CN109810226A - A kind of composite modified styrene-acrylic emulsion of epoxy silane coupling agent-Organic fluoride and preparation method - Google Patents
A kind of composite modified styrene-acrylic emulsion of epoxy silane coupling agent-Organic fluoride and preparation method Download PDFInfo
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- CN109810226A CN109810226A CN201811639147.XA CN201811639147A CN109810226A CN 109810226 A CN109810226 A CN 109810226A CN 201811639147 A CN201811639147 A CN 201811639147A CN 109810226 A CN109810226 A CN 109810226A
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Abstract
The invention discloses a kind of composite modified styrene-acrylic emulsion of epoxy silane coupling agent-Organic fluoride and preparation methods, the use of methyl methacrylate, styrene, n-butyl acrylate, methacrylic acid, dodecafluoroheptyl methacrylate, 3- glycidyl ether oxypropyltrimethoxysilane, octyl phenol polyoxyethylene ether, neopelex, ammonium persulfate and distilled water is primary raw material, is synthesized by way of emulsion polymerization and the composite modified styrene-acrylic emulsion of epoxy silane coupling agent-Organic fluoride is made.Modifying cinepazid emulsion made from the invention compared to traditional modifying cinepazid emulsion have more excellent coating strength, film adhesive, film water absorption rate, film corrosion resistance, lotion the performances such as conversion ratio.Its film pencil hardness 1 grade or more, water absorption rate are below 8% and lotion conversion ratio is 99% or more, there is very big application prospect in 4H or more, adhesive force.
Description
Technical field
The present invention relates to a kind of composite modified styrene-acrylic emulsion of epoxy silane coupling agent-Organic fluoride and preparation methods, belong to and build
Build technical field of coatings.
Background technique
Styrene-acrylic emulsion manufacturing cost is cheap, and have it is nontoxic, tasteless, non-ignitable, pollution less, weatherability, stain resistance, corrosion resistant
The features such as corrosion is excellent is used widely in paint field.However due to traditional styrene-acrylic emulsion hardness of film, attachment
The properties such as power, solvent resistance, water resistance are performed poor, and greatly limit its use scope, therefore use changes
Property method so that its is obtained more excellent performance, be on the basis of playing styrene-acrylic emulsion good characteristics further expansion its make
With the important breakthrough mouth of range.In recent years, there is good achievement to the research that styrene-acrylic emulsion is modified, such as obtain film
Hardness is stronger or corrosion resistance more preferably modifying cinepazid emulsion coating, but most of styrene-acrylic emulsions modified can not have both more
There is more apparent defect in more performances.
Summary of the invention
Based on the above the deficiencies in the prior art, technical problem solved by the invention is to provide a kind of organosilicon (epoxy
Silane coupling agent) the composite modified styrene-acrylic emulsion of/Organic fluoride, product obtained both remained the excellent spy of traditional styrene-acrylic emulsion itself
Point, and more excellent hardness of film, adhesive force, solvent resistance, water resistance and lotion conversion ratio are obtained, there is very big answer
Use prospect.
In order to solve the above technical problem, the present invention provides a kind of composite modified phenylpropyl alcohols of epoxy silane coupling agent-Organic fluoride
Lotion and preparation method, the present invention use methyl methacrylate (MMA), styrene (St), n-butyl acrylate (BA), methyl
Acrylic acid (MAA), dodecafluoroheptyl methacrylate (DFMA), 3- glycidyl ether oxypropyltrimethoxysilane (KH-
560), based on octyl phenol polyoxyethylene ether (OP-10), neopelex (SDS), ammonium persulfate (APS) and distilled water
Raw material (all analysis pure) is wanted, synthesizes that the epoxy silane coupling agent-Organic fluoride is made is compound by way of emulsion polymerization
Modifying cinepazid emulsion.
A kind of composite modified styrene-acrylic emulsion of epoxy silane coupling agent-Organic fluoride:
The material quality number of every 1000 mass fraction lotion of the present invention are as follows: 340-460 parts of A material, 337-342 parts of B
Material and 272.7-273.5 parts of C material；
Wherein A material includes 309.6-412.4 parts of matrixes, and 11.6-19.4 parts of modified monomers one, 18.8-28.2 parts modified single
Body two；B material includes 11-15.7 parts of compound emulsifying agents, 2-2.3 parts of buffers, 324 parts of distilled water；C material includes 2.7-3.5 parts and draws
Send out agent, 270 parts of distilled water；
Wherein,
Matrix is that the mass ratio of methyl methacrylate, styrene and n-butyl acrylate is 1:1:(2-3.33) mixing
Object；
Modified monomer one is dodecafluoroheptyl methacrylate；
Modified monomer two is that the mass ratio of methacrylic acid and 3- glycidyl ether oxypropyltrimethoxysilane is (3-
5): 1 mixture；
Compound emulsifying agent is that the mass ratio of neopelex and octyl phenol polyoxyethylene ether is 1:(1.5-2.5)
Mixture；
Buffer is NaHCO3；
Initiator is ammonium persulfate.
A kind of preparation method of the composite modified styrene-acrylic emulsion of epoxy silane coupling agent-Organic fluoride, comprises the following steps:
Step 1: matrix, modified monomer one and modified monomer two are mixed to obtain A material, by compound emulsifying agent, buffer and steaming
Distilled water is mixed to prepare B material, and initiator and distilled water are mixed to prepare C material；Again A, B are expected to mix, at 30-40 DEG C, stirs 0.5-
Pre-emulsion is made in 1h；
Step 2: by the pre-emulsion of pre-emulsion 50%-60% mass fraction obtained by step 1 and accounting for C obtained by step 1
Expect 30% mass fraction C material mixing and under the conditions of 70-75 DEG C, be stirred to react 0.5-1h；
Remaining pre-emulsion is dropped evenly and C expects and stirs Step 3: synchronizing into the mixture after step 2 reaction；
Step 4: mixture obtained by step 3 is stirred to react 1-1.5h under the conditions of 80-85 DEG C；
Step 5: the epoxy silane coupling is made through supercooling, cooling, discharging, filtering in liquid obtained by step 4
The composite modified styrene-acrylic emulsion of agent-Organic fluoride.
As an improvement of the above technical solution, in the step 1, wherein
Matrix is that the mass ratio of methyl methacrylate, styrene and n-butyl acrylate is 1:1:(2-3.33) mixing
Object；
Modified monomer one is dodecafluoroheptyl methacrylate；
Modified monomer two is that the mass ratio of methacrylic acid and 3- glycidyl ether oxypropyltrimethoxysilane is (3-
5): 1 mixture；
Compound emulsifying agent is that the mass ratio of neopelex and octyl phenol polyoxyethylene ether is 1:(1.5-2.5)
Mixture；
Buffer is NaHCO3；
Initiator is ammonium persulfate；
The material quality number of every 1000 mass fraction lotion of the present invention are as follows: 340-460 parts of A material, 337-342 parts of B
Material and 272-273 parts of C material.
As an improvement of the above technical solution, in the step 1, stirring rate when stirring is 2000-2250r/min.
As an improvement of the above technical solution, it in the step 3, drops evenly remaining pre-emulsion and C material needs
It is dripped off in 2h.
As an improvement of the above technical solution, described Step 2: stirring rate when stirring in step 3 and step 4
For 400-800r/min.
As an improvement of the above technical solution, the composite modified styrene-acrylic emulsion of epoxy silane coupling agent-Organic fluoride applies
Film pencil hardness is in 4H or more, adhesive force 1 grade or more, water absorption rate are below 8% and lotion conversion ratio is 99% or more.
Compared with prior art, technical solution of the present invention has the following beneficial effects:
The composite modified styrene-acrylic emulsion of epoxy silane coupling agent-Organic fluoride produced by the present invention is compared to traditional modification benzene
Acrylic emulsion have more excellent hardness of film, film adhesive, film water absorption rate, film corrosion resistance, lotion conversion ratio
Etc. performances.Its film pencil hardness 4H or more, adhesive force in 1 grade or more, water absorption rate below 8% and the conversion ratio of lotion
99% or more.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention,
And it can be implemented in accordance with the contents of the specification, and in order to allow above and other objects, features and advantages of the invention can
It is clearer and more comprehensible, below in conjunction with preferred embodiment, detailed description are as follows.
Specific embodiment
The following detailed description of a specific embodiment of the invention, as part of this specification, by embodiment come
Illustrate that the principle of the present invention, other aspects of the present invention, feature and its advantage will become apparent by the detailed description.
Embodiment
Prepare the raw material of 1000 parts of composite modified styrene-acrylic emulsions of epoxy silane coupling agent-Organic fluoride of the present invention are as follows:
340-460 parts of A material, 337-342 parts of B material, 272-273 parts of C material.Wherein A material includes 310-414 parts of matrixes, and 11.6-19.4 parts change
Property monomer one, 18.8-28.2 parts of modified monomers two；B material include 11.3-15.8 parts of compound emulsifying agents, 2-2.4 parts of buffers, 324
Part distilled water；C material includes 2.7-3.5 parts of initiators, 270 parts of distilled water.Wherein
Matrix: the mass ratio of MMA, St and BA are MMA:St:BA=1:1:(2-3.33)；
Modified monomer one is DFMA；
The mass ratio of modified monomer two: MAA and KH-560 are MAA:KH-560=(3-5): 1；
Compound emulsifying agent: the mass ratio of SDS and OP-10 is SDS:OP-10=1:(1.5-2.5)；
Buffer is NaHCO3；
Initiator is APS.
Preparation step is as follows:
(1) matrix of the number, modified monomer one and modified monomer two obtained A is sufficiently mixed to expect, the number
Compound emulsifying agent and distilled water are mixed to prepare B material, and the initiator and distilled water of the number are mixed to prepare C material.A, B are expected again mixed
It closes liquid to pour into the three-necked flask fixed, opens thermal-arrest constant-temperature heating magnetic stirring apparatus immediately, adjusting revolving speed is high speed
(2000-2250r/min), reaction temperature are 40 DEG C, persistently stir 1h, close blender, and pre-emulsion is made；
(2) 50%-60% (in mass) that pre-emulsion is made is taken out, then by 30% number (in mass)
C material pours into three-necked flask, turn on agitator, and adjusting revolving speed is low speed (500-600r/min), reaction temperature is 75 DEG C, continues
Stir 1h；
(3) after step (2), the feed rate of peristaltic pump is adjusted, will be taken in step (2) respectively within the time of 2h
Pre-emulsion out is synchronous with the remaining C material of number uniformly to be instilled in three-necked flask, and low speed (500-600r/min) stirring is anti-
It answers；
(4) after step (3), 80 DEG C of reaction temperature are adjusted, constant temperature low speed (500-600r/min) is stirred to react 1h；
(5) after the completion of keeping the temperature, stop reaction, cooling, cooling, discharging, filtering, the epoxy silane coupling agent-, which is made, to be had
The composite modified styrene-acrylic emulsion of machine fluorine.
Wherein embodiment proportion is as shown in table 1.
1 embodiment of table and its proportion
Embodiment performance evaluation is as shown in table 2.
2 embodiment performance evaluation effect of table
The bound of each raw material cited by the present invention and each raw material of the present invention, section value and technological parameter
Bound, the section value of (such as temperature, time) can realize the present invention, embodiment numerous to list herein.
The above is a preferred embodiment of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, it is noted that for those skilled in the art, without departing from the principle of the present invention, may be used also
To make several improvement and variation, these, which improve and change, is also considered as protection scope of the present invention.
Claims (7)
1. a kind of composite modified styrene-acrylic emulsion of epoxy silane coupling agent-Organic fluoride, it is characterised in that:
The material quality number of every 1000 mass fraction lotion of the present invention are as follows: 340-460 parts of A material, 337-342 part B expect and
272.7-273.5 part C expects；
Wherein A material includes 309.6-412.4 parts of matrixes, 11.6-19.4 parts of modified monomers one, 18.8-28.2 parts of modified monomers two；
B material includes 11-15.7 parts of compound emulsifying agents, 2-2.3 parts of buffers, 324 parts of distilled water；C material includes 2.7-3.5 parts of initiators,
270 parts of distilled water；
Wherein,
Matrix is that the mass ratio of methyl methacrylate, styrene and n-butyl acrylate is 1:1:(2-3.33) mixture；
Modified monomer one is dodecafluoroheptyl methacrylate；
Modified monomer two is that the mass ratio of methacrylic acid and 3- glycidyl ether oxypropyltrimethoxysilane is (3-5): 1
Mixture；
Compound emulsifying agent is that the mass ratio of neopelex and octyl phenol polyoxyethylene ether is 1:(1.5-2.5) mixing
Object；
Buffer is NaHCO3；
Initiator is ammonium persulfate.
2. a kind of preparation method of the composite modified styrene-acrylic emulsion of epoxy silane coupling agent-Organic fluoride, which is characterized in that comprising as follows
Step:
Step 1: matrix, modified monomer one and modified monomer two are mixed to obtain A material, by compound emulsifying agent, buffer and distilled water
It is mixed to prepare B material, initiator and distilled water are mixed to prepare C material；Again A, B are expected to mix, at 30-40 DEG C, stirs 0.5-1h, system
Obtain pre-emulsion；
Step 2: by the pre-emulsion of pre-emulsion 50%-60% mass fraction obtained by step 1 and accounting for the material of C obtained by step 1
The C material of 30% mass fraction mixes and under the conditions of 70-75 DEG C, is stirred to react 0.5-1h；
Remaining pre-emulsion is dropped evenly and C expects and stirs Step 3: synchronizing into the mixture after step 2 reaction；
Step 4: mixture obtained by step 3 is stirred to react 1-1.5h under the conditions of 80-85 DEG C；
Step 5: the epoxy silane coupling agent-, which is made, to be had by liquid obtained by step 4 through supercooling, cooling, discharging, filtering
The composite modified styrene-acrylic emulsion of machine fluorine.
3. the preparation method of the composite modified styrene-acrylic emulsion of epoxy silane coupling agent-Organic fluoride as claimed in claim 2, feature
It is: in the step 1, wherein
Matrix is that the mass ratio of methyl methacrylate, styrene and n-butyl acrylate is 1:1:(2-3.33) mixture；
Modified monomer one is dodecafluoroheptyl methacrylate；
Modified monomer two is that the mass ratio of methacrylic acid and 3- glycidyl ether oxypropyltrimethoxysilane is (3-5): 1
Mixture；
Compound emulsifying agent is that the mass ratio of neopelex and octyl phenol polyoxyethylene ether is 1:(1.5-2.5) mixing
Object；
Buffer is NaHCO3；
Initiator is ammonium persulfate；
The material quality number of every 1000 mass fraction lotion of the present invention are as follows: 340-460 parts of A material, 337-342 part B expect and
272-273 parts of C material.
4. the preparation method of the composite modified styrene-acrylic emulsion of epoxy silane coupling agent-Organic fluoride as claimed in claim 2, feature
Be: in the step 1, stirring rate when stirring is 2000-2250r/min.
5. the preparation method of the composite modified styrene-acrylic emulsion of epoxy silane coupling agent-Organic fluoride as claimed in claim 2, feature
It is: in the step 3, drops evenly remaining pre-emulsion and C material needs to drip off in 2h.
6. the preparation method of the composite modified styrene-acrylic emulsion of epoxy silane coupling agent-Organic fluoride as claimed in claim 2, feature
It is: described Step 2: stirring rate when stirring in step 3 and step 4 is 400-800r/min.
7. the composite modified styrene-acrylic emulsion of epoxy silane coupling agent-Organic fluoride as described in claim 1, it is characterised in that: described
The composite modified styrene-acrylic emulsion of epoxy silane coupling agent-Organic fluoride, film pencil hardness 4H or more, adhesive force 1 grade or more,
Water absorption rate is below 8% and lotion conversion ratio is 99% or more.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811639147.XA CN109810226A (en) | 2018-12-29 | 2018-12-29 | A kind of composite modified styrene-acrylic emulsion of epoxy silane coupling agent-Organic fluoride and preparation method |
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| CN113563545A (en) * | 2021-08-19 | 2021-10-29 | 广州市斯洛柯高分子聚合物有限公司 | Organic silicon modified acrylic emulsion for glass coating and preparation method thereof |
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Application publication date: 20190528 |