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Submicron organic spiro aluminum phosphate flame retardant and preparation method thereof

A spirocyclic 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: 2015-12-30
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Submicron organic spiro aluminum phosphate flame retardant and preparation method thereof
  • Submicron organic spiro aluminum phosphate flame retardant and preparation method thereof
  • Submicron organic spiro aluminum phosphate flame retardant and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

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

[0035]

[0036] Add 1500ml of water and 300ml of alcohol-water mixed solution prepared by ethanol into the container, add 2.7g of polyvinylpyrrolidone to the above-mentioned alcohol-water mixed solution and dissolve under stirring, add 130g of DPP to the solution, dissolve under stirring, and then add alkali aqueous solution to adjust When the pH value reaches 6.7, stir and mix evenly, then add 140g of aluminum nitrate nonahydrate to the above solution, mix evenly under stirring, add an aqueous alkali solution to adjust the pH value to 6.3, stir and react at 70°C for 4 hours, cool to room temperature after the reaction, and filter , washed with water, and vacuum-dried at 80°C to obtain 131g of submicron organic spirocyclic aluminum phosphate, with a purity of 99.3%, a particle size of 457nm, and a nar...

Embodiment 2

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

[0039]

[0040] Add 1200ml water and 300ml alcohol-water mixed solution prepared by methanol in the container, add 2.3g sodium dodecylbenzenesulfonate to the above-mentioned alcohol-water mixed solution and dissolve under stirring, add 104g DPP to the solution, dissolve under stirring condition, Then add an aqueous alkali solution to adjust the pH value to 6.6, stir and mix evenly, then add 72g of aluminum trichloride hexahydrate to the above solution, mix evenly under stirring, add an aqueous alkali solution to adjust the pH value to 6.5, stir and react at 60°C for 3 hours, and react After finishing, cool to room temperature, filter, wash with water, and vacuum-dry at 110° C. to obtain 106 g of submicron organospirocyclic aluminum phosphate, with a purity of 98.3% and a particle size of 503 nm.

Embodiment 3

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

[0043]

[0044] Add 3000ml of water and 800ml of alcohol-water mixed solution prepared by ethanol into the container, add 8.7g of polyvinyl alcohol to the above-mentioned alcohol-water mixed solution and dissolve under stirring, add 182g of DPP to the solution, dissolve under stirring, and then add alkaline aqueous solution to adjust When the pH value reaches 6.7, stir and mix evenly, then add 171g of aluminum sulfate octadecahydrate to the above solution, mix evenly under stirring, add an aqueous alkali solution to adjust the pH value to 6.4, stir and react at 50°C for 3 hours, and cool to room temperature after the reaction is completed. Filtration, washing with water, and vacuum drying at 120° C. yielded 190 g of submicron organic spirocyclic aluminum phosphate, with a purity of 99.1% and a particl...

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Abstract

The invention relates to a submicron organic spiro aluminum phosphate flame retardant and a preparation method thereof, which belong to the field of fire retardants. The structural formula of the submicron organic spiro aluminum phosphate flame retardant is as follows (see the description). The preparation method comprises the steps of firstly, hydrolyzing pentaerythritol phosphate (DPP) in an alcohol-water solution under the action of alkali, so as to prepare a solution of sodium salt or sylvite II, and then reacting the prepared pentaerythritol phosphate sodium or sylvite in heating and violent mixing conditions, so as to prepare the organic spiro aluminum phosphate flame retardant. The particle size of prepared organic spiro aluminum phosphate is less than 0.7 mum, the particle size distribution range is narrow and achieves the submicron level, and the consumption of the flame retardant in polymers can be effectively reduced. According to the preparation method, the phosphorus based flame retardant and aluminum salt with good flame retardation are designed in a molecule, so that the problems of formulation of the flame retardant in the flame retardant process of materials and unevenness of distribution of respective components of a flame retardant system are basically solved.

Description

technical field [0001] The invention relates to a submicron organic spirocyclic aluminum phosphate flame retardant and a preparation method thereof, belonging to the field of flame retardants. Background technique [0002] With the growing demand for environmental protection and the rapid development of my country's economy and technology, the non-halogenation of flame retardants has become a hot research topic. Phosphorus-based flame retardants are a class of halogen-free flame retardants with excellent flame retardant properties. They can exert flame retardant effects in the aggregate phase and gas phase, and have less smoke formation, less heat release, and lower toxicity. They have been widely used in high polymer In the flame retardant of material. However, the phosphorus-based 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 t...

Claims

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Application Information

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Patent Type & Authority Applications(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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