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Phosphorus-containing methyl vinyl flame-retardant silicone rubber crude rubber, preparation method therefor and application thereof

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

Active Publication Date: 2015-10-21
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

AI Technical Summary

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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  • Phosphorus-containing methyl vinyl flame-retardant silicone rubber crude rubber, preparation method therefor and application thereof
  • Phosphorus-containing methyl vinyl flame-retardant silicone rubber crude rubber, preparation method therefor and application thereof
  • Phosphorus-containing methyl vinyl flame-retardant silicone rubber crude rubber, preparation method therefor and application thereof

Examples

Experimental program
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Effect test

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 phosphorus-containing methyl vinyl flame-retardant silicone rubber crude rubber, a preparation method therefor and an application thereof. The material has a following structural unit: FORMULA as shown in the specification, wherein X is 2-4, y is 3-6, z is 300-325 and Mw is equal to 18900-27600. The invention further discloses the preparation method for the phosphorus-containing methyl vinyl flame-retardant silicone rubber crude rubber; linear methyl vinyl phosphorus-containing silicone rubber crude rubber with a 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide structure in a side chain is obtained; compared with conventional addition methyl vinyl flame-retardant silicone rubber, the phosphorus-containing methyl vinyl flame-retardant silicone rubber crude rubber disclosed by the invention has better flame resistance; and problems of high filling volume and low flame resistance efficiency in a conventional flame-retardant rubber blending process are overcome; and physical characteristics such as good tensile strength, good impact strength and the like of the silicone rubber are kept.

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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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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