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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- 239000000839 emulsion Substances 0.000 title claims abstract description 57
- 229920001909 styrene-acrylic polymer Polymers 0.000 title claims abstract description 36
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 239000004593 Epoxy Substances 0.000 title claims abstract description 24
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 230000008878 coupling Effects 0.000 title claims abstract description 23
- 238000010168 coupling process Methods 0.000 title claims abstract description 23
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 23
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title abstract 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000012153 distilled water Substances 0.000 claims abstract description 14
- 238000000576 coating method Methods 0.000 claims abstract description 13
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000011248 coating agent Substances 0.000 claims abstract description 11
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 9
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 8
- MTEZSDOQASFMDI-UHFFFAOYSA-N 1-trimethoxysilylpropan-1-ol Chemical compound CCC(O)[Si](OC)(OC)OC MTEZSDOQASFMDI-UHFFFAOYSA-N 0.000 claims abstract description 6
- DUIOKRXOKLLURE-UHFFFAOYSA-N 2-octylphenol Chemical compound CCCCCCCCC1=CC=CC=C1O DUIOKRXOKLLURE-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000010521 absorption reaction Methods 0.000 claims abstract description 6
- 239000000853 adhesive Substances 0.000 claims abstract description 6
- 230000001070 adhesive effect Effects 0.000 claims abstract description 6
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 6
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 38
- 239000000178 monomer Substances 0.000 claims description 22
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 20
- 229910052731 fluorine Inorganic materials 0.000 claims description 20
- 239000011737 fluorine Substances 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 13
- 239000003995 emulsifying agent Substances 0.000 claims description 11
- 239000003999 initiator Substances 0.000 claims description 11
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical group [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 10
- 239000011159 matrix material Substances 0.000 claims description 9
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 8
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 8
- 239000000872 buffer Substances 0.000 claims description 5
- 239000006172 buffering agent Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 5
- SMGIMBKCWODARY-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,7,7,7-dodecafluoroheptyl 2-methylprop-2-enoate Chemical group CC(=C)C(=O)OC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)CC(F)(F)F SMGIMBKCWODARY-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- YJKHMSPWWGBKTN-UHFFFAOYSA-N 2,2,3,3,4,4,5,5,6,6,7,7-dodecafluoroheptyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)F YJKHMSPWWGBKTN-UHFFFAOYSA-N 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract description 4
- 238000007720 emulsion polymerization reaction Methods 0.000 abstract description 2
- 239000006210 lotion Substances 0.000 abstract 2
- 230000006872 improvement Effects 0.000 description 5
- 230000007547 defect Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
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- Polymerisation Methods In General (AREA)
- Compositions Of Macromolecular Compounds (AREA)
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 invention relates to an epoxy silane coupling agent-organic fluorine composite modified styrene-acrylic emulsion and a preparation method thereof, belonging to the technical field of building coatings.
Background
The styrene-acrylic emulsion has the characteristics of low manufacturing cost, no toxicity, no smell, no combustion, less pollution, excellent weather resistance, stain resistance, corrosion resistance and the like, and is widely applied in the field of coatings. However, the traditional styrene-acrylic emulsion has poor performance on various properties such as hardness, adhesion, solvent resistance, water resistance and the like of a coating film, and the application range of the traditional styrene-acrylic emulsion is limited to a great extent, so that the traditional styrene-acrylic emulsion obtains more excellent properties by using a modification method, and the traditional styrene-acrylic emulsion is an important breakthrough for further expanding the application range of the traditional styrene-acrylic emulsion on the basis of exerting the excellent characteristics of the styrene-acrylic emulsion. In recent years, researches on modification of styrene-acrylic emulsion have been carried out, for example, modified styrene-acrylic emulsion paint with higher coating film hardness or better corrosion resistance is obtained, but most of modified styrene-acrylic emulsion cannot have more performances, and the defects are obvious.
Disclosure of Invention
Based on the defects of the prior art, the technical problem solved by the invention is to provide the organic silicon (epoxy silane coupling agent)/organic fluorine composite modified styrene-acrylic emulsion, and the prepared product not only keeps the excellent characteristics of the traditional styrene-acrylic emulsion, but also obtains more excellent coating hardness, adhesive force, solvent resistance, water resistance and emulsion conversion rate, and has great application prospect.
In order to solve the technical problems, the invention provides an epoxy silane coupling agent-organic fluorine composite modified styrene-acrylic emulsion and a preparation method thereof, wherein Methyl Methacrylate (MMA), styrene (St), n-Butyl Acrylate (BA), methacrylic acid (MAA), dodecafluoro heptyl methacrylate (DFMA), 3-glycidyl ether oxypropyltrimethoxysilane (KH-560), octyl phenol polyoxyethylene ether (OP-10), sodium dodecyl benzene sulfonate (SDS), Ammonium Persulfate (APS) and distilled water are used as main raw materials (all are analytically pure), and the epoxy silane coupling agent-organic fluorine composite modified styrene-acrylic emulsion is synthesized by an emulsion polymerization mode.
An epoxy silane coupling agent-organic fluorine composite modified styrene-acrylic emulsion:
every 1000 parts by weight of the emulsion comprises the following raw materials in parts by weight: 340-460 parts of material A, 337-342 parts of material B and 272.7-273.5 parts of material C;
wherein the A material comprises 309.6-412.4 parts of matrix, 11.6-19.4 parts of modified monomer I and 18.8-28.2 parts of modified monomer II; the material B comprises 11-15.7 parts of composite emulsifier, 2-2.3 parts of buffering agent and 324 parts of distilled water; the material C comprises 2.7-3.5 parts of initiator and 270 parts of distilled water;
wherein,
the matrix is a mixture of methyl methacrylate, styrene and n-butyl acrylate in a mass ratio of 1:1 (2-3.33);
the first modified monomer is methacrylic acid dodecafluoroheptyl ester;
the second modified monomer is a mixture of methacrylic acid and 3-glycidyl ether oxypropyltrimethoxysilane in the mass ratio of (3-5) to 1;
the composite emulsifier is a mixture of sodium dodecyl benzene sulfonate and octyl phenol polyoxyethylene ether in a mass ratio of 1 (1.5-2.5);
the buffer is NaHCO3；
The initiator is ammonium persulfate.
A preparation method of epoxy silane coupling agent-organic fluorine composite modified styrene-acrylic emulsion comprises the following steps:
step one, mixing a matrix, a modified monomer I and a modified monomer II to obtain a material A, mixing a composite emulsifier, a buffering agent and distilled water to obtain a material B, and mixing an initiator and distilled water to obtain a material C; mixing the A, B materials, and stirring at 30-40 deg.C for 0.5-1h to obtain pre-emulsion;
step two, mixing 50-60 mass percent of pre-emulsion obtained in the step one with 30 mass percent of material C obtained in the step one, and stirring and reacting for 0.5-1h at 70-75 ℃;
step three, synchronously and uniformly dropwise adding the remaining pre-emulsion and the material C into the mixture reacted in the step two, and stirring;
step four, stirring the mixture obtained in the step three at the temperature of 80-85 ℃ for reaction for 1-1.5 h;
and step five, cooling, discharging and filtering the liquid obtained in the step four to obtain the epoxy silane coupling agent-organic fluorine composite modified styrene-acrylic emulsion.
As an improvement of the above technical solution, in the first step, wherein,
the matrix is a mixture of methyl methacrylate, styrene and n-butyl acrylate in a mass ratio of 1:1 (2-3.33);
the first modified monomer is methacrylic acid dodecafluoroheptyl ester;
the second modified monomer is a mixture of methacrylic acid and 3-glycidyl ether oxypropyltrimethoxysilane in the mass ratio of (3-5) to 1;
the composite emulsifier is a mixture of sodium dodecyl benzene sulfonate and octyl phenol polyoxyethylene ether in a mass ratio of 1 (1.5-2.5);
the buffer is NaHCO3；
The initiator is ammonium persulfate;
every 1000 parts by weight of the emulsion comprises the following raw materials in parts by weight: 460 parts of material A at 340-.
As an improvement of the technical proposal, in the first step, the stirring speed during stirring is 2000-2250 r/min.
As an improvement of the technical scheme, in the third step, the residual pre-emulsion and the material C need to be dripped in 2 hours.
As an improvement of the above technical scheme, the stirring speed in the second step, the third step and the fourth step is 400-800 r/min.
As an improvement of the technical scheme, the epoxy silane coupling agent-organic fluorine composite modified styrene-acrylic emulsion has the advantages that the coating pencil hardness is more than 4H, the adhesive force is more than 1 grade, the water absorption is less than 8 percent, and the emulsion conversion rate is more than 99 percent.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
compared with the traditional modified styrene-acrylic emulsion, the epoxy silane coupling agent-organic fluorine composite modified styrene-acrylic emulsion prepared by the invention has the advantages of excellent performances of coating hardness, coating adhesion, coating water absorption, coating corrosion resistance, emulsion conversion rate and the like. The coating film has pencil hardness of more than 4H, adhesive force of more than 1 grade, water absorption of less than 8 percent and emulsion conversion rate of more than 99 percent.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood, the present invention may be implemented in accordance with the contents of the description, and in order to make the above and other objects, features, and advantages of the present invention more clearly understood, the following detailed description is given in conjunction with the preferred embodiments.
Detailed Description
Other aspects, features and advantages of the present invention will become apparent from the following detailed description, which, when taken in conjunction with the drawings, illustrate by way of example the principles of the invention.
Examples
The raw materials for preparing 1000 parts of the epoxy silane coupling agent-organic fluorine composite modified styrene-acrylic emulsion are as follows: 460 parts of material A at 340-. Wherein, the A material comprises 310-414 parts of matrix, 11.6-19.4 parts of modified monomer I and 18.8-28.2 parts of modified monomer II; the B material comprises 11.3-15.8 parts of composite emulsifier, 2-2.4 parts of buffering agent and 324 parts of distilled water; the material C comprises 2.7-3.5 parts of initiator and 270 parts of distilled water. Wherein
The mass ratio of MMA to St to BA is MMA to St to BA 1 to 1 (2-3.33);
the first modified monomer is DFMA;
the mass ratio of the second modified monomer to the MAA to the KH-560 is MAA: KH-560 ═ (3-5): 1;
compound emulsifier: the mass ratio of SDS to OP-10 is SDS: OP-10 is 1 (1.5-2.5);
the buffer is NaHCO3；
The initiator is APS.
The preparation steps are as follows:
(1) and fully mixing the base body, the modified monomer I and the modified monomer II in parts to obtain a material A, mixing the composite emulsifier in parts with distilled water to obtain a material B, and mixing the initiator in parts with distilled water to obtain a material C. Pouring the A, B material mixed solution into a fixed three-neck flask, immediately starting a heat-collecting constant-temperature heating magnetic stirrer, adjusting the rotating speed to be high speed (2000-;
(2) taking out 50-60% by mass of the prepared pre-emulsion, pouring 30% by mass of the material C into a three-neck flask, starting a stirrer, adjusting the rotating speed to be low (500-;
(3) after the step (2) is finished, adjusting the feeding rate of a peristaltic pump, synchronously and uniformly dropping the pre-emulsion taken out in the step (2) and the residual part of the material C into a three-neck flask within 2 hours, and stirring at a low speed (500-;
(4) after the step (3) is finished, adjusting the reaction temperature to 80 ℃, and stirring and reacting at constant temperature and low speed (500- & gt 600r/min) for 1 h;
(5) and after the heat preservation is finished, stopping the reaction, cooling, discharging and filtering to obtain the epoxy silane coupling agent-organic fluorine composite modified styrene-acrylic emulsion.
The proportions of the examples are shown in Table 1.
TABLE 1 examples and their compounding ratios
The evaluation of the properties of the examples is shown in Table 2.
Table 2 effects of evaluating the properties of examples
The raw materials listed in the invention, the upper and lower limits and interval values of the raw materials of the invention, and the upper and lower limits and interval values of the process parameters (such as temperature, time and the like) can all realize the invention, and the examples are not listed.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (7)
1. An epoxy silane coupling agent-organic fluorine composite modified styrene-acrylic emulsion is characterized in that:
every 1000 parts by weight of the emulsion comprises the following raw materials in parts by weight: 340-460 parts of material A, 337-342 parts of material B and 272.7-273.5 parts of material C;
wherein the A material comprises 309.6-412.4 parts of matrix, 11.6-19.4 parts of modified monomer I and 18.8-28.2 parts of modified monomer II; the material B comprises 11-15.7 parts of composite emulsifier, 2-2.3 parts of buffering agent and 324 parts of distilled water; the material C comprises 2.7-3.5 parts of initiator and 270 parts of distilled water;
wherein,
the matrix is a mixture of methyl methacrylate, styrene and n-butyl acrylate in a mass ratio of 1:1 (2-3.33);
the first modified monomer is methacrylic acid dodecafluoroheptyl ester;
the second modified monomer is a mixture of methacrylic acid and 3-glycidyl ether oxypropyltrimethoxysilane in the mass ratio of (3-5) to 1;
the composite emulsifier is a mixture of sodium dodecyl benzene sulfonate and octyl phenol polyoxyethylene ether in a mass ratio of 1 (1.5-2.5);
the buffer is NaHCO3；
The initiator is ammonium persulfate.
2. The preparation method of the epoxy silane coupling agent-organic fluorine composite modified styrene-acrylic emulsion is characterized by comprising the following steps:
step one, mixing a matrix, a modified monomer I and a modified monomer II to obtain a material A, mixing a composite emulsifier, a buffering agent and distilled water to obtain a material B, and mixing an initiator and distilled water to obtain a material C; mixing the A, B materials, and stirring at 30-40 deg.C for 0.5-1h to obtain pre-emulsion;
step two, mixing 50-60 mass percent of pre-emulsion obtained in the step one with 30 mass percent of material C obtained in the step one, and stirring and reacting for 0.5-1h at 70-75 ℃;
step three, synchronously and uniformly dropwise adding the remaining pre-emulsion and the material C into the mixture reacted in the step two, and stirring;
step four, stirring the mixture obtained in the step three at the temperature of 80-85 ℃ for reaction for 1-1.5 h;
and step five, cooling, discharging and filtering the liquid obtained in the step four to obtain the epoxy silane coupling agent-organic fluorine composite modified styrene-acrylic emulsion.
3. The method for preparing the epoxy silane coupling agent-organic fluorine composite modified styrene-acrylic emulsion as claimed in claim 2, wherein: in the first step, wherein,
the matrix is a mixture of methyl methacrylate, styrene and n-butyl acrylate in a mass ratio of 1:1 (2-3.33);
the first modified monomer is methacrylic acid dodecafluoroheptyl ester;
the second modified monomer is a mixture of methacrylic acid and 3-glycidyl ether oxypropyltrimethoxysilane in the mass ratio of (3-5) to 1;
the composite emulsifier is a mixture of sodium dodecyl benzene sulfonate and octyl phenol polyoxyethylene ether in a mass ratio of 1 (1.5-2.5);
the buffer is NaHCO3；
The initiator is ammonium persulfate;
every 1000 parts by weight of the emulsion comprises the following raw materials in parts by weight: 460 parts of material A at 340-.
4. The method for preparing the epoxy silane coupling agent-organic fluorine composite modified styrene-acrylic emulsion as claimed in claim 2, wherein: in the first step, the stirring speed during stirring is 2000-2250 r/min.
5. The method for preparing the epoxy silane coupling agent-organic fluorine composite modified styrene-acrylic emulsion as claimed in claim 2, wherein: in the third step, the residual pre-emulsion and the material C need to be dripped off within 2 hours.
6. The method for preparing the epoxy silane coupling agent-organic fluorine composite modified styrene-acrylic emulsion as claimed in claim 2, wherein: the stirring speed in the second step, the third step and the fourth step is 400-800 r/min.
7. The epoxy silane coupling agent-organofluorine composite modified styrene-acrylic emulsion according to claim 1, wherein: the epoxy silane coupling agent-organic fluorine composite modified styrene-acrylic emulsion has the coating pencil hardness of more than 4H, the adhesive force of more than 1 grade, the water absorption of less than 8 percent and the emulsion conversion rate of more than 99 percent.
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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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Application publication date: 20190528 |