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Amino-containing organic silicon resin fire retardant and preparation method thereof

A silicone and amino-containing technology, which is used in the field of flame retardants and their preparation, can solve the problems of poor thermal stability and flame retardancy, achieve improved mechanical properties and processing properties, less corrosive gases, and inhibit thermal oxidation degradation reactions Effect

Inactive Publication Date: 2011-06-08
QINGDAO UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing amino-functional silicone resins have poor thermal stability and flame retardancy, and cannot meet the existing requirements for high stability and high flame retardancy of flame retardants

Method used

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  • Amino-containing organic silicon resin fire retardant and preparation method thereof
  • Amino-containing organic silicon resin fire retardant and preparation method thereof
  • Amino-containing organic silicon resin fire retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A 2000ml four-neck flask is equipped with a stirrer, a thermometer, a spherical condenser and a 500ml constant pressure funnel, and 300ml deionized water and 300ml xylene mixed solvent are added to prepare 41.2g N-β-aminoethyl-γ-aminopropyl methyl Dimethoxysilane, 16.8g methyltriethoxysilane and 211.2g diphenyldiethoxysilane were mixed evenly and added to the constant pressure funnel, the temperature was controlled at 40°C, and added dropwise to the flask at a constant speed , added dropwise for 40-50 minutes; continued hydrolysis for 6 hours, then added 60ml of 0.1mol / l hydrochloric acid solution for 4 hours of reaction, added 5.0 grams of hexamethyldisilazane, and reacted for 2 hours, then added 40ml of 0.1mol / l hydrogen Sodium oxide solution neutralized the reaction system, filtered, washed and dried to obtain a white resinous solid, which is an amino group-containing silicone resin. The mass is 194.8g, the yield is 92.3%, the number average molecular weight is about...

Embodiment 2

[0026] A 1000ml four-necked flask is equipped with a stirrer, a thermometer, a spherical condenser and a 100ml constant pressure funnel, and in 500ml deionized water and xylene mixed solvent (volume ratio 2: 1), 25.6 grams of aminopropylmethyl dimethyl Oxysilane, 8.4 grams of methyltriethoxysilane, and 106.5 grams of diphenyldiethoxysilane were mixed evenly and added to the constant pressure funnel. The reaction temperature was controlled at 60 ° C, and the solvent was added dropwise at a uniform speed. After 28-32 minutes, the dropwise addition is completed; continue hydrolysis for 3 hours, then add 30ml of 0.1mol / l sodium hydroxide solution, continue the reaction for 4 hours, add 4.0 grams of dimethyltetraphenyldisiloxane, and react for 2 hours, then add 0.1mol / l hydrochloric acid solution 30ml to neutralize the reaction system, filter, wash and dry to obtain a white resinous solid which is an amino group-containing silicone resin. The mass is 94.2 g, the yield is 89.2%, th...

Embodiment 3

[0028] A 1000ml four-neck flask is equipped with a stirrer, a thermometer, a spherical condenser and a 100ml constant pressure funnel, and 500ml of deionized water is added, and 60.4 grams of aminopropyltrimethoxysilane and 118.8 grams of phenyltrimethoxysilane are mixed evenly. Add it into a constant pressure funnel, control the reaction temperature at 50°C, add it dropwise to deionized water at a constant speed, and drop it in 30-45 minutes to complete the dropwise addition; continue hydrolysis for 4 hours, then add 25ml of 0.1mol / l sulfuric acid dilute solution, and continue the reaction for 4 hours Finally, add 4.0 g of dimethyltetraphenyldisiloxane, react for 2 hours, add 50 ml of 0.1 mol / l ammonia solution to neutralize the reaction system, filter, wash and dry to obtain a white resinous solid that is amino-containing organosilicon resin. The mass is 150.9 g, the yield is 88.7%, the number average molecular weight is 14000, and the structure is polysiloxane with branched...

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Abstract

The invention discloses an amino-containing organic silicon resin fire retardant and a preparation method thereof. The preparation method comprises the steps of: with amino silane and trialkoxysilane as raw materials or with amino silane, dialkoxysilane and trialkoxysilane as the raw materials, adding water or a mixed solvent of water and an organic solvent, carrying out hydrolytic polycondensation under the action of a catalyst, finally adding blocking agent to block the end, adding a neutralizer to neutralize before the reaction is finished, and then filtering, washing and drying to obtain the amino-containing organic silicon resin fire retardant. The fire retardant contains two fire-retardant elements of nitrogen and silicon, has with high efficiency and low toxicity and is an environment-friendly macromolecular fire retardant; the chemical structure is shown as follows: wherein R1, R2, R3, R4, and R6 are H, CH3 or C6H5; R5 is CH2, CH2CH2, CH2CH2CH2, CH2NHCH2CH2 or C6H5; R7 and R8 are CH3, C2H5 or C6H5; and n, p, q are integers of 1-50.

Description

technical field [0001] The invention relates to a flame retardant and a preparation method thereof, in particular to an amino group-containing silicone resin flame retardant and a preparation method thereof. Background technique [0002] Flame retardants widely used in plastics, fibers, coatings and other fields are generally divided into two categories: halogen-containing and halogen-free flame retardants. Among them, halogen-free flame retardants are widely used and have better effects, which are in line with the sustainable development strategy of the environment. Silicone-based flame retardant is a new type of halogen-free flame retardant and a carbon-forming smoke suppressant. As a class of polymer flame retardant, it has the characteristics of high efficiency, non-toxic, smoke-free, and pollution-free. Polysiloxane can be divided into two types from the molecular structure, one is linear and the other is branched, both of which can contain aromatic groups and aliphatic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/26C08L23/00C08L69/00C08L55/02C08L77/00C08L67/02C08L71/12C08L59/02C08L83/08
Inventor 吴宁晶牛民卜
Owner QINGDAO UNIV OF SCI & TECH
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