CN113185947A - Mixed crosslinking system two-component hollow sealant - Google Patents
Mixed crosslinking system two-component hollow sealant Download PDFInfo
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- 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
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- 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
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- 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
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- 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
- C09J11/08—Macromolecular additives
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
Abstract
The application relates to the field of sealant, and particularly discloses a mixed cross-linked two-component hollow sealant. The hollow sealant comprises a main sealing component and a curing component, wherein the main sealing component comprises 50-60 parts of hydroxyl-terminated polydimethylsiloxane, 30-40 parts of inorganic filler, 5-10 parts of dimethyl silicone oil, 2-5 parts of modified silicone oil, 1-3 parts of ethyl orthosilicate and 0.4-0.6 part of water; the curing component comprises: 25-35 parts of a mixed crosslinking agent; 10-15 parts of a coupling agent; 0.5-0.8 part of organic tin catalyst; the main seal component and the curing component of the mixed cross-linking system two-component hollow sealant are independently packaged, and the main seal component and the curing component are 8-10: 1 by volume. The mixed crosslinking system two-component hollow sealant can be used for sealing double-layer glass and has the advantages of short surface drying time, fast curing speed and high curing strength.
Description
Technical Field
The application relates to the field of sealants, in particular to a mixed crosslinking system two-component hollow sealant.
Background
The hollow sealant is a new-generation green environment-friendly sealing material produced under the policy of high efficiency, energy conservation, sealing and environment protection of the national building engineering, and can be solidified into a tough rubber solid by contacting with moisture in the air, so that the requirements of sealing and strength are met, the material can be sealed, and the sealing part is not easy to damage by external force.
The hollow sealant is generally a two-component hollow sealant, a curing component and a main sealing component in the hollow sealant are separately and independently packaged, the two components are mixed according to a specific proportion when in use, the hollow sealant can be mixed for use after a long time and meets the standard, and the two-component hollow sealant has high strength, excellent weather-proof aging resistance, ultraviolet resistance, ozone resistance, water resistance and good adhesion property, and can form good adhesion with various kinds of glass and spacer bars.
The existing two-component hollow sealant has the disadvantages that the performance of each aspect is weakened after 6 months of storage, the working life (more than 90min) and the surface drying time are prolonged along with the lapse of time, the bonding strength of the sealant is reduced, and the sealant can not be cured even after being mixed, so the construction period and the quality are prolonged, the application of the two-component sealant is limited, and therefore, the application space is improved.
Disclosure of Invention
In order to obtain the hollow sealant with shorter pot life, shorter surface drying time and better curing strength under the condition of longer storage time, the application provides the mixed crosslinking system two-component hollow sealant.
The application provides a mix two ingredient cavity of cross-linking system and seal glue with following technical scheme:
the mixed cross-linking system two-component hollow sealant comprises a main sealing component and a curing component, wherein the main sealing component comprises the following components in parts by volume:
50-60 parts of hydroxyl-terminated polydimethylsiloxane;
30-40 parts of an inorganic filler;
5-10 parts of dimethyl silicone oil;
2-5 parts of modified silicone oil;
1-3 parts of ethyl orthosilicate;
0.4-0.6 part of water;
the curing component comprises the following components in parts by volume:
25-35 parts of a mixed crosslinking agent;
10-15 parts of a silane coupling agent;
0.5-0.8 part of organic tin catalyst;
the modified silicone oil is prepared by modifying 4-vinyl epoxy cyclohexane and chloroplatinic acid;
the main seal component and the curing component of the mixed cross-linking system two-component hollow sealant are independently packaged, and the main seal component and the curing component are 8-10: 1 by volume.
Preferably, the preparation method of the mixed crosslinking agent comprises the following steps:
the preparation method of the mixed cross-linking agent comprises the following steps:
dripping methyl trialkoxysilane into butanone oxime silane, reacting for 5-7 h at the water bath temperature of 40-65 ℃, heating to 100-110 ℃ to obtain butanone oxime alkoxysilane, and removing low boiling points to obtain a mixed crosslinking agent;
the molar ratio of the butanone oxime silane to the methyl trialkoxysilane is 1: 0.3 to 0.35.
According to the technical scheme, the modified silicone oil prepared by modifying the prepared curing component, the 4-vinyl epoxy cyclohexane, the chloroplatinic acid and the hydrogen-containing silicone oil is matched in a specific proportion and acts on a curing system when in use, so that a strong interface layer is formed on the surface of the sealant, the bond bridge effect in the system is enhanced, the concentrated stress generated in the curing process is weakened, the stress is uniformly distributed, the texture of the cured sealing adhesive is uniform and is not easy to break at a weak part, the bonding strength of the cured sealant is good, the curing process is accelerated, the surface drying time of the two-component sealant is shorter on the premise of good bonding strength, the quality of the two-component sealant is ensured, and the construction period is shortened.
Preferably, the butanone oxime silane is any one of methyl tributyrinoxime silane and tetrabutoxime silane.
Preferably, the methyltrialkylsilane is any one of methyltrioxysilane and methyltriethylsilane.
By adopting the technical scheme, the methyl/ethyl tributyrinoxime silane and the tetrabutoximino silane are respectively adopted to form the mixture of butanone oxime dimethyl/ethoxy silane and tributyroximino methyl/ethoxy silane with the dibutyloximino dimethyl/ethoxy silane and the tributyroximino methyl/ethoxy silane, so that the bonding strength of the cured sealant is better, the curing process is further accelerated, the surface drying time of the two-component sealant is shorter, the quality of the two-component sealing sealant is ensured, and the construction period is shortened.
Preferably, the inorganic filler is nano calcium carbonate.
By adopting the technical scheme, as the nano calcium carbonate is adopted, the nano calcium carbonate particles have small particle size and narrow particle size distribution width, and are better dispersed in a curing system, so that a better reinforcing effect is realized, the curing strength of the sealing adhesive is better, and the sealing adhesive is not easy to be damaged due to the action of external force.
Preferably, the preparation method of the modified silicone oil comprises the following steps:
dissolving 4-vinyl epoxy cyclohexane by using toluene, adding chloroplatinic acid, heating to 50-55 ℃, dripping hydrogen-containing silicone oil into the dissolved 4-vinyl epoxy cyclohexane, vacuumizing, protecting, heating to 90-100 ℃, reacting for 6-8 hours, and depressurizing to evaporate the toluene to obtain modified silicone oil;
the molar ratio of the 4-vinyl cyclohexene oxide to the hydrogen-containing silicone oil is 1.1-1.3: 1, and 1-3 mL of chloroplatinic acid is added into each 1mL of the 4-vinyl cyclohexene oxide.
By adopting the technical scheme, the modified silicone oil prepared by the preparation method is added in a specific proportion and acts on a reaction system formed by mixing the main sealing component and the curing component, the concentrated stress generated in the curing process is further weakened, the stress is uniformly distributed in the sealing adhesive structure, the cured sealing adhesive is not easy to crack, the bonding strength of the sealing adhesive is enhanced, the surface drying speed is improved, the surface drying time of the two-component sealing adhesive is shortened, the quality of the two-component sealing adhesive is ensured, and the time cost of construction is saved.
Preferably, the silane coupling agent is a compound of 3-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma- (2, 3-glycidoxy) propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane in a volume ratio of 1:1.3: 1.3-1: 1.2:1.2:1:1.3: 1.
By adopting the technical scheme, the compound of various silane coupling agents is adopted to form stable spatial structure connection with the molecules of the hydroxyl-terminated polydimethylsiloxane, so that the stability of the formed sealant is improved, and the sealant is not easy to crack and degum due to external environmental change.
Preferably, the organic tin catalyst is prepared by compounding stannous octoate, dibutyltin laurate and dibutyltin acetate according to the volume ratio of 1:3: 5-1: 2: 5.
By adopting the technical scheme, the main sealing component and the curing component are mixed by compounding the stannous octoate, the dibutyltin laurate and the dibutyltin acetate, so that the reaction activity in a system is reduced, the surface drying speed of the sealant is accelerated, the surface drying time of the sealant is reduced, and the construction period is shortened.
Preferably, the preparation method of the curing component comprises the following steps: and (2) uniformly mixing and stirring 100-150 parts by volume of the mixed crosslinking agent and 250-350 parts by volume of the silane coupling agent in vacuum to prepare a curing agent, then mixing the prepared curing agent with 5-8 parts by volume of the catalyst, and vacuumizing and stirring to prepare the curing component.
By adopting the technical scheme, because the curing agent that makes after mixing cross-linking agent and silane coupling agent stirring, make the surface of curing agent smooth and particle-free, make the curing agent form viscous paste, stir under vacuum environment simultaneously, make the curing agent reduce the participation with oxygen in the preparation process, make catalyst, coupling agent and mixed cross-linking agent mix the curing component more stably, the quality of curing component has been promoted, thereby make the curing component still shorter in the application life behind longer time, make the surface dry time shorter, construction period of having shortened the execution, make sealed glue keep better adhesive strength simultaneously.
Preferably, the main sealing component further comprises 1-2 parts by volume of fumed silica.
By adopting the technical scheme, as the fumed silica is adopted, after the fumed silica is dispersed in the main sealing component and the curing component, hydrogen bonds are generated among different particles through silicon hydroxyl on the surfaces of the particles, a fumed silica aggregate network is formed, the fluidity of the system is limited, the viscosity is increased, the thickening effect is achieved, the fumed silica network is damaged under the action of shearing force, the viscosity of the system is reduced, the thixotropic effect is generated, the construction is convenient, once the shearing force is eliminated, the network structure can be formed again, the sagging of the two-component sealant in the curing process is effectively prevented, the extrudability of the sealant is good, the formed sealant is uniform in texture, and the bonding strength of the sealant is enhanced.
In summary, the present application has the following beneficial effects:
1. according to the application, the curing component prepared by the method, the 4-vinyl epoxy cyclohexane, the chloroplatinic acid and the modified silicone oil prepared by modifying the hydrogen-containing silicone oil are matched in a specific proportion and act on a curing system when in use, so that the bonding strength of the cured sealant is good, the curing process is accelerated, the surface drying time of the two-component sealant is shorter on the premise of good bonding strength, the quality of the two-component sealant is ensured, and the construction period is shortened.
2. Preferentially adopt in this application because mix the curing agent that cross-linking agent and silane coupling agent stir back and make for the smooth no granule in surface of curing agent, thereby make the curing component application period still shorter behind longer time, make the surface dry time shorter, shortened the time limit for a project of construction, make sealed glue keep better cohesive strength simultaneously.
3. The modified silicone oil prepared by the specific preparation method is preferentially adopted in the application, and is added and acted in a reaction system after the main sealing component and the curing component are mixed, so that the bonding strength of the sealant is enhanced, and meanwhile, the surface drying time of the two-component sealant is shorter, so that the quality of the two-component sealant is ensured, and the construction period is shortened.
Detailed Description
The present application is described in further detail below with reference to preparation examples and examples.
The information on the raw materials used in the preparation examples and examples is shown in Table 1.
Preparation example 1
The preparation example discloses a preparation method of modified silicone oil.
100mL of toluene and 50mL of 4-vinyl epoxy cyclohexane are added into a three-neck flask, 1.5mL of chloroplatinic acid is added and heated to 50 ℃, 66mL of hydrogen-containing silicone oil is dripped into the dissolved 4-alkenyl epoxy cyclohexane, the mixture is vacuumized, protected and heated to 90 ℃ for reaction for 6 hours, and the toluene is evaporated under reduced pressure to obtain the modified silicone oil.
Preparation example 2
The preparation example discloses a preparation method of modified silicone oil.
100mL of toluene and 50mL of 4-vinyl epoxy cyclohexane are added into a three-neck flask, 1.7mL of chloroplatinic acid is added and heated to 53 ℃, 60mL of hydrogen-containing silicone oil is dripped into the dissolved 4-alkenyl epoxy cyclohexane, the mixture is vacuumized, protected and heated to 95 ℃ for reaction for 7 hours, and the toluene is evaporated under reduced pressure to obtain the modified silicone oil.
Preparation example 3
The preparation example discloses a preparation method of modified silicone oil.
100mL of toluene and 50mL of 4-vinyl epoxy cyclohexane are added into a three-neck flask, 2mL of chloroplatinic acid is added and heated to 55 ℃, 56mL of hydrogen-containing silicone oil is dripped into the dissolved 4-alkenyl epoxy cyclohexane, the mixture is vacuumized, protected and heated to 100 ℃ for reaction for 8 hours, and the toluene is evaporated under reduced pressure to obtain the modified silicone oil.
Example 1
The embodiment discloses a preparation method of a mixed crosslinking system two-component hollow sealant.
Step 1), preparing a main sealant component: adding 50mL of hydroxy polydimethylsiloxane, 30g of nano calcium carbonate, 1g of fumed silica, 5mL of dimethyl silicone oil, 2mL of modified silicone oil prepared in preparation example 1 and 0.4mL of water into a power mixer for dispersing and dehydrating, stirring at the rotating speed of 30 r/s, heating, adding 1mL of ethyl orthosilicate at the temperature of 90 ℃, performing 110 ℃ and the vacuum degree of 0.09MPa for 110 minutes, and cooling to room temperature to obtain the main sealing component.
And step 2), preparing a curing agent component.
Step 2-1), preparing a mixed cross-linking agent: dripping methyl tributyrinoxime silane into a 20L reaction kettle filled with methyl trimethoxy silane, reacting for 5h under the condition that the water bath temperature is 40 ℃, then heating to 100 ℃, obtaining butanone oxime methoxy silane, and then removing low boiling point in a power mixer to prepare a mixed crosslinking agent;
the molar ratio of the butanone oxime silane to the methyl trialkoxysilane is 1: 0.3.
step 2-2) preparation of a silane coupling agent: adding kh540, kh550, kh560, kh570 and kh792 into a 20L reaction kettle according to the volume ratio of 1:1.2:1.2: 1.5:1, and stirring for 15 minutes to obtain the silane coupling agent.
Step 2-3), preparing an organic tin catalyst: adding stannous octoate, dibutyltin laurate and dibutyltin acetate into a 20L reaction kettle according to the volume ratio of 1:2:5, and stirring for 5 minutes to obtain the organotin catalyst.
Step 2-4), preparing a curing component: 100mL of the prepared silane coupling agent and 250mL of the mixed crosslinking agent are added into a power mixer to be stirred, the negative pressure is-0.085 mpa, the temperature is controlled at 45 ℃, the stirring speed is 30Hz, 5mL of the prepared organic tin catalyst and 100mL of dimethyl silicone oil are added to be stirred for 80 minutes, and the curing component is prepared.
Example 2
The embodiment discloses a preparation method of a mixed crosslinking system two-component hollow sealant.
Step 1), preparing a main sealing component: adding 55mL of hydroxy polydimethylsiloxane, 35g of nano calcium carbonate, 1.5g of fumed silica, 8mL of dimethyl silicone oil, 2.5mL of modified silicone oil prepared in preparation example 2 and 0.5mL of water into a power mixer, stirring, heating, adding 2mL of tetraethoxysilane at the temperature of 95 ℃, dispersing and dehydrating for 120 minutes at the temperature of 120 ℃ and the vacuum degree of 0.092MPa, and cooling to room temperature to obtain the main sealing component.
And 2) preparing a curing component.
Step 2-1), preparing a mixed cross-linking agent: 50ml of methyl tributyrinoxime silane is dripped into a 20L reaction kettle filled with methyl tributyrinoxime silane, the reaction is carried out for 5h under the condition that the water bath temperature is 40 ℃, then the temperature is raised to 100 ℃, butanone oxime methoxysilane is obtained, and low boiling is removed in a power mixer, thus obtaining the mixed crosslinking agent.
Step 2-2) preparation of a silane coupling agent: adding kh540, kh550, kh560, kh570 and kh792 into a 20L reaction kettle according to the volume ratio of 1:1.2:1.2:1:1.5:1, and stirring for 15 minutes to obtain the silane coupling agent.
Step 2-3), preparing an organic tin catalyst: adding stannous octoate, dibutyltin laurate and dibutyltin acetate into a 20L reaction kettle according to the volume ratio of 1:2:5, and stirring for 5 minutes to obtain the organotin catalyst.
Step 2-4), preparing a curing component: 100mL of prepared silane coupling agent and 250mL of mixed crosslinking agent are added into a power mixer to be stirred, the negative pressure is-0.085 mpa, the temperature is controlled at 45 ℃, the stirring speed is 30Hz, 5mL of prepared organic tin catalyst, 200g of fumed silica, 30g of carbon powder and 100mL of dimethyl silicone oil are added to be stirred for 80 minutes, and the curing component is prepared.
Example 3
The embodiment discloses a preparation method of a mixed crosslinking system two-component hollow sealant.
Step 1), preparing a main sealing component: adding 60mL of hydroxy polydimethylsiloxane, 40g of nano calcium carbonate, 2g of fumed silica, 10mL of dimethyl silicone oil, 5mL of modified silicone oil prepared in preparation example 3 and 0.6mL of water into a power mixer, stirring, heating, adding 3mL of tetraethoxysilane at the temperature of 110 ℃, carrying out 130 minutes at the temperature of 130 ℃ and the vacuum degree of 0.095MPa, and cooling to room temperature to obtain the main sealing component.
And 2) preparing a curing component.
Step 2-1), preparing a mixed cross-linking agent: dripping methyl tributyrinoxime silane into a 20L reaction kettle filled with methyl triethoxy silane, reacting for 6h under the condition that the water bath temperature is 50 ℃, then heating to 105 ℃, obtaining butanone oxime ethoxy silane, and then removing low boiling point in a power mixer to prepare a mixed crosslinking agent;
the molar ratio of the methyl tributyl ketoxime silane to the methyl triethoxysilane is 1: 0.32.
step 2-2) preparation of a silane coupling agent: adding kh540, kh550, kh560, kh570 and kh792 into a 20L reaction kettle according to the volume ratio of 1:1.3:1.3, and stirring for 15 minutes to obtain the silane coupling agent.
Step 2-3), preparing an organic tin catalyst: adding stannous octoate, dibutyltin laurate and dibutyltin acetate into a 20L reaction kettle according to the volume ratio of 1:3:5, and stirring for 5 minutes to obtain the organotin catalyst.
Step 2-4), preparing a curing component: adding 120mL of prepared silane coupling agent and 300mL of mixed crosslinking agent into a power mixer, stirring at negative pressure of-0.085 mpa, controlling the temperature at 45 ℃ and stirring speed at 30Hz, adding 6mL of prepared organic tin catalyst, 220g of fumed silica, 30g of carbon powder and 150mL of dimethyl silicone oil, and stirring for 90 minutes to obtain the curing component.
Example 4
The embodiment discloses a preparation method of a mixed crosslinking system two-component hollow sealant.
Compared with the example 3, the difference lies in the preparation method of the curing component, which is as follows:
and 2) preparing a curing component.
Step 2-1), preparing a mixed cross-linking agent: dripping tetrabutyl ketoxime silane into a 20L reaction kettle containing methyltrimethoxy silane, reacting for 7h under the condition that the water bath temperature is 65 ℃, then heating to 110 ℃, obtaining butanone oxime methoxy silane, and then removing low boiling in a power mixer to prepare a mixed crosslinking agent;
the molar ratio of the tetrabutoximino silane to the methyltrimethoxy silane is 1: 0.35.
step 2-2) preparation of a silane coupling agent: adding kh540, kh550, kh560, kh570 and kh792 into a 20L reaction kettle according to the volume ratio of 1:1.2:1.2: 1.3:1, and stirring for 15 minutes to obtain the silane coupling agent.
Step 2-3), preparing an organic tin catalyst: adding stannous octoate, dibutyltin laurate and dibutyltin acetate into a 20L reaction kettle according to the volume ratio of 1:4:5, and stirring for 5 minutes to obtain the organotin catalyst.
Step 2-4), preparing a curing component: 150mL of prepared silane coupling agent and 350mL of mixed crosslinking agent are added into a power mixer to be stirred, the negative pressure is-0.085 mpa, the temperature is controlled to be 45 ℃, the stirring speed is 30Hz,
8mL of the prepared organotin catalyst, 300g of fumed silica, 240g of carbon powder and 110mL of dimethyl silicone oil were added and stirred for 100 minutes to obtain a curing component.
Example 5
The only difference from example 4 is that methyltrimethoxysilane is replaced by methyltriethoxysilane in step 1), butanone oximinoethoxysilane is obtained and then low-boiling is removed.
Comparative example 1
The only difference from example 3 is that:
and step 2-4), adding the methyl tributyl ketoxime silane, the silane coupling agent prepared in the step 2-2), the organotin catalyst in the step 2-3), the fumed silica, the carbon powder and the dimethyl silicone oil into a power mixer.
Comparative example 2
The only difference from example 3 is that:
step 2-4), adding the tetrabutoxime silane, the silane coupling agent prepared in the step 2-2), the organotin catalyst prepared in the step 2-3), the fumed silica, the carbon powder and the dimethyl silicone oil into a power mixer.
Comparative example 4
The only difference from example 3 is that:
step 2-4), adding the mixed cross-linking agent prepared in the step 2-1), the silane coupling agent prepared in the step 2-2), the organotin catalyst prepared in the step 2-3), the fumed silica, the carbon powder and the dimethyl silicone oil into a power mixer, stirring at the negative pressure of-0.085 mpa, controlling the temperature to be 45 ℃ and the stirring speed to be 30 Hz.
Comparative example 5
The only difference from example 3 is that:
replacing the modified silicone oil in the step 1) with dimethyl silicone oil.
Experiment 1
Test pot life
Taking the mixed cross-linking system two-component hollow sealant prepared in the examples 1-5 and the comparative examples 1-5, mixing the main sealing component and the curing component in a volume ratio of 8:1 and 10:1, and testing the qualified standard of the pot life according to GB/T-29755-2013 elastic sealant for hollow glass: the time is 20min, t and 90min are qualified, and the results are shown in Table 2.
TABLE 2
Experiment 2
Testing the curing speed
The mixed cross-linking system two-component hollow sealant prepared in the examples 1-5 and the comparative examples 1-5 is taken, the main sealing component and the curing component are mixed according to the volume ratio of 8:1 and 10:1, the surface drying time is tested according to GB/T13477.5-2003, the surface drying time is measured according to the test method of building sealing materials part 5, the surface drying time is qualified after 20min > T >90min, and the result is shown in the table 3.
TABLE 3
Experiment 3
Testing of bond Strength
The mixed cross-linking system two-component hollow sealant prepared in the examples 1 to 5 and the comparative examples 1 to 5 is taken, the main sealing component and the curing component are mixed according to the volume ratio of 8:1 and 10:1, the bonding strength is tested at normal temperature according to GB/T13477.8-2017 'determination of tensile bonding strength of part 8 of test method of building sealing materials', the sealant is qualified when the sealant is larger than 0.6MPa, and the result is shown in Table 4.
TABLE 4
According to the comparison of the data of the example 3 in the tables 2 to 4 with the data of the comparative examples 1 and 2, the working life of the comparative examples 1 and 2 is 1 to 3 months, the surface drying time is basically the same as that of the example 3, the surface drying time is longer at the beginning of 8 months than that of the example 3, and the product is completely failed after 12 months; and in example 3, the pot life of 1-12 months, the surface dryness are unchanged, the pot life of 12 months starts to change slightly, and the curing speed becomes slow after 18 months, which shows that the pot life of the sealant is shortened by using the curing component prepared by using the mixed crosslinking agent, so that the surface dryness time is shortened.
According to the comparison of the data of the example 3 and the comparative examples 3 and 4 in the tables 2 to 4, the pot life and the open time of 1 to 9 months in the comparative examples 3 and 4 are basically the same as those of the example 3, the pot life is started at 9 months, the bonding strength is smaller than that of the example 3, the open time is longer than that of the example 3 after 12 months, the pot life is slightly changed after 12 months in the example 3, and the solid open time is longer after 18 months, which shows that the performances of all aspects of the curing component formed by adding the mixed crosslinking agent and the coupling agent into the catalyst after uniformly stirring are better than those of the curing component directly adding the mixed crosslinking agent into the curing component.
According to the comparison of the data of the example 3 and the comparative example 5 in the tables 2 to 4, the bonding strength of the example 3 is far greater than that of the comparative example 5, and the surface drying speed is lower than that of the comparative example 5, which shows that the bonding strength and the curing speed of the sealant can be improved only by proportionally combining the modified silicone oil prepared by the specific preparation method and the curing component, so that the two-component sealant is not easy to crack and the construction period is shortened.
Claims (10)
1. A mixed cross-linking system two-component hollow sealant is characterized in that: comprises a main sealing component and a curing component,
the main sealing component comprises the following components in parts by volume:
50-60 parts of hydroxyl-terminated polydimethylsiloxane;
30-40 parts of an inorganic filler;
5-10 parts of dimethyl silicone oil;
2-5 parts of modified silicone oil;
1-3 parts of ethyl orthosilicate;
0.4-0.6 part of water;
the curing component comprises the following components in parts by volume:
25-35 parts of a mixed crosslinking agent;
10-15 parts of a silane coupling agent;
0.5-0.8 part of organic tin catalyst;
the modified silicone oil is prepared by modifying 4-vinyl epoxy cyclohexane and chloroplatinic acid;
the main seal component and the curing component of the mixed cross-linking system two-component hollow sealant are independently packaged, and the main seal component and the curing component are 8-10: 1 in a volume ratio;
the preparation method of the mixed cross-linking agent comprises the following steps:
dropping butanone oxime silane into methyl trialkoxysilane, reacting for 5-7 h at the water bath temperature of 40-65 ℃, heating to 100-110 ℃ to obtain butanone oxime alkoxysilane, and removing low boiling point to obtain the mixed crosslinking agent.
2. The hybrid crosslinking system two-component hollow sealant as claimed in claim 1, which is characterized in that: the molar ratio of the butanone oxime silane to the methyl trialkoxysilane is 1: 0.3 to 0.35.
3. The hybrid crosslinking system two-component hollow sealant as claimed in claim 2, which is characterized in that: the butanone oxime silane is any one of methyl tributyl oxime silane and tetrabutoxime silane.
4. The hybrid crosslinking system two-component hollow sealant as claimed in claim 2, which is characterized in that: the methyl trialkyl silane is any one of methyl trioxymethylene and methyl triethyl silane.
5. The hybrid crosslinking system two-component hollow sealant as claimed in claim 1, which is characterized in that: the inorganic filler is nano calcium carbonate.
6. The hybrid crosslinking system two-component hollow sealant as claimed in claim 1, which is characterized in that: the preparation method of the modified silicone oil comprises the following steps:
dissolving 4-vinyl epoxy cyclohexane by using toluene, adding chloroplatinic acid, heating to 50-55 ℃, dripping hydrogen-containing silicone oil into the dissolved 4-vinyl epoxy cyclohexane, vacuumizing, protecting, heating to 90-100 ℃, reacting for 6-8 hours, and decompressing and steaming out the toluene to obtain modified silicone oil;
the molar ratio of the 4-vinyl cyclohexene oxide to the hydrogen-containing silicone oil is 1.1-1.3: 1, and 1-3 mL of chloroplatinic acid is added into each 1mL of the 4-vinyl cyclohexene oxide.
7. The hybrid crosslinking system two-component hollow sealant as claimed in claim 1, which is characterized in that: the silane coupling agent is prepared by compounding 3-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane according to the volume ratio of 1:1.3: 1.3-1: 1.2:1.2: 1.3:1.
8. The hybrid crosslinking system two-component hollow sealant as claimed in claim 1, which is characterized in that: the organic tin catalyst is prepared by compounding stannous octoate, dibutyltin laurate and dibutyltin acetate according to the volume ratio of 1:3: 5-1: 2: 5.
9. The hybrid crosslinking system two-component hollow sealant as claimed in claim 1, which is characterized in that: the preparation method of the curing component comprises the following steps: and (2) uniformly mixing and stirring 100-150 parts by volume of the mixed crosslinking agent and 250-350 parts by volume of the silane coupling agent in vacuum to prepare a curing agent, mixing the prepared curing agent with 5-8 parts by volume of the catalyst, and vacuumizing and stirring to prepare the curing component.
10. The hybrid crosslinking system two-component hollow sealant according to any one of claims 1 to 9, characterized in that: the main sealing component further comprises 1-2 parts by volume of fumed silica.
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