CN108192561A - Ketoxime removing type silicone sealant and preparation method thereof - Google Patents
Ketoxime removing type silicone sealant and preparation method thereof Download PDFInfo
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- CN108192561A CN108192561A CN201711492790.XA CN201711492790A CN108192561A CN 108192561 A CN108192561 A CN 108192561A CN 201711492790 A CN201711492790 A CN 201711492790A CN 108192561 A CN108192561 A CN 108192561A
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- Prior art keywords
- silane
- type silicone
- removing type
- silicone sealant
- ketoxime removing
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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
-
- 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
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
-
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- 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
Abstract
The present invention relates to a kind of ketoxime removing type silicone sealants and preparation method thereof.The ketoxime removing type silicone sealant, in parts by weight, including the following raw material component:100 parts of polysiloxanediol, 40~80 parts of dimethicone, composition A0.5~2 part, composition B0.5~2 part, 15~25 parts of filler, 5~12 parts of crosslinking agent, 0.5~3 part of silane coupling agent, 0.05~0.5 part of catalyst;Wherein, the composition A includes the nano silver being carried on carrier;The composition B includes thiazole compound.It is good that the ketoxime removing type silicone sealant is not easy xanthochromia, anti-mold effect, and surface drying, hardening time are short, facilitate construction.
Description
Technical field
The present invention relates to silicone sealant, more particularly to ketoxime removing type silicone sealant and preparation method thereof.
Background technology
In recent years, house decoration silicone sealant increasingly payes attention to anti-mold effect, particularly high-grade hotel and villa
Kitchen and bath fits up.These application sites are chronically at the environment of warmed moist, and fluid sealant uses preceding less clean position or use in addition
Adherency spot provides nutriment for mould afterwards, and fluid sealant is caused to go mouldy, and seriously affects beauty, pollutes environment or even causes close
Sealing disabler.
Transparent silicone fluid sealant is widely used in design of glass lighting roof joint seal, organic glass because of its transparent characteristic
Etc. materials light canopy joint seal, coated glass and two-way mirror sealing etc. fields.With the expansion in interior decoration market, transparent silicon
Ketone seal gum is gradually applied to kitchen and bath's waterproof sealing, so the mildew resistance to transparent adhesive tape also there are certain requirements.Therefore, moldproof transparent
Silicone sealant product has very big market potential and development space.
Addition mould inhibitor is to prepare the most direct effective method of mildewproof sealant, but some mould inhibitors be easy to cause colloid
Xanthochromia seriously affects the transparency and aesthetics of fluid sealant.Part Methods are utilized using polyether polyol as the organo-arsenic of carrier
Object is closed as mould inhibitor, is prepared for Single-component moldproof transparent Dealcoholization type silicone sealant, but its mould proof long-term effect is also needed checking
It examines.Separately there is method by the use of thiazole compound as mould inhibitor, be prepared for the single-component room temperature vulcanized mould proof silicone of transparent dealcoholized type
Fluid sealant, but the easy xanthochromia of the colloid of such fluid sealant.
Invention content
Based on this, it is necessary to provide a kind of ketoxime removing type silicone sealant.The ketoxime removing type silicone sealant be not easy xanthochromia,
Anti-mold effect is good, and surface drying, hardening time are short, facilitate construction.
A kind of ketoxime removing type silicone sealant, in parts by weight, including the following raw material component:
Wherein, the composition A includes the nano silver being carried on carrier;
The composition B includes thiazole compound.
The ketoxime removing type silicone sealant in one of the embodiments, in parts by weight, including the following raw material group
Point:
The carrier includes at least one of apatite, calcium phosphate, basic zirconium phosphate in one of the embodiments,.
It can be by conventional method by the nano-silver loaded on carrier.In one embodiment of the invention, can lead to
The carrier is crossed to load the ion exchange or suction-operated of silver ion.
The composition B includes 1,2-benzisothiazolin-3-one, the different thiophenes of 2-n- octyl groups -4- in one of the embodiments,
At least one of oxazoline -3- ketone, 2-methyl-4-isothiazolin-3-one, 5- chloro-2-methyl -4- isothiazole beautiful jade -3- ketone.
The polysiloxanediol structural formula is in one of the embodiments,Viscosity is 8
~200Pa.s (25 DEG C).
The viscosity of the dimethicone is 0.1~50Pa.s (25 DEG C) in one of the embodiments,.
The crosslinking agent is the silane of the base containing ketoxime in one of the embodiments,.
The crosslinking agent is methyl tributanoximo silane, vinyl tributanoximo silicon in one of the embodiments,
Alkane, propyl tributanoximo silane, phenyl tributanoximo silane, four butanone oximino silanes, (the methyl tert-butyl ketoxime of methyl three
Base) silane, vinyl three (methylisobutylketone oximido) silane, four (methylisobutylketone oximido) silane, methyl tri acetylacetonate oximido silicon
At least one of alkane, vinyl tri acetylacetonate oximino silane.Preferably as above in type of crosslinking agent at least two.
The crosslinking agent is methyl tributanoximo silane and vinyl tributanoximo silicon in one of the embodiments,
Alkane, the preferably weight ratio of the two are 5~9:2~3;Or, (methyl is different for (methylisobutylketone oximido) silane of methyl three and vinyl three
Butanone oximido) silane, the preferably weight ratio of the two is 5~7:1~3;Or, four butanone oximino silane and methyl tributanoximo silicon
Alkane, the preferably weight ratio of the two are 3~5:5~7.
The silane coupling agent is chloropropyl triethoxysilane, γ-aminopropyl trimethoxy in one of the embodiments,
Base silane, gamma-aminopropyl-triethoxy-silane, N- β aminoethyls γ-aminopropyltrimethoxysilane, N- β aminoethyls γ-ammonia third
At least one of ethyl triethoxy silicane alkane, glycidyl triethoxysilane, mercaptopropyl trimethoxysilane.
In one of the embodiments, the silane coupling agent for gamma-aminopropyl-triethoxy-silane, N- β aminoethyls γ-
Aminopropyl trimethoxysilane or N- β aminoethyl gamma-aminopropyl-triethoxy-silanes.
The catalyst is dibutyl tin laurate, dibutyltin diacetate, two bays in one of the embodiments,
At least one of sour dioctyl tin, two (dodecyl sulphur) dibutyl tins, stannous octoate, two fourth acetylacetone,2,4-pentanedione tin.
The filler is inorganic filler in one of the embodiments,.Preferably aerosil (white carbon).
The present invention also provides the preparation methods of the ketoxime removing type silicone sealant, include the following steps:
By the polysiloxanediol, dimethicone, composition A, composition B, filler, crosslinking agent, silane coupling agent, urge
Agent is mixed, and control vacuum degree is 0.09~0.10MPa, 10~800rpm of rotating speed, stirs 30~180min, you can.
Compared with prior art, the invention has the advantages that:
The ketoxime removing type silicone sealant of the present invention, the silicone body formed with polysiloxanediol and dimethicone
Based on system, ketoxime removing type silicone sealant, each original are prepared with reference to the nano silver and thiazole compound being carried on carrier
Material, which matches, shows good synergistic effect, so as to make the ketoxime removing type silicone sealant in the premise for keeping the transparency
Under, anti-mold effect is excellent and long-acting, suitable for mould proof more demanding interior decoration, while avoids colloid during storage
Xanthochromia, surface drying, hardening time are shorter, have good caking property with most of matrix, can be widely used for the anti-of interior decoration
Water-stop, and constructing operation is convenient, construction efficiency is high.
Specific embodiment
Ketoxime removing type silicone sealant of the present invention and preparation method thereof is made below in conjunction with specific embodiment further detailed
Thin explanation.
The polysiloxanediol structural formula used in the embodiment of the present invention forViscosity for 8~
200Pa.s (25 DEG C), purchased from Dow Corning;
The viscosity of dimethicone is 0.1~50Pa.s (25 DEG C), purchased from Dow Corning;
The nano silver on carrier is carried on purchased from Lonza, the carrier is apatite, calcium phosphate or basic zirconium phosphate.
Embodiment 1:
A kind of ketoxime removing type silicone sealant of the present embodiment, in parts by weight, is made of the following raw material:
100 parts of polysiloxanediol, 60 parts of dimethicone, 20 parts of gas-phase silica are carried on receiving on apatite
1 part of rice silver, 1 part of 1,2-benzisothiazolin-3-one, 6 parts of methyl tributanoximo silane, vinyl tributyl ketoximyl silane 2
Part, 1.5 parts of gamma-aminopropyl-triethoxy-silane, 0.25 part of dibutyltin diacetate.
The preparation method of above-mentioned ketoxime removing type silicone sealant, includes the following steps:
Above-mentioned raw materials composition is added in into double-planet equipment, is 0.09MPa in vacuum degree, rotating speed is to be carried out under 300rpm
90min is chemically reacted, product performance index is shown in Table 1.
Embodiment 2:
A kind of ketoxime removing type silicone sealant of the present embodiment, in parts by weight, is made of the following raw material:
100 parts of polysiloxanediol, 80 parts of dimethicone, 25 parts of gas-phase silica are carried on receiving on apatite
2 parts of rice silver, 2 parts of 1,2-benzisothiazolin-3-one, 9 parts of methyl tributanoximo silane, vinyl tributyl ketoximyl silane 3
Part, 3 parts of gamma-aminopropyl-triethoxy-silane, 0.5 part of dibutyltin diacetate.
The preparation method of above-mentioned ketoxime removing type silicone sealant, includes the following steps:
Above-mentioned raw materials are added in into double-planet equipment, are 0.09MPa in vacuum degree, rotating speed is that chemistry is carried out under 300rpm
90min is reacted, product performance index is shown in Table 1.
Embodiment 3:
A kind of ketoxime removing type silicone sealant of the present embodiment, in parts by weight, is made of the following raw material:
100 parts of polysiloxanediol, 40 parts of dimethicone, 15 parts of gas-phase silica are carried on receiving on calcium phosphate
0.5 part of rice silver, 0.5 part of 2-methyl-4-isothiazolin-3-one, 5 parts of methyl tributanoximo silane, vinyl tributanoximo
2 parts of silane, 0.5 part of gamma-aminopropyl-triethoxy-silane, 0.05 part of dibutyltin diacetate.
The preparation method of above-mentioned ketoxime removing type silicone sealant, includes the following steps:
Above-mentioned raw materials are added in into double-planet equipment, are 0.09MPa in vacuum degree, rotating speed is that chemistry is carried out under 300rpm
90min is reacted, product performance index is shown in Table 1.
Embodiment 4:
A kind of ketoxime removing type silicone sealant of the present embodiment, in parts by weight, is made of the following raw material:
100 parts of polysiloxanediol, 60 parts of dimethicone, 20 parts of gas-phase silica are carried on receiving on basic zirconium phosphate
0.5 part of rice silver, 2 parts of 2-n- octyl group -4- isothiazoline -3- ketone, 4 parts of four butanone oximino silane, methyl tributanoximo silane 6
Part, 1.5 parts of N- β aminoethyls γ-aminopropyltrimethoxysilane, 0.25 part of dibutyltin diacetate.
The preparation method of above-mentioned ketoxime removing type silicone sealant, includes the following steps:
Above-mentioned raw materials are added in into double-planet equipment, are 0.09MPa in vacuum degree, rotating speed is that chemistry is carried out under 300rpm
90min is reacted, product performance index is shown in Table 1.
Embodiment 5:
A kind of ketoxime removing type silicone sealant of the present embodiment, in parts by weight, is made of the following raw material:
100 parts of polysiloxanediol, 60 parts of dimethicone, 20 parts of gas-phase silica are carried on receiving on basic zirconium phosphate
2 parts of rice silver, 0.5 part of 5- chloro-2-methyl -4- isothiazole beautiful jade -3- ketone, 6 parts of methyl three (methylisobutylketone oximido) silane, vinyl
Three 2 parts of (methylisobutylketone oximido) silane, 1.5 parts of N- β aminoethyls gamma-aminopropyl-triethoxy-silane, di lauric dibutyl
0.5 part of tin.
The preparation method of above-mentioned ketoxime removing type silicone sealant, includes the following steps:
Above-mentioned raw materials are added in into double-planet equipment, are 0.0MPa in vacuum degree, rotating speed is that chemistry is carried out under 300rpm
90min is reacted, product performance index is shown in Table 1.
Comparative example 1:
A kind of ketoxime removing type silicone sealant of this comparative example, in parts by weight, is made of the following raw material:
100 parts of polysiloxanediol, 60 parts of dimethicone, 20 parts of gas-phase silica are carried on receiving on apatite
Rice silver-colored 1 part, 6 parts of methyl tributanoximo silane, 2 parts of vinyl tributyl ketoximyl silane, gamma-aminopropyl-triethoxy-silane
1.5 parts, 0.25 part of dibutyltin diacetate.
The preparation method of above-mentioned ketoxime removing type silicone sealant, includes the following steps:
Above-mentioned raw materials are added in into double-planet equipment, are 0.09MPa in vacuum degree, rotating speed is that chemistry is carried out under 300rpm
90min is reacted, product performance index is shown in Table 1.
Comparative example 2:
A kind of ketoxime removing type silicone sealant of this comparative example, in parts by weight, is made of the following raw material:
100 parts of polysiloxanediol, 60 parts of dimethicone, 20 parts of gas-phase silica, 1,2- benzisothiazole -3-
1 part of ketone, 6 parts of methyl tributanoximo silane, 2 parts of vinyl tributyl ketoximyl silane, gamma-aminopropyl-triethoxy-silane 1.5
Part, 0.25 part of dibutyltin diacetate.
The preparation method of above-mentioned ketoxime removing type silicone sealant, includes the following steps:
Above-mentioned raw materials are added in into double-planet equipment, are 0.09MPa in vacuum degree, rotating speed is that chemistry is carried out under 300rpm
90min is reacted, product performance index is shown in Table 1.
The ketoxime removing type silicone sealant of embodiment 1-5 and comparative example 1-2 are tested for the property:
Test method is as follows:
1st, surface drying time:It is tested according to method as defined in GB 13477.5-2002;
2nd, shore hardness:It is made according to method as defined in GB 16776-2005 and conserves test sample, according to GB/T
531-2008 is tested using shore A type hardness tester meters;
3rd, curing degree:It is tested according to method as defined in 32369 appendix As -2015 of GB/T;
4th, aging xanthochromia situation:The ketoxime removing type silicone sealant that range estimation embodiment 1-5 and comparative example 1-2 has just been prepared
It is transparence, ketoxime removing type silicone sealant is then placed into 7d in 70 DEG C, glue sample xanthochromia situation is observed after aging, range estimation is sentenced
It is disconnected;
5th, displacement capacity:The regulation of 25 grades of mildewproof sealant is tested according to JC/T 885-2016;
6th, fungicidal properties:Mould proof level estimate is carried out according to method as defined in GB/T 1741-2007;
7th, long-acting mould-proof performance:2 times according to GB/T 1741-2007 regulation test periods carry out mould proof level estimate.
The performance comparison of 1 each embodiment and comparative example of table
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, it is all considered to be the range of this specification record.
Embodiment described above only expresses the several embodiments of the present invention, and description is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that those of ordinary skill in the art are come
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of ketoxime removing type silicone sealant, which is characterized in that in parts by weight, including the following raw material component:
Wherein, the composition A includes the nano silver being carried on carrier;
The composition B includes thiazole compound.
2. ketoxime removing type silicone sealant according to claim 1, which is characterized in that in parts by weight, including following former
Expect component:
3. ketoxime removing type silicone sealant according to claim 1 or 2, which is characterized in that the carrier include apatite,
At least one of calcium phosphate, basic zirconium phosphate.
4. ketoxime removing type silicone sealant according to claim 1 or 2, which is characterized in that the composition B includes 1,2- benzene
And isothiazoline -3- ketone, 2-n- octyl group -4- isothiazoline -3- ketone, 2-methyl-4-isothiazolin-3-one, 5- chloro-2-methyls -
At least one of 4- isothiazole beautiful jade -3- ketone.
5. ketoxime removing type silicone sealant according to claim 1 or 2, which is characterized in that the polysiloxanediol
Structural formula isViscosity is 8~200Pa.s.
6. ketoxime removing type silicone sealant according to claim 1 or 2, which is characterized in that the dimethicone glues
It spends for 0.1~50Pa.s.
7. ketoxime removing type silicone sealant according to claim 1 or 2, which is characterized in that the crosslinking agent is methyl three
Butanone oximino silane, vinyl tributyl ketoximyl silane, propyl tributanoximo silane, phenyl tributanoximo silane, four fourths
Ketoximinosilanes, methyl three (methylisobutylketone oximido) silane, vinyl three (methylisobutylketone oximido) silane, four (methyl is different
Butanone oximido) silane, methyl tri acetylacetonate oximino silane, at least one of vinyl tri acetylacetonate oximino silane.
8. ketoxime removing type silicone sealant according to claim 1 or 2, which is characterized in that the silane coupling agent is chlorine
Propyl-triethoxysilicane, γ-aminopropyltrimethoxysilane, gamma-aminopropyl-triethoxy-silane, N- β aminoethyls γ-ammonia third
Base trimethoxy silane, N- β aminoethyls gamma-aminopropyl-triethoxy-silane, glycidyl triethoxysilane, mercapto propyl front three
At least one of oxysilane.
9. ketoxime removing type silicone sealant according to claim 1 or 2, which is characterized in that the catalyst is two bays
Sour dibutyl tin, dibutyltin diacetate, tin dilaurate dioctyl tin, two (dodecyl sulphur) dibutyl tins, stannous octoate, two
At least one of fourth acetylacetone,2,4-pentanedione tin.
10. the preparation method of claim 1-9 any one of them ketoxime removing type silicone sealants, which is characterized in that including such as
Lower step:
By the polysiloxanediol, dimethicone, composition A, composition B, filler, crosslinking agent, silane coupling agent, catalyst
It is mixed, control vacuum degree is 0.09~0.1MPa, 10~800rpm of rotating speed, stirs 30~180min, you can.
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CN115247037A (en) * | 2021-04-28 | 2022-10-28 | 安徽汇杰新材料科技有限公司 | Novel long-acting mildew-proof adhesive and preparation method thereof |
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CN115247037A (en) * | 2021-04-28 | 2022-10-28 | 安徽汇杰新材料科技有限公司 | Novel long-acting mildew-proof adhesive and preparation method thereof |
CN113773790A (en) * | 2021-09-17 | 2021-12-10 | 北京天山新材料技术有限公司 | High-thixotropy fast-curing silicone sealant and preparation method thereof |
CN113773790B (en) * | 2021-09-17 | 2023-01-10 | 北京天山新材料技术有限公司 | High-thixotropy fast-curing silicone sealant and preparation method thereof |
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Application publication date: 20180622 |