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A kind of submicron organic spirocyclic aluminum phosphate flame retardant and preparation method thereof

A spiro aluminum phosphate, sub-micron technology, applied in the field of flame retardants, can solve the problems of long reaction time, low solubility, large product particle size, etc., and achieve good flame retardant effect, high thermal stability, and simple post-processing. Effect

Active Publication Date: 2018-03-02
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent (CN102086401A) discloses a method for preparing an organic aluminum phosphonate flame retardant, aluminum methyl phosphonate, which has a thermal decomposition temperature higher than 325°C and can be applied to flame retardancy of thermoplastic polymer materials. However, this The reaction steps of the production method are complicated, there are by-products, and the particle size of the product is large, and the dispersion in the substrate is not good
Chinese patent (CN103102508A) has reported a kind of nano organic phosphonic acid aluminum salt flame retardant and preparation method thereof, has made the product that particle diameter is all below 1 μ m, has good flame retardant effect in ABS plastics, but its reaction time If it is too long, there are many types of additives required, and the particle size range is widely distributed, which is not conducive to industrial production
U.S. Patent (US4973727) reacts aluminum hydroxide and dimethyl methyl phosphonate to prepare organic phosphonic acid aluminum flame retardants. Aluminum hydroxide has less solubility in solvents and lower reactivity. The reaction is not only time-consuming, but also increases energy consumption
The above patents have successfully prepared aluminum organophosphate flame retardants, but there are still many shortcomings, which limit the industrial production and application of such flame retardants

Method used

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  • A kind of submicron organic spirocyclic aluminum phosphate flame retardant and preparation method thereof
  • A kind of submicron organic spirocyclic aluminum phosphate flame retardant and preparation method thereof
  • A kind of submicron organic spirocyclic aluminum phosphate flame retardant and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0034] A submicron organic spiro aluminum phosphate flame retardant, white powder, particle size less than 0.7μm, melting point 261~263℃, structural formula is as follows:

[0035]

[0036] Add 1500ml of water and 300ml of ethanol to a mixed solution of alcohol and water, add 2.7g of polyvinylpyrrolidone to the above mixed solution of alcohol and water to dissolve under stirring, add 130g of DPP to the solution, dissolve under stirring, and then add alkaline aqueous solution Adjust the pH to 6.7, stir and mix well, then add 140g of aluminum nitrate nonahydrate to the above solution, mix well under stirring, add an aqueous alkali solution to adjust the pH to 6.3, stir for 4 hours at 70°C, cool to room temperature after the reaction, Filtered, washed with water, and dried under vacuum at 80°C to obtain 131g of sub-micron organic spiro aluminum phosphate. The purity of the product obtained is 99.3%, the particle size is 457nm, and the distribution range is narrow. figure 1 Shown.

Embodiment 2

[0038] A submicron organic spiro aluminum phosphate flame retardant, white powder, particle size less than 0.7μm, melting point 261~263℃, structural formula is as follows:

[0039]

[0040] Add 1200ml of water and 300ml of methanol to a mixed solution of alcohol and water in the container, add 2.3g of sodium dodecylbenzene sulfonate to the above mixed solution of alcohol and water to dissolve under stirring, add 104g of DPP to the solution, and dissolve under stirring , Then add alkaline aqueous solution to adjust the pH value to 6.6, stir and mix uniformly, then add 72g of aluminum trichloride hexahydrate to the above solution, mix uniformly under stirring, add alkaline aqueous solution to adjust the pH value to 6.5, and stir for 3 hours at 60°C. After the reaction is completed, it is cooled to room temperature, filtered, washed with water, and dried under vacuum at 110°C to obtain 106 g of sub-micron organic spiro aluminum phosphate. The purity of the obtained product reaches 98...

Embodiment 3

[0042] A submicron organic spiro aluminum phosphate flame retardant, white powder, particle size less than 0.7μm, melting point 261~263℃, structural formula is as follows:

[0043]

[0044] Add 3000ml of water and 800ml of ethanol to the alcohol-water mixed solution in the container, add 8.7g of polyvinyl alcohol to the above-mentioned alcohol-water mixed solution to dissolve under stirring, add 182g of DPP to the solution, dissolve under stirring, and then add alkaline aqueous solution Adjust the pH to 6.7, stir and mix well, then add 171g of aluminum sulfate octahydrate to the above solution, mix well under stirring, add alkaline aqueous solution to adjust the pH to 6.4, stir for 3 hours at 50°C, cool to room temperature after the reaction is complete , Filtered, washed with water, vacuum-dried at 120°C to obtain 190g of submicron organic spiro aluminum phosphate. The purity of the product obtained is 99.1%, and the particle size is 481nm.

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Abstract

The invention relates to a submicron organic spirocyclic aluminum phosphate flame retardant and a preparation method thereof, belonging to the field of flame retardants. A submicron organic spirocyclic aluminum phosphate flame retardant, the structural formula is as follows: the preparation method is: firstly, the pentaerythritol diphosphate (DPP) is hydrolyzed in the alcohol aqueous solution under the action of alkali to obtain its sodium salt or potassium salt II solution, and then react the prepared pentaerythritol diphosphate sodium or potassium salt under heating and vigorous stirring conditions to prepare an organic spirocyclic aluminum phosphate flame retardant. The particle size of the prepared organic spirocyclic aluminum phosphate is less than 0.7 μm, and the particle size distribution range is narrow, reaching the submicron level, which can effectively reduce the consumption amount of the flame retardant in the polymer. The preparation method designs phosphorus-based flame retardants and aluminum salts with excellent flame-retardant properties in one molecule, which fundamentally solves the problem of the compounding of flame retardants in the process of material flame-retardant and the uneven distribution of components in the flame-retardant system. Equality issues.

Description

Technical field [0001] The invention relates to a submicron organic spiro aluminum phosphate flame retardant and a preparation method thereof, and belongs to the field of flame retardants. Background technique [0002] With the increasing demand for environmental protection and the rapid development of my country's economy and technology, halogen-free flame retardants have become a hot research topic. Phosphorus flame retardant is a kind of halogen-free flame retardant with superior flame retardant performance. It can exert the flame retardant effect in the aggregation phase and the gas phase, and has less smoke generation, small heat release and low toxicity. It has been widely used in high polymer The flame retardant of the material. However, the phosphorus flame retardants currently used have poor heat resistance, high volatility, easy migration, poor compatibility, and the flame retardant effect of the flame retardant is roughly proportional to the phosphorus content. These ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/527C07F9/6574C08L67/02C08L77/00
Inventor 刘吉平李泓成赵伟
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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