CN110452594A - A kind of alcohol-soluble organic-inorganic hybrid resin and preparation method thereof - Google Patents
A kind of alcohol-soluble organic-inorganic hybrid resin and preparation method thereof Download PDFInfo
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- CN110452594A CN110452594A CN201910486223.6A CN201910486223A CN110452594A CN 110452594 A CN110452594 A CN 110452594A CN 201910486223 A CN201910486223 A CN 201910486223A CN 110452594 A CN110452594 A CN 110452594A
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- Prior art keywords
- alcohol
- soluble organic
- inorganic hybrid
- hybrid resin
- inorganic
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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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/062—Copolymers with monomers not covered by C09D133/06
- C09D133/066—Copolymers with monomers not covered by C09D133/06 containing -OH 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
- C09D5/10—Anti-corrosive paints containing metal dust
- C09D5/106—Anti-corrosive paints containing metal dust containing Zn
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/20—Diluents or solvents
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0893—Zinc
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Paints Or Removers (AREA)
Abstract
The present invention discloses a kind of alcohol-soluble organic-inorganic hybrid resin and preparation method thereof, the alcohol-soluble organic-inorganic hybrid resin is made of organic phase component and inorganic phase component, by percentage to the quality, the inorganic phase component is made of following component: ethyl orthosilicate, 30~50%wt；γ-glycidyl ether oxygen propyl trimethoxy silicane, 1~5%wt；Deionized water, 0.65~18%wt；Dehydrated alcohol, 30~50%wt；Acetic acid, 0.2~0.5%wt；By percentage to the quality, organic phase component is made of following component: acrylate monomer blend, 50~70%wt；Initiator, 1~5%wt；Chain-transferring agent, 0.5~2%wt；Propylene glycol methyl ether acetate, 25~45%wt.The present invention uses the dehydrated alcohol of low toxicity as solvent, smaller to human injury, in addition, zinc powder class functional filler is added in prepared alcohol-soluble organic-inorganic hybrid resin, can be used widely in high temperature resistant or heavy antisepsis field.
Description
Technical field
The present invention relates to anticorrosive paint field, in particular to a kind of alcohol-soluble organic-inorganic hybrid resin and its preparation side
Method.
Background technique
Anti-corrosion is exactly to protect the metal for being easy corrosion by taking various means, and to reach extension, it uses the longevity
The purpose of life.Anti-decaying paint is many kinds of, can be generally divided into according to ingredient: epoxy anticorrosive paint, polyurethane anti-corrosion paint, acrylic acid are anti-
Rotten paint, inorganic anti-corrosion paint, vinyl perchloride anti-corrosion paint, chlorinated rubber anticorrosive paint, highly-chlorinated polyethylene anti-decaying paint.It can be in severe item
Used under part, and there is preferable durability, weather resistance, can ocean, use 10 years or 15 years under inferior mal-condition
More than, even if in acid, alkali, salt and solvent medium, and under the conditions of certain temperature, it could be used that 5 years or more.
Traditional anticorrosive paint has certain penetrating odor and biology poison usually using organic solvents such as benzene class, ketone, esters
Property, and the resin of solvent is done with water, due to the defect of water, if surface tension is big, volatility is poor, needs to be added a large amount of cosolvents etc.
Problem, there are also many defects.In addition, pure organic polymer resin in coating in use, its mechanical property, heat-resisting ageing-resisting
Also defect.In view of this, it is really necessary to develop a kind of alcohol-soluble organic-inorganic hybrid resin and preparation method thereof, to
Overcome the above problem.
Summary of the invention
For the shortcomings of the prior art, the object of the present invention is to provide a kind of alcohol-soluble organic and inorganic is miscellaneous
Change resin and preparation method thereof, uses the dehydrated alcohol of low toxicity as solvent, it is smaller to human injury, in addition, in institute
It prepares and zinc powder class functional filler is added in alcohol-soluble organic-inorganic hybrid resin, can be obtained in high temperature resistant or heavy antisepsis field
To extensive use.
In order to realize above-mentioned purpose according to the present invention and other advantages, a kind of alcohol-soluble hybrid inorganic-organic is provided
Resin is made of organic phase component and inorganic phase component, wherein by percentage to the quality, the inorganic phase component by below at
Divide and be made:
By percentage to the quality, organic phase component is made of following component:
Preferably, by percentage to the quality, the acrylate monomer blend is made of following component:
Further, this case also provides a kind of method for preparing above-mentioned alcohol-soluble organic-inorganic hybrid resin, including following
Step:
Step 1: ethyl orthosilicate, γ-glycidyl ether oxygen propyl trimethoxy silicane, dehydrated alcohol are mixed, it is added
Then acetic acid regulation system pH value is gradually added dropwise to deionized water, time for adding is controlled at 0.5 hour~2 hours, is added dropwise to 4
After, continue to be stirred to react 2-6 hours, obtains modified silicasol；
Step 2: acrylate monomer blend is stirred evenly, initiator and chain-transferring agent is added, after mixing,
It is gradually added dropwise in propylene glycol methyl ether acetate, during dropwise addition, reaction system is stirred evenly, and by temperature of reaction system
It is controlled 2~6 hours within the scope of 90~120 DEG C, after being added dropwise, by temperature of reaction system control within the scope of 100~150 DEG C
Insulation reaction 2-8 hours, be down to room temperature obtain designing it is molten using propylene glycol methyl ether acetate as the acrylate polymer of solvent
Liquid；
Step 3: by acrylate polymer solution made from modified silicasol made from step 1 and step 2 according to one
Certainty ratio mixing, is warming up to 60 DEG C, the reaction was continued in lasting stirring 2~24 hours to get to designed alcohol-soluble it is organic-nothing
Machine hybrid resin.
Preferably, in step 2, the initiator is benzoyl peroxide or di t-amyl peroxide.
Preferably, the chain-transferring agent is sulfydryl dehydrated alcohol.
Preferably, in step 3, the mixed proportion of the modified silicasol and acrylate polymer be 1:10~
1:4。
Compared with prior art, the present invention the beneficial effect is that:
1. organic/inorganic two are keyed using chemistry in system, two problem of phase separation of hydridization are effectively overcome, favorably
In performance compound two comprehensive performances of system.
2. mainly making the solvent of system using ethyl alcohol, the big organic solvents of pollutions such as traditional dimethylbenzene are substituted, favorably
In reducing energy consumption, the pollution to environment is reduced.
3. the hybrid resin of design synthesis has good weatherability and corrosion resistance, bottom surface conjunction can be applied to
One anticorrosive paint.
Detailed description of the invention:
Fig. 1 is alcohol-soluble organic-inorganic hybrid resin solidify coating scanning electron microscopic picture prepared by embodiment one；
Fig. 2 is that the piece zinc anticorrosive paint solidification of the alcohol-soluble organic-inorganic hybrid resin prepared based on embodiment one is applied
Layer.
Specific embodiment
Present invention will be described in further detail below with reference to the accompanying drawings, foregoing end other objects of the invention, feature, side
Face and advantage will be apparent, and so that those skilled in the art can carry out according to the description.
Embodiment one
A kind of alcohol-soluble organic-inorganic hybrid resin, is made, wherein with quality of organic phase component and inorganic phase component
Percentages, the inorganic phase component are made of following component:
Further, by percentage to the quality, organic phase component is made of following component:
Further, by percentage to the quality, the acrylate monomer blend is made of the following components:
Further, this case also provides a kind of method for preparing above-mentioned alcohol-soluble organic-inorganic hybrid resin, including following
Step:
Step 1: ethyl orthosilicate, γ-glycidyl ether oxygen propyl trimethoxy silicane, dehydrated alcohol are mixed, it is added
Then acetic acid regulation system pH value is gradually added dropwise to deionized water to 4, time for adding was controlled at 2 hours, after being added dropwise, after
It is continuous to be stirred to react 2 hours, obtain modified silicasol；
Step 2: acrylate monomer blend is stirred evenly, initiator and chain-transferring agent, after mixing, gradually
It is added dropwise in propylene glycol methyl ether acetate, during dropwise addition, reaction system is stirred evenly, and by temperature of reaction system 90
It controls 6 hours within the scope of DEG C, after being added dropwise, temperature of reaction system control is reacted 8 hours in 100 DEG C of range inside holdings, drop
It is to be designed using propylene glycol methyl ether acetate as the acrylate polymer solution of solvent to room temperature；
Step 3: by acrylate polymer solution made from modified silicasol made from step 1 and step 2 according to one
Certainty ratio mixing, is warming up to 60 DEG C, the reaction was continued in lasting stirring 24 hours to get arriving designed alcohol-soluble organic and inorganic
Hybrid resin.
Further, in step 2, the initiator is benzoyl peroxide.
Further, the chain-transferring agent is sulfydryl dehydrated alcohol.
Further, in step 3, the mixed proportion of the modified silicasol and acrylate polymer is 1:4.
Fig. 1 is the scanning electron microscope (SEM) photograph of the alcohol-soluble organic-inorganic hybrid resin solidify coating arrived by scanning electron microscopic observation
Piece, surface uniform ground do not have the appearance of two-phase split-phase problem, show the connection of chemical bond, be conducive to hybrid inorganic-organic two
The microfacies of phase is compatible, is conducive to compound two comprehensive performances of performance system.
Fig. 2 is that the piece zinc anticorrosive paint solidification of the alcohol-soluble organic-inorganic hybrid resin prepared based on embodiment one is applied
Layer, coating show that uniform silvery white pattern, zinc flake are uniformly distributed in system, are conducive to play its decoration and its prevent
Rotten efficiency.
Embodiment two
A kind of alcohol-soluble organic-inorganic hybrid resin, is made, wherein with quality of organic phase component and inorganic phase component
Percentages, the inorganic phase component are made of following component:
Further, by percentage to the quality, organic phase component is made of following component:
Further, by percentage to the quality, the acrylate monomer blend is made of the following components:
Further, this case also provides a kind of method for preparing above-mentioned alcohol-soluble organic-inorganic hybrid resin, including following
Step:
Step 1: ethyl orthosilicate, γ-glycidyl ether oxygen propyl trimethoxy silicane, dehydrated alcohol are mixed, it is added
Then acetic acid regulation system pH value is gradually added dropwise to deionized water to 4, time for adding was controlled at 1 hour, after being added dropwise, after
It is continuous to be stirred to react 4 hours, obtain modified silicasol；
Step 2: acrylate monomer blend is stirred evenly, initiator and chain-transferring agent is added, after mixing,
It is gradually added dropwise in propylene glycol methyl ether acetate, during dropwise addition, reaction system is stirred evenly, and reaction system is stirred
Uniformly, and by temperature of reaction system it controls 4 hours within the scope of 100 DEG C, after being added dropwise, temperature of reaction system control is existed
120 DEG C of range inside holdings react 4 hours, be down to that room temperature designed using propylene glycol methyl ether acetate as the acrylic acid of solvent
Ester polymer solution；
Step 3: by acrylate polymer solution made from modified silicasol made from step 1 and step 2 according to one
Certainty ratio mixing, is warming up to 60 DEG C, the reaction was continued in lasting stirring 12 hours to get arriving designed alcohol-soluble organic and inorganic
Hybrid resin.
Further, in step 2, the initiator is di t-amyl peroxide.
Further, the chain-transferring agent is sulfydryl dehydrated alcohol.
Further, in step 3, the mixed proportion of the modified silicasol and acrylate polymer is 1:5.
Embodiment three
A kind of alcohol-soluble organic-inorganic hybrid resin, is made, wherein with quality of organic phase component and inorganic phase component
Percentages, the inorganic phase component are made of following component:
By percentage to the quality, organic phase component is made of following component:
Further, by percentage to the quality, the acrylate monomer blend is made of the following components:
Further, this case also provides a kind of method for preparing above-mentioned alcohol-soluble organic-inorganic hybrid resin, including following
Step:
Step 1: ethyl orthosilicate, γ-glycidyl ether oxygen propyl trimethoxy silicane, dehydrated alcohol are mixed, it is added
Then acetic acid regulation system pH value is gradually added dropwise to deionized water to 4, time for adding was controlled at 1.5 hours, after being added dropwise,
Continue to be stirred to react 3 hours, obtains modified silicasol；
Step 2: acrylate monomer blend is stirred evenly, initiator and chain-transferring agent is added, after mixing,
It is gradually added dropwise in propylene glycol methyl ether acetate, during dropwise addition, reaction system is stirred evenly, and by temperature of reaction system
It is controlled 2.5 hours within the scope of 105 DEG C, after being added dropwise, by temperature of reaction system control in 140 DEG C of range inside holding reactions 3
Hour, it is down to room temperature and obtains designing the acrylate polymer solution using propylene glycol methyl ether acetate as solvent；
Step 3: by acrylate polymer solution made from modified silicasol made from step 1 and step 2 according to one
Certainty ratio mixing, is warming up to 60 DEG C, the reaction was continued in lasting stirring 10 hours to get arriving designed alcohol-soluble organic and inorganic
Hybrid resin.
Further, in step 2, the initiator is benzoyl peroxide or di t-amyl peroxide.
Further, the chain-transferring agent is sulfydryl dehydrated alcohol.
Further, in step 3, the mixed proportion of the modified silicasol and acrylate polymer is 1:8.
In designed kind alcohol-soluble organic-inorganic hybrid resin, the zinc flake that partial size is 400 mesh, matter is added
Amount ratio is organic-inorganic hybrid resin: piece zinc=1:1 (w/w) obtains organic and inorganic after high speed dispersion is mixed
Hydridization piece zinc anticorrosive paint, performance are as follows:
One, alcohol-soluble hybrid inorganic-organic piece zinc anticorrosive paint of table
Number of devices and treatment scale described herein are for simplifying explanation of the invention.To application of the invention,
Modifications and variations will be readily apparent to persons skilled in the art.
Although the embodiments of the present invention have been disclosed as above, but it is not limited in listed fortune in specification and embodiments
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily real
Now other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is not limited to
Specific details and legend shown and described herein.
Claims (6)
1. a kind of alcohol-soluble organic-inorganic hybrid resin, which is characterized in that it is made of organic phase component and inorganic phase component,
In, by percentage to the quality, the inorganic phase component is made of following component:
By percentage to the quality, organic phase component is made of following component:
2. alcohol-soluble organic-inorganic hybrid resin as described in claim 1, which is characterized in that by percentage to the quality, described
Acrylate monomer blend is made of following component:
3. a kind of preparation method of such as described in any item alcohol-soluble organic-inorganic hybrid resins of claim 1~2, feature
It is, comprising the following steps:
Step 1: ethyl orthosilicate, γ-glycidyl ether oxygen propyl trimethoxy silicane, dehydrated alcohol are mixed, acetic acid is added
Then regulation system pH value is gradually added dropwise to deionized water, time for adding is controlled at 0.5 hour~2 hours, is added dropwise to 4
Afterwards, continue to be stirred to react 2-6 hours, obtain modified silicasol；
Step 2: acrylate monomer blend is stirred evenly, initiator and chain-transferring agent is added, after mixing, gradually
It is added dropwise in propylene glycol methyl ether acetate, during dropwise addition, reaction system is stirred evenly, and by temperature of reaction system 90
It controls 2~6 hours within the scope of~120 DEG C, after being added dropwise, temperature of reaction system is controlled in 100~150 DEG C of range inside holdings
Reaction 2-8 hours, is down to room temperature and obtains designing the acrylate polymer solution using propylene glycol methyl ether acetate as solvent；
Step 3: by acrylate polymer solution made from modified silicasol made from step 1 and step 2 according to certain ratio
Example mixing, is warming up to 60 DEG C, the reaction was continued in lasting stirring 2~24 hours to get miscellaneous to designed alcohol-soluble organic and inorganic
Change resin.
4. the preparation method of alcohol-soluble organic-inorganic hybrid resin as claimed in claim 3, which is characterized in that in step 2
In, the initiator is benzoyl peroxide or di t-amyl peroxide.
5. the preparation method of alcohol-soluble organic-inorganic hybrid resin as claimed in claim 3, which is characterized in that the chain turns
Shifting agent is sulfydryl dehydrated alcohol.
6. the preparation method of alcohol-soluble organic-inorganic hybrid resin as claimed in claim 3, which is characterized in that in step 3
In, the mixed proportion of the modified silicasol and acrylate polymer is 1:10~1:4.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910486223.6A CN110452594A (en) | 2019-06-05 | 2019-06-05 | A kind of alcohol-soluble organic-inorganic hybrid resin and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910486223.6A CN110452594A (en) | 2019-06-05 | 2019-06-05 | A kind of alcohol-soluble organic-inorganic hybrid resin and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102007032886A1 (en) * | 2007-07-14 | 2009-01-15 | Bayer Materialscience Ag | Hydrophilic hardcoat coatings |
| CN104558450A (en) * | 2014-12-30 | 2015-04-29 | 北京金汇利应用化工制品有限公司 | Organic-inorganic compound modified water-based acrylic resin and preparation method thereof |
| EP3301138A1 (en) * | 2016-09-30 | 2018-04-04 | Daw Se | Aqueous treatment mass for building walls, ceilings or floors |
| CN108546485A (en) * | 2017-12-04 | 2018-09-18 | 苏州吉人高新材料股份有限公司 | A kind of organic-inorganic hybrid resin of high solids content and preparation method thereof |
-
2019
- 2019-06-05 CN CN201910486223.6A patent/CN110452594A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102007032886A1 (en) * | 2007-07-14 | 2009-01-15 | Bayer Materialscience Ag | Hydrophilic hardcoat coatings |
| CN104558450A (en) * | 2014-12-30 | 2015-04-29 | 北京金汇利应用化工制品有限公司 | Organic-inorganic compound modified water-based acrylic resin and preparation method thereof |
| EP3301138A1 (en) * | 2016-09-30 | 2018-04-04 | Daw Se | Aqueous treatment mass for building walls, ceilings or floors |
| CN108546485A (en) * | 2017-12-04 | 2018-09-18 | 苏州吉人高新材料股份有限公司 | A kind of organic-inorganic hybrid resin of high solids content and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 朱万强: "《涂料基础教程》", 30 June 2012, 西南交通大学出版社 * |
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