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A kind of phosphorous methyl vinyl flame retardant silicone rubber raw rubber and its preparation method and application

A silicone rubber raw rubber, methyl vinyl technology, applied in the field of flame retardant silicone rubber, can solve the problems affecting the scope of use, mechanical properties such as tensile strength, impact strength decline, low flame retardant efficiency, etc., to achieve good flame retardant properties, good tensile strength and impact strength, excellent flame retardancy

Active Publication Date: 2017-10-10
湖北省兴发磷化工研究院有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Mg(OH) 2 As an environmentally friendly flame retardant and smoke suppressant, it is widely used in rubber flame retardant. The main disadvantage is that the flame retardant efficiency is low. It is necessary to increase the filling amount to improve the flame retardancy of the entire system. With the increase of the filling amount, its mechanical properties such as tensile strength and impact strength are significantly reduced, which also seriously affects its scope of use.

Method used

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  • A kind of phosphorous methyl vinyl flame retardant silicone rubber raw rubber and its preparation method and application
  • A kind of phosphorous methyl vinyl flame retardant silicone rubber raw rubber and its preparation method and application
  • A kind of phosphorous methyl vinyl flame retardant silicone rubber raw rubber and its preparation method and application

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Embodiment 1

[0040] A kind of phosphorous methyl vinyl flame retardant silicone rubber raw rubber and preparation method thereof, comprises the following steps:

[0041] 1) Add DOPO (3.24g, 0.015mol) into a three-necked flask, under nitrogen protection, add chloroform (3mL), heat up to 65°C, after DOPO is completely dissolved in chloroform, add azobisisobutyronitrile (0.017g), then VMDMS (2.2 mL, 0.015 mol) was added dropwise and the reaction was stirred for 20 h. NaOH solution (6 wt%, 1.2 mL) was added to the product mixture, and stirring was continued at 60 °C for 2 h. Separate the liquid, extract the organic phase, and extract the aqueous phase with chloroform for 2 to 3 times, combine the organic phases, and distill under reduced pressure to obtain a viscous light yellow transparent solid, which is a phosphorus-containing silanol oligomer, with a yield of 85%. FTIR (cm -1 ,KBr):3240cm -1 (OH),3064cm -1 (C-H in phenyl group),2800-3000cm -1 (CH 2 ,CH 3 ),1595cm -1 (phenyl group),...

Embodiment 2

[0044] A kind of phosphorous methyl vinyl flame retardant silicone rubber raw rubber and preparation method thereof, comprises the following steps:

[0045] 1) Add DOPO (6.48g, 0.03mol) into a three-necked flask, under nitrogen protection, add acetonitrile (6mL), heat up to 90°C, after DOPO is completely dissolved in acetonitrile, add azobisisobutyronitrile (0.052g), and then VMDMS (5.3 mL, 0.036 mol) was added dropwise, and the reaction was stirred for 20 h. NaOH solution (5 wt%, 3 mL) was added to the product mixture, and stirring was continued at 60 °C for 2 h. Separate the liquid, extract the organic phase, extract the water phase with acetonitrile for 2 to 3 times, combine the organic phases, and distill under reduced pressure. The obtained viscous light yellow transparent solid is phosphorus-containing silanol oligomer, and the yield is about 88%.

[0046] 2) Add D to a reaction flask equipped with a thermometer and a stirring bar 4 (8g, 0.027mol), D 4 Vi (0.653g, 0...

Embodiment 3

[0048] A kind of phosphorous methyl vinyl flame retardant silicone rubber raw rubber and preparation method thereof, comprises the following steps:

[0049] 1) Add DOPO (10.83g, 0.05mol) into a three-necked flask, under nitrogen protection, add benzene (10mL), raise the temperature to 85°C, after DOPO is completely dissolved in benzene, add azobisisobutyronitrile (0.108g), then VMDMS (11.2 mL, 0.075 mol) was added dropwise and the reaction was stirred for 24 h. NaOH solution (5 wt%, 5.7 mL) was added to the product mixture, and stirring was continued at 60 °C for 2 h. Separate the liquid, extract the organic phase, extract the water phase with benzene for 2 to 3 times, combine the organic phases, and distill under reduced pressure to obtain a viscous light yellow transparent solid that is a phosphorus-containing silanol oligomer with a yield of 93%.

[0050] 2) Add D to a reaction flask equipped with a thermometer and a stirring bar 4 (15g, 0.051mol), D 4 Vi (1.09g, 0.0032...

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Abstract

The invention discloses a novel phosphorus-containing methyl vinyl flame-retardant silicone rubber raw rubber and its preparation method and application. The material has the following structural units: wherein, x is 2-4, y is 3-6, z It is 300‑325, Mw=18900~27600. This paper also discloses the preparation method of the methyl vinyl silicone rubber raw rubber, and a linear formazan with a side chain containing 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide structure is obtained. Phosphorus-based flame retardant silicone rubber raw rubber, compared with traditional additive methyl vinyl flame retardant silicone rubber, the present invention has better flame retardancy, and overcomes the traditional flame retardant rubber blending process The filling amount is large, the flame retardant efficiency is low, and the physical properties such as good tensile strength and impact strength of silicone rubber are retained.

Description

technical field [0001] The invention belongs to the technical field of flame-retardant silicone rubber, and in particular relates to a halogen-free, high-performance, high-efficiency and environment-friendly raw phosphorus-containing methyl vinyl flame-retardant silicone rubber and its preparation method and application. Background technique [0002] A common flame retardant method for silicone rubber materials is to add various flame retardants for blending and flame retardant. This method must be filled with a large amount of fillers to improve the flame retardant performance of the entire system, but at the same time adding a large amount of fillers, it affects various physical properties of the rubber, such as tensile strength, impact strength, etc. are significantly reduced, seriously restricting The application of rubber products in daily life. With the increasing requirements for high-performance, high-efficiency, and environmentally friendly flame-retardant silicone...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/30C08L83/08
Inventor 马会娟张旺李永刚杨桂春陈海平鄢烈祥艾聪
Owner 湖北省兴发磷化工研究院有限公司
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