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Phosphor-nitrogen containing silane A, phosphite ester halogen-free flame retardant containing nitrogen phosphor silicon and preparation method of phosphite ester halogen-free flame retardant

A nitrogen silane and flame retardant technology, which is applied in the field of phosphite halogen-free flame retardants and their preparation, can solve the problems of low flame retardant efficiency, achieve small color influence, high flame retardant effect, and broad industrial application prospects Effect

Active Publication Date: 2013-11-13
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the above problems, the purpose of the present invention is to overcome the disadvantages of low flame retardant efficiency of conventional phosphorus-based flame retardants, combine the advantages of phosphorus / silicon and phosphorus / nitrogen flame retardant systems, and provide a new phosphorus, nitrogen, silicon Phosphite organic-inorganic hybrid environment-friendly halogen-free flame retardant

Method used

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  • Phosphor-nitrogen containing silane A, phosphite ester halogen-free flame retardant containing nitrogen phosphor silicon and preparation method of phosphite ester halogen-free flame retardant
  • Phosphor-nitrogen containing silane A, phosphite ester halogen-free flame retardant containing nitrogen phosphor silicon and preparation method of phosphite ester halogen-free flame retardant
  • Phosphor-nitrogen containing silane A, phosphite ester halogen-free flame retardant containing nitrogen phosphor silicon and preparation method of phosphite ester halogen-free flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1) In a 500ml three-necked flask equipped with mechanical stirring and a constant pressure dropping funnel, add 66.3g (0.3mol) 3-aminopropyltriethoxysilane and 200ml tetrahydrofuran, and stir at 30-40°C for 10 minutes, Add 9g (0.3mol) of paraformaldehyde, warm up to 65-70°C after 1 hour of heat preservation reaction, then add 66.0g (0.6mol) of dimethyl phosphite dropwise within 2 hours, and stop the reaction after 12 hours of heat preservation reaction. Remove the solvent, dissolve the crude product in 200ml chloroform, wash three times with 0.1mol / L sodium hydroxide solution, wash three times with deionized water, dry over anhydrous magnesium sulfate and remove chloroform to obtain a light yellow transparent liquid, which is reactant a.

[0033] Product A structural characterization:

[0034] FTIR (KBr, cm -1 ):2984-2905(ν C-H ),1269(ν P=O ),1196(ν C-N ),1103-1080(ν Si-O ), 1046-965 (ν P-O ). 1 H-NMR (400MHz, CDCl 3 -d,ppm):3.83(dd,6H),3.66(d,12H),2.84(d,4H),2...

Embodiment 2

[0038] 1) In a 500ml three-necked flask equipped with mechanical stirring and constant pressure dropping funnel, add 70.6g (0.3mol) N-methyl-3-aminopropyltrimethoxysilane and 200ml tetrahydrofuran, and stir at 30-40°C After 10 minutes, add 9g (0.3mol) paraformaldehyde, warm up to 65-70°C after 1 hour of heat preservation reaction, then add 33.0g (0.3mol) of dimethyl phosphite dropwise within 2 hours, and heat preservation reaction for 12 hours Stop responding. Remove the solvent, dissolve the crude product in 200ml chloroform, wash three times with 0.1mol / L sodium hydroxide solution, wash three times with deionized water, dry over anhydrous magnesium sulfate and remove chloroform to obtain a light yellow transparent liquid, which is Reactant A.

[0039] Product A structural characterization:

[0040] FTIR (KBr, cm -1 ):2984-2905(ν C-H ),1269(ν P=O ),1196(ν C-N ),1103-1080(ν Si-O ), 1046-965 (ν P-O ). 1 H-NMR (400MHz, CDCl 3 -d,ppm):3.83(dd,6H),3.66(d,6H),2.84(d,2H),2...

Embodiment 3

[0044] 1) In a 500ml three-necked flask equipped with mechanical stirring and a constant pressure dropping funnel, add 76.6g (0.3mol) N-phenyl-3-aminopropyltrimethoxysilane and 200ml tetrahydrofuran, and stir at 30-40°C After 10 minutes, add 9g (0.3mol) paraformaldehyde, warm up to 65-70°C after 1 hour of heat preservation reaction, then add 33.0g (0.3mol) of dimethyl phosphite dropwise within 2 hours, and heat preservation reaction for 12 hours Stop responding. Remove the solvent, dissolve the crude product in 200ml chloroform, wash three times with 0.1mol / L sodium hydroxide solution, wash three times with deionized water, dry over anhydrous magnesium sulfate and remove chloroform to obtain a light yellow transparent liquid, which is reactant a.

[0045] Product A structural characterization:

[0046] FTIR (KBr, cm -1 ):2984-2905(ν C-H ),1600-1490(δ aromatic C=C ),1269(ν P=O ),1196(ν C-N ),1103-1080(ν Si-O ), 1046-965 (ν P-O ). 1 H-NMR (400MHz, CDCl 3 -d,ppm):6.7-...

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Abstract

The invention provides phosphor-nitrogen containing silane A and a preparation method thereof. Furthermore, the invention also provides phosphite ester halogen-free flame retardant containing nitrogen phosphor silicon and a preparation method of the phosphite ester halogen-free flame retardant. The phosphite ester halogen-free flame retardant containing nitrogen phosphor silicon is used for synthesizing phosphite ester silane containing phosphor nitrogen elements by using silane containing an imino group, an aldehyde compound and dialkyl phosphate as the materials through Kabachnik-Fields reaction; and the prepared silane and tetraethyl orthosilicate are used for preparing organic-inorganic hybrid halogen-free flame retardant containing phosphor, nitrogen and silicon under the action of acid / alkaline catalyst. The flame retardant is halogen-free and non-toxic and is organically combined with the advantages of phosphor / nitrogen, phosphor / silicon flame retardant synergic system, and has very high flame retardant efficiency for a polymer material. The appearance of the flame retardant is white solid powder, and therefore, the interferences for the color of the base body are smaller. Moreover, the preparation method is simple and easy to implement, low in cost and convenient for realizing industrialization.

Description

technical field [0001] The invention relates to the technical field of flame retardant materials, in particular to a phosphorus-nitrogen-containing silane A, a nitrogen-phosphorus-silicon-containing phosphite halogen-free flame retardant and a preparation method thereof. Background technique [0002] With the continuous development of science and technology, polymer materials are widely used in various industries such as electronics, automobiles, and construction because of their excellent physical and chemical properties. However, as we all know, synthetic polymer materials are basically derived from petrochemicals, and are composed of carbon and hydrogen elements, so they are extremely flammable. In recent years, major fire accidents directly caused by the ignition of polymer materials are not uncommon, whether at home or abroad. Therefore, the research and development of flame-retardant polymers is an extremely important direction of material science at present. The dev...

Claims

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Application Information

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IPC IPC(8): C07F9/40C07F9/6596C08K5/549C08L23/12
Inventor 胡源江赛华桂宙
Owner UNIV OF SCI & TECH OF CHINA
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