CN103951789B - A kind of resistant to elevated temperatures minute surface silver resin and preparation method thereof - Google Patents
A kind of resistant to elevated temperatures minute surface silver resin and preparation method thereof Download PDFInfo
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- CN103951789B CN103951789B CN201410137281.5A CN201410137281A CN103951789B CN 103951789 B CN103951789 B CN 103951789B CN 201410137281 A CN201410137281 A CN 201410137281A CN 103951789 B CN103951789 B CN 103951789B
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Abstract
The invention discloses a kind of resistant to elevated temperatures minute surface silver resin, which is made up of following raw material：First component：Acetylbutyrylcellulose, solvent；Second component：Methyl methacrylate, methacrylic acid butyl acetate, hydroxyethyl methacrylate, hydroxy propyl methacrylate,（Methyl）Acrylic acid epoxy ester, vinylsiloxane, isobornyl methacrylate, lauryl methacrylate, acrylic acid, initiator；Third component：Initiator, solvent.The preparation method of the minute surface silver resin, including step：Acetylbutyrylcellulose in first component is added in solvent and is dissolved, heated while stirring, be warming up to 70 95 DEG C, lead to nitrogen；Second component is mixed, the first component is added drop-wise to, is incubated, is warming up to 85 110 DEG C；Add third component, insulation, finally cooling, filtration.Minute surface silver resin prepared by the present invention has resistance to elevated temperatures, and there is the adhesive force of wide spectrum to base material, and the solvent resistance of product is preferable, and synthesis technique environmental protection.
Description
Technical field
The present invention relates to a kind of resistant to elevated temperatures minute surface silver resin and preparation method thereof.
Background technology
Minute surface silver resin is generally acrylic resin modified, minute surface silver resin of the prior art often exist following these
One or more in problem：1. resistance to elevated temperatures is not fully up to expectations, the substrate adhesion 2. without wide spectrum, i.e., resin is the bottom of to
The adaptability of material is often bad, and 3. the solvent resistance of resin is poor, and 4. raw materials used or synthesis technique is not environmentally；5. synthesize work
Skill is relatively costly.
For this purpose, forefathers have done substantial amounts of research work, Chinese patent CN102432777A first synthesizes active acetic acid
Cellulose butyrate intermediate, then again with functional acrylic monomer copolymerization, step is more, high cost.
Chinese patent CN101157813A, be acetylbutyrylcellulose acrylic resin etc. be directly mixed to prepare, belong to altogether
Mixed modification, during without chemical reaction.
《Acrylic acid modified acetylbutyrylcellulose is used for imitative plating aluminium paint》In one text, changed using Solution Free Radical method
Property, monomer used is styrene, methyl methacrylate, ethyl acrylate, methacrylic acid butyl acetate.If according to this article
The polymer that the method that offers is made is not then curable.
Content of the invention
It is an object of the invention to provide a kind of resistant to elevated temperatures minute surface silver resin and preparation method thereof.
The technical solution used in the present invention is：
A kind of resistant to elevated temperatures minute surface silver resin, which is made up of the raw material of three below component：First component：Acetate butyrate
Cellulose 50-60 parts, solvent 200-300 parts；Second component：Methyl methacrylate 40-50 parts, methacrylic acid butyl acetate
20-30 parts, hydroxyethyl methacrylate 20-25 parts, hydroxy propyl methacrylate 10-15 parts,（Methyl）Acrylic acid epoxy
Ester 30-40 parts, vinylsiloxane 0-15 parts, isobornyl methacrylate 0-15 parts, lauryl methacrylate 0-20 parts,
Acrylic acid 0-2 parts, initiator 1-2 parts；Third component：Initiator 1-2 parts, solvent 20-30 parts.
Described acetylbutyrylcellulose be CAB381-0.1, CAB381-0.5, CAB381-2, CAB381-20 in extremely
Few one kind.
Described initiator is oil soluble peroxides or azo-compound.
Described oil soluble peroxides be benzoyl peroxide, peroxidized t-butyl perbenzoate, cumyl peroxide,
At least one in di-t-butyl peroxide, methyl ethyl ketone peroxide.
Described azo-compound is azodiisobutyronitrile, at least one in 2,2'-Azobis(2,4-dimethylvaleronitrile).
Described solvent is esters solvent, ketones solvent, at least one in aromatic hydrocarbon solvent.
Described solvent be ethyl acetate, butyl acetate, glycol methyl ether acetate, ethylene glycol ether acetate, the third two
In alcohol methyl ether acetate, butyl acetate, hexone, Ketohexamethylene, butanone, toluene, dimethylbenzene extremely
Few one kind.
A kind of preparation method of resistant to elevated temperatures minute surface silver resin, including step：By the acetate butyrate fiber in the first component
Element is added in solvent and dissolves, and heats while stirring, is warming up to 70-95 DEG C, leads to nitrogen protection；Will be complete for the material in the second component
Portion mixes, and is added drop-wise in the first component with 3.5-4.5 hours, is incubated 1-1.5 hours, is warming up to 85-110 DEG C；Add the 3rd group
Point, 2-2.5 hours are incubated, finally cooling, filtration.
The invention has the beneficial effects as follows：Minute surface silver resin prepared by the present invention has resistance to elevated temperatures, base material is had wide
The adhesive force of spectrum, the solvent resistance of product are preferable, and synthesis technique environmental protection.
Description of the drawings
Fig. 1 be the embodiment of the present invention 3 synthesis minute surface silver resin mirror effect test in, spray on glass dry after
Picture in kind.
Specific embodiment
A kind of resistant to elevated temperatures minute surface silver resin, which is made up of the raw material of three below component（Described part is quality
Part）：First component：Acetylbutyrylcellulose 50-60 parts, solvent 200-300 parts；Second component：Methyl methacrylate 40-50
Part, methacrylic acid butyl acetate 20-30 parts, hydroxyethyl methacrylate 20-25 parts, hydroxy propyl methacrylate 10-
15 parts,（Methyl）Acrylic acid epoxy ester 30-40 parts, vinylsiloxane 0-15 parts, isobornyl methacrylate 0-15 parts, first
Base lauryl acrylate 0-20 parts, acrylic acid 0-2 parts, initiator 1-2 parts；Third component：Initiator 1-2 parts, solvent 20-30
Part.
The preparation method of above-mentioned resistant to elevated temperatures minute surface silver resin, including step：Will be fine for the acetate butyrate in the first component
Dimension element is added in solvent and dissolves, and heats while stirring, is warming up to 70-95 DEG C, leads to nitrogen protection；By the material in the second component
All mix, be added drop-wise in the first component with 3.5-4.5 hours, be incubated 1-1.5 hours, be warming up to 85-110 DEG C；Add the 3rd
Component, is incubated 2-2.5 hours, finally cooling, filtration.
Preferably, described acetylbutyrylcellulose is CAB381-0.1, CAB381-0.5, CAB381-2, CAB381-20
In at least one.
Described initiator is oil soluble peroxides or azo-compound；Preferably, described oil soluble peroxides
For benzoyl peroxide, peroxidized t-butyl perbenzoate, cumyl peroxide, di-t-butyl peroxide, methyl ethyl ketone peroxide
In at least one；Described azo-compound is azodiisobutyronitrile, at least one in 2,2'-Azobis(2,4-dimethylvaleronitrile).
Described solvent is esters solvent, ketones solvent, at least one in aromatic hydrocarbon solvent；Preferably, described molten
Agent is ethyl acetate, butyl acetate, glycol methyl ether acetate, ethylene glycol ether acetate, propylene glycol methyl ether acetate, diethyl
At least one in glycol monobutyl ether acetate, hexone, Ketohexamethylene, butanone, toluene, dimethylbenzene.
With reference to specific embodiment, the present invention is described further：
Embodiment 1:
Lead to nitrogen in four-hole boiling flask, add 200 parts of butyl acetates, 50 parts of dimethylbenzene to heat while stirring, be subsequently adding
50 parts of CAB381-2 dissolvings, are warming up to 80 DEG C.Start the following mixture of Deca, 40 parts of methyl methacrylates 20 parts of methyl-props
Olefin(e) acid butyl acetate 10 parts of hydroxyethyl methacrylates 10 parts of hydroxy propyl methacrylates 40 parts of glycidyls
Ester 1 part of initiator azodiisobutyronitrile, dripped off with 4 hours, after dripping off be incubated 1 hour.Again by 1 part of azodiisobutyronitrile 20 parts
Butyl acetate is added, and is incubated 2 hours, is filtered.
Embodiment 2:
Lead to nitrogen in four-hole boiling flask, add 300 parts of glycol methyl ether acetates, heat while stirring, be subsequently adding 50
Part CAB381-20 dissolvings, are warming up to 85-90 DEG C.Start the following mixture of Deca, 50 parts of methyl methacrylates 20 parts of methyl
Acrylic acid butyl acetate 10 parts of hydroxyethyl methacrylates 10 parts of hydroxy propyl methacrylates 30 parts of methacrylic acid rings
Oxygen ester 10 parts of isobornyl methacrylates 1.5 parts of benzoyl peroxides mixing, dripped off with 4 hours, after dripping off, insulation 1 is little
When.Again by 1 part of benzoyl peroxide 20 parts of butyl acetates add, be incubated 2 hours, filter.
Embodiment 3:
Lead to nitrogen in four-hole boiling flask, add 200 parts of glycol methyl ether acetates, 100 parts of dimethylbenzene to stir in heating
Mix, be subsequently adding 60 parts of CAB381-0.5 dissolvings, be warming up to 85-90 DEG C.Start the following mixture of Deca, 45 parts of methacrylic acids
Methyl ester 20 parts of methacrylic acid butyl acetates 10 parts of hydroxyethyl methacrylates 15 parts of hydroxy propyl methacrylates 40
Part epoxymethacrylate, 10 parts of VTESs 1 part of azodiisobutyronitrile 0.5 part of benzoyl peroxide,
Dripped off with 4 hours, after dripping off, be incubated 1 hour.Again by 1 part of benzoyl peroxide 20 parts of butyl acetates add, be incubated 2 hours, mistake
Filter.
Following test is carried out to the resin of present invention synthesis：
First, resin adhesive force test
Electrosilvering proportioning：15 mass parts of resin of the synthesis of embodiment 3,3 mass parts of minute surface silver paste, solvent ethylene glycol methyl ether vinegar
82 mass parts of acid esters；Mirror-like silver proportioning：1 mass parts of resin of the synthesis of embodiment 3,2 mass parts of minute surface silver paste, solvent ethylene glycol first
17 mass parts of ether acetate.
Form of construction work：Spraying；Drying mode：70 DEG C are toasted 1 hour.
Following test result is obtained in electroplating effect test and mirror effect test
| Ground | Glass | PC | PET | ABS | PS |
| Adhesive force grade | 0 grade | 0 grade | 1 grade | 0 grade | 1 grade |
Fig. 1 be the embodiment of the present invention 3 synthesis minute surface silver resin in this secondary mirror measure of merit, spray on glass do
Picture in kind after dry.
2nd, resin high temperature test
Test mode：The resin sample of embodiment 1-3 synthesis directly toasts 30 parts at 180 DEG C, and visualization of color changes.
Test result：It was found that obvious color change
3rd, resin recoating examination
Construction proportioning
Ink with mirror effect：Embodiment 2-in-1 into 1 mass parts of minute surface resin, 2 mass parts of silver paste, 17 mass parts of Tianna solution；
PU varnish：PU 5 mass parts of resin, 1.6 mass parts of TDI firming agent, 5 mass parts of Tianna solution；
Baking vanish varnish：Baking vanish 5 mass parts of resin, 5 mass parts of Tianna solution；
Form of construction work：Ink with mirror effect is sprayed on glass first, is toasted 30 minutes in 150 DEG C；Difference is painted again in minute surface
Spraying PU varnish or baking vanish varnish, PU varnish-dryings mode be 70 DEG C 30 minutes, baking vanish be 130 DEG C 30 minutes.
Test result：PU varnish, baking vanish varnish adhesive force on ink with mirror effect reaches 0 grade.
4th, solvent resistance test
Solvent resistance（Butanone is wiped）：100 times.
Claims (8)
1. a kind of resistant to elevated temperatures minute surface silver resin, it is characterised in that：Which is made up of the raw material of three below component：First group
Point：
Acetylbutyrylcellulose 50-60 mass parts, solvent 200-300 mass parts；Second component：Methyl methacrylate 40-50
Mass parts, methacrylic acid butyl acetate 20-30 mass parts, hydroxyethyl methacrylate 20-25 mass parts, methacrylic acid
Hydroxy propyl ester 10-15 mass parts,（Methyl）Acrylic acid epoxy ester 30-40 mass parts, vinylsiloxane 0-15 mass parts, methyl
Isobornyl acrylate 0-15 mass parts, lauryl methacrylate 0-20 mass parts, acrylic acid 0-2 mass parts, initiator 1-2
Mass parts；Third component：Initiator 1-2 mass parts, solvent 20-30 mass parts.
2. a kind of resistant to elevated temperatures minute surface silver resin according to claim 1, it is characterised in that：Described acetate butyrate fiber
Element is at least one in CAB381-0.1, CAB381-0.5, CAB381-2, CAB381-20.
3. a kind of resistant to elevated temperatures minute surface silver resin according to claim 1, it is characterised in that：Described initiator is oil soluble
Property peroxide or azo-compound.
4. a kind of resistant to elevated temperatures minute surface silver resin according to claim 3, it is characterised in that：Described oil-soluble peroxidating
Thing is benzoyl peroxide, peroxidized t-butyl perbenzoate, cumyl peroxide, di-t-butyl peroxide, peroxidating first and second
At least one in ketone.
5. a kind of resistant to elevated temperatures minute surface silver resin according to claim 3, it is characterised in that：Described azo-compound is
At least one in azodiisobutyronitrile, 2,2'-Azobis(2,4-dimethylvaleronitrile).
6. a kind of resistant to elevated temperatures minute surface silver resin according to claim 1, it is characterised in that：Described solvent is that esters are molten
Agent, ketones solvent, at least one in aromatic hydrocarbon solvent.
7. a kind of resistant to elevated temperatures minute surface silver resin according to claim 6, it is characterised in that：Described solvent is acetic acid second
Ester, butyl acetate, glycol methyl ether acetate, ethylene glycol ether acetate, propylene glycol methyl ether acetate, butyl vinegar
At least one in acid esters, hexone, Ketohexamethylene, butanone, toluene, dimethylbenzene.
8. the preparation method of a kind of resistant to elevated temperatures minute surface silver resin described in claim 1, it is characterised in that：Including step：Will
Acetylbutyrylcellulose in first component is added in solvent and dissolves, and heats while stirring, is warming up to 70-95 DEG C, leads to nitrogen
Protection；Material in second component is all mixed, is added drop-wise in the first component with 3.5-4.5 hours, be incubated 1-1.5 hours,
It is warming up to 85-110 DEG C；Third component is added, 2-2.5 hours are incubated, finally cooling, filtration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410137281.5A CN103951789B (en) | 2014-04-04 | 2014-04-04 | A kind of resistant to elevated temperatures minute surface silver resin and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410137281.5A CN103951789B (en) | 2014-04-04 | 2014-04-04 | A kind of resistant to elevated temperatures minute surface silver resin and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN103951789A CN103951789A (en) | 2014-07-30 |
| CN103951789B true CN103951789B (en) | 2017-03-15 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104479444B (en) * | 2014-12-05 | 2017-04-19 | 广州致辉精化股份有限公司 | Boiling-resistant mirror resin and preparation method thereof |
| CN104710558A (en) * | 2015-02-09 | 2015-06-17 | 扬州市政兴树脂有限公司 | Solid thermoplastic acrylic acid high-temperature-resistant cold-stamped mold-pressed resin and preparation method thereof |
| CN104926997A (en) * | 2015-06-02 | 2015-09-23 | 清远雅克化工有限公司 | Preparation method of resin for water based metallic flashing paint |
| CN105669906B (en) * | 2016-03-09 | 2017-11-21 | 广州伊德尔化学科技有限公司 | A kind of resistance to alcohol is washed, High temperature resistance mirror-like silver resin and preparation method thereof |
| CN107141857A (en) * | 2017-05-22 | 2017-09-08 | 上海天地涂料有限公司 | A kind of minute surface silver resin and preparation method thereof |
| CN109836754B (en) * | 2019-01-17 | 2021-08-10 | 广州致辉精化股份有限公司 | Solvent-resistant and boiling-resistant PC mirror resin and preparation method thereof |
| CN118126621A (en) * | 2024-03-05 | 2024-06-04 | 大一(云浮)新材料科技有限公司 | Multicomponent polyurethane coating and manufacturing process thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432777A (en) * | 2011-08-29 | 2012-05-02 | 华南理工大学 | Method for modifying cellulose acetate butyrate (CAB) for electro-silvered simulating coating |
-
2014
- 2014-04-04 CN CN201410137281.5A patent/CN103951789B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432777A (en) * | 2011-08-29 | 2012-05-02 | 华南理工大学 | Method for modifying cellulose acetate butyrate (CAB) for electro-silvered simulating coating |
Non-Patent Citations (1)
| Title |
|---|
| 《丙烯酸改性醋酸丁酸纤维素用于仿电镀铝粉漆的研究》;郭芳等;《上海涂料》;20101231;第48卷(第4期);5-8 * |
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| CN103951789A (en) | 2014-07-30 |
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Address after: 511400, two, room 506, building 15, Cheonan headquarters, 555 Panyu Avenue, east ring street, Guangzhou, Guangdong, Panyu District Patentee after: Guangzhou EDL Chemical Technology Co.,Ltd. Address before: 511400 Guangdong city in Guangzhou Province, four West Street, Guangzhou economic and Technological Development Zone No. nine science park sapphire plant No. 2 6 floor (602-1) Patentee before: Guangzhou EDL Chemical Technology Co.,Ltd. |