthesize is tested
Being equipped with agitator, prolong, temperature take into account in the reactor of Dropping feeder, adds the phenolic rosin resin of 700kg, 72kg butyl acrylate, after mixing, be heated to 95 DEG C, make phenolic rosin resin be dissolved as molten state completely.Add the homemade reactive emulsifier of 260kg, stir, holding temperature, between 90-100 DEG C, starts the deionized water 1000kg dripping about 95 DEG C heat, within about 1 hour, dropwises.First 8kg Potassium Persulphate is dissolved in 240kg deionized water, is then slowly added dropwise in above-mentioned emulsion, within about 0.5 hour, dropwises, remain on about 90 DEG C insulation reaction 5 hours.Be cooled to less than 40 DEG C, filter and package, obtained phenolic rosin resin emulsion.
Embodiment 7: polymeric rosin resin (softening temperature 140 DEG C) emulsion synthesize is tested
Being equipped with agitator, prolong, temperature take into account in the reactor of Dropping feeder, add the polymeric rosin resin of 18kg, 1.8kg Isooctyl acrylate monomer and 0.5kg butyl acrylate, after mixing, be heated to 95 DEG C, make polymeric rosin resin be dissolved as molten state completely.Add the MS-1 emulsifying agent of 6kg, stir, holding temperature, between 90-100 DEG C, starts the deionized water 15kg dripping about 95 DEG C heat, within about 1 hour, dropwises.First 100g Sodium Persulfate is dissolved in 3kg deionized water, is then slowly added dropwise in above-mentioned emulsion, within about 0.5 hour, dropwises, remain on about 90 DEG C insulation reaction 5 hours.Be cooled to less than 40 DEG C, filter and package, obtained polymeric rosin resin emulsion.
Embodiment 8: phenolic rosin resin (softening temperature 146 DEG C) emulsion synthesize is tested
Being equipped with agitator, prolong, temperature take into account in the reactor of Dropping feeder, add the phenolic rosin resin of 15kg, 1kg ethyl propenoate, 0.2kg Isooctyl acrylate monomer and 0.2kg methacrylic acid, after mixing, be heated to 95 DEG C, make phenolic rosin resin be dissolved as molten state completely.Add the MS-1 emulsifying agent of 6kg, stir, holding temperature, between 90-100 DEG C, starts the deionized water 15kg dripping about 95 DEG C heat, within about 1 hour, dropwises.First 200g ammonium persulphate is dissolved in 6kg deionized water, is then slowly added dropwise in above-mentioned emulsion, within about 0.5 hour, dropwises, remain on about 90 DEG C insulation reaction 5 hours.Be cooled to less than 40 DEG C, filter and package, obtained phenolic rosin resin emulsion.
In sum, the present invention is not limited to above-mentioned embodiment, and persons skilled in the art are in the technical scope disclosed by the present invention, and the change that can expect easily, all within protection scope of the present invention.
Claims (5)
1. a synthetic method for high softening-point modified rosin resin emulsion, is characterized in that, its composition and weight percent are:
Add high softening-point modified rosin resin and acrylic ester monomer according to the above ratio in a kettle., be heated with stirring to 90-100 DEG C in molten state, then add emulsifying agent, stir.Then, add the deionized water of about 95 DEG C, constantly stir, maintain the temperature between 90-95 DEG C.Finally, add initiator solution, about 90 DEG C insulation reaction 5 hours, be cooled to less than 40 DEG C and filter and package, obtained high softening-point modified rosin resin emulsion.
2. the synthetic method of high softening-point modified rosin resin emulsion as claimed in claim 1, is characterized in that: high softening-point modified rosin resin is the one in polymeric rosin resin, phenolic rosin resin, rosin glycerin ester resin.
3. the synthetic method of high softening-point modified rosin resin emulsion as claimed in claim 1, is characterized in that: acrylic ester monomer be in vinylformic acid, butyl acrylate, ethyl propenoate, Isooctyl acrylate monomer, methacrylic acid any one or multiple.
4. the synthetic method of high softening-point modified rosin resin emulsion as claimed in claim 1, is characterized in that: emulsifying agent is the one in MS-1 emulsifying agent, homemade reactive emulsifier.
5. the synthetic method of high softening-point modified rosin resin emulsion as claimed in claim 1, is characterized in that: initiator is the one in ammonium persulphate, Potassium Persulphate, Sodium Persulfate.
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| CN201310549645.6A CN104610513A (en) | 2013-11-02 | 2013-11-02 | Synthetic method for high-softening point modified rosin resin emulsion |
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| CN201310549645.6A CN104610513A (en) | 2013-11-02 | 2013-11-02 | Synthetic method for high-softening point modified rosin resin emulsion |
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Cited By (3)
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| CN105542562A (en) * | 2016-03-14 | 2016-05-04 | 石狮市恒升环保型油墨技术研发中心 | Water-based ink as all-natural renewable resource and preparation method of water-based ink |
| CN107254023A (en) * | 2017-06-26 | 2017-10-17 | 四会市邦得利化工有限公司 | Preparation method and application of graft modified tackifying resin |
| CN111072830A (en) * | 2019-12-31 | 2020-04-28 | 黎月清 | Preparation method of phellandrene resin emulsion |
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| CN105542562A (en) * | 2016-03-14 | 2016-05-04 | 石狮市恒升环保型油墨技术研发中心 | Water-based ink as all-natural renewable resource and preparation method of water-based ink |
| CN107254023A (en) * | 2017-06-26 | 2017-10-17 | 四会市邦得利化工有限公司 | Preparation method and application of graft modified tackifying resin |
| CN107254023B (en) * | 2017-06-26 | 2018-06-29 | 四会市邦得利化工有限公司 | Preparation method and application of graft modified tackifying resin |
| CN111072830A (en) * | 2019-12-31 | 2020-04-28 | 黎月清 | Preparation method of phellandrene resin emulsion |
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Application publication date: 20150513 |