CN110938089A - Preparation method of silane for synthesizing water-based acrylic emulsion and silane - Google Patents
Preparation method of silane for synthesizing water-based acrylic emulsion and silane Download PDFInfo
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- CN110938089A CN110938089A CN201911207291.0A CN201911207291A CN110938089A CN 110938089 A CN110938089 A CN 110938089A CN 201911207291 A CN201911207291 A CN 201911207291A CN 110938089 A CN110938089 A CN 110938089A
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- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 42
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 239000000839 emulsion Substances 0.000 title claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims abstract description 20
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- 239000012043 crude product Substances 0.000 claims abstract description 4
- 238000004821 distillation Methods 0.000 claims abstract description 4
- YDSWCNNOKPMOTP-UHFFFAOYSA-N mellitic acid Chemical compound OC(=O)C1=C(C(O)=O)C(C(O)=O)=C(C(O)=O)C(C(O)=O)=C1C(O)=O YDSWCNNOKPMOTP-UHFFFAOYSA-N 0.000 claims description 26
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 18
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 14
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 12
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 12
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 10
- CHPNMYQJQQGAJS-UHFFFAOYSA-N 3-tri(propan-2-yloxy)silylpropyl 2-methylprop-2-enoate Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)CCCOC(=O)C(C)=C CHPNMYQJQQGAJS-UHFFFAOYSA-N 0.000 claims description 9
- VAONRJSBKBYQRM-UHFFFAOYSA-N C(C(=C)C)(=O)OCCC[Si](OC(C)C)(OC)OC Chemical compound C(C(=C)C)(=O)OCCC[Si](OC(C)C)(OC)OC VAONRJSBKBYQRM-UHFFFAOYSA-N 0.000 claims description 9
- -1 methacryloxypropyldiisopropoxymethoxysilane Chemical compound 0.000 claims description 9
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 7
- 238000003786 synthesis reaction Methods 0.000 claims description 7
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 claims description 7
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 claims description 7
- NHJVRSWLHSJWIN-UHFFFAOYSA-N 2,4,6-trinitrobenzenesulfonic acid Chemical compound OS(=O)(=O)C1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O NHJVRSWLHSJWIN-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 4
- 238000007720 emulsion polymerization reaction Methods 0.000 abstract description 3
- 238000004321 preservation Methods 0.000 abstract description 2
- 239000004925 Acrylic resin Substances 0.000 description 7
- 229920000178 Acrylic resin Polymers 0.000 description 7
- 239000006087 Silane Coupling Agent Substances 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 150000004756 silanes Chemical class 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 125000005587 carbonate group Chemical group 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- MABAWBWRUSBLKQ-UHFFFAOYSA-N ethenyl-tri(propan-2-yloxy)silane Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)C=C MABAWBWRUSBLKQ-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- HCOKJWUULRTBRS-UHFFFAOYSA-N propan-2-yloxysilane Chemical compound CC(C)O[SiH3] HCOKJWUULRTBRS-UHFFFAOYSA-N 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/188—Preparation; Treatments not provided for in C07F7/20 by reactions involving the formation of Si-O linkages
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F230/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
- C08F230/04—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal
- C08F230/08—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon
-
- 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
- C09D143/00—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 containing boron, silicon, phosphorus, selenium, tellurium, or a metal; Coating compositions based on derivatives of such polymers
- C09D143/04—Homopolymers or copolymers of monomers containing silicon
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Silicon Polymers (AREA)
Abstract
The invention discloses a preparation method of silane for synthesizing water-based acrylic emulsion and silane, and relates to the technical field of silane preparation, wherein the temperature of a reaction kettle is controlled to be 30-40 ℃, 100 parts by mass of methacryloxypropyltrimethoxysilane and 0.3-0.5 part by mass of a catalyst are added into the reaction kettle, the reaction kettle is stirred and slowly dripped with 40-50 parts by mass of isopropanol, and after dripping is finished, the reaction kettle is subjected to heat preservation reaction at 30-40 ℃ for 2-3 hours; adding 0.7-1.5 parts by mass of a neutralizing agent, stirring for 2-3 hours, and filtering out salt in the system to obtain a crude product; distilling out alcohol under negative pressure, and controlling the distillation temperature below 50 ℃ to obtain the silane synthesized by the water-based acrylic emulsion. Compared with the traditional silane, the preparation method can greatly improve the stability of the product, reduce the occurrence of gel phenomenon in the emulsion polymerization process, improve the addition amount of the silane in the water-based acrylic emulsion and further improve the performance of the acrylic emulsion.
Description
Technical Field
The invention relates to the technical field of silane preparation, in particular to a preparation method of silane for synthesizing aqueous acrylic emulsion and silane.
Background
The acrylic resin has good adhesive force and weather resistance, and is widely applied due to excellent performance, the existing acrylic resin is mainly a solvent type and has great pollution to the environment, compared with the solvent resin of the same type, the water-based acrylic resin has poorer performances such as water resistance, corrosion resistance, chemical resistance and the like, and after the water-based acrylic resin is dried by air to form a film, a coating is formed by accumulating particles, so the performances such as adhesive force, water resistance, salt fog resistance, abrasion resistance, hardness, heat resistance, impact resistance, moisture resistance, solvent resistance and the like are poorer than those of the oil-based acrylic resin. To ameliorate these deficiencies of waterborne acrylic resins, silanes may be incorporated into the polymerization system. The silanes commonly used today are vinyltrimethoxysilane, vinyltriethoxysilane, methacryloxypropyltrimethoxysilane, and the like.
These silane coupling agents have in common that: 1. the organic reactive group can copolymerize with acrylic monomers, thereby enabling the silane coupling agent to be polymerized onto a molecular chain. 2. The hydrolyzable group on the silane coupling agent is easy to generate dehydration condensation in an aqueous system. Particularly, the emulsion polymerization temperature usually reaches 75-88 ℃, and the silanes are hydrolyzed very quickly. In particular, the collision of the coupling agent with water molecules during the migration of the coupling agent from the monomer droplets to the latex bundle is unavoidable, and the hydrolysis thereof is almost instantaneously completed, so that the gel is easily generated. Therefore, the amount of silane added to the aqueous acrylic resin is also greatly limited, and is generally about 1% at most. In order to reduce the hydrolysis speed of the silane, the vinyltriisopropoxy silane is used instead of the vinyltriisopropoxy silane, but the vinyltriisopropoxy has too low activity and is difficult to hydrolyze under heating conditions, and the use of the product is seriously influenced.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of silane for synthesizing aqueous acrylic emulsion and silane, which greatly improve the stability of products.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows: a preparation method of silane for synthesizing aqueous acrylic emulsion comprises the following steps:
controlling the temperature of a reaction kettle to be 30-40 ℃, adding 100 parts by mass of methacryloxypropyltrimethoxysilane and 0.3-0.5 part by mass of a catalyst into the reaction kettle, stirring, slowly dropwise adding 40-50 parts by mass of isopropanol into the kettle, and after dropwise adding, keeping the temperature at 30-40 ℃ for reacting for 2-3 hours;
adding 0.7-1.5 parts by mass of a neutralizing agent, stirring for 2-3 hours, and filtering out salt in the system to obtain a crude product;
distilling out alcohol under negative pressure, and controlling the distillation temperature below 50 ℃ to obtain the silane synthesized by the water-based acrylic emulsion.
On the basis of the technical scheme, the silane for synthesizing the water-based acrylic emulsion comprises the following components in parts by mass: 5 to 10 parts of methacryloxypropyltrimethoxysilane, 40 to 50 parts of methacryloxypropylisopropoxydimethoxysilane, 20 to 40 parts of methacryloxypropyldiisopropoxymethoxysilane and 0 to 10 parts of methacryloxypropyltriisopropoxysilane.
On the basis of the technical scheme, the catalyst is one of organic strong acid, benzene hexacarboxylic acid, trichloroacetic acid, trinitrobenzene sulfonic acid, p-toluenesulfonic acid and trifluoromethanesulfonic acid.
On the basis of the technical scheme, the neutralizing agent is one of carbonate, sodium carbonate, calcium carbonate and potassium carbonate.
The invention also provides silane for synthesizing the water-based acrylic emulsion, which comprises the following raw materials in parts by weight:
100 parts of methacryloxypropyltrimethoxysilane;
0.3-0.5 parts of a catalyst;
40-50 parts of isopropanol;
0.7-1.5 parts of a neutralizing agent.
On the basis of the technical scheme, the silane for synthesizing the water-based acrylic emulsion comprises the following components in parts by mass: 5 to 10 parts of methacryloxypropyltrimethoxysilane, 40 to 50 parts of methacryloxypropylisopropoxydimethoxysilane, 20 to 40 parts of methacryloxypropyldiisopropoxymethoxysilane and 0 to 10 parts of methacryloxypropyltriisopropoxysilane.
On the basis of the technical scheme, the catalyst is one of organic strong acid, mellitic acid, trichloroacetic acid, trinitrobenzenesulfonic acid, p-toluenesulfonic acid and trifluoromethanesulfonic acid, and mellitic acid is preferred.
On the basis of the technical scheme, the neutralizing agent is one of carbonate, sodium carbonate, calcium carbonate and potassium carbonate, and preferably sodium carbonate.
Compared with the prior art, the invention has the advantages that:
compared with the traditional silane, the silane prepared by the preparation method for synthesizing the water-based acrylic emulsion can greatly improve the stability of the product, reduce the occurrence of gel phenomenon in the emulsion polymerization process, improve the addition amount of the silane in the water-based acrylic emulsion and further improve the performance of the acrylic emulsion.
Detailed Description
The embodiment of the invention provides a preparation method of silane for synthesizing aqueous acrylic emulsion, which comprises the following steps:
(1) controlling the temperature of the reaction kettle to be 30-40 ℃, then adding 100 parts by mass of methacryloxypropyltrimethoxysilane and 0.3-0.5 part by mass of a catalyst into the reaction kettle, and starting stirring.
(2) Slowly dripping 40-50 parts by mass of isopropanol into the kettle, and controlling the temperature in the dripping process to be 30-40 ℃.
(3) And after the dropwise addition is finished, carrying out heat preservation reaction at 30-40 ℃ for 2-3 h.
(4) And adding 0.7-1.5 parts by mass of a neutralizing agent, and stirring for 2-3 hours, wherein the pH test paper detects that the mixture is neutral or weakly alkaline.
(5) The crude product was obtained by filtering off the salts in the system with a filter.
(6) Distilling out alcohol under negative pressure, and controlling the distillation temperature below 50 ℃ to obtain the target product.
The silane prepared by the method of the embodiment of the invention contains the isopropoxy silane with large steric hindrance, can greatly reduce the hydrolysis speed of the silane, ensures that the silane is polymerized with acrylic acid and then hydrolyzed, and has the maximum addition amount of 10 percent. The product is synthesized in one step without rectification, so that the energy consumption can be greatly saved. No waste material is generated in the product synthesis process, and the production process is green and environment-friendly.
As a preferred embodiment, the silane for aqueous acrylic emulsion synthesis comprises the following components in parts by weight: 5 to 10 parts of methacryloxypropyltrimethoxysilane, 40 to 50 parts of methacryloxypropylisopropoxydimethoxysilane, 20 to 40 parts of methacryloxypropyldiisopropoxymethoxysilane and 0 to 10 parts of methacryloxypropyltriisopropoxysilane.
In a preferred embodiment, the catalyst is an organic strong acid, and is one of mellitic acid, trichloroacetic acid, trinitrobenzenesulfonic acid, p-toluenesulfonic acid and trifluoromethanesulfonic acid.
In a preferred embodiment, the neutralizing agent is carbonate, and is one of sodium carbonate, calcium carbonate and potassium carbonate.
The embodiment of the invention also provides silane for synthesizing the water-based acrylic emulsion, which comprises the following raw materials in parts by weight:
100 parts of methacryloxypropyltrimethoxysilane;
0.3-0.5 parts of a catalyst;
40-50 parts of isopropanol;
0.7-1.5 parts of a neutralizing agent.
As a preferred embodiment, the silane for aqueous acrylic emulsion synthesis comprises the following components in parts by weight: 5 to 10 parts of methacryloxypropyltrimethoxysilane, 40 to 50 parts of methacryloxypropylisopropoxydimethoxysilane, 20 to 40 parts of methacryloxypropyldiisopropoxymethoxysilane and 0 to 10 parts of methacryloxypropyltriisopropoxysilane.
In a preferred embodiment, the catalyst is an organic strong acid, and is one of mellitic acid, trichloroacetic acid, trinitrobenzenesulfonic acid, p-toluenesulfonic acid and trifluoromethanesulfonic acid, and mellitic acid is preferred.
In a preferred embodiment, the neutralizing agent is a carbonate, which is one of sodium carbonate, calcium carbonate and potassium carbonate, and is preferably a carbonate.
The present invention will be described in further detail with reference to examples.
Example 1
348g of methacryloxypropyltrimethoxysilane was weighed and put into a 1L three-necked flask, and stirring was started. Weighing 1.74g of mellitic acid, dissolving in 152g of isopropanol, stirring uniformly to dissolve, quickly dropping mellitic acid solution into the kettle by using a constant-pressure titration funnel, continuously reacting for 3 hours, and adding about 2.5g of Na2CO3Neutralizing the catalyst, stirring for about 1 hr, pumping alcohol to 70 deg.c under negative pressure (-0.09MPa) and filtering to obtain 365g product, which is analyzed by GC to obtain methacryloxypropyltrimethoxysilane 9%, methacryloxypropylisopropoxydimethoxysilane 45%, methacryloxypropyldiisopropoxymethoxysilane 35% and methacryloxypropyltriisopropoxysilane 8%.
Example 2
350g of methacryloxypropyltrimethoxysilane is weighed and put into a 1L three-neck flask, and stirring is started. Weighing 1.8g of trifluoromethanesulfonic acid, dissolving in 155g of isopropanol, stirring uniformly to dissolve, quickly dropping mellitic acid solution into the kettle by using a constant-pressure titration funnel, continuously reacting for 3h, and adding about 2.6g of Na2CO3After neutralizing the catalyst and continuing stirring for about 1 hour, evacuating to 70 deg.C under negative pressure (-0.09MPa), filtering to obtain 367g of product, which is analyzed by GC to obtain 7% methacryloxypropyltrimethoxysilane, 48% methacryloxypropylisopropoxydimethoxysilane, 36% methacryloxypropyldiisopropoxymethoxysilane and 7% methacryloxypropyltriisopropoxysilane.
Example 3
350g of methacryloxypropyltrimethoxysilane is weighed and put into a 1L three-neck flask, and stirring is started. Weighing 1.8g of trichloroacetic acid, dissolving in 155g of isopropanol, uniformly stirring and dissolving, quickly dropping a mellitic acid solution into a kettle by using a constant-pressure titration funnel, continuously reacting for 3 hours, adding about 2.6g of calcium carbonate to neutralize the catalyst, continuously stirring for about 1 hour, then extracting alcohol to 70 ℃ under negative pressure (-0.09MPa) to obtain 364g of product, and carrying out GC analysis on 7% of methacryloxypropyltrimethoxysilane, 47% of methacryloxypropylisopropoxydimethoxysilane, 34% of methacryloxypropyldiisopropoxymethoxysilane and 10% of methacryloxypropyltriisopropoxysilane.
Example 4
The acrylic emulsion prepared from the silane synthesized in example 1 was formulated as follows and then painted on woodware, with two layers of top coats, left at room temperature for 7 days, and after complete curing, tested for water resistance, boiled water resistance, and 50% ethanol resistance for one hour according to national standards. It has high boiling water resistance, high ethanol resistance, no whitening and no foaming. The normal temperature water is slightly whitish after 24 hours, does not bubble and recovers after one hour after being removed. The formula and the operation details of the wood finish paint are shown in table 1:
TABLE 1
The present invention is not limited to the above-described embodiments, and it will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the principle of the present invention, and such modifications and improvements are also considered to be within the scope of the present invention. Those not described in detail in this specification are within the skill of the art.
Claims (8)
1. A preparation method of silane for synthesizing aqueous acrylic emulsion is characterized by comprising the following steps:
controlling the temperature of a reaction kettle to be 30-40 ℃, adding 100 parts by mass of methacryloxypropyltrimethoxysilane and 0.3-0.5 part by mass of a catalyst into the reaction kettle, stirring, slowly dropwise adding 40-50 parts by mass of isopropanol into the kettle, and after dropwise adding, keeping the temperature at 30-40 ℃ for reacting for 2-3 hours;
adding 0.7-1.5 parts by mass of a neutralizing agent, stirring for 2-3 hours, and filtering out salt in the system to obtain a crude product;
distilling out alcohol under negative pressure, and controlling the distillation temperature below 50 ℃ to obtain the silane synthesized by the water-based acrylic emulsion.
2. The method of claim 1, wherein: the silane for synthesizing the water-based acrylic emulsion comprises the following components in parts by weight: 5 to 10 parts of methacryloxypropyltrimethoxysilane, 40 to 50 parts of methacryloxypropylisopropoxydimethoxysilane, 20 to 40 parts of methacryloxypropyldiisopropoxymethoxysilane and 0 to 10 parts of methacryloxypropyltriisopropoxysilane.
3. The method of claim 1, wherein: the catalyst is one of organic strong acid, benzene hexacarboxylic acid, trichloroacetic acid, trinitrobenzene sulfonic acid, p-toluenesulfonic acid and trifluoromethanesulfonic acid.
4. The method of claim 1, wherein: the neutralizer is one of carbonate, sodium carbonate, calcium carbonate and potassium carbonate.
5. A silane for aqueous acrylic emulsion synthesis, characterized by: the silane for synthesizing the water-based acrylic emulsion comprises the following raw materials in parts by weight:
100 parts of methacryloxypropyltrimethoxysilane;
0.3-0.5 parts of a catalyst;
40-50 parts of isopropanol;
0.7-1.5 parts of a neutralizing agent.
6. The silane for aqueous acrylic emulsion synthesis according to claim 5, characterized in that: the silane for synthesizing the water-based acrylic emulsion comprises the following components in parts by weight: 5 to 10 parts of methacryloxypropyltrimethoxysilane, 40 to 50 parts of methacryloxypropylisopropoxydimethoxysilane, 20 to 40 parts of methacryloxypropyldiisopropoxymethoxysilane and 0 to 10 parts of methacryloxypropyltriisopropoxysilane.
7. The silane for aqueous acrylic emulsion synthesis according to claim 5, characterized in that: the catalyst is organic strong acid, and is one of mellitic acid, trichloroacetic acid, trinitrobenzene sulfonic acid, p-toluenesulfonic acid and trifluoromethanesulfonic acid, and mellitic acid is preferred.
8. The silane for aqueous acrylic emulsion synthesis according to claim 5, characterized in that: the neutralizer is one of carbonate, sodium carbonate, calcium carbonate and potassium carbonate, and is preferably sodium carbonate.
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| CN115748009A (en) * | 2022-11-15 | 2023-03-07 | 安徽南澳地毯有限公司 | Preparation method of water-repellent carpet non-woven fabric |
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| CN115748009A (en) * | 2022-11-15 | 2023-03-07 | 安徽南澳地毯有限公司 | Preparation method of water-repellent carpet non-woven fabric |
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