CN104109504A - Deeply-cured ketoxime type single-component room-temperature vulcanized silicon rubber and preparation method thereof - Google Patents
Deeply-cured ketoxime type single-component room-temperature vulcanized silicon rubber and preparation method thereof Download PDFInfo
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- CN104109504A CN104109504A CN201410323853.9A CN201410323853A CN104109504A CN 104109504 A CN104109504 A CN 104109504A CN 201410323853 A CN201410323853 A CN 201410323853A CN 104109504 A CN104109504 A CN 104109504A
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Abstract
The invention discloses a deeply-cured ketoxime type single-component room-temperature vulcanized silicon rubber which comprises the following components in parts by mass: 35-80 parts of hydroxyl-terminated poly-dimethyl siloxane, 25-80 parts of filler, 2-10 parts of plasticizer, 1-8 parts of crosslinking agent, 0.1-5 parts of tackifier, 0.01-1 part of catalyst, 0.1-5 parts of deep curing accelerator and 1-10 parts of color paste. Compared with the prior art, the deeply-cured ketoxime type single-component room-temperature vulcanized silicon rubber has the advantages that the deep curing is greatly improved, the curing depth is greater than 5mm for 24 hours, the rubber is free from corroding base materials of stone, glass, metal and the like, good in binding property and low in energy consumption during production process and has no three wastes and no environmental pollution.
Description
[technical field]
The invention belongs to construction sealing materials category, particularly the technical field of single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type and preparation method thereof.
[background technology]
Room temperature vulcanized silicone rubber is because have good dielectric properties, chemical property, well heat-resisting, weathering resistance and bonding strength, can be in the scope of-65～232 DEG C the premium properties such as life-time service, become widely used a kind of sealing material, be called as liquid packing.
Press composition, sulfuration mechanism different with operation, room temperature vulcanized silicone rubber can be divided into single-component, bicomponent condensed type room temperature sulfidization silicon rubber and dual composition addition type room temperature vulcanized silicone rubber.The sulfuration of single-component room temperature vulcanized silicon rubber is undertaken by absorbing airborne moisture, and curing time depends on the thickness of vulcanization system, temperature, humidity and silastic-layer.Sulfuration is from outward appearance to inner essence carried out, and deeply-curing is slow.The sulfuration of double component room temperature vulcanization silicon rubber causes by catalyzer, can carry out on surface and inside simultaneously, can deeply-curing.Curing time can be by catalyst levels control.The curing time of addition type room temperature vulcanized silicone rubber depends primarily on temperature, therefore, utilizes temperature can control its vulcanization rate.
[summary of the invention]
Object of the present invention solves the problems of the prior art exactly, proposes the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type, can overcome the slow problem of single-component room temperature vulcanized silicon rubber deeply-curing in the market.
For achieving the above object, the present invention proposes the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type, comprise that following component and each constituent mass ratio are: hydroxyl-terminated injecting two methyl siloxane: 35～80 parts, filler: 35～80 parts, softening agent: 2～10 parts, linking agent: 1～8 part, tackifier: 0.1～5 part, catalyzer: 0.01～1 part, deeply-curing promotor: 0.1～5 part, mill base: 1～10 part.
As preferably, the viscosity of described hydroxyl-terminated injecting two methyl siloxane in the time that temperature is 25 DEG C is 10000～80000 centipoises.
As preferably, described filler is at least one or two the above mixtures in gas-phase silica, precipitated silica, light calcium carbonate or water-ground limestone, and described light calcium carbonate is nm-class active calcium carbonate.
As preferably, described softening agent is at least one or two the above mixtures in dibutyl phthalate, dioctyl phthalate (DOP), Dinonylphthalate or the different ester of phthalic acid two.
As preferably, described linking agent is at least one or two the above mixtures in dimethyl two Diacetylmonoxime base silanes, methyl tributanoximo silane, vinyl tributyl ketoximyl silane, phenyl tributanoximo silane, propyl group tributanoximo silane or four Diacetylmonoxime base silanes.
As preferably, described tackifier are at least one or two the above mixtures in γ-aminopropyl triethoxysilane, γ-(2,3-glycidoxy) propyl trimethoxy silicane, N-β-aminoethyl-γ-aminopropyltrimethoxysilane or anilinomethyl triethoxysilane.
As preferably, described catalyzer is at least one or two above mixtures in dibutyltin diacetate, dibutyl tin laurate, isopropyl titanate, tetrabutyl titanate, ethylacetoacetate titanium inner complex.
As preferably, described deeply-curing promotor is at least one or two above mixtures in ketone compounds, etheric acid compounds, Carbox amide.
For achieving the above object, the invention allows for the preparation method of the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type, comprise the following steps successively:
1) prepare base-material:
A) after 35～80 parts of hydroxyl-terminated injecting two methyl siloxanes and 35～80 parts of fillers are dropped into kneaders stirring, vacuumize-0.06～-0.1MPa, stir 20～40min;
B) add 2～10 parts of softening agent, vacuumize-0.06～-0.1MPa, stir 20～40min;
C) base-material preparing is proceeded to planet machine for subsequent use.
2) prepare the single-component room temperature vulcanized silicon rubber of deeply-curing ketoxime type:
A) in planet machine, add 1～10 part of mill base and step 1) in the base-material mix and blend for preparing, vacuumize-0.06～-0.1MPa, stir 20～40min;
B) 1～8 part of linking agent is added to planetary mixer, vacuumize-0.06～-0.1MPa, stir 20～40min;
C) 0.1～5 part of tackifier, 0.01～1 part of catalyzer are added to planetary mixer, vacuumize-0.06～-0.1MPa, stir 20～40min;
D) 0.1～5 part of deeply-curing promotor is added to planetary mixer, vacuumize-0.06～-0.1MPa, stir 20～40min; Make the single-component room temperature vulcanized silicon rubber of deeply-curing ketoxime type.
Beneficial effect of the present invention:
1, the room temperature vulcanized silicone rubber deeply-curing that prepared by formula provided by the invention is largely increased, and within 24 hours, curing depth is greater than 5mm.
2, the silicon rubber that prepared by the present invention is corrosion-free to base materials such as stone material, glass, metals, and cementability is good.
3, preparation method provided by the invention, in production process, energy consumption is low, produces environmentally safe without the three wastes.
Feature of the present invention and advantage will be elaborated by embodiment.
[embodiment]
Embodiment:
Sample 1:
After 100g viscosity 20000cps (25 DEG C) hydroxyl-terminated injecting two methyl siloxane and 100g nm-class active calcium carbonate are stirred in kneader, vacuumize-0.096～-0.1MPa, stir 20-40min; Unload vacuum, drop into 8g dibutyl phthalate, vacuumize-0.096～-0.1MPa, stir 20-40min; The sizing material making is proceeded to planetary mixer for subsequent use.
Add planetary mixer to mix with the base-material preparing 10g vinyl tributyl ketoximyl silane, vacuumize-0.096～-0.1MPa, stir 20-40min; 2.5g γ-aminopropyl triethoxysilane, 0.1g dibutyl tin dilaurate are added to planetary mixer, vacuumize-0.096～-0.1MPa, stir 20-40min; 1.5g acetic acid acetyl triethyl is added to planetary mixer, vacuumize-0.096～-0.1MPa, stir 20-40min.Obtain paste and be designated as sample 1, test result is as shown in table 1.
Sample 2:
After 100g viscosity 50000cps (25 DEG C) hydroxyl-terminated injecting two methyl siloxane and 80g nm-class active calcium carbonate are stirred in kneader, vacuumize-0.096～-0.1MPa, stir 20-40min; Unload vacuum, drop into 15g dibutyl phthalate, vacuumize-0.096～-0.1MPa, stir 20-40min; The sizing material making is proceeded to planetary mixer for subsequent use.
10g methyl tributanoximo silane is added to planetary mixer, vacuumize-0.096～-0.1MPa, stir 20-40min; Then 1.3gN-β-aminoethyl-γ-aminopropyltrimethoxysilane, 0.1g dibutyl tin dilaurate are added to planetary mixer, vacuumize-0.096～-0.1MPa, stir 20-40min; 1g methane amide is added to planetary mixer, vacuumize-0.096～-0.1MPa, stir 20-40min.Obtain paste and be designated as sample 2, test result is as shown in table 1.
Sample 3:
After 100g viscosity 80000cps (25 DEG C) hydroxyl-terminated injecting two methyl siloxane and 80g nm-class active calcium carbonate are stirred in kneader, vacuumize-0.096～-0.1MPa, stir 20-40min; Unload vacuum, drop into 20g dibutyl phthalate, vacuumize-0.096～-0.1MPa, stir 20-40min; The sizing material making is proceeded to planetary mixer for subsequent use.
2g methyl tributanoximo silane, 8g vinyl tributyl ketoximyl silane are added to planetary mixer, vacuumize-0.096～-0.1MPa, stir 20-40min; Then 1.25g γ-aminopropyl triethoxysilane, 1.25N-β-aminoethyl-γ-aminopropyltrimethoxysilane, 0.1g dibutyl tin dilaurate are added to planetary mixer, vacuumize-0.096～-0.1MPa, stir 20-40min; 1.5g acetic acid acetyl triethyl is added to planetary mixer, vacuumize-0.096～-0.1MPa, stir 20-40min.Obtain paste and be designated as sample 3, test result is as shown in table 1.
Table 1 sample test record
Above-described embodiment is to explanation of the present invention, is not limitation of the invention, any scheme after simple transformation of the present invention is all belonged to protection scope of the present invention.
Claims (9)
1. the single-component room temperature vulcanized silicon rubber of deeply-curing ketoxime type, it is characterized in that: comprise that following component and each constituent mass ratio are: hydroxyl-terminated injecting two methyl siloxane: 35～80 parts, filler: 35～80 parts, softening agent: 2～10 parts, linking agent: 1～8 part, tackifier: 0.1～5 part, catalyzer: 0.01～1 part, deeply-curing promotor: 0.1～5 part, mill base: 1～10 part.
2. the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type as claimed in claim 1, is characterized in that: the viscosity of described hydroxyl-terminated injecting two methyl siloxane in the time that temperature is 25 DEG C is 10000～80000 centipoises.
3. the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type as claimed in claim 1, it is characterized in that: described filler is at least one or two the above mixtures in gas-phase silica, precipitated silica, light calcium carbonate or water-ground limestone, and described light calcium carbonate is nm-class active calcium carbonate.
4. the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type as claimed in claim 1, is characterized in that: described softening agent is at least one or two the above mixtures in dibutyl phthalate, dioctyl phthalate (DOP), Dinonylphthalate or the different ester of phthalic acid two.
5. the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type as claimed in claim 1, is characterized in that: described linking agent is at least one or two the above mixtures in dimethyl two Diacetylmonoxime base silanes, methyl tributanoximo silane, vinyl tributyl ketoximyl silane, phenyl tributanoximo silane, propyl group tributanoximo silane or four Diacetylmonoxime base silanes.
6. the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type as claimed in claim 1, it is characterized in that: described tackifier are at least one or two the above mixtures in γ-aminopropyl triethoxysilane, γ-(2,3-glycidoxy) propyl trimethoxy silicane, N-β-aminoethyl-γ-aminopropyltrimethoxysilane or anilinomethyl triethoxysilane.
7. the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type as claimed in claim 1, is characterized in that: described catalyzer is at least one or two above mixtures in dibutyltin diacetate, dibutyl tin laurate, isopropyl titanate, tetrabutyl titanate, ethylacetoacetate titanium inner complex.
8. the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type as described in any one in claim 1 to 7, is characterized in that: described deeply-curing promotor is at least one or two above mixtures in ketone compounds, etheric acid compounds, Carbox amide.
9. a preparation method for the single-component room temperature vulcanized silicon rubber of deeply-curing ketoxime type, is characterized in that: comprise the following steps successively:
1) prepare base-material:
A) after 35～80 parts of hydroxyl-terminated injecting two methyl siloxanes and 35～80 parts of fillers are dropped into kneaders stirring, vacuumize-0.06～-0.1MPa, stir 20～40min;
B) add 2～10 parts of softening agent, vacuumize-0.06～-0.1MPa, stir 20～40min;
C) base-material preparing is proceeded to planet machine for subsequent use.
2) prepare the single-component room temperature vulcanized silicon rubber of deeply-curing ketoxime type:
A) in planet machine, add 1～10 part of mill base and step 1) in the base-material mix and blend for preparing, vacuumize-0.06～-0.1MPa, stir 20～40min;
B) 1～8 part of linking agent is added to planetary mixer, vacuumize-0.06～-0.1MPa, stir 20～40min;
C) 0.1～5 part of tackifier, 0.01～1 part of catalyzer are added to planetary mixer, vacuumize-0.06～-0.1MPa, stir 20～40min;
D) 0.1～5 part of deeply-curing promotor is added to planetary mixer, vacuumize-0.06～-0.1MPa, stir 20～40min; Make the single-component room temperature vulcanized silicon rubber of deeply-curing ketoxime type.
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Cited By (9)
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| CN106190015A (en) * | 2016-08-22 | 2016-12-07 | 深圳市新亚新材料有限公司 | A kind of no-solvent type organosilicon coating glue and preparation method thereof |
| CN107129790A (en) * | 2017-04-19 | 2017-09-05 | 常熟市恒信粘胶有限公司 | Neutral silicone sealant for stone material |
| CN107142074A (en) * | 2017-05-09 | 2017-09-08 | 江苏天辰新材料股份有限公司 | A kind of preparation method of de-oxime type one component room temperature fluid sealant |
| CN108219739A (en) * | 2017-12-30 | 2018-06-29 | 广州市白云化工实业有限公司 | Single-component ketonic oxime organosilicon adhesive glue of deeply-curing and preparation method thereof |
| CN111205650A (en) * | 2018-11-21 | 2020-05-29 | 王长杰 | Production process flow and formula of high-voltage bare conductor insulating material |
| CN112920764A (en) * | 2021-01-28 | 2021-06-08 | 四川省俊川科技有限公司 | Preparation method of single-component ketoxime-removing type organosilicon sealant for system doors and windows |
| CN113667306A (en) * | 2020-05-15 | 2021-11-19 | 江西蓝星星火有机硅有限公司 | Light diffusion type organic silicon composite material and preparation method thereof |
| CN115785527A (en) * | 2022-12-28 | 2023-03-14 | 佛山市普力达科技有限公司 | Coupling agent for accelerating deep curing, preparation method and transparent RTV (room temperature vulcanized) applied by coupling agent |
| CN115851216A (en) * | 2022-11-29 | 2023-03-28 | 湖北兴瑞硅材料有限公司 | High-thixotropy bi-component room temperature vulcanized silicone rubber and preparation method thereof |
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| CN101565599A (en) * | 2008-05-14 | 2009-10-28 | 广州市回天精细化工有限公司 | Deeply-curing non-corrosive single-component ketonic oxime potting adhesive and preparation method thereof |
| CN102321450A (en) * | 2011-08-23 | 2012-01-18 | 杭州之江有机硅化工有限公司 | Solar energy photovoltaic assembly organosilicon sealant material and preparation method thereof |
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| CN101565599A (en) * | 2008-05-14 | 2009-10-28 | 广州市回天精细化工有限公司 | Deeply-curing non-corrosive single-component ketonic oxime potting adhesive and preparation method thereof |
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| CN106190015B (en) * | 2016-08-22 | 2019-01-15 | 深圳市新亚新材料有限公司 | A kind of no-solvent type organosilicon coating glue and preparation method thereof |
| CN106190015A (en) * | 2016-08-22 | 2016-12-07 | 深圳市新亚新材料有限公司 | A kind of no-solvent type organosilicon coating glue and preparation method thereof |
| CN107129790A (en) * | 2017-04-19 | 2017-09-05 | 常熟市恒信粘胶有限公司 | Neutral silicone sealant for stone material |
| CN107142074A (en) * | 2017-05-09 | 2017-09-08 | 江苏天辰新材料股份有限公司 | A kind of preparation method of de-oxime type one component room temperature fluid sealant |
| CN108219739B (en) * | 2017-12-30 | 2020-11-10 | 广州市白云化工实业有限公司 | Deep-cured single-component ketoxime-removed organic silicon adhesive and preparation method thereof |
| CN108219739A (en) * | 2017-12-30 | 2018-06-29 | 广州市白云化工实业有限公司 | Single-component ketonic oxime organosilicon adhesive glue of deeply-curing and preparation method thereof |
| CN111205650A (en) * | 2018-11-21 | 2020-05-29 | 王长杰 | Production process flow and formula of high-voltage bare conductor insulating material |
| CN113667306A (en) * | 2020-05-15 | 2021-11-19 | 江西蓝星星火有机硅有限公司 | Light diffusion type organic silicon composite material and preparation method thereof |
| CN113667306B (en) * | 2020-05-15 | 2023-02-03 | 江西蓝星星火有机硅有限公司 | Photodiffusion type organic silicon composite material and preparation method thereof |
| CN112920764A (en) * | 2021-01-28 | 2021-06-08 | 四川省俊川科技有限公司 | Preparation method of single-component ketoxime-removing type organosilicon sealant for system doors and windows |
| CN115851216A (en) * | 2022-11-29 | 2023-03-28 | 湖北兴瑞硅材料有限公司 | High-thixotropy bi-component room temperature vulcanized silicone rubber and preparation method thereof |
| CN115785527A (en) * | 2022-12-28 | 2023-03-14 | 佛山市普力达科技有限公司 | Coupling agent for accelerating deep curing, preparation method and transparent RTV (room temperature vulcanized) applied by coupling agent |
| CN115785527B (en) * | 2022-12-28 | 2023-09-12 | 佛山市普力达科技有限公司 | Accelerated deep curing coupling agent, preparation method and transparent RTV (real time kinematic) applied to same |
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Application publication date: 20141022 |