Preparation method of addition type liquid fluorinated silicone rubber

Abstract

The invention relates to a preparation method of addition type liquid fluorinated silicone rubber. D3F, ViD4 and MM with the purity larger than 99.5% are adopted as raw materials and evenly mixed according to a certain ratio, and vinyl fluorosilicone oil is obtained; the vinyl fluorosilicone oil is used as base gum, a reinforcement agent, a cross-linking agent and a catalyst are added in the vinyl fluorosilicone oil, kneading, grinding, tabletting and other technologies are performed, and the liquid fluorinated silicone rubber (FSR) is obtained; the insulation performance, hydrophobic property, the high-temperature resistance and the like of the LSR are better than that of liquid silicone rubber (LSR) with the same technology and formula. The preparation method is short in production period, the product has the good heat tear resistance, demolding is convenient, various machining ways of mold pressing, extrusion, injection molding and the like can be achieved, and automatic production materials can be achieved.

Description

technical field

[0001] The invention belongs to the technical field of new chemical materials, and in particular relates to a preparation method of addition-type liquid fluorosilicone rubber. Background technique

[0002] Silicone materials have excellent high and low temperature resistance (-60°C to 310°C), superior physical and mechanical properties at high temperatures, aging resistance, and self-extinguishing properties; while fluorocarbon materials have good thermal stability (-27°C to 300°C), has extremely superior oil resistance and solvent resistance. However, with the continuous development of industrial technology, silicone materials have gradually exposed their shortcomings of poor oil resistance and solvent resistance, while organic fluorine materials have defects of poor low temperature resistance and difficult processing.

[0003] Liquid Fluorosilicone Rubber (Liquid Fluorosilicone Rubber referred to as FSR) is also known as fluorinated polysiloxane. It is ...

Examples

preparation example Construction

[0035] A preparation method of addition-type liquid fluorosilicone rubber, comprising the steps of:

[0036] 1) Synthesis of base rubber: Synthesis of base rubber: the raw material D 3 F.ViD 4 Mix 60-70 parts, 0.4-0.5 parts and 0.2-0.3 parts of MM with MM in a three-necked flask, remove low boilers under reduced pressure at 50°C-70°C, and add 0.2-0.4 parts by mass of Catalyst, filled with nitrogen as a protective gas, the reaction temperature is 60 ℃ ~ 80 ℃, the reaction time is 40min ~ 60min, and the homopolyvinyl fluorosilicone oil is the base rubber, and the vinyl content in the base rubber is 0.02mol% ~ 1mol %, trifluoropropyl content is 20mol%~50mol%; Described catalyst is alkali glue;

[0037] 2) Reinforcement of base rubber: mix 100 parts by mass of base rubber and 10-70 parts of reinforcing agent, and knead in vacuum at 120°C-140°C for 3h-6h to form a uniformly mixed compound; The mixed material is passed through a three-roll machine until there are no visible parti...

Embodiment 1

[0052] Addition-type liquid fluorosilicone rubber is prepared as follows:

[0053] 1) Synthesis of the base rubber: the raw material D 3 F.ViD 4 Mix 62 parts, 0.4 parts and 0.2 parts of MM with a three-necked flask by mass parts, remove low boilers under reduced pressure at 65°C, add catalyst alkali gel with a mass part of 0.23, and fill with nitrogen as a protective gas. Make the reaction temperature at 65°C, the reaction time is 45min, and the monomer D 3 F is converted into a linear polymer, which ends before the linear polymer transforms into a stable tetracyclic body, thereby obtaining vinyl fluorosilicone oil with a higher conversion rate; the reaction temperature is 65 ° C, and the activity temperature of the catalyst alkali gel is lower than that of cesium hydroxide (70 °C), a higher temperature will result in a wider molecular weight distribution of the product.

[0054] 2) Reinforcement of the base rubber: mix the base rubber and the reinforcing agent white carbon...

Embodiment 2

[0060] Addition-type liquid fluorosilicone rubber is prepared as follows:

[0061] 1) Synthesis of the base rubber: the raw material D 3 F.ViD 4Mix 69 parts, 0.48 parts and 0.28 parts of MM with MM in a three-necked flask, remove low boilers under reduced pressure at 68°C, add alkali gum with a mass part of 0.4, fill with nitrogen as a protective gas, and make the reaction The temperature is 76°C, and the reaction time is 55 minutes;

[0062] 2) Reinforcement of the base rubber: mix the base rubber and the reinforcing agent white carbon black in parts by mass of 100 parts and 50 parts, knead in vacuum at 140°C for 6 hours to form a uniformly mixed mixture; pass the mixture through three The roll machine is thinly passed until there are no visible particles, and the reinforced base rubber is obtained;

[0063] 3) Cross-linking and curing of addition-type liquid fluorosilicone rubber: Mix the reinforcing base rubber, cross-linking agent, catalyst and polymerization inhibitor ...

technical field

[0001] The invention belongs to the technical field of new chemical materials, and in particular relates to a preparation method of addition-type liquid fluorosilicone rubber. Background technique

[0002] Silicone materials have excellent high and low temperature resistance (-60°C to 310°C), superior physical and mechanical properties at high temperatures, aging resistance, and self-extinguishing properties; while fluorocarbon materials have good thermal stability (-27°C to 300°C), has extremely superior oil resistance and solvent resistance. However, with the continuous development of industrial technology, silicone materials have gradually exposed their shortcomings of poor oil resistance and solvent resistance, while organic fluorine materials have defects of poor low temperature resistance and difficult processing.

[0003] Liquid Fluorosilicone Rubber (Liquid Fluorosilicone Rubber referred to as FSR) is also known as fluorinated polysiloxane. It is ...

Examples

preparation example Construction

[0035] A preparation method of addition-type liquid fluorosilicone rubber, comprising the steps of:

[0036] 1) Synthesis of base rubber: Synthesis of base rubber: the raw material D 3 F.ViD 4 Mix 60-70 parts, 0.4-0.5 parts and 0.2-0.3 parts of MM with MM in a three-necked flask, remove low boilers under reduced pressure at 50°C-70°C, and add 0.2-0.4 parts by mass of Catalyst, filled with nitrogen as a protective gas, the reaction temperature is 60 ℃ ~ 80 ℃, the reaction time is 40min ~ 60min, and the homopolyvinyl fluorosilicone oil is the base rubber, and the vinyl content in the base rubber is 0.02mol% ~ 1mol %, trifluoropropyl content is 20mol%~50mol%; Described catalyst is alkali glue;

[0037] 2) Reinforcement of base rubber: mix 100 parts by mass of base rubber and 10-70 parts of reinforcing agent, and knead in vacuum at 120°C-140°C for 3h-6h to form a uniformly mixed compound; The mixed material is passed through a three-roll machine until there are no visible parti...

Embodiment 1

[0052] Addition-type liquid fluorosilicone rubber is prepared as follows:

[0053] 1) Synthesis of the base rubber: the raw material D 3 F.ViD 4 Mix 62 parts, 0.4 parts and 0.2 parts of MM with a three-necked flask by mass parts, remove low boilers under reduced pressure at 65°C, add catalyst alkali gel with a mass part of 0.23, and fill with nitrogen as a protective gas. Make the reaction temperature at 65°C, the reaction time is 45min, and the monomer D 3 F is converted into a linear polymer, which ends before the linear polymer transforms into a stable tetracyclic body, thereby obtaining vinyl fluorosilicone oil with a higher conversion rate; the reaction temperature is 65 ° C, and the activity temperature of the catalyst alkali gel is lower than that of cesium hydroxide (70 °C), a higher temperature will result in a wider molecular weight distribution of the product.

[0054] 2) Reinforcement of the base rubber: mix the base rubber and the reinforcing agent white carbon...

Embodiment 2

[0060] Addition-type liquid fluorosilicone rubber is prepared as follows:

[0061] 1) Synthesis of the base rubber: the raw material D 3 F.ViD 4Mix 69 parts, 0.48 parts and 0.28 parts of MM with MM in a three-necked flask, remove low boilers under reduced pressure at 68°C, add alkali gum with a mass part of 0.4, fill with nitrogen as a protective gas, and make the reaction The temperature is 76°C, and the reaction time is 55 minutes;

[0062] 2) Reinforcement of the base rubber: mix the base rubber and the reinforcing agent white carbon black in parts by mass of 100 parts and 50 parts, knead in vacuum at 140°C for 6 hours to form a uniformly mixed mixture; pass the mixture through three The roll machine is thinly passed until there are no visible particles, and the reinforced base rubber is obtained;

[0063] 3) Cross-linking and curing of addition-type liquid fluorosilicone rubber: Mix the reinforcing base rubber, cross-linking agent, catalyst and polymerization inhibitor ...