Preparation method of cyclodextrin-based phosphated flame retardant

A phosphorus-based flame retardant and cyclodextrin technology, which is applied in the field of preparation of cyclodextrin-based phosphorus-based flame retardants, can solve the problem that phosphorus-based flame retardants are unstable, cannot achieve flame retardant effect, and produce dioxins, etc. problem, to prevent outward diffusion, high-efficiency flame retardant effect, and improve the effect of dehydration

Inactive Publication Date: 2017-12-22
宣城市聚源精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Among the existing flame retardants, the traditional halogenated flame retardants have the characteristics of high flame retardant efficiency and are used by most enterprises, but they will produce a large amount of toxic substances during combustion. For example: the most widely used in the market now is Decabromodiphenyl ether has a high flame retardant effect, but it will produce dioxins during the combustion process, causing great harm to the environment
Therefore, it is gradually being replaced by halogen-free flame retardants. Among them, organophosphorus flame retardants are developing rapidly, especially halogen-free phosphorus-nitrogen flame retardants have been recognized by green environmental protection. They have the characteristics of high Flame retardant, low toxicity, low smoke, and no corrosive gas generation, but most of the phosphorus-based flame retardants are unstable and not resistant to hydrolysis, so they cannot achieve the best flame retardant effect

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A preparation method of a cyclodextrin-based phosphorus-based flame retardant, comprising the following steps:

[0019] (1) Add 15-18g of cyclodextrin to 75mL of 2% sodium hydroxide aqueous solution, stir at 50°C for 30min, then add 3.2g of glycidyl ether dropwise, drop it in 15min, and then add it at 10°C , stirred for 3 hours, and then stood still for 10 hours to obtain a reaction solution, then adjusted the pH to neutral with a sulfuric acid solution, then carried out rotary evaporation and drying of the reaction solution to obtain a solid reactant, which was ground and passed through 200 Mesh sieve, then uniformly disperse into ammonia water in a mass ratio of 5:50, then add 0.35% of its mass of alkaline activated nano-silica to ammonia water, stir at 80°C for 2 hours at a speed of 1800r / min, and then Stand at room temperature for 5 hours to obtain the modified cyclodextrin base liquid;

[0020] (2) Add phosphorus oxychloride dropwise to the modified cyclodextrin b...

Embodiment 2

[0030] A preparation method of a cyclodextrin-based phosphorus-based flame retardant, comprising the following steps:

[0031] (1) Add 18g of cyclodextrin to 80mL of 2% sodium hydroxide aqueous solution, stir at 50°C for 30min, then add 3.5g of glycidyl ether dropwise, drop it for 15min, then at 10°C, Stir for 5 hours, then stand still for 10 hours to obtain a reaction solution, then adjust the pH to neutral with a sulfuric acid solution, then carry out rotary evaporation and drying of the reaction solution to obtain a solid reactant, grind the obtained solid reactant, and pass through a 200-mesh sieve , then uniformly dispersed in ammonia water in a mass ratio of 5:50, then add its mass of 0.40% alkaline activated nano-silicon dioxide to ammonia water, stir at 80°C for 2 hours at a speed of 1800r / min, and then Stand at room temperature for 5 hours to obtain the modified cyclodextrin base liquid;

[0032] (2) Add phosphorus oxychloride dropwise to the modified cyclodextrin ba...

Embodiment 3

[0042] A preparation method of a cyclodextrin-based phosphorus-based flame retardant, comprising the following steps:

[0043] (1) Add 16g of cyclodextrin to 78mL of 2% sodium hydroxide aqueous solution, stir at 50°C for 30min, then add 3.3g of glycidyl ether dropwise, drop it for 15min, then at 10°C, Stir for 4 hours, then stand still for 10 hours to obtain the reaction solution, then adjust the pH to neutral with sulfuric acid solution, then carry out rotary evaporation and drying of the reaction solution to obtain a solid reactant, grind the obtained solid reactant, and pass through a 200-mesh sieve , and then uniformly dispersed in ammonia water at a mass ratio of 5:50, and then add 0.38% of its mass of alkaline activated nano-silica to the ammonia water, stir at 80°C for 2 hours at a speed of 1800r / min, and then Stand still for 5 hours to obtain the modified cyclodextrin base liquid;

[0044](2) Add phosphorus oxychloride dropwise to the modified cyclodextrin base soluti...

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PUM

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Abstract

The invention discloses a preparation method of a cyclodextrin-based phosphated flame retardant and relates to the technical field of flame retardant. The preparation method comprises the following steps: (1) preparing a modified cyclodextrin base solution; (2) dropwise adding phosphorus oxychloride into the modified cyclodextrin base solution; stirring and carrying out rotary evaporation and drying to obtain solid matters; (3) crushing the solid matters prepared by step (2) and immersing the crushed solid matters in absolute ethyl alcohol; then filtering and washing with de-ionized water; then carrying out the rotary evaporation and drying to obtain the cyclodextrin-based phosphated flame retardant. The cyclodextrin-based phosphated flame retardant provided by the invention not only has a good flame-retarding effect, but also is green and environmentally friendly.

Description

technical field [0001] The invention belongs to the technical field of flame retardants, and in particular relates to a preparation method of a cyclodextrin-based phosphorus-based flame retardant. Background technique [0002] Among the existing flame retardants, the traditional halogenated flame retardants have the characteristics of high flame retardant efficiency and are used by most enterprises, but they will produce a large amount of toxic substances during combustion. For example: the most widely used in the market now is Decabromodiphenyl ether has a high flame retardant effect, but it will produce dioxins during the combustion process, causing great harm to the environment. Therefore, it is gradually being replaced by halogen-free flame retardants. Among them, organophosphorus flame retardants are developing rapidly, especially halogen-free phosphorus-nitrogen flame retardants have been recognized by green environmental protection. They have the characteristics of hi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L5/16C08K9/04C08K3/36C08B37/16
CPCC08K9/04C08B37/0012C08K3/36C08K2201/011C08L2201/02C08L2201/22C08L5/16
Inventor 程聚光
Owner 宣城市聚源精细化工有限公司
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