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A kind of high tear strength addition type liquid fluorosilicone rubber and preparation method thereof

A high tear strength, liquid fluorosilicone technology, applied in the field of rubber materials, can solve the problems of oily environment use restrictions, unstable product performance, low physical and mechanical strength of addition-type liquid fluorosilicone rubber, etc., to avoid reactivity ratio and Structural difference, reduction of steric hindrance effect, significant effect of ring-opening copolymerization

Active Publication Date: 2022-07-15
新元化学(山东)股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the small molecular weight, the physical and mechanical strength of addition-type liquid fluorosilicone rubber is low, especially the tear strength is usually only 10-20kN / m, which cannot meet the high tear resistance requirements of modern industry, and limits the product to a certain extent. application
[0004] Patent document CN201110146226.9 discloses a high-strength fluorosilicone rubber compound and its preparation method. Raw materials such as fluorosilicone raw rubber, fluorosilicone rubber crosslinking agent, white carbon black, reinforcing additives, and vulcanizing agents are kneaded It can be mixed evenly on the machine or internal mixer, and the fluorosilicone rubber compound can be obtained after discharging, which solves the problem of unstable product performance caused by uneven distribution of vinyl groups in fluorosilicone raw rubber.
This document uses high molecular weight fluorosilicone raw rubber, which is applied in the field of fluorosilicone compound rubber by peroxide vulcanization, and cannot be used in the field of addition type liquid fluorosilicone rubber.
Patent document CN201811003198.3 discloses an addition-type fluorosilicone rubber composition and its preparation method, fluorosilicone rubber and coating, which uses ethylene dimethylsiloxane copolymerized with trifluoropropylmethylsiloxane chains. Fluorosilicone liquid rubber is used as the base rubber. Due to the introduction of more dimethyl silicone chain links, the base rubber has poor oil resistance and has too many restrictions on the use of oily environments, and the fluorosilicone rubber composition is based on Implemented in the form of a single component, the stability is poor, affecting product quality
Patent document CN201510614864.7 discloses a preparation method of addition-type liquid fluorosilicone rubber, which uses D with a purity greater than 99.5%. 3 F.ViD 4 , MM as raw materials to prepare vinyl fluorosilicone oil, then use it as base rubber to add reinforcing agent, crosslinking agent, catalyst, and then prepare liquid fluorosilicone rubber through kneading, grinding, tableting and other processes. The base is distributed in the main chain of silicone, which is different from the cross-linking effect of the terminal vinyl group. The vinyl group of the molecular side chain will have a certain degree of influence on the mechanical properties of the product after vulcanization, especially the tear strength. The crosslinking density of the liquid fluorosilicone rubber is too high, and the tear strength of the liquid fluorosilicone rubber is poor

Method used

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  • A kind of high tear strength addition type liquid fluorosilicone rubber and preparation method thereof
  • A kind of high tear strength addition type liquid fluorosilicone rubber and preparation method thereof
  • A kind of high tear strength addition type liquid fluorosilicone rubber and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0089] The preparation of high tear resistance additive 1 comprises the following steps:

[0090] (1) Add 3245g of trimethyltris(3,3,3-trifluoropropyl)cyclotrisiloxane (D 3 F), 924g octamethylcyclotetrasiloxane (D) 4 ) and 716g of tetramethyltetravinylcyclotetrasiloxane (D 4 Vi ), stir evenly, dehydrate for 2h at 30~40℃, -0.099MPa to -0.1MPa;

[0091] (2) use nitrogen to restore the pressure, add 130 g of divinyltetramethyldisiloxane (MM Vi ), 3g potassium hydroxide alkali glue (KOH content 4.58%) and 20g dimethyl sulfoxide, the system exotherm has a polymerization phenomenon to occur, and the heating is turned on and slowly heats up, and the system gradually becomes thinner by the colloid during the heating, and continues to be warmed up to The copolymerization reaction was carried out at 90-100°C, and the reaction was maintained for 4h;

[0092] (3) after the reaction is complete, add 3.1g phosphoric acid gum (H 3 PO 4 content 4.12%) to maintain 90~100 ℃ stirring for ...

Embodiment 2

[0097] The preparation of high tear resistance additive 2, comprises the steps:

[0098] (1) Add 2710g of trimethyltris(3,3,3-trifluoropropyl)cyclotrisiloxane (D 3 F), 964g octamethylcyclotetrasiloxane (D) 4 ) and 1120 g of tetramethyltetravinylcyclotetrasiloxane (D 4 Vi ), stir evenly, dehydrate for 2h at 30~40℃, -0.099MPa to -0.1MPa;

[0099] (2) use nitrogen to restore the pressure, add 120 g of divinyltetramethyldisiloxane (MM Vi ), 3g potassium hydroxide alkali glue (KOH content 4.58%) and 18g dimethyl sulfoxide, the system exothermic polymerization phenomenon occurs, and the heating is turned on and slowly heats up, during the heating period, the system gradually becomes thinner by the colloid, and continues to heat up to The copolymerization reaction was carried out at 90-100°C, and the reaction was maintained for 4h;

[0100] (3) after the reaction is complete, add 3.1g phosphoric acid gum (H 3 PO 4 content 4.12%) to maintain 90~100 ℃ stirring for 1h to neutrali...

Embodiment 3

[0104] The preparation of high tear strength addition type liquid fluorosilicone rubber includes the following steps:

[0105] (1) Add 1100g fluorosilicone base rubber I (viscosity 126000mPa.s, vinyl mass fraction 0.12%) and 110g high tear resistance additive 1 (viscosity 318mPa.s, vinyl mass fraction 5.35%) into the vacuum kneader, and then add Hydrophobically modified 660g fumed silica (hexamethyldisilazane, specific surface area 220m 2 / g, carbon content 3.05%) were added in five times, and the kneading interval was 0.5h after each addition, and the heating was turned on, and the material temperature was raised to 180 ° C for kneading and mixing for 1 h, and then 990g of fluorosilicon base rubber II was added to the kneader. (viscosity 30500mPa.s, vinyl mass fraction 0.20%) and pump the system pressure to -0.098MPa and continue kneading for 3h;

[0106] (2) Lower the sizing material to room temperature, and use a three-roll mill to continue thinning the mixed sizing materi...

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Abstract

The invention relates to a high tear strength addition type liquid fluorosilicone rubber and a preparation method thereof. The rubber is formed by mixing two components, A and B, and the A component includes: 40-60 parts of fluorosilicone base rubber I, 37 parts ~54 parts of fluorosilicon base rubber II, 3 to 6 parts of high tear resistance additives, 25 to 30 parts of fumed silica, 1 to 2 parts of platinum catalyst, 1 to 3 parts of heat-resistant additives; component B includes: 40 to 60 parts of fluorosilicone base rubber I, 37 to 54 parts of fluorosilicon base rubber II, 3 to 6 parts of high tear resistance additive, 25 to 30 parts of fumed silica, 6 to 12 parts of fluorosilicon crosslinking agent, 0.1 to 0.5 parts 1 part inhibitor, 1 to 3 parts heat resistant additive. The invention prepares a high tear-resistant additive for addition type fluorosilicone rubber, and then makes the three synergistic effects in the form of high and low viscosity base rubber compounding, and then there is a two-dimension between the side group hydrogen and the main chain silicon-oxygen chain link. The polyfluorosiloxane with methylsiloxane chain structure is used as a cross-linking agent to form cross-linking points with different densities by simultaneous vulcanization, which greatly improves the tear resistance.

Description

technical field [0001] The invention relates to the technical field of rubber materials, in particular to a high tear strength addition type liquid fluorosilicone rubber and a preparation method thereof. Background technique [0002] Addition type liquid fluorosilicone rubber is based on vinyl-containing polyfluorosiloxane as the base polymer, with silicon-hydrogen bond-containing oligofluorosiloxane as the cross-linking agent, under the action of platinum catalyst, through the addition reaction It forms an elastomer with a network structure, has excellent oil resistance, and has a low volume swelling rate in an oily environment. It is very suitable for the production of oil-resistant parts used in the automotive industry, ships, aviation manufacturing and other fields. The addition also has the characteristics of fast and convenient molding, short processing cycle, no by-products in the reaction, and wide operating temperature. [0003] In order to meet the process conditi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L83/08C08K9/06C08K7/26C08K3/22C08G77/24C08G77/06
CPCC08L83/08C08G77/24C08G77/06C08K2003/2213C08L2205/025C08L2205/035C08K9/06C08K7/26C08K3/22
Inventor 于鹏飞杜辉田志钢侯志伟刘晓敏丛洋王华杰
Owner 新元化学(山东)股份有限公司
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