CN112708393B - Dealcoholized silicone sealant and preparation method thereof - Google Patents
Dealcoholized silicone sealant and preparation method thereof Download PDFInfo
- Publication number
- CN112708393B CN112708393B CN202011593533.7A CN202011593533A CN112708393B CN 112708393 B CN112708393 B CN 112708393B CN 202011593533 A CN202011593533 A CN 202011593533A CN 112708393 B CN112708393 B CN 112708393B
- Authority
- CN
- China
- Prior art keywords
- parts
- oligomers
- gamma
- silicone sealant
- compound
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000004590 silicone sealant Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 39
- 239000007822 coupling agent Substances 0.000 claims abstract description 30
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 30
- RJMRIDVWCWSWFR-UHFFFAOYSA-N methyl(tripropoxy)silane Chemical compound CCCO[Si](C)(OCCC)OCCC RJMRIDVWCWSWFR-UHFFFAOYSA-N 0.000 claims abstract description 27
- -1 polysiloxane, dimethyl Polymers 0.000 claims abstract description 19
- 229920002545 silicone oil Polymers 0.000 claims abstract description 15
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 13
- INJVFBCDVXYHGQ-UHFFFAOYSA-N n'-(3-triethoxysilylpropyl)ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CCCNCCN INJVFBCDVXYHGQ-UHFFFAOYSA-N 0.000 claims abstract description 12
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims abstract description 12
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims abstract description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 239000011256 inorganic filler Substances 0.000 claims abstract description 10
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 10
- DCQBZYNUSLHVJC-UHFFFAOYSA-N 3-triethoxysilylpropane-1-thiol Chemical compound CCO[Si](OCC)(OCC)CCCS DCQBZYNUSLHVJC-UHFFFAOYSA-N 0.000 claims abstract description 9
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000539 dimer Substances 0.000 claims description 27
- 239000013638 trimer Substances 0.000 claims description 27
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 25
- 239000000203 mixture Substances 0.000 claims description 21
- 229920001296 polysiloxane Polymers 0.000 claims description 18
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 14
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 13
- 239000013522 chelant Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- NOGBEXBVDOCGDB-NRFIWDAESA-L (z)-4-ethoxy-4-oxobut-2-en-2-olate;propan-2-olate;titanium(4+) Chemical group [Ti+4].CC(C)[O-].CC(C)[O-].CCOC(=O)\C=C(\C)[O-].CCOC(=O)\C=C(\C)[O-] NOGBEXBVDOCGDB-NRFIWDAESA-L 0.000 claims description 11
- MTEZSDOQASFMDI-UHFFFAOYSA-N 1-trimethoxysilylpropan-1-ol Chemical compound CCC(O)[Si](OC)(OC)OC MTEZSDOQASFMDI-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000005909 Kieselgur Substances 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 238000004898 kneading Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 238000010276 construction Methods 0.000 abstract description 20
- 230000000052 comparative effect Effects 0.000 description 20
- 238000012360 testing method Methods 0.000 description 19
- 238000012423 maintenance Methods 0.000 description 9
- 239000000565 sealant Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 238000006073 displacement reaction Methods 0.000 description 5
- 239000004566 building material Substances 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000002390 adhesive tape Substances 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-IGMARMGPSA-N Calcium-40 Chemical group [40Ca] OYPRJOBELJOOCE-IGMARMGPSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- WHIVNJATOVLWBW-PLNGDYQASA-N (nz)-n-butan-2-ylidenehydroxylamine Chemical compound CC\C(C)=N/O WHIVNJATOVLWBW-PLNGDYQASA-N 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 229920005601 base polymer Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 229940008099 dimethicone Drugs 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 229910021487 silica fume Inorganic materials 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Silicon Polymers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention discloses a dealcoholized silicone sealant and a preparation method thereof. The dealcoholized silicone sealant is prepared from the following raw materials: alpha, omega-dihydroxy polysiloxane, dimethyl silicone oil, inorganic filler, compound cross-linking agent, compound coupling agent and titanate vulcanizing agent; the compound cross-linking agent consists of methyltripropoxysilane and oligomeric cross-linking agent, and the oligomeric cross-linking agent is selected from at least one of oligomers of methyltriethoxysilane, methyltripropoxysilane and oligomers of vinyl triethoxysilane; the compound coupling agent consists of gamma-glycidoxypropyltrimethoxysilane and an oligomeric coupling agent, wherein the oligomeric coupling agent is selected from at least one of oligomers of gamma-aminopropyltriethoxysilane, oligomers of N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane and oligomers of 3-mercaptopropyltriethoxysilane. The dealcoholized silicone sealant has the characteristic of no bubble in high-temperature construction.
Description
Technical Field
The invention relates to the technical field of sealants, in particular to a dealcoholized silicone sealant and a preparation method thereof.
Background
The silicone sealant is used for sealing joints between building curtain wall plates and between door and window plates, and is a preferred sealing material in the building industry due to good ultraviolet resistance, displacement resistance, elastic recovery capacity and excellent adhesion to common building materials.
After being vulcanized, the alcohol-type silicone sealant has higher elasticity, namely high displacement resistance, excellent bonding property and water-resistant bonding property and excellent weather resistance. The low molecules released in the curing process of the alcohol-type silicone sealant are alcohol substances, and compared with butanone oxime released by the common ketoxime-type silicone sealant on the market, the alcohol-type silicone sealant is obviously more environment-friendly. However, the common alcohol-type sealant on the market is easy to foam under the influence of high temperature of a curtain wall plate in the construction process of an outdoor curtain wall, so that the attractiveness and the waterproof performance of the seal can be influenced.
Disclosure of Invention
Based on the situation, the invention aims to provide a dealcoholization type silicone sealant which does not generate bubbles in high-temperature construction.
In order to achieve the purpose, the invention adopts the following scheme:
the dealcoholized silicone sealant is prepared from the following raw materials in parts by weight:
the compound cross-linking agent consists of methyltripropoxysilane and oligomeric cross-linking agent, and the oligomeric cross-linking agent is selected from at least one of oligomers of methyltriethoxysilane, methyltripropoxysilane and oligomers of vinyl triethoxysilane;
the compound coupling agent consists of gamma-glycidoxypropyltrimethoxysilane and an oligomeric coupling agent, wherein the oligomeric coupling agent is selected from at least one of oligomers of gamma-aminopropyltriethoxysilane, oligomers of N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane and oligomers of 3-mercaptopropyltriethoxysilane.
In some embodiments, the dealcoholized silicone sealant is prepared from the following raw materials in parts by weight:
in some embodiments, the compounded crosslinking agent is prepared from a mixture of 1: 2-7 of methyl tripropoxysilane and an oligomeric cross-linking agent.
In some embodiments, the compounded coupling agent is prepared from a mixture of 1: 0.8-3.5 of gamma-glycidoxypropyltrimethoxysilane and an oligomeric coupling agent.
In some embodiments, the compound cross-linking agent consists of oligomers of methyl tripropoxysilane and methyl triethoxysilane in a mass ratio of 1: 2-3, and the compound coupling agent consists of oligomers of gamma-glycidoxypropyltrimethoxysilane and gamma-aminopropyltriethoxysilane in a mass ratio of 1: 0.8-1.5.
In some embodiments, the compound cross-linking agent consists of oligomers of methyl tripropoxysilane and methyl tripropoxysilane in a mass ratio of 1: 3-4, and the compound coupling agent consists of oligomers of gamma-glycidoxypropyltrimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane in a mass ratio of 1: 1.5-2.5.
In some embodiments, the compound cross-linking agent consists of oligomers of methyltripropoxysilane and vinyltriethoxysilane in a mass ratio of 1: 3.5-4.5, and the compound coupling agent consists of oligomers of gamma-glycidoxypropyltrimethoxysilane and 3-mercaptopropyltriethoxysilane in a mass ratio of 1: 2-3.
In some embodiments, the compound cross-linking agent consists of oligomers of methyltripropoxysilane and methyltriethoxysilane in a mass ratio of 1: 5.5-6.5, and the compound coupling agent consists of oligomers of gamma-glycidoxypropyltrimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane in a mass ratio of 1: 2.5-3.5.
In some embodiments, the oligomer of the methyltriethoxysilane is a mixture of a dimer and a trimer thereof, the oligomer of the methyltripropoxysilane is a mixture of a dimer and a trimer thereof, the oligomer of the vinyltriethoxysilane is a mixture of a dimer and a trimer thereof, and the mass ratio of the dimer to the trimer is preferably 1: 0.8-1.5;
the oligomer of the gamma-aminopropyltriethoxysilane is a mixture of a dimer and a trimer thereof, the oligomer of the N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane is a mixture of a dimer and a trimer thereof, the oligomer of the 3-mercaptopropyltriethoxysilane is a mixture of a dimer and a trimer thereof, and the mass ratio of the dimer to the trimer is preferably 1: 0.8-1.5.
In some of these embodiments, the α, ω -dihydroxy polysiloxane has a viscosity at 25 ℃ of 0.5pa.s to 150 pa.s.
In some of these embodiments, the dimethicone has a viscosity of 0.1Pa.s to 50Pa.s at 25 ℃.
In some of these embodiments, the inorganic filler is at least one of nano-active calcium carbonate, ground calcium carbonate, micro-silica powder, and diatomaceous earth.
In some of these embodiments, the titanate vulcanizing agent is diisopropoxytitanium bis (ethylacetoacetate) chelate.
The invention also provides a preparation method of the dealcoholized silicone sealant.
The specific technical scheme is as follows:
the preparation method of the dealcoholized silicone sealant comprises the following steps:
dehydrating and blending the alpha, omega-dihydroxy polysiloxane, the dimethyl silicone oil and the inorganic filler for 30-300 minutes at the temperature of 80-150 ℃ and the vacuum degree of-0.06-0.099 MPa, and cooling to obtain a base material;
and (3) reacting the base material with the compound cross-linking agent, the compound coupling agent and the titanate vulcanizing agent for 30-180 minutes under the conditions that the vacuum degree is-0.06-0.099 MPa and the rotating speed is 10-800 rpm, so as to obtain the dealcoholized silicone sealant.
In some of these embodiments, the method of making the dealcoholized silicone sealants comprises the steps of:
adding the alpha, omega-dihydroxy polysiloxane, the dimethyl silicone oil and the inorganic filler into a kneading machine, dehydrating and blending for 60-120 minutes under the conditions that the temperature is 100-120 ℃ and the vacuum degree is-0.08-0.099 MPa, and cooling to obtain a base material;
adding the base material into a planetary stirrer or a high-speed dispersion stirrer, adding the compound cross-linking agent, the compound coupling agent and the titanate vulcanizing agent, and reacting for 60-120 minutes under the conditions that the vacuum degree is-0.08-0.099 MPa and the rotating speed is 200-400 rpm to obtain the dealcoholized silicone sealant.
Compared with the prior art, the invention has the following beneficial effects:
in order to solve the problem that the dealcoholized silicone sealant on the market is easy to foam when constructed under the condition of high temperature (higher than 60 ℃), the invention uses alpha, omega-dihydroxy polysiloxane as a base polymer, is matched with a compound cross-linking agent and a compound coupling agent with specific types and dosage, and then is added with a certain amount of inorganic filler and titanate vulcanizing agent to prepare the novel dealcoholized silicone sealant in an alcohol system, and the sealant can not generate bubbles in the curing process. Construction comparison is carried out on a curtain wall with the surface temperature of 65 ℃, bubbles are generated on the surface of the adhesive tape within half an hour of the construction of the conventional dealcoholized silicone sealant, and after the sealant disclosed by the invention is constructed for 8 hours, the surface of the adhesive tape is still flat, no bubbles are generated, and the sealant has the characteristic of no bubbles in high-temperature construction. Meanwhile, the dealcoholized silicone sealant has good caking property, water-resistant caking property, excellent weather resistance and high displacement capacity, and has no corrosion to most building materials; the sealant is an alcohol micromolecule which is separated in the curing process, and has the characteristic of being more environment-friendly compared with the commercially available butanone oxime-removed sealant. Therefore, the dealcoholized silicone sealant has the following advantages:
1. during high-temperature construction, no bubbles are generated in the curing process, and the construction conditions of outdoor high-temperature base materials in summer can be met.
2. The adhesive has good adhesion, water-resistant adhesion, excellent weather resistance and high displacement capacity, and can form strong adhesion with most building materials after being cured without a primer.
3. The micromolecules released in the curing process are alcohol micromolecules and are environment-friendly.
4. The neutral curing system is adopted, and the paint has no corrosion to most building materials such as metal, glass, concrete and the like, and is widely applied.
5. The product is convenient to construct and meets the normal requirements of production, storage and transportation.
Drawings
FIG. 1 is a graph showing the effect of the dealcoholized silicone sealant prepared in example 1 after 8 hours of maintenance in a simulated curtain wall construction test.
FIG. 2 is a graph showing the effect of the dealcoholized silicone sealant prepared in example 2 after 8 hours of maintenance in a simulated curtain wall construction test.
FIG. 3 is a graph showing the effect of the dealcoholized silicone sealant prepared in example 3 after 8 hours of maintenance in a simulated curtain wall construction test.
FIG. 4 is a graph showing the effect of the dealcoholized silicone sealant prepared in example 4 after 8 hours of maintenance in a simulated curtain wall construction test.
FIG. 5 is a graph showing the effect of the dealcoholized silicone sealant prepared in comparative example 1 after 8 hours of maintenance in a simulated curtain wall construction test.
FIG. 6 is a graph showing the effect of the dealcoholized silicone sealant prepared in comparative example 2 after 8 hours of maintenance in a simulated curtain wall construction test.
FIG. 7 is a graph showing the effect of the dealcoholized silicone sealant prepared in comparative example 3 after 8 hours of maintenance in a simulated curtain wall construction test.
FIG. 8 is a graph showing the effect of the dealcoholized silicone sealant prepared in comparative example 4 after 8 hours of maintenance in a simulated curtain wall construction test.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The terms "comprising" and "having," and any variations thereof, are intended to cover non-exclusive inclusions. For example, a process, method, apparatus, article, or device that comprises a list of steps is not limited to only those steps or modules listed, but may alternatively include other steps not listed or inherent to such process, method, article, or device.
The "plurality" referred to in the present invention means two or more. "and/or" describes the association relationship of the associated objects, meaning that there may be three relationships, e.g., a and/or B, which may mean: a exists alone, A and B exist simultaneously, and B exists alone. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.
The following are specific examples.
The room temperature described in the following examples refers to a room temperature of 10 to 30 ℃.
In the following examples and comparative examples, the viscosity of the α, ω -dihydroxypolysiloxane was 50 pas/25 ℃; the viscosity of the dimethylsilicone fluid was 0.35 pas/25 ℃.
The oligomers of methyltriethoxysilane in the following examples and comparative examples were mixtures of dimers and trimers thereof, the mass ratio of dimers to trimers was 1:1.
the oligomers of methyltripropoxysilane in the following examples and comparative examples were a mixture of dimer and trimer thereof, and the mass ratio of dimer and trimer was 1:1.
the oligomers of vinyltriethoxysilane in the following examples and comparative examples are mixtures of their dimers and trimers, the mass ratio of dimer to trimer being 1:1.
the oligomers of gamma-aminopropyltriethoxysilane in the following examples and comparative examples are mixtures of dimers and trimers thereof, the mass ratio of dimer to trimer being 1:1.
the oligomers of N- (. beta. -aminoethyl) - γ -aminopropyltriethoxysilane in the following examples and comparative examples were mixtures of dimers and trimers thereof, the mass ratio of dimer to trimer being 1:1.
the oligomer of 3-mercaptopropyltriethoxysilane in the following examples and comparative examples was a mixture of dimer and trimer thereof, the mass ratio of dimer and trimer being 1:1.
diisopropoxytitanium bis (ethylacetoacetate) chelate compound in the following examples and comparative examples, i.e.
726 titanate chelate having the formula:
example 1:
the embodiment provides a dealcoholized silicone sealant which is prepared from the following raw materials in parts by weight:
the preparation method of the dealcoholized silicone sealant comprises the following steps:
adding 100 parts of alpha, omega-dihydroxy polysiloxane, 20 parts of dimethyl silicone oil and 120 parts of nano active calcium carbonate into a kneader, dehydrating and blending for 90min under the conditions that the temperature is 110 ℃ and the vacuum degree is-0.09 MPa, and cooling to room temperature to obtain a base material;
adding the base material into a planetary stirrer, adding 2 parts of methyltripropoxysilane and 5 parts of oligomer of methyltriethoxysilane, 0.6 part of gamma-glycidyl ether oxypropyltrimethoxysilane and 0.6 part of oligomer of gamma-aminopropyltriethoxysilane, finally adding 4 parts of diisopropoxytitanium bis (ethyl acetoacetate) chelate, and carrying out chemical reaction for 90 minutes at the vacuum degree of-0.09 MPa and the rotating speed of 300rpm to obtain the dealcoholization type silicone sealant, wherein the product test indexes are shown in Table 1.
Example 2:
the embodiment provides a dealcoholized silicone sealant which is prepared from the following raw materials in parts by weight:
the preparation method of the dealcoholized silicone sealant comprises the following steps:
100 parts of alpha, omega-dihydroxy polysiloxane, 40 parts of dimethyl silicone oil, 100 parts of nano active calcium carbonate and 100 parts of heavy calcium carbonate are added into a kneader, dehydrated and blended for 90min under the conditions that the temperature is 110 ℃ and the vacuum degree is-0.09 MPa, and cooled to room temperature to obtain a base material;
adding the base material into a planetary stirrer, adding 2 parts of methyltripropoxysilane and 7 parts of oligomer of methyltripropoxysilane, 1 part of gamma-glycidyl ether oxypropyltrimethoxysilane and 2 parts of oligomer of N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, finally adding 6 parts of diisopropoxytitanium bis (ethyl acetoacetate) chelate, and carrying out chemical reaction for 90 minutes at a vacuum degree of-0.09 MPa and a rotating speed of 300rpm to obtain the dealcoholization type silicone sealant, wherein the product test indexes are shown in Table 1.
Example 3:
the embodiment provides a dealcoholized silicone sealant which is prepared from the following raw materials in parts by weight:
the preparation method of the dealcoholized silicone sealant comprises the following steps:
100 parts of alpha, omega-dihydroxy polysiloxane, 40 parts of nano active calcium carbonate and 40 parts of silicon micropowder are added into a kneader, dehydrated and blended for 90min under the conditions that the temperature is 110 ℃ and the vacuum degree is-0.09 MPa, and cooled to room temperature to obtain a base material;
adding the base material into a planetary stirrer, adding 1 part of methyl tripropoxysilane and 4 parts of an oligomer of vinyl triethoxysilane, 0.3 part of gamma-glycidyl ether oxypropyl trimethoxysilane and 0.7 part of an oligomer of 3-mercaptopropyl triethoxysilane, finally adding 2 parts of diisopropoxy titanium bis (ethyl acetoacetate) chelate, and carrying out chemical reaction for 90 minutes at the vacuum degree of-0.09 MPa and the rotating speed of 300rpm to obtain the dealcoholization type silicone sealant, wherein the product test indexes are shown in table 1.
Example 4:
the embodiment provides a dealcoholized silicone sealant which is prepared from the following raw materials in parts by weight:
the preparation method of the dealcoholized silicone sealant comprises the following steps:
100 parts of alpha, omega-dihydroxy polysiloxane, 20 parts of dimethyl silicone oil, 100 parts of nano active calcium carbonate and 50 parts of diatomite are added into a kneader, dehydrated and blended for 90min under the conditions that the temperature is 110 ℃ and the vacuum degree is-0.09 MPa, and cooled to room temperature to obtain a base material;
adding the base material into a planetary stirrer, adding 1 part of methyltripropoxysilane and 6 parts of oligomers of methyltriethoxysilane, 0.5 part of gamma-glycidyl ether oxypropyltrimethoxysilane and 1.5 parts of oligomers of N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, finally adding 4 parts of diisopropoxytitanium bis (ethyl acetoacetate) chelate, and carrying out chemical reaction for 90 minutes at a vacuum degree of-0.09 MPa and a rotating speed of 300rpm to obtain the dealcoholized silicone sealant, wherein the performance index of the product is shown in Table 1.
Comparative example 1:
the comparison example provides a dealcoholized silicone sealant, which is different from the sealant in example 1 in the composition of a cross-linking agent and a coupling agent and is prepared from the following raw materials in parts by weight:
the preparation method of the dealcoholized silicone sealant comprises the following steps:
100 parts of alpha, omega-dihydroxy polysiloxane, 20 parts of dimethyl silicone oil and 120 parts of nano active calcium carbonate are added into a kneader, dehydrated and blended for 90min under the conditions that the temperature is 110 ℃ and the vacuum degree is-0.09 MPa, and cooled to room temperature to obtain a base material;
adding the base material into a planetary stirrer, adding 7 parts of methyltrimethoxysilane and 1.2 parts of gamma-aminopropyltrimethoxysilane, finally adding 4 parts of diisopropoxytitanium bis (ethyl acetoacetate) chelate, and carrying out chemical reaction for 90 minutes at a vacuum degree of-0.09 MPa and a rotating speed of 300rpm to obtain the dealcoholized silicone sealant, wherein the product test indexes are shown in Table 1.
Comparative example 2:
the comparison example provides a dealcoholized silicone sealant, which is different from the sealant in example 3 in the composition of a cross-linking agent and a coupling agent and is prepared from the following raw materials in parts by weight:
the preparation method of the dealcoholized silicone sealant comprises the following steps:
100 parts of alpha, omega-dihydroxy polysiloxane, 40 parts of nano active calcium carbonate and 40 parts of silicon micropowder are added into a kneader, dehydrated and blended for 90min under the conditions that the temperature is 110 ℃ and the vacuum degree is-0.09 MPa, and cooled to room temperature to obtain a base material;
adding the base material into a planetary stirrer, adding 5 parts of methyltrimethoxysilane and 1 part of N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, finally adding 2 parts of diisopropoxytitanium bis (ethyl acetoacetate) chelate, and carrying out chemical reaction for 90 minutes at a vacuum degree of-0.09 MPa and a rotating speed of 300rpm to obtain the dealcoholized silicone sealant, wherein the product test indexes are shown in Table 1.
Comparative example 3
This comparative example provides a dealcoholized silicone sealant which differs from example 1 in that oligomers of methyltripropoxysilane instead of methyltriethoxysilane and gamma-glycidoxypropyltrimethoxysilane instead of gamma-aminopropyltriethoxysilane were prepared from the following raw materials in parts by weight:
the preparation method of the dealcoholized silicone sealant comprises the following steps:
adding 100 parts of alpha, omega-dihydroxy polysiloxane, 20 parts of dimethyl silicone oil and 120 parts of nano active calcium carbonate into a kneader, dehydrating and blending for 90min under the conditions that the temperature is 110 ℃ and the vacuum degree is-0.09 MPa, and cooling to room temperature to obtain a base material;
adding the base material into a planetary stirrer, adding 2 parts of methyl tripropoxysilane, 0.6 part of gamma-glycidyl ether oxypropyltrimethoxysilane and finally 4 parts of diisopropoxy titanium bis (ethyl acetoacetate) chelate, and carrying out chemical reaction for 90 minutes at a vacuum degree of-0.09 MPa and a rotating speed of 300rpm to obtain the dealcoholized silicone sealant, wherein the product test indexes are shown in Table 1.
Comparative example 4:
this comparative example provides a dealcoholized silicone sealant which differs from example 1 in that methyltrimethoxysilane is used in place of methyltripropoxysilane and gamma-aminopropyltrimethoxysilane is used in place of gamma-glycidoxypropyltrimethoxysilane, and is specifically prepared from the following raw materials in parts by weight:
the preparation method of the dealcoholized silicone sealant comprises the following steps:
adding 100 parts of alpha, omega-dihydroxy polysiloxane, 20 parts of dimethyl silicone oil and 120 parts of nano active calcium carbonate into a kneader, dehydrating and blending for 90min under the conditions that the temperature is 110 ℃ and the vacuum degree is-0.09 MPa, and cooling to room temperature to obtain a base material;
adding the base material into a planetary stirrer, adding 2 parts of methyltrimethoxysilane and 5 parts of oligomer of methyltriethoxysilane, 0.6 part of gamma-aminopropyltrimethoxysilane and 0.6 part of oligomer of gamma-aminopropyltriethoxysilane, finally adding 4 parts of diisopropoxytitanium bis (ethyl acetoacetate) chelate, and carrying out chemical reaction for 90 minutes at the vacuum degree of-0.09 MPa and the rotating speed of 300rpm to obtain the dealcoholized silicone sealant, wherein the product test indexes are shown in table 1.
The dealcoholized silicone sealants prepared in examples 1 to 4 and comparative examples 1 to 4 were subjected to the performance tests shown in Table 1.
The test method for simulating curtain wall construction comprises the following steps: a testing plate for curtain wall construction is manufactured by using edge folding aluminum plates with the thickness of 400mm multiplied by 400mm and reserving glue seams with the thickness of 18mm among 2 aluminum plates, the testing plate is placed in a 65 ℃ drying oven for 4 hours, the testing plate is immediately glued in the reserved glue seams according to a weather-resistant glue construction method after being taken out, the gluing plate is immediately placed in the 65 ℃ drying oven for maintenance, the foaming condition of the glue strip after being maintained for 8 hours is observed, and the experimental results are shown in figures 1-8 and table 1.
TABLE 1
As can be seen by comparison, the dealcoholized silicone sealants prepared in examples 1 to 4 were smooth in appearance and did not foam after 8 hours of curing at 65 ℃ in a simulation test, and the dealcoholized silicone sealants prepared in comparative examples 1 to 4 were remarkably foamed on the surface of the adhesive tape after 8 hours of curing at 65 ℃. Therefore, the dealcoholized silicone sealant can achieve the aim of no bubble in high-temperature construction while ensuring good caking property, water-resistant caking property, excellent weather resistance and high displacement capacity.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent should be subject to the appended claims.
Claims (8)
1. The dealcoholized silicone sealant is characterized by being prepared from the following raw materials in parts by weight:
100 parts of alpha, omega-dihydroxy polysiloxane
0-40 parts of dimethyl silicone oil
80-200 parts of inorganic filler
5-9 parts of compound cross-linking agent
1-3 parts of compound coupling agent
2-6 parts of a titanate vulcanizing agent;
the compound cross-linking agent is prepared from the following components in percentage by mass of 1: 2-7 parts of methyltripropoxysilane and an oligomeric cross-linking agent, wherein the oligomeric cross-linking agent is selected from at least one of oligomers of methyltriethoxysilane, methyltripropoxysilane and oligomers of vinyl triethoxysilane;
the compound coupling agent is prepared from the following components in a mass ratio of 1: 0.8-3.5 of gamma-glycidoxypropyltrimethoxysilane and an oligomeric coupling agent, wherein the oligomeric coupling agent is selected from at least one of oligomers of gamma-aminopropyltriethoxysilane, oligomers of N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane and oligomers of 3-mercaptopropyltriethoxysilane;
the oligomer of the methyltriethoxysilane is a mixture of a dimer and a trimer thereof, and the oligomer of the vinyltriethoxysilane is a mixture of a dimer and a trimer thereof;
the oligomer of the gamma-aminopropyl triethoxysilane is a mixture of a dimer and a trimer thereof, the oligomer of the N- (beta-aminoethyl) -gamma-aminopropyl triethoxysilane is a mixture of a dimer and a trimer thereof, and the oligomer of the 3-mercaptopropyl triethoxysilane is a mixture of a dimer and a trimer thereof;
the mass ratio of the dimer to the trimer in the oligomeric cross-linking agent is 1: 0.8-1.5; the mass ratio of the dimer to the trimer in the oligomeric coupling agent is 1: 0.8-1.5.
2. The dealcoholized silicone sealant according to claim 1, which is prepared from the following raw materials in parts by weight:
100 parts of alpha, omega-dihydroxy polysiloxane
15-25 parts of dimethyl silicone oil
110-130 parts of inorganic filler
6-8 parts of compound cross-linking agent
1-2 parts of compound coupling agent
3-5 parts of a titanate vulcanizing agent.
3. The dealcoholization type silicone sealant as claimed in claim 1, wherein the compound cross-linking agent is composed of oligomers of methyltripropoxysilane and methyltriethoxysilane in a mass ratio of 1: 2-3, and the compound coupling agent is composed of oligomers of gamma-glycidoxypropyltrimethoxysilane and gamma-aminopropyltriethoxysilane in a mass ratio of 1: 0.8-1.5; or,
the compound cross-linking agent consists of oligomers of methyl tripropoxysilane and methyl tripropoxysilane in a mass ratio of 1: 3-4, and the compound coupling agent consists of oligomers of gamma-glycidoxypropyltrimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane in a mass ratio of 1: 1.5-2.5; or,
the compound cross-linking agent consists of oligomers of methyl tripropoxysilane and vinyl triethoxysilane in a mass ratio of 1: 3.5-4.5, and the compound coupling agent consists of oligomers of gamma-glycidyl ether oxypropyl trimethoxysilane and 3-mercaptopropyl triethoxysilane in a mass ratio of 1: 2-3; or,
the compound cross-linking agent is composed of oligomers of methyl tripropoxysilane and methyl triethoxysilane at a mass ratio of 1: 5.5-6.5, and the compound coupling agent is composed of oligomers of gamma-glycidyl ether oxypropyltrimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane at a mass ratio of 1: 2.5-3.5.
4. The dealcoholized silicone sealant according to any one of claims 1 to 3, wherein the α, ω -dihydroxy polysiloxane has a viscosity at 25 ℃ of 5 to 100 Pa.s; and/or the presence of a gas in the gas,
the viscosity of the dimethyl silicone oil at 25 ℃ is 0.1 Pa.s-5 Pa.s.
5. The dealcoholized silicone sealant according to claim 4, wherein the α, ω -dihydroxy polysiloxane has a viscosity at 25 ℃ of 45 to 55 Pa.s; and/or the presence of a gas in the gas,
the viscosity of the dimethyl silicone oil at 25 ℃ is 0.2 Pa.s-0.5 Pa.s.
6. The dealcoholized silicone sealant according to any one of claims 1 to 3, wherein the inorganic filler is at least one of nano-active calcium carbonate, ground calcium carbonate, fine silica powder and diatomaceous earth; and/or the presence of a gas in the gas,
the titanate vulcanizing agent is diisopropoxytitanium bis (ethyl acetoacetate) chelate.
7. A method of preparing the dealcoholized silicone sealant according to any one of claims 1 to 3, comprising the steps of:
dehydrating and blending the alpha, omega-dihydroxy polysiloxane, the dimethyl silicone oil and the inorganic filler for 30-300 minutes at the temperature of 80-150 ℃ and the vacuum degree of-0.06-0.099 MPa, and cooling to obtain a base material;
and (3) reacting the base material with the compound cross-linking agent, the compound coupling agent and the titanate vulcanizing agent for 30-180 minutes under the conditions that the vacuum degree is-0.06-0.099 MPa and the rotating speed is 10-800 rpm, so as to obtain the dealcoholized silicone sealant.
8. The method for preparing the dealcoholized silicone sealant according to claim 7, comprising the steps of:
adding the alpha, omega-dihydroxy polysiloxane, the dimethyl silicone oil and the inorganic filler into a kneading machine, dehydrating and blending for 60-120 minutes under the conditions that the temperature is 100-120 ℃ and the vacuum degree is-0.08-0.099 MPa, and cooling to obtain a base material;
adding the base material into a planetary stirrer or a high-speed dispersion stirrer, adding the compound cross-linking agent, the compound coupling agent and the titanate vulcanizing agent, and reacting for 60-120 minutes under the conditions that the vacuum degree is-0.08-0.099 MPa and the rotating speed is 200-400 rpm to obtain the dealcoholized silicone sealant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011593533.7A CN112708393B (en) | 2020-12-29 | 2020-12-29 | Dealcoholized silicone sealant and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011593533.7A CN112708393B (en) | 2020-12-29 | 2020-12-29 | Dealcoholized silicone sealant and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112708393A CN112708393A (en) | 2021-04-27 |
| CN112708393B true CN112708393B (en) | 2022-08-23 |
Family
ID=75546168
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011593533.7A Active CN112708393B (en) | 2020-12-29 | 2020-12-29 | Dealcoholized silicone sealant and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112708393B (en) |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101153076B (en) * | 2006-09-29 | 2011-04-27 | 北京化工大学 | Polysiloxane resin with lateral group containing alkoxyl, producing method and use of the same |
| CN104559910A (en) * | 2014-12-26 | 2015-04-29 | 广州市白云化工实业有限公司 | Spray for accelerating curing of silicone sealant |
| CN107936908A (en) * | 2017-12-06 | 2018-04-20 | 苏州铂邦胶业有限公司 | Silicone sealant |
| CN109666447A (en) * | 2019-01-16 | 2019-04-23 | 江西奋发科技有限公司 | A kind of single-component dealcoholization-type silicone rubber sealant and preparation method thereof |
| CN111892906B (en) * | 2020-08-13 | 2022-07-01 | 广州市白云化工实业有限公司 | Dealcoholized single-component silicone sealant capable of being rapidly and deeply cured and preparation method thereof |
-
2020
- 2020-12-29 CN CN202011593533.7A patent/CN112708393B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN112708393A (en) | 2021-04-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108179003B (en) | Dealcoholized silicone weather-resistant sealant with low modulus and high displacement capacity and preparation method thereof | |
| CN107286897A (en) | A kind of Single-component low-viscosity dealcoholized type organic silicon potting adhesive and preparation method thereof | |
| CN109135660A (en) | A kind of dealcoholized type bi-component sealant and preparation method thereof | |
| CN112143446A (en) | Bi-component silicone sealant and preparation method and application thereof | |
| US5300611A (en) | Room temperature curable organopolysiloxane compositions | |
| CN113337245A (en) | Dealcoholized photovoltaic module sealant and preparation method thereof | |
| CN105778512A (en) | Environment-friendly dealcoholized room-temperature vulcanized silicone rubber and preparation method thereof | |
| CN108517198A (en) | A kind of single-component room-temperature vulcanized organosilicon adhesive and preparation method thereof | |
| CN110982448B (en) | Tackifier, dealcoholized RTV (room temperature vulcanized) silicone rubber and preparation method thereof | |
| CN106244091A (en) | A kind of high intensity dealcoholized type double component room temperature vulcanization silicon rubber building sealant and preparation method thereof | |
| CN108219739B (en) | Deep-cured single-component ketoxime-removed organic silicon adhesive and preparation method thereof | |
| CN106634806B (en) | Single-component silicone structural sealant and preparation method thereof | |
| CN106190013B (en) | silicone resin type bi-component elastic silicone sealant for hollow glass and preparation method thereof | |
| CN112708393B (en) | Dealcoholized silicone sealant and preparation method thereof | |
| CN104531050A (en) | Low-modulus high-elongation-percentage room-temperature-vulcanization silicon rubber and preparation method thereof | |
| CN112961645B (en) | Self-curing insulating silicone rubber and preparation method and application thereof | |
| CN111073577A (en) | Environment-friendly MS sealant and preparation method thereof | |
| CN112210341B (en) | Double-vulcanization system building sealant and preparation method thereof | |
| CN114773379A (en) | Modified siloxane, heat-resistant silicone structural sealant and preparation method thereof | |
| CN114874744A (en) | Mildew-proof beauty glue for interior decoration and preparation method thereof | |
| CN114149783B (en) | Low-temperature-resistant neutral silicone sealant and preparation method thereof | |
| CN109096945A (en) | A kind of tackifier and preparation method thereof applied to silicone sealant | |
| CN110257002B (en) | Two-component silicone sealant for projection lamp | |
| CN113337197B (en) | Sealing rubber primer coating liquid and preparation method thereof | |
| CN114316888B (en) | Single-component ketoxime type silicone adhesive and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder |
Address after: Guangzhou private science and Technology Park Yunan road Baiyun District of Guangzhou City, Guangdong Province, No. 1 510540 Patentee after: Guangzhou Baiyun Technology Co.,Ltd. Address before: Guangzhou private science and Technology Park Yunan road Baiyun District of Guangzhou City, Guangdong Province, No. 1 510540 Patentee before: GUANGZHOU BAIYUN CHEMICAL INDUSTRY Co.,Ltd. |
|
| CP01 | Change in the name or title of a patent holder |