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Aluminum diethyl phosphinate material and preparation method thereof

A technology of diethylphosphinic acid and aluminum ethylphosphinate, applied in the field of flame retardant materials, can solve the problems of large dust, poor dispersion effect, and affecting the flame retardant and mechanical properties of polymer materials

Active Publication Date: 2020-10-23
ZHEJIANG XINHUA CHEM +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Due to the low specific surface energy and small intermolecular force of ultra-fine aluminum diethylphosphinate powder, there is a lot of air between the powder during the production process, resulting in a low bulk density of only 0.20g / cm 3 -0.30g / cm 3 , so that it is not easy to be compatible with polymers during use, and it is difficult to produce "bridging" phenomenon in the process of extrusion molding or extrusion granulation, and the dispersion effect is not good, which seriously affects the flame retardancy and mechanical properties of polymer materials. performance, and the dust is large, which seriously pollutes the environment
[0003] Although surface modification of ultrafine aluminum diethylphosphinate powder can effectively increase its bulk density, traditional ultrafine aluminum diethylphosphinate powder is usually pulverized by wet ball milling or jet milling. Obtained, the surface is irregular, and it is easy to form uneven coating when the surface is modified
And the traditional surface modification mainly adopts liquid phase surface treatment method, on the one hand, its process is loaded down with trivial details, and processing time is long, and production cost height is unfavorable for industrialized production; Regulator, and the introduction of acidic substances is easy to corrode equipment

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  • Aluminum diethyl phosphinate material and preparation method thereof
  • Aluminum diethyl phosphinate material and preparation method thereof

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preparation example Construction

[0023] The preparation method of aluminum diethylphosphinate material provided by the invention comprises:

[0024] S1, providing a mixed acid solution and a suspension containing an aluminum source, wherein the mixed acid solution includes dialkylphosphinic acid and a crystallization aid;

[0025] S2, mixing the mixed acid solution with the suspension, reacting to obtain aluminum diethylphosphinate particles, and stacking a plurality of aluminum diethylphosphinate particles to form a powder with a porous structure, wherein The powder has a D95 particle size distribution of 5 μm-30 μm;

[0026] S3, the powder is placed in a mixer for mixing, the coupling agent is added to the mixer by spraying and mixed with the powder, and the coupling agent is combined with the powder Obtain aluminum diethylphosphinate material, wherein the bulk density of aluminum diethylphosphinate material is 0.45g / cm 3 -0.70g / cm 3 .

[0027] In step S1, the aluminum source includes at least one of al...

Embodiment 1

[0055] Aluminum sulfate is pre-dispersed in water, and the pH value is adjusted to 7.8 by sodium hydroxide to obtain a suspension.

[0056] 90kg of dialkylphosphinic acid and 10kg of crystallization aid di-sec-butylphosphinic acid (bis(1-methylpropyl)phosphinic acid) were mixed to form a mixed acid solution.

[0057] At 50°C and 1 bar, under the condition that the molar ratio of aluminum sulfate to diethylphosphinic acid is 1:3, mix the above mixed acid solution and suspension to react to obtain aluminum diethylphosphinate powder . The aluminum diethylphosphinate powder is formed by stacking a plurality of aluminum diethylphosphinate particles, has a porous structure, the particle diameter D95 is 15.12 μm, and the bulk density of the powder is 0.23 g / cm 3 .

[0058] Weigh 50kg of the above-prepared aluminum diethylphosphinate powder and 0.5kg of titanate coupling agent, and pour the weighed aluminum diethylphosphinate powder into the preheated to 120°C In a high-speed mixer...

Embodiment 2

[0060] The sodium metaaluminate is pre-dispersed in water, and the pH value is adjusted to 4.1 by hydrochloric acid to obtain a suspension.

[0061] The dialkylphosphinic acid of 99.9kg is mixed with the crystallization aid dibutylphosphinic acid of 0.1kg, forms mixed acid solution.

[0062] At 150°C and 25 bar, under the condition that the molar ratio of sodium metaaluminate to diethylphosphinic acid is 1:10, the above mixed acid solution and suspension are mixed to react to obtain aluminum diethylphosphinate Powder. The aluminum diethylphosphinate powder is formed by stacking a plurality of aluminum diethylphosphinate particles, has a porous structure, the particle diameter D95 is 29.21 μm, and the bulk density of the powder is 0.310 g / cm 3 .

[0063] Weigh 50kg of the above-prepared aluminum diethylphosphinate powder and 1.5kg of silane coupling agent, and pour the weighed aluminum diethylphosphinate powder into a high-speed In the mixer, mix at a speed of 400r / min for 6...

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Abstract

The invention relates to an aluminum diethyl phosphinate material and a preparation method thereof. The preparation method comprises the steps that a mixed acid solution and a turbid liquid containingan aluminum source are provided, wherein the mixed acid solution comprises dialkyl phosphinic acid and a crystallization assisting agent; the mixed acid solution and the turbid liquid are mixed and react to obtain aluminum diethyl phosphinate particles, the multiple aluminum diethyl phosphinate particles are stacked to form powder of a porous structure, and the powder has D95 particle size distribution of 5-30 microns; putting the powder into a mixing machine to be mixed; and a coupling agent is added into the mixing machine in a spraying mode and mixed with the powder, the coupling agent andthe powder are combined to obtain the diethyl aluminum phosphinate material, and the bulk density of the diethyl aluminum phosphinate material is 0.45 g / cm < 3 > to 0.70 g / cm < 3 >. The diethyl aluminum phosphinate material can be uniformly dispersed in a polymer in the use process, so that the polymer material has excellent flame retardancy and mechanical properties, and dust pollution is small.

Description

technical field [0001] The invention relates to the technical field of flame retardant materials, in particular to an aluminum diethylphosphinate material and a preparation method thereof. Background technique [0002] Due to the low specific surface energy and small intermolecular force of ultra-fine aluminum diethylphosphinate powder, there is a lot of air between the powder during the production process, resulting in a low bulk density of only 0.20g / cm 3 -0.30g / cm 3 , so that it is not easy to be compatible with the polymer during use, and it is difficult to produce "bridging" phenomenon in the process of extrusion molding or extrusion granulation, and the dispersion effect is not good, which seriously affects the flame retardancy and mechanical properties of polymer materials. performance, and the dust is large, which seriously pollutes the environment. [0003] Although surface modification of ultrafine aluminum diethylphosphinate powder can effectively increase its b...

Claims

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Application Information

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IPC IPC(8): C07F9/30C08K5/5313C08L75/08
CPCC07F9/301C08K5/5313C08L2201/02C08L75/08Y02E60/10
Inventor 应思斌蒋铭豪谢自强周健章震王超远
Owner ZHEJIANG XINHUA CHEM
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