CN104725592A - Preparation method of maleopimaric double-component waterborne polyurethane - Google Patents
Preparation method of maleopimaric double-component waterborne polyurethane Download PDFInfo
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Abstract
The invention discloses a preparation method of maleopimaric double-component waterborne polyurethane. The preparation method sequentially comprises the following steps: preparing a hydrophilic polyester intermediate; preparing maleopimaric polyester polyol; preparing a maleopimaric polyester polyol aqueous dispersion; and preparing the maleopimaric double-component waterborne polyurethane. According to the preparation method of the maleopimaric double-component waterborne polyurethane disclosed by the invention, a rosin tricyclophenanthrene framework is introduced into the double-component waterborne polyurethane in form of the polyester polyol component, so that the performances of the double-component waterborne polyurethane such as drying time, water resistance, hardness, glossiness and the like are remarkably improved; rosin is an important characteristic forest product resource in China and has the characteristics of being reproducible, green and environment-friendly, low in cost and the like. Rosin is introduced into the double-component waterborne polyurethane, so that not only is the comprehensive performance of a material improved, but also a novel path for development of rosin in direction of high additional value deep processing and utilization is further provided.
Description
Technical field
The present invention relates to a kind of preparation method of maleopimaric acid dual-component aqueous polyurethane, belong to paint field.
Background technology
Waterborne two-component polyurethane coating not only inherits the advantage of water-borne coatings low VOC VOC content, and have mechanical property, the weathering resistance and film formation at low temp etc. of solvent-type double-component urethane excellence concurrently, demonstrate vast potential for future development, become the focus of coatings industry research.Dual-component aqueous polyurethane is primarily of the polyalcohol water dispersoid containing-OH and the polyisocyanate curing agent composition containing-NCO.Polyalcohol water dispersoid is as the hydroxy component of dual-component aqueous polyurethane, its the Nomenclature Composition and Structure of Complexes also has important impact to the performance of dual-component aqueous polyurethane, therefore to the research of polyalcohol water dispersoid be also improve that dual-component aqueous polyurethane is slow at rate of drying, one of the important channel of deficiency in water tolerance and mechanical property etc.
Along with the worsening shortages of fossil resources, polyalcohol water dispersoid synthesis material is to renewable biomass resource future development, develop biomass polyalcohol water dispersion is not only conducive to reducing dual-component aqueous polyurethane cost for the preparation of dual-component aqueous polyurethane, and contribute to realizing polyurethane industrial and transform to the direction of environmental protection and Sustainable development.
Also relevant report rosin or derivatives thereof being introduced aqueous polyurethane is had at present, the application being 101497685 as publication number utilizes rosinyl polyester polyol to prepare aqueous polyurethane, publication number is that a kind of aqueous dispersion of the urethane resin based on rosin has been prepared in the application of 104185647A, but above-mentioned application synthesis be monocomponent waterborne polyurethane.And compared with monocomponent waterborne polyurethane coating, waterborne two-component polyurethane coating due to its cross-linking density high, more excellent in water tolerance, chemical resistant properties, mechanical properties.In addition, because rosin molecular skeleton is comparatively large, steric effect is serious, so it is higher that fat polymerization desired reaction temperature occurs, the polyester viscosity of synthesis is larger.When rosin is incorporated in monocomponent waterborne polyurethane with the form of polyester polyol, required polyester polyol is obtained by rosin derivative and small molecules diol reaction, do not need to consider water dispersible, and required polyester polyol is by rosin derivative and other acid constituents when being incorporated in dual-component aqueous polyurethane, alkoxide component and hydrophilic monomer reaction obtain, and be necessary for water and dispersible type, for time in monocomponent waterborne polyurethane required polyester polyol, time in dual-component aqueous polyurethane, the viscosity of required polyester polyol can not be excessive otherwise affect follow-up dispersion process, and the influence factor of its synthetic technological condition is more, so synthesis comparatively difficulty.The research utilizing rosin polyester polyhydric-alcohol water dispersion to prepare waterborne two-component polyurethane coating aspect at present have not been reported.
Summary of the invention
The invention provides a kind of preparation method of maleopimaric acid dual-component aqueous polyurethane, considerably improve the performances such as the water tolerance of gained maleopimaric acid dual-component aqueous polyurethane, glossiness, gloss and hardness, be conducive to realizing dual-component aqueous polyurethane and transform to the direction of Sustainable development.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is as follows:
A preparation method for maleopimaric acid dual-component aqueous polyurethane, comprises the following steps that order connects:
A, by the mixing of 35 ~ 60 parts of dibasic alcohol, 2 ~ 5 parts of 5-sodium sulfo isophthalates and 0.05 ~ 0.25 part of monohydroxy butyl stannic oxide, at N
2190 ~ 210 DEG C are warming up to, insulation 20 ~ 50min under protection;
B, the reaction mass of steps A gained is cooled to 130 ~ 160 DEG C, adds 5 ~ 45 parts of maleopimaric acids, 20 ~ 45 parts of aromatic acids, 10 ~ 35 parts of hexanodioic acids and 5 ~ 13 parts of TriMethylolPropane(TMP)s, be warming up to 210 ~ 240 DEG C, insulation 40 ~ 70min; Then, in reaction system, add 2 ~ 8 parts of dimethylbenzene, at 210 ~ 240 DEG C after back flow reaction 130 ~ 160min, be cooled to 130 ~ 160 DEG C, decompression vacuum pumping 15 ~ 30min;
C, at 60 ~ 90 DEG C, in step B gained material, add quality and be 70 ~ 140 parts of water and diethylene glycol ether acetate alone, high-speed stirring, obtains the water dispersion that solid content is 45 ~ 60%, wherein, the mass ratio of water and diethylene glycol ether acetate alone is (3.5 ~ 4.5): 1;
D, by the water dispersion of water-based isocyanate and step C gained according to n
(-NCO): n
(-OH)the ratio mixing of=(1.1:1) ~ (3:1), and thin up, obtained solid content is 45% ~ 60% maleopimaric acid dual-component aqueous polyurethane;
In each step, number is mass fraction.
Above-mentioned steps A gained is hydrophilic polyester intermediate HPI, and step B gained is maleopimaric acid polyester polyol MPP, and step C gained is maleopimaric acid aqueous polyester polyol dispersoid MPPD.
Aforesaid method passes through esterification, luxuriant and rich with fragrance for rosin three ring skeleton is introduced in polyester polyol, and the polyester polyol of gained can well be dispersed in water, and considerably improve water tolerance, glossiness, the performance such as gloss and hardness of gained maleopimaric acid dual-component aqueous polyurethane.
In order to improve the over-all properties of products obtained therefrom further, in steps A, at N
2with ramp to 190 ~ 210 DEG C of 1 ± 0.5 DEG C/min under protection.
Be controlled better in order to reaction process can be made, thus improve the over-all properties of products obtained therefrom further, the reaction mass of steps A gained is cooled to 130 ~ 160 DEG C by step B, add 5 ~ 45 parts of maleopimaric acids, 20 ~ 45 parts of aromatic acids, 10 ~ 35 parts of hexanodioic acids and 5 ~ 13 parts of TriMethylolPropane(TMP)s, 210 ~ 240 DEG C are warming up to, insulation 40 ~ 70min with the temperature rise rate of 0.5 ± 0.2 DEG C/min; Then, in reaction system, add 2 ~ 8 parts of dimethylbenzene, at 210 ~ 240 DEG C after back flow reaction 130 ~ 160min, be cooled to 130 ~ 160 DEG C, then be warming up to 185 ~ 195 DEG C with the temperature rise rate of 4 ± 1 DEG C/min, decompression vacuum pumping while intensification.
The above-mentioned object vacuumized removes the by product of removal xylene and small-molecular-weight, dimethylbenzene removing can without the need to too high-temperature at 150 ~ 160 DEG C, follow-up temperature progressively rising is by product in order to remove unreacted alcohol and small-molecular-weight and purified product, if directly vacuumize the splashing that liquid easily occurs at 210 ~ 240 DEG C after back flow reaction 130 ~ 160min, if directly cool the temperature to 185 ~ 195 DEG C to vacuumize, product viscosity then synthesized by same time is large, thus, preferably first lower the temperature, and then with decompression vacuum pumping while specific ramp, such product property that can make reaches best.
In order to improve stability dispersions obtained in step C further, the speed of high-speed stirring is 1800 ~ 2200r/min, and churning time is 30 ~ 50min.
In above-mentioned steps D, do not add any auxiliary agent and also can reach good levelling property, but in order to improve the levelling property of products obtained therefrom further, before thin up, preferably add the flow agent of 0.1 ~ 0.3 part, described number is mass fraction.
Above-mentioned flow agent can select existing conventional any type, but in order on the basis ensureing levelling property, make the synergistic effect between each component perform to the best, described flow agent is Byk 348 flow agent.
Dibasic alcohol in above-mentioned steps A can select existing conventional any type, but in order to further ensure the over-all properties of products obtained therefrom, is preferably 2-ethyl-2 butyl-1,3-PD, neopentyl glycol or 1,4 cyclohexane dimethanol; More preferably neopentyl glycol.
In above-mentioned steps B, aromatic acid can select existing conventional any type, but in order to further ensure the over-all properties of products obtained therefrom, is preferably m-phthalic acid, phthalate anhydride or phthalic acid; More preferably m-phthalic acid.
Above-mentioned water-based isocyanate can select existing conventional any type, but in order to the over-all properties of products obtained therefrom can be made to perform to the best, is preferably Bayer water-based isocyanate solidifying agent 3100.
The NM technology of the present invention is all with reference to prior art.
Luxuriant and rich with fragrance for rosin three ring skeleton is introduced in dual-component aqueous polyurethane with the form of polyester polyol component by the preparation method of maleopimaric acid dual-component aqueous polyurethane of the present invention, significantly improves the performances such as the time of drying of dual-component aqueous polyurethane, water tolerance, hardness and glossiness; And the rosin characteristic Forest products resource that to be China important, there is renewable, environmental protection and the characteristic such as cost is low, be introduced in dual-component aqueous polyurethane the over-all properties not only contributing to improving material, and provide new way for rosin to high added value and deep processing and utilization future development.
Accompanying drawing explanation
Fig. 1 is the infrared spectrum of embodiment 1 gained hydrophilic polyester intermediate (HPI), MPP (reaction 0h) and MPP (reaction terminates);
Fig. 2 is embodiment 1 gained maleopimaric acid polyester polyol
13c NMR schemes;
Fig. 3 is the infrared spectrum of embodiment 1 gained maleopimaric acid dual-component aqueous polyurethane.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
Embodiment 1
40 parts of neopentyl glycol, 2.5 parts of 5-sodium sulfo isophthalates, 0.1 part of monohydroxy butyl stannic oxide are joined in reaction vessel, at N
2with the ramp to 190 DEG C of 1 DEG C/min under protection, insulation 50min, obtains hydrophilic polyester intermediate (HPI).When above-mentioned reaction system is cooled to 150 DEG C, add 9.2 parts of maleopimaric acids, 40 parts of m-phthalic acids, 30 parts of hexanodioic acids, 10 parts of TriMethylolPropane(TMP)s, 210 DEG C are warming up to the temperature rise rate of 0.5 DEG C/min, insulation 70min, then, 7 parts of dimethylbenzene are added in reaction system, at 210 DEG C after back flow reaction 160min, start when being cooled to 150 DEG C to be warming up to 190 DEG C with the temperature rise rate of 4 DEG C/min, decompression vacuum pumping while heating up, obtained maleopimaric acid polyester polyol (MPP).At 60 DEG C, in MPP, add quality and be diethylene glycol ether acetate alone and the water (mass ratio of water and diethylene glycol ether acetate alone is 4:1) of 80 parts, after high-speed stirring (stir speed (S.S.) is 2000r/min) 40min, obtained solid content is 50 ~ 55% maleopimaric acid aqueous polyester polyol dispersoids (MPPD).By 50 parts of MPPD, 14 parts
3100 water-based isocyanates, 0.23 part of Byk 348 flow agent, after mixing, thin up, obtained solid content 50 ~ 55% maleopimaric acid dual-component aqueous polyurethane.
Comparative example 1
40 parts of neopentyl glycol, 2.5 parts of 5-sodium sulfo isophthalates, 0.1 part of monohydroxy butyl stannic oxide are joined in reaction vessel, at N
2with the ramp to 190 DEG C of 1 DEG C/min under protection, insulation 50min, obtains hydrophilic polyester intermediate (HPI).When above-mentioned reaction system is cooled to 150 DEG C, add 0 part of maleopimaric acid, 40 parts of m-phthalic acids, 30 parts of hexanodioic acids, 10 parts of TriMethylolPropane(TMP)s, 210 DEG C are warming up to the temperature rise rate of 0.5 DEG C/min, insulation 70min, then, 7 parts of dimethylbenzene are added in reaction system, at 210 DEG C after back flow reaction 160min, start when being cooled to 150 DEG C to be warming up to 190 DEG C with the temperature rise rate of 4 DEG C/min, decompression vacuum pumping while heating up, cooling discharge, obtained maleopimaric acid polyester polyol (MPP).At 60 DEG C, in MPP, add quality and be diethylene glycol ether acetate alone and the water (mass ratio of water and diethylene glycol ether acetate alone is 4:1) of 80 parts, after high-speed stirring (stir speed (S.S.) is 2000r/min) 40min, obtained solid content is 50 ~ 55% maleopimaric acid aqueous polyester polyol dispersoids (MPPD).By 50 parts of MPPD, 14 parts
3100 water-based isocyanates, 0.23 part of Byk 348 flow agent, after mixing, thin up, obtained solid content 50 ~ 55% maleopimaric acid dual-component aqueous polyurethane.
Embodiment 2
55 parts of neopentyl glycol, 4 parts of 5-sodium sulfo isophthalates, 0.25 part of monohydroxy butyl stannic oxide are joined in reaction vessel, at N
2with the ramp to 210 DEG C of 1 DEG C/min under protection, insulation 20min, obtains hydrophilic polyester intermediate (HPI).When above-mentioned reaction system is cooled to 150 DEG C, add 43 parts of maleopimaric acids, 25 parts of m-phthalic acids, 20 parts of hexanodioic acids, 7 parts of TriMethylolPropane(TMP)s, 240 DEG C are warming up to the temperature rise rate of 0.5 DEG C/min, insulation 40min, then, 5.5 parts of dimethylbenzene are added in reaction system, at 240 DEG C after back flow reaction 130min, start when being cooled to 140 DEG C to be warming up to 190 DEG C with the temperature rise rate of 4 DEG C/min, decompression vacuum pumping while heating up, cooling discharge, obtained maleopimaric acid polyester polyol (MPP).At 90 DEG C, in MPP, add quality and be diethylene glycol ether acetate alone and the water (mass ratio of water and diethylene glycol ether acetate alone is 4:1) of 110 parts, after high-speed stirring (stir speed (S.S.) is 2000r/min) 40min, obtained solid content is 50 ~ 55% maleopimaric acid aqueous polyester polyol dispersoids (MPPD).By 50 parts of MPPD, 14 parts
3100 water-based isocyanates, 0.23 part of Byk 348 flow agent, after mixing, thin up, obtained solid content 50 ~ 55% maleopimaric acid dual-component aqueous polyurethane.
Comparative example 2
55 parts of neopentyl glycol, 4 parts of 5-sodium sulfo isophthalates, 0.25 part of monohydroxy butyl stannic oxide are joined in reaction vessel, at N
2with the ramp to 210 DEG C of 1 DEG C/min under protection, insulation 20min, obtains hydrophilic polyester intermediate (HPI).When above-mentioned reaction system is cooled to 150 DEG C, add 0 part of maleopimaric acid, 25 parts of m-phthalic acids, 20 parts of hexanodioic acids, 7 parts of TriMethylolPropane(TMP)s, 240 DEG C are warming up to the temperature rise rate of 0.5 DEG C/min, insulation 40min, then, 5.5 parts of dimethylbenzene are added in reaction system, at 240 DEG C after back flow reaction 130min, start when being cooled to 140 DEG C to be warming up to 190 DEG C with the temperature rise rate of 4 DEG C/min, decompression vacuum pumping while heating up, cooling discharge, obtained maleopimaric acid polyester polyol (MPP).At 90 DEG C, in MPP, add quality and be diethylene glycol ether acetate alone and the water (mass ratio of water and diethylene glycol ether acetate alone is 4:1) of 110 parts, after high-speed stirring (stir speed (S.S.) is 2000r/min) 40min, obtained solid content is 50 ~ 55% maleopimaric acid aqueous polyester polyol dispersoids (MPPD).By 50 parts of MPPD, 14 parts
3100 water-based isocyanates, 0.23 part of Byk 348 flow agent, after mixing, thin up, obtained solid content 50 ~ 55% maleopimaric acid dual-component aqueous polyurethane.
Embodiment 3
45 parts of neopentyl glycol, 3 parts of 5-sodium sulfo isophthalates, 0.15 part of monohydroxy butyl stannic oxide are joined in reaction vessel, at N
2with the ramp to 200 DEG C of 1 DEG C/min under protection, insulation 35min, obtains hydrophilic polyester intermediate (HPI).When above-mentioned reaction system is cooled to 150 DEG C, add 19 parts of maleopimaric acids, 35 parts of m-phthalic acids, 25 parts of hexanodioic acids, 9 parts of TriMethylolPropane(TMP)s, 220 DEG C are warming up to the temperature rise rate of 0.5 DEG C/min, insulation 60min, then, 6 parts of dimethylbenzene are added in reaction system, at 220 DEG C after back flow reaction 150min, start when being cooled to 150 DEG C to be warming up to 190 DEG C with the temperature rise rate of 4 DEG C/min, decompression vacuum pumping while heating up, cooling discharge, obtained maleopimaric acid polyester polyol (MPP).At 70 DEG C, in MPP, add quality and be diethylene glycol ether acetate alone and the water (mass ratio of water and diethylene glycol ether acetate alone is 4:1) of 90 parts, after high-speed stirring (stir speed (S.S.) is 2000r/min) 40min, obtained solid content is 50 ~ 55% maleopimaric acid aqueous polyester polyol dispersoids (MPPD).By 50 parts of MPPD, 14 parts
3100 water-based isocyanates, 0.23 part of Byk 348 flow agent, after mixing, thin up, obtained solid content 50 ~ 55% maleopimaric acid dual-component aqueous polyurethane.
Embodiment 4
50 parts of neopentyl glycol, 3.5 parts of 5-sodium sulfo isophthalates, 0.2 part of monohydroxy butyl stannic oxide are joined in reaction vessel, at N
2with the ramp to 210 DEG C of 1 DEG C/min under protection, insulation 20min, obtains hydrophilic polyester intermediate (HPI).When above-mentioned reaction system is cooled to 150 DEG C, add 29.6 parts of maleopimaric acids, 30 parts of m-phthalic acids, 20 parts of hexanodioic acids, 8 parts of TriMethylolPropane(TMP)s, 230 DEG C are warming up to the temperature rise rate of 0.5 DEG C/min, insulation 50min, then, 5 parts of dimethylbenzene are added in reaction system, at 230 DEG C after back flow reaction 140min, start when being cooled to 150 DEG C to be warming up to 190 DEG C with the temperature rise rate of 4 DEG C/min, decompression vacuum pumping while heating up, cooling discharge, obtained maleopimaric acid polyester polyol (MPP).At 80 DEG C, in MPP, add quality and be diethylene glycol ether acetate alone and the water (mass ratio of water and diethylene glycol ether acetate alone is 4:1) of 95 parts, after high-speed stirring (stir speed (S.S.) is 2000r/min) 40min, obtained solid content is 50 ~ 55% maleopimaric acid aqueous polyester polyol dispersoids (MPPD).By 50 parts of MPPD, 14 parts
3100 water-based isocyanates, 0.23 part of Byk 348 flow agent, after mixing, thin up, obtained solid content 50 ~ 55% maleopimaric acid dual-component aqueous polyurethane.
The performances such as time of drying of maleopimaric acid dual-component aqueous polyurethane, pencil hardness, snappiness, glossiness and shock-resistance are detected respectively according to standard GB/T/T 1728-1989, GB/T 6739-2006, GB/T 1731-1993, GB/T1743-1989, GB/T 1732-1993, and contrast with the performance of the dual-component aqueous polyurethane prepared by commercially available polyester water dispersion Bayhydrol D 270 (specifically preparing the preparation method see maleopimaric acid dual-component aqueous polyurethane in embodiment 1), the results are shown in Table 1.
The performance of table 1 maleopimaric acid dual-component aqueous polyurethane
Respectively example 1 and 2 and comparative example 1 and 2 are compared discovery, the application's dual-component aqueous polyurethane all has obvious lifting in time of drying, hardness, glossiness and water-intake rate etc.; The dual-component aqueous polyurethane prepared from MPPD and Bayhydrol D 270 and the application are carried out contrast, and the correlated performance of the application's maleopimaric acid dual-component aqueous polyurethane is better than the performance of the dual-component aqueous polyurethane prepared by commercially available water dispersion.In addition, compared with the water-intake rate of maleopimaric acid monocomponent waterborne polyurethane (24h 14.4%), the water-intake rate of maleopimaric acid dual-component aqueous polyurethane obviously reduces.Therefore, rosin structure to be introduced in dual-component aqueous polyurethane by special preparation and is not only contributed to the performance improving dual-component aqueous polyurethane by the application, and is conducive to realizing dual-component aqueous polyurethane and transforms to the direction of Sustainable development.
Claims (10)
1. a preparation method for maleopimaric acid dual-component aqueous polyurethane, is characterized in that: comprise the following steps that order connects:
A, by the mixing of 35 ~ 60 parts of dibasic alcohol, 2 ~ 5 parts of 5-sodium sulfo isophthalates and 0.05 ~ 0.25 part of monohydroxy butyl stannic oxide, at N
2190 ~ 210 DEG C are warming up to, insulation 20 ~ 50min under protection;
B, the reaction mass of steps A gained is cooled to 130 ~ 160 DEG C, adds 5 ~ 45 parts of maleopimaric acids, 20 ~ 45 parts of aromatic acids, 10 ~ 35 parts of hexanodioic acids and 5 ~ 13 parts of TriMethylolPropane(TMP)s, be warming up to 210 ~ 240 DEG C, insulation 40 ~ 70min; Then, in reaction system, add 2 ~ 8 parts of dimethylbenzene, at 210 ~ 240 DEG C after back flow reaction 130 ~ 160min, be cooled to 130 ~ 160 DEG C, decompression vacuum pumping;
C, at 60 ~ 90 DEG C, in step B gained material, add quality and be 70 ~ 140 parts of water and diethylene glycol ether acetate alone, high-speed stirring, obtains the water dispersion that solid content is 45 ~ 60%, wherein, the mass ratio of water and diethylene glycol ether acetate alone is (3.5 ~ 4.5): 1;
D, by the water dispersion of water-based isocyanate and step C gained according to n
(-NCO): n
(-OH)the ratio mixing of=(1.1:1) ~ (3:1), and thin up, obtained solid content is 45% ~ 60% maleopimaric acid dual-component aqueous polyurethane;
In each step, number is mass fraction.
2. preparation method as claimed in claim 1, is characterized in that: the dibasic alcohol in steps A is 2-ethyl-2 butyl-1,3-PD, neopentyl glycol or 1,4 cyclohexane dimethanol.
3. preparation method as claimed in claim 2, is characterized in that: the dibasic alcohol in steps A is neopentyl glycol.
4. the preparation method as described in claim 1-3 any one, is characterized in that: in steps A, at N
2with ramp to 190 ~ 210 DEG C of 1 ± 0.5 DEG C/min under protection.
5. the preparation method as described in claim 1-3 any one, is characterized in that: in step B, aromatic acid is m-phthalic acid, phthalate anhydride or phthalic acid.
6. preparation method as claimed in claim 5, is characterized in that: in step B, aromatic acid is m-phthalic acid.
7. the preparation method as described in claim 1-3 any one, it is characterized in that: the reaction mass of steps A gained is cooled to 130 ~ 160 DEG C by step B, add 5 ~ 45 parts of maleopimaric acids, 20 ~ 45 parts of aromatic acids, 10 ~ 35 parts of hexanodioic acids and 5 ~ 13 parts of TriMethylolPropane(TMP)s, 210 ~ 240 DEG C are warming up to, insulation 40 ~ 70min with the temperature rise rate of 0.5 ± 0.2 DEG C/min; Then, in reaction system, add 2 ~ 8 parts of dimethylbenzene, at 210 ~ 240 DEG C after back flow reaction 130 ~ 160min, be cooled to 130 ~ 160 DEG C, then be warming up to 185 ~ 195 DEG C with the temperature rise rate of 4 ± 1 DEG C/min, decompression vacuum pumping while intensification.
8. the preparation method as described in claim 1-3 any one, is characterized in that: in step C, and the speed of high-speed stirring is 1800 ~ 2200r/min, and churning time is 30 ~ 50min.
9. the preparation method as described in claim 1-3 any one, is characterized in that: in step D, before thin up, adds the flow agent of 0.1 ~ 0.3 part, and described number is mass fraction.
10. preparation method as claimed in claim 9, it is characterized in that: in step D, described flow agent is Byk 348 flow agent.
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| CN111019074A (en) * | 2019-12-31 | 2020-04-17 | 苏州世华新材料科技股份有限公司 | Self-extinction resin emulsion, preparation method and application thereof in water-based matte ink |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105504216A (en) * | 2015-12-21 | 2016-04-20 | 桂林市和鑫防水装饰材料有限公司 | Preparation method of rosin-based waterborne polyurethane waterproof material |
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| CN111019074A (en) * | 2019-12-31 | 2020-04-17 | 苏州世华新材料科技股份有限公司 | Self-extinction resin emulsion, preparation method and application thereof in water-based matte ink |
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| CN115141341A (en) * | 2022-06-26 | 2022-10-04 | 瀚寅(苏州)新材料科技有限公司 | Combined polyether for full-water-blown polyurethane and preparation method thereof |
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