CN103627182B - The liquid silastic of a kind of low compression set and preparation method - Google Patents
The liquid silastic of a kind of low compression set and preparation method Download PDFInfo
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- CN103627182B CN103627182B CN201310638771.9A CN201310638771A CN103627182B CN 103627182 B CN103627182 B CN 103627182B CN 201310638771 A CN201310638771 A CN 201310638771A CN 103627182 B CN103627182 B CN 103627182B
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Abstract
The present invention relates to liquid glue of a kind of low compression set and preparation method thereof, it is mixed by a certain percentage by the quality of component A and B component and forms；Wherein, component A is made up of 100 parts of liquid silicon rubber sizings and 0.2 0.5 parts of catalyst, and B component is made up of 100 parts of liquid silicon rubber sizings, 6 25 parts of cross-linking agent and 0.1 0.3 parts of inhibitor.
Description
Technical field
The present invention relates to liquid silastic and the preparation method of a kind of low compression set, have low after referring mainly to molding
Compression set, high resilience, the liquid silastic goods of soft, belong to add-on type liquid silicon rubber technical field.
Background technology
Owing to liquid silastic has high-low temperature resistant, ultraviolet resistance, radiation hardness, weather-proof, electric insulation, highly-breathable, physiology
The performance that inertia etc. are excellent, has therefore obtained extensively at aspects such as Aeronautics and Astronautics, electronic apparatus, chemical industry, machinery, medical science, article of everyday use
Apply generally.The rubber roll silicone rubber being applied on the devices such as laser printer, photocopier, facsimile machine and ATM requires to have low
The performances such as hardness, low compression set, dimensional stability.
The crosslinked elastomer that obtains has the compositions that low compression becomes forever and is early described.US2008287603A1 adds nothing
Machine acidizer, adds 10 parts of calcium carbonate and reduces the compression set of goods, and the goods prepared not only compress forever
Deformation is unstable, rubber mobility is poor, and Article Stiffness Determination is too high.EP432761 describes the peroxide being added with a kind of alkenyl
The silicone elastomer of compound crosslinking.Its shortcoming is that with the addition of this peroxide containing alkenyl can affect the hard of goods
Degree.EP-A415180 describes the organosiloxane of the peroxide crosslinking using cerium compound or Magnesium dioxide.Institute in patent
The Main Function stating cerium compound is that ageing-resistant, the Magnesium dioxide of raising goods are to improve the oil resistivity of goods.They
Add and simply compression set is played the least effect.EP0581504A2 adds containing alkyl titanate.Alkane described in patent
Base titanate simply improves the adhesive force of goods, and compression set is not had too much influence.These compositionss all can not be same
Time meet low compression set, soft and dimensional stability.
For an existing difficult problem, the beneficial effects of the present invention is: the end-vinyl containing multiple vinyl chain links with centre gathers
Polysiloxanes be main body to improve compression set, add partial filler carry out reinforcement, and other auxiliary agents of specific use
As added antiager etc., occur addition anti-under the effect of platinum catalyst by the polydimethylsiloxanes blocked to add hydrogen
Should, prepare a kind of liquid silastic with low compression set, soft.Wherein by adding hydrogeneous mole
It is the hardness that 0.6:1～0.8:1 realizes reducing goods with the ratio of the mole of vinyl, and don't affects the permanent change of its compression
Shape.
Summary of the invention
One to be solved by this invention technical problem is that: providing a kind of soft, compression set is little, resilience is high
Add-on type liquid silicon rubber sizing material and preparation method thereof.
A kind of low compression set liquid silastic that the present invention provides, including following component:
1) component (A): 100 parts of liquid silicon rubber sizings, 0.2-0.5 part catalyst；
2) component (B): 100 parts of liquid silicon rubber sizings, 4-25 part cross-linking agent, 0.01-0.3 part inhibitor；
Liquid silicon rubber sizing described in component (A) and component (B) is by 100 parts of vinylsiloxanes (a), 5-30
Part filler (b), 0.5-5 part auxiliary agent (c) composition, wherein vinyl polysiloxane (a), its structural formula such as following formula 1:
[wherein, R=C2H3；M, n are integer, m=500～2000, n=4～20]
In component (B), cross-linking agent is the containing hydrogen silicone oil of hydrogen end-blocking, and hydrogen content is 0.01-1.0%, preferably 0.02-
0.1%,
Structural formula such as following formula 2:
[wherein, R1=H, R2=CH3Or C6H5, m, n are integer, m=10～100, n=0～15]
Present invention additionally comprises the preparation method of a kind of described liquid silicon rubber sizing, comprise the steps:
1) 50 parts of vinylsiloxanes (a), 5-30 part filler (b) and 0.5-5 part auxiliary agent (c) are mixed in vacuum kneader
Close 2-3 hour；
2) it is warming up to 150-170 DEG C and adds hot milling 3-5 hour；
3) add 50 parts of vinyl polysiloxane (a) after cooling to mix 0.5-1 hour, be uniformly dispersed.
The present invention farther includes the preparation method of aforesaid liquid silicone rubber, specifically includes:
1) prepare component (A) and component (B) according to component (A) and the composition of (B) and formula, stir respectively, vacuum
Deaeration, filters；
2) by component (A) and (B) quality mix homogeneously according to a certain percentage, be heating and curing prepared liquid silicon rubber material.
The hydrogen content of containing hydrogen silicone oil and vinyl polysiloxane in mesolow compression permanent deformation liquid silastic of the present invention
The mol ratio of contents of ethylene is 0.6-0.8:1.
Described inhibitor is the one in alkynol compound, including 1--acetylene-1-Hexalin, 3-methyl isophthalic acid-butine-
3-alcohol, 3,5-dimethyl-1-hexin-3-alcohol, 3-Phenyl-1-butyn-3-ol.
Described catalyst is platinum catalyst.
Described filler (b) be mean diameter be the fume colloidal silica of 20-200 nanometer, precipitated silica, wollastonite powder
Any or two or more mixing.
Described auxiliary agent (c) is in hexamethyldisiloxane, vinyl silazane, hydroxyvinyl silicone oil, hydroxy silicon oil
Any one or more.
The present invention contains the poly-polysiloxanes of end-vinyl of multiple vinyl chain links and improves compression forever for main body with centre
Deformation, adds partial filler and carries out reinforcement, and other auxiliary agents of specific use such as add antiager, such as ferrum oxide, oxidation
Cerium, magnesium oxide etc., occur addition anti-by the polysiloxanes blocked to add hydrogen acting on of platinum catalyst under heating condition
Should, prepare a kind of liquid silastic with low compression set, soft.Wherein by adding hydrogeneous mole
It is the hardness that 0.6:1～0.8:1 realizes reducing goods with the ratio of the mole of vinyl, and don't affects the permanent change of its compression
Shape.The liquid silicon rubber material of the present invention has that compression set is little, hardness is low after molding, rebound degree advantages of higher.
Detailed description of the invention
Below by embodiment, present aspect done concrete description, it is necessary to it is pointed out here that be that following example are served only for
The present invention is further described, it is impossible to be interpreted as limiting the scope of the invention, the person skilled in the art in this field
Nonessential improvement and adjustment can be made according to the present invention.
The preparation of sizing: by 50 parts of vinyl polysiloxane (a) and 5-30 part filler (b) and 0.5-5 part auxiliary agent (c)
Vacuum kneader mixes 2-3 hour, is warming up to 150-170 DEG C and adds hot milling 3-5 hour, after cooling, add residue 50 parts
Vinyldimethicone (a) mixes 0.5-1 hour, prepares liquid silicon rubber sizing.
The composition of liquid silastic: by the sizing of 100 parts of above-mentioned preparations, the mixing of 0.2-0.5 part platinum catalyst, stirring
Uniformly, vacuum defoamation, filter to obtain component (A)；100 parts of sizings and 4-25 part cross-linking agent and 0.01-0.3 part inhibitor are mixed
Conjunction stirs, vacuum defoamation, filters to obtain component (B).And (B) quality mix homogeneously according to a certain percentage (A), injection, heating
Curing molding, detection.
Detection: (1) viscosity: use digital display viscosity meter；
(2) hardness: 170 DEG C, molding in 5 minutes make 6mm thickness hardness bar, use Asker C Durometer measurements；
(3) compression becomes forever: make diameter 25mm, the test block of thickness 12.5mm, first places 4h at 200 DEG C of baking ovens, then
Being compressed to 9.5mm thickness with compression clamp and be positioned over 180 DEG C of baking oven 22h, it is H that cooling records products thickness after half an hour, its pressure
Contracting becomes (12.5-H)/(12.5-9.5) * 100 forever
Example below is all according to the preparation of above-mentioned preparation method and detection.
Embodiment 1
Sizing formula (1):
| Formula | Vinyl polysiloxane | Filler | Auxiliary agent |
| Type | Viscosity 50,000 centipoise contents of ethylene 0.8% | Precipitated silica | Hexamethyldisiloxane |
| Mark | 100 | 30 | 6 |
Liquid silicone rubber formulation:
| Formula | Sizing | Platinum catalyst | Cross-linking agent | Inhibitor |
| Type | Formula (1) | Karst catalyst | Hydrogen content 0.05% | Ethynylcyclohexanol |
| Mark | 100 | 0.2 | 11 | 0.1 |
Embodiment 2
Sizing formula:
| Formula | Vinyl polysiloxane | Filler | Auxiliary agent |
| Type | Viscosity 50,000 centipoise contents of ethylene 0.8% | Precipitated silica | Hexamethyldisiloxane |
| Mark | 100 | 40 | 8 |
Liquid silicone rubber formulation:
| Formula | Sizing | Platinum catalyst | Cross-linking agent | Inhibitor |
| Type | Karst catalyst | Hydrogen content 0.05% | Ethynylcyclohexanol | |
| Mark | 100 | 0.2 | 10 | 0.1 |
Embodiment 3
Sizing formula:
| Formula | Vinyl polysiloxane | Filler | Auxiliary agent |
| Type | Viscosity 50,000 centipoise contents of ethylene 0.8% | Aluminium oxide | KH-560 |
| Mark | 100 | 40 | 1 |
Liquid silicone rubber formulation:
| Formula | Sizing | Platinum catalyst | Cross-linking agent | Inhibitor |
| Type | Karst catalyst | Hydrogen content 0.05 | Ethynylcyclohexanol | |
| Mark | 100 | 0.2 | 10 | 0.1 |
Embodiment 4
Sizing formula:
| Formula | Vinyl polysiloxane | Filler | Auxiliary agent |
| Type | Viscosity 50,000 centipoise contents of ethylene 1.0% | Aluminium oxide | KH-560 |
| Mark | 100 | 40 | 1 |
Liquid silicone rubber formulation:
| Formula | Sizing | Platinum catalyst | Cross-linking agent | Inhibitor |
| Type | Karst catalyst | Hydrogen content 0.05% | Ethynylcyclohexanol | |
| Mark | 100 | 0.2 | 12.5 | 0.1 |
Embodiment 5
Sizing formula:
| Formula | Vinyl polysiloxane | Filler | Auxiliary agent |
| Type | Viscosity 50,000 centipoise contents of ethylene 0.8% | Aluminium oxide | KH-560 |
| Mark | 100 | 40 | 1 |
Liquid silicone rubber formulation:
| Formula | Sizing | Platinum catalyst | Cross-linking agent | Inhibitor |
| Type | Karst catalyst | Hydrogen content 0.03% | Ethynylcyclohexanol | |
| Mark | 100 | 0.2 | 16.7 | 0.1 |
Embodiment 6
Sizing formula:
| Formula | Vinyl polysiloxane | Filler | Auxiliary agent |
| Type | Viscosity 50,000 centipoise contents of ethylene 0.8% | Aluminium oxide | KH-560 |
| Mark | 100 | 40 | 1 |
Liquid silicone rubber formulation:
| Formula | Sizing | Platinum catalyst | Cross-linking agent | Inhibitor |
| Type | Karst catalyst | Hydrogen content 0.1% | Ethynylcyclohexanol | |
| Mark | 100 | 0.2 | 5 | 0.1 |
Comparative example 1
Preparation method, detection method ibid implementation is the same.
Sizing formula:
| Formula | Vinyl polysiloxane | Filler | Auxiliary agent |
| Type | Viscosity 50,000 centipoise contents of ethylene 0.23% | Precipitated silica | Hexamethyldisiloxane |
| Mark | 100 | 30 | 6 |
Liquid silicone rubber formulation:
| Formula | Sizing | Platinum catalyst | Cross-linking agent | Inhibitor |
| Type | Karst catalyst | Hydrogen content 0.1% | Ethynylcyclohexanol | |
| Mark | 100 | 0.2 | 3.5 | 0.1 |
Comparative example 2
Sizing formula:
| Formula | Vinyl polysiloxane | Filler | Auxiliary agent |
| Type | Viscosity 50,000 centipoise contents of ethylene 0.23% | Precipitated silica | Hexamethyldisiloxane |
| Mark | 100 | 30 | 6 |
Liquid silicone rubber formulation:
| Formula | Sizing | Platinum catalyst | Cross-linking agent | Inhibitor | Multi-vinyl silicone oil |
| Type | Karst catalyst | Hydrogen content 0.1% | Ethynylcyclohexanol | Contents of ethylene 10% | |
| Mark | 100 | 0.2 | 9 | 0.1 | 4 |
Comparative example 3
Sizing formula:
Liquid silicone rubber formulation:
Comparative example 4
Sizing formula:
| Formula | Vinyl polysiloxane | Filler | Auxiliary agent |
| Type | Viscosity 5000 centipoise contents of ethylene 0.46% | Aluminium oxide | KH-560 |
| Mark | 100 | 40 | 1 |
Liquid silicone rubber formulation:
| Formula | Sizing | Platinum catalyst | Cross-linking agent | Inhibitor |
| Type | Karst catalyst | Hydrogen content 0.1% | Ethynylcyclohexanol | |
| Mark | 100 | 0.2 | 7 | 0.1 |
Embodiment 1-6 and comparative example 1-4 detection data such as following table:
Claims (8)
1. a low compression set liquid silastic, including following component:
1) component (A): 100 parts of liquid silicon rubber sizings, 0.2-0.5 part catalyst；
2) component (B): 100 parts of liquid silicon rubber sizings, 4-25 part cross-linking agent, 0.01-0.3 part inhibitor；
It is characterized in that, described liquid silicon rubber sizing is filled out by 100 parts of vinyldimethicone (a), 5-30 part
Material (b), 0.5-5 part auxiliary agent (c) composition, wherein the viscosity of vinyldimethicone (a) is 10000-100000mPa
S, contents of ethylene is 0.5-2%, its structural formula such as:
Wherein, R=C2H3；M, n are integer, m=500-2000, n=4-20；
Described cross-linking agent be hydrogen end-blocking containing hydrogen silicone oil, hydrogen content is 0.01-1.0%, structural formula such as:
Wherein, R1=H, R2=CH3Or C6H5, m, n are integer, m=10-100, n=0-15；Described containing hydrogen silicone oil hydrogen content
It is 0.6-0.8: 1 with the mol ratio of vinyldimethicone contents of ethylene.
2. the preparation method of a liquid silicon rubber sizing as claimed in claim 1, it is characterised in that include walking as follows
Rapid:
1) 50 parts of vinyldimethicone (a) as claimed in claim 1,5-30 part filler (b) and 0.5-5 part are helped
Agent (c) mixes 2-3 hour in vacuum kneader；
2) it is warming up to 150-170 DEG C and adds hot milling 3-5 hour；
3) add 50 parts of vinyldimethicone (a) after cooling to mix 0.5-1 hour, be uniformly dispersed.
3. the preparation method of a liquid silastic as claimed in claim 1, it is characterised in that including:
1) component (A) described in claim 1 and (B) are stirred respectively, vacuum defoamation, filter；
2) by component (A) and (B) according to 1: 1 mix homogeneously, be heating and curing prepared liquid silicon rubber material.
4. liquid silastic as claimed in claim 1, it is characterised in that inhibitor is the one in alkynol compound, including
1-acetenyl-1-Hexalin, 3-methyl isophthalic acid-butine-3-alcohol, 3,5-dimethyl-1-hexin-3-alcohol, 3-phenyl-ethyl acetylene-3-
Alcohol.
5. liquid silastic as claimed in claim 1, it is characterised in that described catalyst is platinum catalyst.
6. liquid silastic as claimed in claim 1, it is characterised in that described containing hydrogen silicone oil, hydrogen content is 0.02-0.1%.
7. as claimed in claim 2 method, it is characterised in that described filler (b) be mean diameter be the vapor phase method of 20-200 nanometer
White carbon, precipitated silica, any one of wollastonite powder or two or more mixing.
8. as claimed in claim 2 method, it is characterised in that described auxiliary agent (c) be hexamethyldisiloxane, vinyl silazane,
Any one of hydroxyvinyl silicone oil, hydroxy silicon oil or several.
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| CN104098916A (en) * | 2014-07-29 | 2014-10-15 | 东莞兆舜有机硅新材料科技有限公司 | Addition type ultra-soft silicone rubber, as well as preparation method and application thereof |
| CN104371326B (en) * | 2014-11-27 | 2016-02-17 | 深圳市森日有机硅材料有限公司 | A kind of preparation method of liquid silicon rubber composition |
| CN105985646A (en) * | 2015-02-05 | 2016-10-05 | 镇江高美新材料有限公司 | Bicomponent low-hardness silicone rubber and preparation method therefor |
| CN105419341B (en) * | 2015-12-15 | 2018-04-10 | 江苏天辰新材料股份有限公司 | A kind of low compression set silicon rubber and preparation method thereof and application method |
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| CN105968819A (en) * | 2016-05-12 | 2016-09-28 | 浙江新安化工集团股份有限公司 | Key liquid silicone rubber composition with ultralong striking life and preparation method of key liquid silicone rubber composition |
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| CN108219671A (en) * | 2018-01-11 | 2018-06-29 | 佛山市天宝利硅工程科技有限公司 | A kind of bi-component addition type liquid silastic and preparation method thereof |
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| CN110606986B (en) * | 2019-09-20 | 2020-05-22 | 杭州聚丰新材料有限公司 | Silicone rubber cross-linking agent, and preparation method and application thereof |
| CN110684358A (en) * | 2019-10-14 | 2020-01-14 | 东莞市跨越电子有限公司 | Filling foaming encapsulation silica gel for new energy power battery, preparation method and application |
| CN112852167B (en) * | 2021-01-12 | 2023-04-28 | 江西蓝星星火有机硅有限公司 | Low-hardness transparent liquid silicone rubber composition with low compression deformation, and preparation method and application thereof |
| CN114479466A (en) * | 2021-12-17 | 2022-05-13 | 江阴市鸿萌橡塑制品有限公司 | High-resilience high-wear-resistance peristaltic pump tube and manufacturing method thereof |
| CN114479467A (en) * | 2021-12-18 | 2022-05-13 | 航天长屏科技有限公司 | Ultra-soft high-resilience electromagnetic shielding rubber and preparation method thereof |
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| US5717010A (en) * | 1992-01-23 | 1998-02-10 | General Electric Company | Low compression set silicone elastomers |
| CN101983989B (en) * | 2010-11-01 | 2012-03-28 | 深圳市森日有机硅材料有限公司 | Liquid silicon rubber composition and preparation method thereof |
| CN102876046B (en) * | 2012-07-31 | 2014-01-15 | 深圳市森日有机硅材料有限公司 | Liquid silicon rubber composition and preparation method thereof |
| CN102936484A (en) * | 2012-11-21 | 2013-02-20 | 江苏创景科技有限公司 | Double-component low-hardness high-heat-conductivity room-temperature-curing organosilicon heat conducting adhesive |
| CN102936415B (en) * | 2012-11-22 | 2013-12-25 | 深圳市森日有机硅材料有限公司 | Liquid silicone rubber composition having low permanent compression deformation and preparation method thereof |
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