CN115491165B - Flame-retardant silicone adhesive for hollow glass and preparation method thereof - Google Patents
Flame-retardant silicone adhesive for hollow glass and preparation method thereof Download PDFInfo
- Publication number
- CN115491165B CN115491165B CN202211280981.0A CN202211280981A CN115491165B CN 115491165 B CN115491165 B CN 115491165B CN 202211280981 A CN202211280981 A CN 202211280981A CN 115491165 B CN115491165 B CN 115491165B
- Authority
- CN
- China
- Prior art keywords
- component
- flame retardant
- preparation
- coupling agent
- modified
- 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
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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
-
- 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
- C08L2201/02—Flame or fire retardant/resistant
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The application relates to the field of silicone adhesive, and relates to flame-retardant silicone adhesive for hollow glass and a preparation method thereof. The flame-retardant silicone adhesive for the hollow glass comprises a component A and a component B, wherein the component A comprises the following components: nano calcium carbonate; a base adhesive; dimethyl silicone oil; modifying the mixed flame-retardant filler; the component B comprises: pigment carbon black; fumed silica; dimethyl silicone oil; a cross-linking agent; a coupling agent; a modified silane coupling agent; a catalyst; the preparation method comprises the following steps: mixing nano calcium carbonate, base gum, dimethyl silicone oil and modified mixed flame retardant filler, heating, vacuumizing and stirring at a high speed to obtain a component A; heating pigment carbon black, vacuumizing, stirring at a high speed, adding a cross-linking agent and dimethyl silicone oil, stirring in vacuum, adding fumed silica, stirring in vacuum, adding a coupling agent, a modified silane coupling agent and a catalyst, and stirring in vacuum to obtain a component B; the component A and the component B are mixed to prepare the product, which has the advantage of improving the flame retardant property of the silicone adhesive.
Description
Technical Field
The application relates to the field of silicone adhesive, in particular to flame-retardant silicone adhesive for hollow glass and a preparation method thereof.
Background
Silicone gums are an ointment-like material that cures to a tough, rubbery solid upon exposure to moisture in the air. The silicone adhesive has the characteristics of strong adhesive force, high tensile strength, weather resistance, vibration resistance, moisture resistance, odor resistance and large adaptation to cold and hot changes, so the silicone adhesive is commonly used for bonding building materials, and is commonly used for bonding glass in the aspect of building, and is also called glass adhesive.
The silicone adhesive is also used for bonding glass in building curtain wall doors and windows, and along with the continuous improvement of the fireproof requirements of the building curtain wall doors and windows, the common double-component silicone hollow glass sealant is inflammable when meeting open fire, can not meet the manufacturing requirements of the fireproof hollow glass, and the development of the double-component silicone hollow glass flame-retardant sealant is urgently needed to solve the combustion problem of the common silicone sealant.
Disclosure of Invention
In order to improve the flame retardant property of the silicone adhesive, the application provides the flame retardant silicone adhesive for the hollow glass and a preparation method thereof.
In a first aspect, the application provides a flame-retardant silicone adhesive for hollow glass, which adopts the following technical scheme:
the flame-retardant silicone adhesive for the hollow glass comprises a component A and a component B, wherein the component A is prepared from the following raw materials in parts by weight:
30-60 parts of nano calcium carbonate;
35-65 parts of base adhesive;
5-25 parts of dimethyl silicone oil;
30-60 parts of modified mixed flame retardant filler;
the component B is prepared from the following raw materials in parts by weight:
15-20 parts of pigment carbon black;
5-10 parts of fumed silica;
25-30 parts of dimethyl silicone oil;
30-40 parts of a cross-linking agent;
30-40 parts of a coupling agent;
10-30 parts of modified silane coupling agent;
0.01-0.1 part of catalyst.
By adopting the technical scheme, in the component A, the nano calcium carbonate can improve thixotropy, viscosity, strength and the like of the silicone adhesive, and can improve flame retardant property and ultraviolet resistance after filling due to the high temperature resistance of the nano calcium carbonate; the modified mixed flame-retardant filler can improve the flame retardant property of the silicone adhesive; the compatibility of the nano calcium carbonate and the modified mixed flame-retardant filler with the base adhesive can be improved by the dimethyl silicone oil, so that the nano calcium carbonate and the modified mixed flame-retardant filler are better mixed into the base adhesive; in the component B, the pigment carbon black can effectively block ultraviolet rays, so that the ultraviolet resistance and ageing resistance of the silicone adhesive are improved; the fumed silica can reduce sedimentation and delamination of the pigment carbon black, so that the pigment carbon black is dispersed more uniformly, sedimentation or solidification of the component B can be prevented, and the weather resistance, tearing strength and adhesive property of the silicone adhesive can be improved; the viscosity of the silicone adhesive can be affected to a certain extent by adding the nano calcium carbonate, and the nano calcium carbonate in the component A can be subjected to surface treatment by adding the coupling agent and the modified silane coupling agent, so that the influence of the nano calcium carbonate on the silicone adhesive can be reduced.
Preferably, the modified mixed flame retardant filler comprises 29.2-58.5 parts of flame retardant filler, 0.5-1 part of composite surface treatment agent and 0.3-0.5 part of coupling agent KH-550, wherein the flame retardant filler comprises one or more of 1, 2-ethylene tetra (1-chloro-2-propyl) phosphate, DOP, guanidine sulfamate, zinc borate and antimony oxide.
By adopting the technical scheme, the 1, 2-ethylene tetra (1-chloro-2-propyl) phosphate and DOP are used as flame retardants, so that the flame retardant has good flame retardant property; guanidine sulfamate, zinc borate and antimony oxide are all flame retardant fillers with better flame retardant property, and when the flame retardant filler is compounded for use, better flame retardant property can be exerted; the coupling agent KH-550 can introduce carbon-carbon double bonds on the surface of the flame-retardant filler, so that the flame-retardant filler can strengthen the connection strength and compatibility with the base rubber.
Preferably, the mass ratio of the 1, 2-ethylene tetra (1-chloro-2-propyl) phosphate to the DOP to the guanidine sulfamate to the zinc borate to the antimony oxide is 1:3-4:3-4:1:3-4.
By adopting the technical scheme, when the mass ratio of the 1, 2-ethylene tetra (1-chloro-2-propyl) phosphate, DOP, guanidine sulfamate, zinc borate and antimony oxide is different, the flame retardant effect is different, and the application provides the optimal mass ratio of the 1, 2-ethylene tetra (1-chloro-2-propyl) phosphate, DOP, guanidine sulfamate, zinc borate and antimony oxide, so that the silicone adhesive has good flame retardant property.
Preferably, the composite surface treatment agent comprises one or more of coconut oil, sodium stearate, aluminum titanate coupling agent and silane coupling agent, wherein the silane coupling agent comprises one or more of coupling agent KH-550 and coupling agent KH-792.
By adopting the technical scheme, the coconut oil and the sodium stearate are both surfactants, and have better activation performance on the flame-retardant filler, and after the coconut oil and the sodium stearate are combined, the prepared composite surface treatment agent has better activation performance when being singly used, and the activity of the flame-retardant filler after being subjected to surface treatment is better, so that the composite surface treatment agent has better flame-retardant performance.
Preferably, the mass ratio of the coconut oil to the sodium stearate is 2-4:3-5.
By adopting the technical scheme, when the mass ratio of the coconut oil to the sodium stearate is different, the performances of the prepared composite surface treating agent are different, and the optimal mass ratio of the coconut oil to the sodium stearate is provided, so that the prepared composite surface treating agent has the optimal effect of surface modification of the flame-retardant filler.
Preferably, the preparation of the modified mixed flame retardant filler comprises the following steps:
step 1: preparing a composite surface treating agent, namely heating sodium stearate with accurate measurement to 80-90 ℃, then adding coconut oil with accurate measurement, and continuously stirring for 20-25min to prepare the composite surface treating agent;
step 2: mixing and stirring accurately metered 1, 2-ethylene tetra (1-chloro-2-propyl) phosphate, DOP, guanidine sulfamate, zinc borate and antimony oxide for 1-2 hours, then adding accurately metered silane coupling agent, and mixing and stirring for 15-20 minutes at 100-110 ℃ to prepare a mixture;
step 3: and (3) feeding the mixture into an air flow mill under negative pressure for grinding, and then mixing the ground mixture with a composite surface treating agent for 20-25min at 80-90 ℃ to prepare the modified mixed flame retardant filler.
By adopting the technical scheme, the sodium stearate and the coconut oil are mixed to prepare the composite surface treating agent with better performance; after the flame-retardant filler is uniformly mixed, the compatibility and the mixing uniformity between the flame-retardant fillers are improved by adding the silane coupling agent, and then grinding is performed before the composite surface modifier is mixed, so that the composite surface modifier can better perform surface modification on the flame-retardant filler.
Preferably, the modified silane coupling agent comprises a coupling agent KH-792, a coupling agent HY-102 and E51 epoxy resin, wherein the mass ratio of the coupling agent KH-792 to the coupling agent HY-102 to the E51 epoxy resin is 4-6:10:2.7-3.
By adopting the technical scheme, the E51 epoxy resin has better bonding performance and strength, has hydroxyl and better reaction activity, can react with amino, but the E51 epoxy resin has poorer compatibility, the coupling agent KH-792 can improve the compatibility between the E51 epoxy resin and each component, so that the crosslinking reaction is more complete, the overall performance of the product can be improved, and the coupling agent HY-102 can improve the filling amount of pigment carbon black and fumed silica in the E51 epoxy resin, so that each component is better compatible and mixed, and the flame retardant performance is improved.
Preferably, the cross-linking agent comprises one or more of methyltriethoxysilane, dimethyldiethoxysilane, dimethyldimethoxysilane, methyltrimethoxysilane, methyl orthosilicate, ethyl orthosilicate and ethyl polysilicate; the catalyst comprises one or more of dibutyl tin dilaurate and dibutyl tin diacetate.
Preferably, the coupling agent comprises one or more of gammA-Aminopropyl triethoxysilane (KH-550), gamma-glycidoxypropyl trimethoxysilane (KH-560), N-2-aminoethyl-3-aminopropyl triethoxysilane (KH-791), N-2-aminoethyl-3-aminopropyl trimethoxysilane (KH-792), trisaminosilane N- (piperazinylethyl) -3-aminopropyl methyldimethoxysilane (SCA-A 85T), 3-diethylenetriaminopropyl methyldimethoxysilane (KH-A603), 3-diethylenetriaminopropyl trimethoxysilane (NQ-62).
By adopting the technical scheme, the coupling agent contains secondary amine groups, tertiary amine groups and a small amount of primary amine groups, so that the bonding strength, corrosion resistance and weather resistance of the silicone adhesive can be improved, the dispersibility and the bonding property of the filler can be improved, and the crosslinking density can be greatly improved.
In a second aspect, the application provides a preparation method of flame-retardant silicone adhesive for hollow glass, which adopts the following technical scheme:
the preparation method of the flame-retardant silicone adhesive for the hollow glass comprises the following steps of:
step 1: preparing a component A, namely uniformly mixing nano calcium carbonate, base gum, dimethyl silicone oil and modified mixed flame retardant filler which are accurately measured, heating to 110-150 ℃, vacuumizing, keeping the vacuum degree at 0.09-0.1MPa, and stirring at a high speed for 1-2h to obtain the component A;
step 2: preparing a component B, namely heating pigment carbon black with accurate measurement to 110-150 ℃ and vacuumizing, keeping the vacuum degree at 0.09-0.1MPa, stirring at high speed for 0.5-1h, adding a crosslinking agent with accurate measurement and dimethyl silicone oil, stirring for 30-40min under vacuum, continuing to add fumed silica with accurate measurement, stirring for 30-40min under vacuum, adding a coupling agent with accurate measurement, a modified silane coupling agent and a catalyst, and stirring for 60-70min under vacuum to obtain the component B; step 3: and mixing and stirring the component A and the component B uniformly to obtain the product.
By adopting the technical scheme, the component A and the component B are stirred in a vacuum state, so that sundries such as dust in air are prevented from being mixed into the silicone adhesive, the component A and the component B can be fully expanded, the filler added into the component A and the component B can be fully mixed, air bubbles in the component A and the component B can be prevented from occurring, and the quality is prevented from being influenced.
In summary, the application has the following beneficial effects:
1. the nano calcium carbonate and the modified mixed flame-retardant filler in the component A are used as the filler and added into the base adhesive, so that the flame retardant property, the ultraviolet resistance and the ageing resistance of the silicone adhesive are improved, and the adhesive property of the silicone adhesive is also improved after the flame-retardant filler is treated by the composite surface treating agent; in the component B, pigment carbon black and gas phase silicon dioxide are compounded for use, so that the ultraviolet resistance and the ageing resistance of the silicone adhesive are further improved.
2. In the application, the 1, 2-ethylene tetra (1-chloro-2-propyl) phosphate, DOP, guanidine sulfamate, zinc borate and antimony oxide are preferably used as the flame retardant filler in a compounding way, and the composite surface treatment agent and the silane coupling agent are adopted for surface modification treatment, so that the compatibility of the flame retardant filler and the base adhesive is improved, and the flame retardant property of the flame retardant filler is improved.
3. According to the method, the quality of the component A and the component B is improved by adjusting the adding sequence, the stirring time and the vacuum degree of each component, so that the flame retardant property, the adhesive property and the ageing resistance of the silicone adhesive are further improved.
Detailed Description
Preparation example
Preparation example 1
The preparation of the modified mixed flame-retardant filler comprises the following steps:
step 1: preparing a composite surface treating agent, namely adding 0.06kg of sodium stearate into a stirrer, heating to 85 ℃ to dissolve the sodium stearate into liquid, adding 0.04kg of coconut oil for emulsification, and continuously stirring for 20min at the rotating speed of 300r/min to prepare the composite surface treating agent;
step 2: adding 2.73kg of 1, 2-ethylene tetra (1-chloro-2-propyl) phosphate, 8.18kg of DOP, 8.18kg of guanidine sulfamate, 2.73kg of zinc borate and 8.18kg of antimony oxide into a stirrer, mixing and stirring at the rotating speed of 300r/min for 1.5h, adding 0.03kg of coupling agent KH-550, heating to 100 ℃, and mixing and stirring for 15min to obtain a mixture;
step 3: and (3) feeding the mixture into an air flow mill under negative pressure for grinding until the D50 of the mixture is less than or equal to 40 mu m, then conveying the ground mixture and the composite surface treating agent into a modified coating device, heating to 80 ℃ and mixing for 20min to obtain the modified mixed flame retardant filler.
Preparation example 2
Preparation 2 differs from preparation 1 in that: 0.06kg of sodium stearate and 0.04kg of coconut oil in step 1 were changed to 0.028kg of sodium stearate and 0.072kg of coconut oil.
Preparation example 3
Preparation 3 differs from preparation 1 in that: 0.06kg of sodium stearate and 0.04kg of coconut oil in step 1 were changed to 0.033kg of sodium stearate and 0.067kg of coconut oil.
Preparation example 4
Preparation example 4 differs from preparation example 1 in that: 0.06kg of sodium stearate and 0.04kg of coconut oil in step 1 were changed to 0.05kg of sodium stearate and 0.05kg of coconut oil.
Preparation example 5
Preparation 5 differs from preparation 1 in that: 0.06kg of sodium stearate and 0.04kg of coconut oil in step 1 were changed to 0.043kg of sodium stearate and 0.057kg of coconut oil.
Preparation example 6
Preparation example 6 differs from preparation example 1 in that: the coupling agent KH-550 added in the step 2 is changed into the coupling agent KH-792.
Preparation example 7
Preparation 7 differs from preparation 1 in that: 0.06kg of sodium stearate and 0.04kg of coconut oil in the step 1 are added instead with 0.043kg of sodium stearate and 0.057kg of coconut oil; 2.73kg of 1, 2-ethylenetetra (1-chloro-2-propyl) phosphate, 8.18kg of DOP, 8.18kg of guanidine sulfamate, 2.73kg of zinc borate and 8.18kg of antimony oxide added in step 2 were changed to 2.5kg of 1, 2-ethylenetetra (1-chloro-2-propyl) phosphate, 10kg of DOP, 7.5kg of guanidine sulfamate, 2.5kg of zinc borate and 7.5kg of antimony oxide.
Preparation example 8
Preparation 8 differs from preparation 1 in that: 0.06kg of sodium stearate and 0.04kg of coconut oil in the step 1 are added instead with 0.043kg of sodium stearate and 0.057kg of coconut oil; 2.73kg of 1, 2-ethylenetetra (1-chloro-2-propyl) phosphate, 8.18kg of DOP, 8.18kg of guanidine sulfamate, 2.73kg of zinc borate and 8.18kg of antimony oxide added in step 2 were changed to 3kg of 1, 2-ethylenetetra (1-chloro-2-propyl) phosphate, 6kg of DOP, 9kg of guanidine sulfamate, 3kg of zinc borate and 9kg of antimony oxide.
Preparation example 9
Preparation 9 differs from preparation 1 in that: 0.06kg of sodium stearate and 0.04kg of coconut oil in the step 1 are added instead with 0.043kg of sodium stearate and 0.057kg of coconut oil; 2.73kg of 1, 2-ethylenetetra (1-chloro-2-propyl) phosphate, 8.18kg of DOP, 8.18kg of guanidine sulfamate, 2.73kg of zinc borate and 8.18kg of antimony oxide added in step 2 were changed to 3.3kg of 1, 2-ethylenetetra (1-chloro-2-propyl) phosphate, 6.7kg of DOP, 6.7kg of guanidine sulfamate, 3.3kg of zinc borate and 10kg of antimony oxide.
Preparation example 10
Preparation 10 differs from preparation 1 in that: 0.06kg of sodium stearate and 0.04kg of coconut oil in the step 1 are added instead with 0.043kg of sodium stearate and 0.057kg of coconut oil; 2.73kg of 1, 2-ethylenetetra (1-chloro-2-propyl) phosphate, 8.18kg of DOP, 8.18kg of guanidine sulfamate, 2.73kg of zinc borate and 8.18kg of antimony oxide added in step 2 were changed to 3kg of 1, 2-ethylenetetra (1-chloro-2-propyl) phosphate, 6kg of DOP, 6kg of guanidine sulfamate, 3kg of zinc borate and 12kg of antimony oxide.
PREPARATION EXAMPLE 11
Preparation 11 differs from preparation 1 in that: 0.06kg of sodium stearate and 0.04kg of coconut oil in the step 1 are added instead with 0.043kg of sodium stearate and 0.057kg of coconut oil; 2.73kg of 1, 2-ethylenetetra (1-chloro-2-propyl) phosphate, 8.18kg of DOP, 8.18kg of guanidine sulfamate, 2.73kg of zinc borate and 8.18kg of antimony oxide added in step 2 were changed to 3.75kg of 1, 2-ethylenetetra (1-chloro-2-propyl) phosphate, 7.5kg of DOP, 7.5kg of guanidine sulfamate, 3.75kg of zinc borate and 7.5kg of antimony oxide.
Preparation example 12
The preparation method of the modified silane coupling agent comprises the following steps:
step 1: into a 3000ml three-necked flask, 4kg of N- (. Beta. -aminoethyl) -gamma. -aminopropyl trimethoxysilane and 10kg of isopropyl tris (dioctyl pyrophosphoyloxy) titanate, 2.7kg of E51 epoxy resin, 4.5kg of methanol were charged, and a reflux condenser, a thermometer and a constant pressure dropping funnel were mounted on the three-necked flask, and the temperature was raised to 100℃under stirring to carry out reflux reaction for 3 hours.
Step 2: and (3) distilling under reduced pressure to collect methanol, continuously heating to 145 ℃, reacting for 2.5 hours, and cooling to room temperature to obtain the modified coupling agent.
Preparation example 13
Preparation 13 differs from preparation 12 in that: 4kg of N- (. Beta. -aminoethyl) -gammA-Aminopropyl trimethoxysilane added in step 1 were changed to 6kg of N- (. Beta. -aminoethyl) -gammA-Aminopropyl trimethoxysilane.
PREPARATION EXAMPLE 14
Preparation 14 differs from preparation 12 in that: 4kg of N- (. Beta. -aminoethyl) -gammA-Aminopropyl trimethoxysilane added in step 1 were changed to 5kg of N- (. Beta. -aminoethyl) -gammA-Aminopropyl trimethoxysilane.
Preparation example 15
Preparation 15 differs from preparation 12 in that: 4kg of N- (. Beta. -aminoethyl) -gammA-Aminopropyl trimethoxysilane and 2.7kg of E51 epoxy resin added in step 1 were changed to 5kg of N- (. Beta. -aminoethyl) -gammA-Aminopropyl trimethoxysilane and 3kg of E51 epoxy resin.
PREPARATION EXAMPLE 16
Preparation 16 differs from preparation 12 in that: 4kg of N- (. Beta. -aminoethyl) -gammA-Aminopropyl trimethoxysilane and 2.7kg of E51 epoxy resin added in step 1 were changed to 5kg of N- (. Beta. -aminoethyl) -gammA-Aminopropyl trimethoxysilane and 2.85kg of E51 epoxy resin.
Preparation example 17
Preparation 17 differs from preparation 1 in that: 0.06kg of sodium stearate and 0.04kg of coconut oil in step 1 were changed to 0.025kg of sodium stearate and 0.075kg of coconut oil.
PREPARATION EXAMPLE 18
Preparation 18 differs from preparation 1 in that: 0.06kg of sodium stearate and 0.04kg of coconut oil in step 1 were changed to 0.075kg of sodium stearate and 0.025kg of coconut oil.
Examples
Example 1
The flame-retardant silicone adhesive for the hollow glass comprises a component A and a component B;
component A comprises 3kg of nano calcium carbonate, 3.5kg of 107 base gum, 0.5kg of simethicone and 3kg of modified mixed flame retardant filler in preparation example 1;
component B comprises 1.7kg of pigment carbon black, 0.75kg of fumed silica, 2.5kg of simethicone, 3.5kg of methyltrimethoxysilane, 3.5kg of trisaminosilane N- (piperazinylethyl) -3-aminopropyl methyldimethoxysilane, 1kg of the modified silane coupling agent of preparation 12 and 0.005kg of dibutyltin dilaurate.
The preparation method of the flame-retardant silicone adhesive for the hollow glass comprises the following steps of:
step 1: 3kg of nano calcium carbonate, 3.5kg of 107 base rubber, 0.5kg of dimethyl silicone oil and 3kg of modified mixed flame retardant filler in preparation example 1 are added into a reaction kettle, mixed and stirred uniformly, heated to 110-150 ℃, vacuumized by a vacuumizer, the vacuum degree is kept in the interval of 0.09-0.1MPa, and then stirred at a high speed of 800r/min for 1.5h to prepare the component A;
step 2: preparing a component B, namely adding 1.7kg of pigment carbon black into a planetary disperser, heating to 130 ℃, vacuumizing, keeping the vacuum degree within a range of 0.09-0.1MPa, stirring at a high speed for 0.5h, adding 3.5kg of methyltrimethoxysilane and 2.5kg of simethicone, stirring for 30min under vacuum, continuing adding 0.75kg of fumed silica, continuing stirring for 30min under vacuum, and finally adding 3.5kg of trisilane N- (piperazinylethyl) -3-aminopropyl methyldimethoxysilane, 1kg of the modified silane coupling agent in preparation example 12 and 0.005kg of dibutyltin dilaurate, and finally stirring for 60min under vacuum to obtain the component B;
step 3: before use, the component A and the component B are mixed and stirred uniformly according to the proportion of 10:1, and the product is prepared.
Example 2
Example 2 differs from example 1 in that: 3kg of the modified mixed flame retardant filler in preparation example 1 added in step 1 was changed to 3kg of the modified mixed flame retardant filler in preparation example 2.
Example 3
Example 3 differs from example 1 in that: 3kg of the modified mixed flame retardant filler in preparation example 1 added in step 1 was changed to 3kg of the modified mixed flame retardant filler in preparation example 3.
Example 4
Example 4 differs from example 1 in that: 3kg of the modified mixed flame retardant filler in preparation example 1 added in step 1 was changed to 3kg of the modified mixed flame retardant filler in preparation example 4.
Example 5
Example 5 differs from example 1 in that: 3kg of the modified mixed flame retardant filler in preparation example 1 added in step 1 was changed to 3kg of the modified mixed flame retardant filler in preparation example 5.
Example 6
Example 6 differs from example 1 in that: 3kg of the modified mixed flame retardant filler in preparation example 1 added in step 1 was changed to 3kg of the modified mixed flame retardant filler in preparation example 6.
Example 7
Example 7 differs from example 1 in that: 3kg of the modified mixed flame retardant filler in preparation example 1 added in step 1 was changed to 3kg of the modified mixed flame retardant filler in preparation example 7.
Example 8
Example 8 differs from example 1 in that: 3kg of the modified mixed flame retardant filler in preparation example 1 added in step 1 was changed to 3kg of the modified mixed flame retardant filler in preparation example 8.
Example 9
Example 9 differs from example 1 in that: 3kg of the modified mixed flame retardant filler in preparation example 1 added in step 1 was changed to 3kg of the modified mixed flame retardant filler in preparation example 9.
Example 10
Example 10 differs from example 1 in that: 3kg of the modified mixed flame retardant filler in preparation example 1 added in step 1 was changed to 3kg of the modified mixed flame retardant filler in preparation example 10.
Example 11
Example 11 differs from example 1 in that: 3kg of the modified mixed flame retardant filler in preparation example 1 added in step 1 was changed to 3kg of the modified mixed flame retardant filler in preparation example 11.
Example 12
Example 12 differs from example 1 in that: 3kg of the modified mixed flame retardant filler in preparation example 1 added in step 1 was changed to 6kg of the modified mixed flame retardant filler in preparation example 11.
Example 13
Example 13 differs from example 1 in that: 3kg of the modified mixed flame retardant filler in preparation example 1 added in step 1 was changed to 4.5kg of the modified mixed flame retardant filler in preparation example 11.
Example 14
Example 14 differs from example 1 in that: 3kg of nano calcium carbonate and 3kg of modified mixed flame retardant filler in preparation example 1 added in step 1 were changed to 6kg of nano calcium carbonate and 4.5kg of modified mixed flame retardant filler in preparation example 11.
Example 15
Example 15 differs from example 1 in that: 3kg of nano calcium carbonate and 3kg of modified mixed flame retardant filler in preparation example 1 added in step 1 were changed to 4.5kg of nano calcium carbonate and 4.5kg of modified mixed flame retardant filler in preparation example 11.
Example 16
Example 16 differs from example 1 in that: 3kg of nano calcium carbonate, 3.5kg of 107 base gum and 3kg of modified mixed flame retardant filler in preparation example 1 added in step 1 were changed to 4.5kg of nano calcium carbonate, 6.5kg of 107 base gum and 4.5kg of modified mixed flame retardant filler in preparation example 11.
Example 17
Example 17 differs from example 1 in that: 3kg of nano calcium carbonate, 3.5kg of 107 base gum and 3kg of modified mixed flame retardant filler in preparation example 1 added in step 1 were changed to 4.5kg of nano calcium carbonate, 5kg of 107 base gum and 4.5kg of modified mixed flame retardant filler in preparation example 11.
Example 18
Example 18 differs from example 1 in that: 3kg of nano calcium carbonate, 3.5kg of 107 base gum, 0.5kg of dimethyl silicone oil and 3kg of modified mixed flame retardant filler in preparation example 1 added in step 1 were changed to 4.5kg of nano calcium carbonate, 5kg of 107 base gum, 2.5kg of dimethyl silicone oil and 4.5kg of modified mixed flame retardant filler in preparation example 11.
Example 19
Example 19 differs from example 1 in that: 3kg of nano calcium carbonate, 3.5kg of 107 base gum, 0.5kg of dimethyl silicone oil and 3kg of modified mixed flame retardant filler in preparation example 1 added in step 1 were changed to 4.5kg of nano calcium carbonate, 5kg of 107 base gum, 1.5kg of dimethyl silicone oil and 4.5kg of modified mixed flame retardant filler in preparation example 11.
Example 20
Example 20 differs from example 1 in that: 3kg of nano calcium carbonate, 3.5kg of 107 base gum, 0.5kg of dimethyl silicone oil and 3kg of modified mixed flame retardant filler in preparation example 1 added in the step 1 are changed to 4.5kg of nano calcium carbonate, 5kg of 107 base gum, 1.5kg of dimethyl silicone oil and 4.5kg of modified mixed flame retardant filler in preparation example 11; 1kg of the modified silane coupling agent in preparation example 12 added in step 2 was changed to 1kg of the modified silane coupling agent in preparation example 13.
Example 21
Example 21 differs from example 1 in that: 3kg of nano calcium carbonate, 3.5kg of 107 base gum, 0.5kg of dimethyl silicone oil and 3kg of modified mixed flame retardant filler in preparation example 1 added in the step 1 are changed to 4.5kg of nano calcium carbonate, 5kg of 107 base gum, 1.5kg of dimethyl silicone oil and 4.5kg of modified mixed flame retardant filler in preparation example 11; 1kg of the modified silane coupling agent in preparation example 12 added in step 2 was changed to 1kg of the modified silane coupling agent in preparation example 14.
Example 22
Example 22 differs from example 1 in that: 3kg of nano calcium carbonate, 3.5kg of 107 base gum, 0.5kg of dimethyl silicone oil and 3kg of modified mixed flame retardant filler in preparation example 1 added in the step 1 are changed to 4.5kg of nano calcium carbonate, 5kg of 107 base gum, 1.5kg of dimethyl silicone oil and 4.5kg of modified mixed flame retardant filler in preparation example 11; 1kg of the modified silane coupling agent in preparation example 12 added in step 2 was changed to 1kg of the modified silane coupling agent in preparation example 15.
Example 23
Example 23 differs from example 1 in that: 3kg of nano calcium carbonate, 3.5kg of 107 base gum, 0.5kg of dimethyl silicone oil and 3kg of modified mixed flame retardant filler in preparation example 1 added in the step 1 are changed to 4.5kg of nano calcium carbonate, 5kg of 107 base gum, 1.5kg of dimethyl silicone oil and 4.5kg of modified mixed flame retardant filler in preparation example 11; 3kg of the modified silane coupling agent in preparation example 12 added in step 2 was changed to 1kg of the modified silane coupling agent in preparation example 16.
Example 24
Example 24 differs from example 1 in that: 3kg of nano calcium carbonate, 3.5kg of 107 base gum, 0.5kg of dimethyl silicone oil and 3kg of modified mixed flame retardant filler in preparation example 1 added in the step 1 are changed to 4.5kg of nano calcium carbonate, 5kg of 107 base gum, 1.5kg of dimethyl silicone oil and 4.5kg of modified mixed flame retardant filler in preparation example 11; 2kg of the modified silane coupling agent in preparation example 12 added in step 2 was changed to 3kg of the modified silane coupling agent in preparation example 16.
Example 25
Example 25 differs from example 1 in that: 3kg of nano calcium carbonate, 3.5kg of 107 base gum, 0.5kg of dimethyl silicone oil and 3kg of modified mixed flame retardant filler in preparation example 1 added in the step 1 are changed to 4.5kg of nano calcium carbonate, 5kg of 107 base gum, 1.5kg of dimethyl silicone oil and 4.5kg of modified mixed flame retardant filler in preparation example 11; 2kg of the modified silane coupling agent in preparation example 12 added in step 2 was changed to 2kg of the modified silane coupling agent in preparation example 16.
Comparative example
Comparative example 1
Comparative example 1 differs from example 1 in that: 3kg of the modified mixed flame retardant filler in preparation example 1 added in step 1 was changed to 3kg of the modified mixed flame retardant filler in preparation example 17.
Comparative example 2
Comparative example 2 differs from example 1 in that: 3kg of the modified mixed flame retardant filler in preparation example 1 added in step 1 was changed to 3kg of the modified mixed flame retardant filler in preparation example 18.
Comparative example 3
Comparative example 3 differs from example 1 in that: 3kg of the modified mixed flame retardant filler in preparation example 1 added in step 1 was changed to 2kg of the modified mixed flame retardant filler in preparation example 1.
Comparative example 4
Comparative example 4 differs from example 1 in that: 3kg of the modified mixed flame retardant filler in preparation example 1 added in step 1 was changed to 7kg of the modified mixed flame retardant filler in preparation example 1.
Comparative example 5
Comparative example 5 differs from example 1 in that: 3kg of nano calcium carbonate added in the step 1 is changed into 2kg of nano calcium carbonate.
Comparative example 6
Comparative example 6 differs from example 1 in that: 3kg of nano calcium carbonate added in the step 1 is changed into 7kg of nano calcium carbonate.
Comparative example 7
Comparative example 7 differs from example 1 in that: 3.5kg of the 107 base adhesive added in the step 1 is changed into 2kg of the 107 base adhesive.
Comparative example 8
Comparative example 8 differs from example 1 in that: 3.5kg of the 107 base adhesive added in the step 1 is changed into 8kg of the 107 base adhesive.
Comparative example 9
Comparative example 9 differs from example 1 in that: 2kg of the modified silane coupling agent in preparation example 12 added in step 2 was changed to 0.5kg of the modified silane coupling agent in preparation example 16.
Comparative example 10
Comparative example 10 differs from example 1 in that: 2kg of the modified silane coupling agent in preparation example 12 added in step 2 was changed to 4kg of the modified silane coupling agent in preparation example 16.
Detection method
1. Flame retardant properties: according to GB/T24267-2009 "flame retardant sealants for construction", flame burning times were measured for examples 1-25 and comparative examples 1-10, and flame retardant grades were determined.
2. Tensile bond strength: the tensile bond strength was measured under three conditions of normal conditions, water-ultraviolet treatment and hot air aging for examples 1 to 25 and comparative examples 1 to 10 according to GB/T29755-2013 elastic sealants for hollow glass.
3. Water vapor transmission rate: the water vapor transmission rate was measured according to GB/T29755-2013 elastic sealer for hollow glass for examples 1-25 and comparative examples 1-10.
TABLE 1 determination of tensile bond Strength and Water vapor Transmission Rate for examples 1-6 and comparative examples 1-2
TABLE 2 determination of flame retardant Properties of examples 1-6 and comparative examples 1-2
TABLE 3 determination of tensile bond Strength and Water vapor Transmission Rate for examples 7-13 and comparative examples 3-4
TABLE 4 determination of flame retardant Properties of examples 7-13 and comparative examples 3-4
TABLE 5 determination of tensile bond Strength and Water vapor Transmission Rate for examples 14-19 and comparative examples 5-8
TABLE 6 determination of flame retardant Properties of examples 14-19 and comparative examples 5-8
/>
TABLE 7 determination of tensile bond Strength and Water vapor Transmission Rate for examples 20-25 and comparative examples 9-10
TABLE 8 determination of flame retardant Properties of examples 20-25 and comparative examples 9-10
/>
As can be seen from the combination of examples 1-6 and comparative examples 1-2 and the combination of tables 1-2, the effect of using the coupling agent KH-550 is better than that of the coupling agent KH-792, but the coupling agent KH-792 still has good performance, and when the ratio of coconut oil to sodium stearate in the composite surface treatment agent is different, the effects on the flame retardance, tensile adhesive strength and water vapor transmission rate of the silicone adhesive are different, and the performance of example 5 is better in combination consideration.
It can be seen from the combination of examples 7 to 13 and comparative examples 3 to 4 and the combination of tables 3 to 4 that the mass ratio of 1, 2-ethylenetetra (1-chloro-2-propyl) phosphate, DOP, guanidine sulfamate, zinc borate and antimony oxide in the flame retardant filler is different, and the effects on the flame retardant property, tensile bond strength and water vapor transmission rate of the silicone adhesive are different, and when the addition amount of the flame retardant filler is different, the flame retardant property is lowered but the tensile bond strength is improved, and when the addition amount of the flame retardant filler is excessive, the flame retardant property is improved, but the base adhesive cannot fully absorb the flame retardant filler, but the tensile bond strength of the silicone adhesive is lowered, and the flame retardant property of the flame retardant filler cannot fully exert, and the performance of example 13 is better in combination comprehensive consideration.
As can be seen from the combination of examples 14 to 19 and comparative examples 5 to 8 and the combination of tables 5 to 6, when the amounts of the nano calcium carbonate, the base gum, the dimethyl silicone oil and the modified mixed flame retardant filler are different, the prepared silicone gum has different flame retardant properties, tensile bond strength and water vapor transmittance, when the nano calcium carbonate is excessive, the tensile bond strength of the silicone gum is reduced, the ratio between the base gum and the nano calcium carbonate and the modified mixed flame retardant filler is maintained, and the proper dimethyl silicone oil is added, so that the base gum can be better mixed with the nano calcium carbonate and the modified mixed flame retardant filler, the properties of the components are fully exerted, and the performance of example 19 is better in combination of comprehensive consideration.
As can be seen from the combination of examples 20 to 25 and comparative examples 9 to 10 and the combination of tables 5 to 6, the flame retardant silicone adhesive for hollow glass prepared in example 25 has the best performance in combination with comprehensive consideration, when the mass ratio of the coupling agent KH-792, the coupling agent HY-102 and the E51 epoxy resin in the modified silane coupling agent is different, and when the total amount of the added modified silane coupling agent is different, the influences on the flame retardant performance, tensile bonding strength and water vapor transmission rate of the silicone adhesive are different.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (1)
1. The flame-retardant silicone adhesive for the hollow glass is characterized by comprising a component A and a component B, wherein the component A comprises 4.5kg of nano calcium carbonate, 5kg of 107 base adhesive, 1.5kg of dimethyl silicone oil and 4.5kg of modified mixed flame-retardant filler;
the preparation of the modified mixed flame-retardant filler comprises the following steps:
step 1: preparing a composite surface treating agent, namely adding 0.043kg of sodium stearate into a stirrer and heating to 85 ℃ to dissolve the sodium stearate into liquid, then adding 0.057kg of coconut oil for emulsification, and continuously stirring for 20min at the rotating speed of 300r/min to prepare the composite surface treating agent;
step 2: 3.75kg of 1, 2-ethylene tetra (1-chloro-2-propyl) phosphate, 7.5kg of DOP, 7.5kg of guanidine sulfamate, 3.75kg of zinc borate and 7.5kg of antimony oxide are added into a stirrer to be mixed and stirred at the rotating speed of 300r/min for 1.5h, then 0.03kg of coupling agent KH-550 is added, and the mixture is heated to 100 ℃ and mixed and stirred for 15min to prepare a mixture;
step 3: feeding the mixture into an air flow mill under negative pressure for grinding until the D50 of the mixture is less than or equal to 40 mu m, then conveying the ground mixture and the composite surface treating agent into a modified coating device, heating to 80 ℃ and mixing for 20min to obtain modified mixed flame retardant filler;
component B comprises 1.7kg of pigment carbon black, 0.75kg of fumed silica, 2.5kg of simethicone, 3.5kg of methyltrimethoxysilane, 3.5kg of trisaminosilane N- (piperazinylethyl) -3-aminopropyl methyldimethoxysilane, 2kg of modified silane coupling agent and 0.005kg of dibutyltin dilaurate;
the preparation method of the modified silane coupling agent comprises the following steps:
step 1: 5kg of N- (betA-Aminoethyl) -gammA-Aminopropyl trimethoxysilane, 10kg of isopropyl tri (dioctyl pyrophosphoryl) titanate, 2.85kg of E51 epoxy resin and 4.5kg of methanol are added into a 3000ml three-neck flask, a reflux condenser tube, a thermometer and a constant pressure dropping funnel are arranged on the three-neck flask, the temperature is raised to 100 ℃ under stirring, and reflux reaction is carried out for 3 hours;
step 2: vacuum distilling to collect methanol, continuously heating to 145 ℃, reacting for 2.5h, and cooling to room temperature to obtain the modified coupling agent;
the preparation method of the flame-retardant silicone adhesive for the hollow glass comprises the following steps of:
step 1: preparing a component A, namely adding 4.5kg of nano calcium carbonate, 5kg of 107 base rubber, 1.5kg of dimethyl silicone oil and 4.5kg of modified mixed flame retardant filler into a reaction kettle, uniformly mixing and stirring, heating to 110-150 ℃, vacuumizing by a vacuumizing machine, keeping the vacuum degree within a range of 0.09-0.1MPa, and stirring at a high speed of 800r/min for 1.5h to obtain the component A;
step 2: preparing a component B, namely adding 1.7kg of pigment carbon black into a planetary disperser, heating to 130 ℃, vacuumizing, keeping the vacuum degree within a range of 0.09-0.1MPa, stirring at a high speed for 0.5h, adding 3.5kg of methyltrimethoxysilane and 2.5kg of dimethyl silicone oil, stirring for 30min under vacuum, continuously adding 0.75kg of fumed silica, continuously stirring for 30min under vacuum, and finally adding 3.5kg of trisilane N- (piperazinylethyl) -3-aminopropyl methyldimethoxysilane, 2kg of modified silane coupling agent and 0.005kg of dibutyltin dilaurate, and stirring for 60min under vacuum to obtain the component B;
step 3: before use, the component A and the component B are mixed and stirred uniformly according to the proportion of 10:1, and the product is prepared.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211280981.0A CN115491165B (en) | 2022-10-19 | 2022-10-19 | Flame-retardant silicone adhesive for hollow glass and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211280981.0A CN115491165B (en) | 2022-10-19 | 2022-10-19 | Flame-retardant silicone adhesive for hollow glass and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115491165A CN115491165A (en) | 2022-12-20 |
| CN115491165B true CN115491165B (en) | 2023-08-18 |
Family
ID=84475338
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211280981.0A Active CN115491165B (en) | 2022-10-19 | 2022-10-19 | Flame-retardant silicone adhesive for hollow glass and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115491165B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0472035A2 (en) * | 1990-08-03 | 1992-02-26 | Quantum Chemical Corporation | Flame retardant crosslinkable polymeric compositions |
| CN103897656A (en) * | 2012-12-25 | 2014-07-02 | 锋泾（中国）建材集团有限公司 | Double-component flame-retardant silicone sealant for hollow glass |
| WO2015158257A1 (en) * | 2014-04-18 | 2015-10-22 | 苏州天山新材料技术有限公司 | High-adhesive one-component deoximation type room-temperature vulcanized silicone rubber sealant and preparation method therefor |
| CN114410274A (en) * | 2022-03-10 | 2022-04-29 | 武汉市金辉有机硅有限公司 | Flame-retardant silicone sealant for hollow glass and preparation method thereof |
-
2022
- 2022-10-19 CN CN202211280981.0A patent/CN115491165B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0472035A2 (en) * | 1990-08-03 | 1992-02-26 | Quantum Chemical Corporation | Flame retardant crosslinkable polymeric compositions |
| CN103897656A (en) * | 2012-12-25 | 2014-07-02 | 锋泾（中国）建材集团有限公司 | Double-component flame-retardant silicone sealant for hollow glass |
| WO2015158257A1 (en) * | 2014-04-18 | 2015-10-22 | 苏州天山新材料技术有限公司 | High-adhesive one-component deoximation type room-temperature vulcanized silicone rubber sealant and preparation method therefor |
| CN114410274A (en) * | 2022-03-10 | 2022-04-29 | 武汉市金辉有机硅有限公司 | Flame-retardant silicone sealant for hollow glass and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115491165A (en) | 2022-12-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109627770B (en) | Dealcoholized condensed type double-component room temperature vulcanized silicone rubber and preparation method thereof | |
| CN101942201B (en) | Room-temperature vulcanized antiflaming single-component dealcoholization-type silicone rubber sealant and preparation method thereof | |
| CN106833478B (en) | High-performance flame-retardant two-component silane modified polyether sealant and preparation method thereof | |
| CN107760256A (en) | A kind of lower shrinkage heat conductive flame-retarding double-component condensed type organic silicon potting adhesive and its preparation method and application | |
| CN106147695A (en) | Quick cured silicone glue of one 1 to 1 double-component and preparation method thereof | |
| CN101805585A (en) | One-component flame retardant solar photovoltaic subassembly sealant and preparation method thereof | |
| CN101544881B (en) | Bi-component silicone pouring sealant for LED photoelectric display device and method for manufacturing same | |
| CN109796927B (en) | Quick-curing silicone structural adhesive and application thereof | |
| CN104277759A (en) | Ageing resistant type solar photovoltaic component sealing material and preparation method thereof | |
| CN109810670B (en) | Bi-component fireproof silicone sealant and preparation method thereof | |
| CN107523259B (en) | Preparation of alpha-570 coupling agent modified organosilicon sealant | |
| CN113185947B (en) | Mixed crosslinking system two-component hollow sealant | |
| CN110205084B (en) | Quick-curing type organosilicon sealant | |
| CN103602304A (en) | Fast moisture-cured composition | |
| CN102093721A (en) | Single-component alcohol/ketoxime-removed room temperature vulcanizing silicone rubber and preparation method thereof | |
| CN114106768A (en) | Bi-component flame-retardant silicone sealant and preparation method thereof | |
| CN106833503A (en) | A kind of single-component ketoxime removing type room temperature vulcanized silicone sealant of low modulus and preparation method thereof | |
| CN111073577B (en) | Environment-friendly MS sealant and preparation method thereof | |
| CN113308186B (en) | Flame-retardant silane modified waterproof coating and preparation method thereof | |
| CN115491165B (en) | Flame-retardant silicone adhesive for hollow glass and preparation method thereof | |
| CN108977166A (en) | A kind of silicone sealant and preparation method thereof | |
| CN103740322A (en) | Inflaming retarding type solar photovoltaic module sealant | |
| CN112708135B (en) | Degradable organic silicon elastomer and synthesis method thereof | |
| CN106753204B (en) | Two-component silicone structural sealant and preparation method thereof | |
| CN114525105A (en) | Two-component organic silicon pouring sealant for photovoltaic junction box 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 |