CN105622940A - Multi-branched-chain high-activity water-based resin prepolymer and preparation method thereof - Google Patents
Multi-branched-chain high-activity water-based resin prepolymer and preparation method thereof Download PDFInfo
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- CN105622940A CN105622940A CN201610102621.XA CN201610102621A CN105622940A CN 105622940 A CN105622940 A CN 105622940A CN 201610102621 A CN201610102621 A CN 201610102621A CN 105622940 A CN105622940 A CN 105622940A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
- C08G77/16—Polysiloxanes containing silicon bound to oxygen-containing groups to hydroxyl groups
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
- C09D183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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Abstract
The invention discloses multi-branched-chain high-activity water-based resin prepolymer and a synthetic method thereof.Hydroxide radicals in the prepolymer are associated with hydrogen bonds in water, a polyhydroxy group enables the prepolymer to be dissolved in water easily, and therefore the prepolymer is transparent liquid high in solid content and can be dissolved in water easily.In the crosslinking curing process, the hydroxide radicals disappear with dehydration and polycondensation, and finally a water resistant coating which is extremely high in hardness and fullness is formed.The high-activity hydroxide radicals of the prepolymer can be dehydrated and polycondensated automatically at the normal temperature without action of a catalyst, a film is formed through crosslinking, and the prepolymer is suitable for making various types of water-based paints with wood lacquer as the majority.The synthetic method of the prepolymer is simple in step, the reaction condition is easy to control, the equipment requirement is low, and the production cost is effectively lowered.
Description
Technical field
The present invention relates to organic high molecular compound, in particular to a kind of higly branched chain high reactivity water-based resin prepolymer and its preparation method.
Background technology
Existing decoration coating type is a lot, along with modern's human-subject test and growth in the living standard, house ornamentation environmental requirement is more and more higher. But existing environment-friendly type coating weak effect, it is difficult to promote.
Existing coating resin is taken as the leading factor with the organic polymer such as urethane, polyacrylic ester substantially, will realize the Water-borne modification of solution. Common way is, introduces the hydrophilic radical such as amino, ether base on above-mentioned organic polymer molecules chain, makes it to form W/O or O/W micella, oil phase substance dispersion property in aqueous phase emulsion. And in order to ensure suitable solid content and control the viscosity of emulsion, polymkeric substance often needs to form linear molecule chain. In addition, solvent type curing system is difficult to effect in aqueous phase; Micella is to being cross-linked to form certain barrier; Hydrophilic radical remains in paint film, and therefore, hardness and fullness ratio and water tolerance and even film texture, all do not reach the effect of solvent based coating.
Summary of the invention
It is an object of the invention to provide a kind of higly branched chain high reactivity water-based resin prepolymer and its preparation method, at least can one of solve the problem.
, it provides a kind of higly branched chain high reactivity water-based resin prepolymer, for achieving the above object, according to an aspect of the present invention the general formula of performed polymer is:
Wherein, R ' expression monovalence hydrophobic grouping, M represents metallicity element, and n, m are natural number.
In some embodiments, R ' expression alkyl, halohydrocarbon, nitro-NO2, ester group-COO-, M represents C, Sn, Si, Ti, Zr or Ge.
In some embodiments, n=4.
Correspondingly, present invention also offers the synthetic method of a kind of higly branched chain high reactivity water-based resin prepolymer, comprise the following steps:
By the chain polymer that initial cell element polycondensation is hydroxyl, wherein, m is natural number, and R ' all represents monovalence hydrophobic grouping;
By the chain polymer that initial cell element polycondensation is band short-chain branch, reaction formula is:
In some embodiments, also comprise step: metal alkoxide hydrolysis is formed initial cell, and reaction formula is:
R��M(OH)n-1+xH2O��R��M(OR)n-1+ xR-OH, wherein, x=n-1, R and R ' all represent monovalence hydrophobic grouping;
In some embodiments, the chain polymer polycondensation of hydroxyl chain polymer and band short-chain branch being obtained higly branched chain high reactivity water-based resin prepolymer, reaction formula is:
In some embodiments, the synthetic method of higly branched chain high reactivity water-based resin prepolymer, concrete steps are as follows:
Raw material prepares: the mol ratio of Union carbide A-162 and dimethyldiethoxysilane is 1��1.4:1, the mol ratio of lauryl alcohol and methyltrimethoxy silane is 0.8��0.95:1, the mol ratio of deionized water and Union carbide A-162 is 1.2��1.8:1, catalyst A is the 0.6% of reactant total mass, catalyst B is the 1.8% of reactant total mass, and wherein catalyst A and catalyst B are organometallic catalysts;
Polycondensation: in above-mentioned raw materials ratio, two kinds of silane and catalyst A are added in four-hole bottle, stirs and heat to 75 DEG C, drip ionized water, within 20 minutes, drip, 85 DEG C of back flow reaction two hours, 85 DEG C steam ethanol, then, add catalyst B and lauryl alcohol, heat to 130 DEG C, reflux 2��4 hours, obtain higly branched chain high reactivity water-based resin prepolymer.
In some embodiments, the synthetic method of higly branched chain high reactivity water-based resin prepolymer, concrete steps are as follows:
Raw material prepares: the mol ratio of Union carbide A-162 and dimethyldiethoxysilane is 1.2:1, the mol ratio of lauryl alcohol and methyltrimethoxy silane is 0.9:1, the mol ratio of deionized water and Union carbide A-162 is 1.6:1, catalyst A is the 0.6% of reactant total mass, and catalyst B is the 1.8% of reactant total mass;
Polycondensation: in above-mentioned raw materials ratio, two kinds of silane and catalyst A are added in four-hole bottle, stirs and heat to 75 DEG C, drip ionized water, within 20 minutes, drip, 85 DEG C of back flow reaction two hours, 85 DEG C steam ethanol, then, add catalyst B and lauryl alcohol, heat to 130 DEG C, reflux 3 hours, obtain higly branched chain high reactivity water-based resin prepolymer.
The useful effect of the present invention is: the higly branched chain high reactivity water-base resin of the present invention is in crosslinking curing process, and hydroxyl disappears along with dehydrating polycondensation, finally forms the water-fast rete that hardness, fullness ratio are extremely high. The high reactivity hydroxyl of this performed polymer can under normal temperature and catalyst-free effect dehydrating polycondensation voluntarily, crosslinked film forming, all kinds of water-borne coatingss of suitable for making based on wood lacquer. The synthetic method step of this performed polymer is simple, and easily-controlled reaction conditions is low for equipment requirements, effectively reduces production cost.
Embodiment
The present invention is further detailed explanation below.
The higly branched chain high reactivity water-based resin prepolymer of the present invention, performed polymer is linear polymer, and its general formula is:
Wherein, R ' expression monovalence hydrophobic grouping, such as alkyl, halohydrocarbon, nitro-NO2, ester group-COO-; M represents metallicity element, C, Sn, Si, Ti, Zr or Ge; M is natural number, n=4. Ester group-COO-is ester group-COO-ester or ester group-COO-grease
The synthetic method of above-mentioned higly branched chain high reactivity water-based resin prepolymer, comprises the following steps:
A, by metal alkoxide hydrolysis formed initial cell, reaction formula is:
R��M(OR)n-1+xH2O��R��M(OH)n-1+ xR-OH, wherein, x=n-1, R and R ' all representing monovalence hydrophobic grouping, M represents metallicity element;
B, being hydroxyl chain polymer by initial cell element polycondensation, wherein, m is natural number,
C, being the chain polymer of band short-chain branch by initial cell element polycondensation, reaction formula is:
D, the chain polymer polycondensation of hydroxyl chain polymer and band short-chain branch being obtained higly branched chain high reactivity water-based resin prepolymer, reaction formula is:
Specifically, the synthetic method of above-mentioned performed polymer is:
Raw material prepares: the mol ratio of Union carbide A-162 and dimethyldiethoxysilane is 1��1.4:1, the mol ratio of lauryl alcohol and methyltrimethoxy silane is 0.8��0.95:1, the mol ratio of deionized water and Union carbide A-162 is 1.2��1.8:1, catalyst A is the 0.6% of reactant total mass, catalyst B is the 1.8% of reactant total mass, and wherein catalyst A and catalyst B are organometallic catalysts;
Polycondensation: in above-mentioned raw materials ratio, two kinds of silane and catalyst A are added in four-hole bottle, stirs and heat to 75 DEG C, drip ionized water, within 20 minutes, drip, 85 DEG C of back flow reaction two hours, 85 DEG C steam ethanol, then, add catalyst B and lauryl alcohol, heat to 130 DEG C, reflux 2��4 hours, obtain higly branched chain high reactivity water-based resin prepolymer.
Raw material adopts Union carbide A-162, dimethyldiethoxysilane and lauryl alcohol, and three is formed under specific reaction conditions and meets general formula R ' M (OH)n-1Initial cell, then obtains higly branched chain high reactivity water-based resin prepolymer through series reaction.
Under the existence of lauryl alcohol, the carbon chain lengths of the side chain of the higly branched chain high reactivity water-based resin prepolymer obtained reaches 12, side chain has greater depth so that higly branched chain high reactivity water-based resin prepolymer is applied in coating, can form the good paint film of pliability fullness ratio.
Adopt above-mentioned reaction conditions so that the backbone length of higly branched chain high reactivity water-based resin prepolymer is m, and m >=6 so that higly branched chain high reactivity water-based resin prepolymer is applied in coating, can form the good paint film of hardness.
The synthetic method embodiment 1 of higly branched chain high reactivity water-based resin prepolymer
Raw material prepares: the mol ratio of Union carbide A-162 and dimethyldiethoxysilane is 1.2:1, the mol ratio of lauryl alcohol and methyltrimethoxy silane is 0.9:1, the mol ratio of deionized water and Union carbide A-162 is 1.6:1, catalyst A is the 0.6% of reactant total mass, and catalyst B is the 1.8% of reactant total mass;
Polycondensation: in above-mentioned raw materials ratio, two kinds of silane and catalyst A are added in four-hole bottle, stirs and heat to 75 DEG C, drip ionized water, within 20 minutes, drip, 85 DEG C of back flow reaction two hours, 85 DEG C steam ethanol, then, add catalyst B and lauryl alcohol, heat to 130 DEG C, reflux 3 hours, obtain higly branched chain high reactivity water-based resin prepolymer.
The synthetic method embodiment 2 of higly branched chain high reactivity water-based resin prepolymer
Raw material prepares: the mol ratio of Union carbide A-162 and dimethyldiethoxysilane is 1:1, the mol ratio of lauryl alcohol and methyltrimethoxy silane is 0.8:1, the mol ratio of deionized water and Union carbide A-162 is 1.2:1, catalyst A is the 0.6% of reactant total mass, and catalyst B is the 1.8% of reactant total mass;
Polycondensation: in above-mentioned raw materials ratio, two kinds of silane and catalyst A are added in four-hole bottle, stirs and heat to 75 DEG C, drip ionized water, within 20 minutes, drip, 85 DEG C of back flow reaction two hours, 85 DEG C steam ethanol, then, add catalyst B and lauryl alcohol, heat to 130 DEG C, reflux 4 hours, obtain higly branched chain high reactivity water-based resin prepolymer.
The synthetic method embodiment 3 of higly branched chain high reactivity water-based resin prepolymer
Raw material prepares: the mol ratio of Union carbide A-162 and dimethyldiethoxysilane is 1.4:1, the mol ratio of lauryl alcohol and methyltrimethoxy silane is 0.95:1, the mol ratio of deionized water and Union carbide A-162 is 1.8:1, catalyst A is the 0.6% of reactant total mass, and catalyst B is the 1.8% of reactant total mass;
Polycondensation: in above-mentioned raw materials ratio, two kinds of silane and catalyst A are added in four-hole bottle, stirs and heat to 75 DEG C, drip ionized water, within 20 minutes, drip, 85 DEG C of back flow reaction two hours, 85 DEG C steam ethanol, then, add catalyst B and lauryl alcohol, heat to 130 DEG C, reflux 2 hours, obtain higly branched chain high reactivity water-based resin prepolymer.
Above-described is only some embodiments of the present invention. , it is also possible to make some distortion and improvement, for the person of ordinary skill of the art, without departing from the concept of the premise of the invention these all belong to protection scope of the present invention.
Claims (6)
1. higly branched chain high reactivity water-based resin prepolymer, it is characterised in that, the general formula of described performed polymer is:
Wherein, R ' expression monovalence hydrophobic grouping, M represents metallicity element, and n, m are natural number.
2. higly branched chain high reactivity water-based resin prepolymer according to claim 1, it is characterised in that, the functional group of R ' is alkyl, halohydrocarbon, nitro-NO2Or ester group-COO-, M represents C, Sn, Si, Ti, Zr or Ge.
3. higly branched chain high reactivity water-based resin prepolymer according to claim 2, it is characterised in that, n=4.
4. the synthetic method of higly branched chain high reactivity water-based resin prepolymer, it is characterised in that, comprise following chemical reaction step:
Metal alkoxide hydrolysis forms initial cell, and reaction formula is:
R��M(OR)n-1+xH2O��R��M(OH)n-1+ xR-OH, wherein, x=n-1, R and R ' all represent monovalence hydrophobic grouping;
Initial cell element polycondensation is hydroxyl chain polymer, and wherein, m is natural number, and R ' all represents monovalence hydrophobic grouping, and M represents metallicity element,
Initial cell element polycondensation is the chain polymer of band short-chain branch, and reaction formula is:
The chain polymer polycondensation of hydroxyl chain polymer and band short-chain branch obtains higly branched chain high reactivity water-based resin prepolymer, and reaction formula is:
5. the synthetic method of higly branched chain high reactivity water-based resin prepolymer according to claim 4, it is characterised in that, concrete steps are as follows:
Raw material prepares: the mol ratio of Union carbide A-162 and dimethyldiethoxysilane is 1��1.4:1, the mol ratio of lauryl alcohol and methyltrimethoxy silane is 0.8��0.95:1, the mol ratio of deionized water and Union carbide A-162 is 1.2��1.8:1, catalyst A is the 0.6% of reactant total mass, catalyst B is the 1.8% of reactant total mass, and wherein catalyst A and catalyst B are organometallic catalysts;
Polycondensation: in above-mentioned raw materials ratio, two kinds of silane and catalyst A are added in four-hole bottle, stirs and heat to 75 DEG C, drip ionized water, within 20 minutes, drip, 85 DEG C of back flow reaction two hours, 85 DEG C steam ethanol, then, add catalyst B and lauryl alcohol, heat to 130 DEG C, reflux 2��4 hours, obtain higly branched chain high reactivity water-based resin prepolymer.
6. the synthetic method of higly branched chain high reactivity water-based resin prepolymer according to claim 5, it is characterised in that, concrete steps are as follows:
Raw material prepares: the mol ratio of Union carbide A-162 and dimethyldiethoxysilane is 1.2:1, the mol ratio of lauryl alcohol and methyltrimethoxy silane is 0.9:1, the mol ratio of deionized water and Union carbide A-162 is 1.6:1, catalyst A is the 0.6% of reactant total mass, and catalyst B is the 1.8% of reactant total mass;
Polycondensation: in above-mentioned raw materials ratio, two kinds of silane and catalyst A are added in four-hole bottle, stirs and heat to 75 DEG C, drip ionized water, within 20 minutes, drip, 85 DEG C of back flow reaction two hours, 85 DEG C steam ethanol, then, add catalyst B and lauryl alcohol, heat to 130 DEG C, reflux 3 hours, obtain higly branched chain high reactivity water-based resin prepolymer.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100092686A1 (en) * | 2007-04-27 | 2010-04-15 | Nora Laryea | Method for the production of a coating material |
| CN102153753A (en) * | 2011-02-21 | 2011-08-17 | 黄山阳昕涂料有限公司 | Method for preparing water-based nano silicon resin compound |
| CN102492142A (en) * | 2011-11-24 | 2012-06-13 | 上海久安水质稳定剂厂 | Scratch resistant silicone resin for wooden floor, preparation method and application thereof |
| CN103265702A (en) * | 2013-05-28 | 2013-08-28 | 哈尔滨工业大学 | Preparation method of ultraviolet-resistant and high-temperature-resistant methyl silicone resin |
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- 2016-02-24 CN CN201610102621.XA patent/CN105622940A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100092686A1 (en) * | 2007-04-27 | 2010-04-15 | Nora Laryea | Method for the production of a coating material |
| CN102153753A (en) * | 2011-02-21 | 2011-08-17 | 黄山阳昕涂料有限公司 | Method for preparing water-based nano silicon resin compound |
| CN102492142A (en) * | 2011-11-24 | 2012-06-13 | 上海久安水质稳定剂厂 | Scratch resistant silicone resin for wooden floor, preparation method and application thereof |
| CN103265702A (en) * | 2013-05-28 | 2013-08-28 | 哈尔滨工业大学 | Preparation method of ultraviolet-resistant and high-temperature-resistant methyl silicone resin |
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