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A kind of preparation and modification method of magnesium hydroxide flame retardant

A magnesium hydroxide and flame retardant technology, applied in magnesium hydroxide and other directions, can solve the problems of easy product agglomeration, large reaction rate, large particle size range, etc., to reduce particle agglomeration, enhance application ability, and uniform appearance. Effect

Active Publication Date: 2019-08-09
自然资源部天津海水淡化与综合利用研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the magnesium hydroxide produced by the precipitation reaction usually has a large reaction rate and does not have a long enough time for lattice arrangement, and the resulting precipitated crystal form is incomplete, and the product is easy to agglomerate, with a large particle size range and low quality; Magnesium has a strong surface polarity and exhibits "hydrophilic and oleophobic" properties. When it is added to polymer materials as a flame retardant, it has poor compatibility with polymer materials, which in turn affects the mechanical properties and properties of polymer materials. Processing performance
In order to improve the application ability of magnesium hydroxide, it is usually necessary to carry out additional modification operations, that is, to improve the magnesium hydroxide particles and polymers through surfactant treatment, coupling agent treatment, microencapsulation or polymerization grafting. Material compatibility, operational difficulty and process cost have all been improved

Method used

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  • A kind of preparation and modification method of magnesium hydroxide flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] First mix 5mL styrene (PS) and 5mL cyclohexane in a 150mL Erlenmeyer flask, then add 4g cetyltrimethylammonium bromide (CTAB) and 10mL of 1mol / L magnesium chloride solution successively, and then 10 mL of isopropanol was added dropwise under stirring, and stirred for 30 min to obtain a clear and transparent inverse microemulsion. Under magnetic stirring, add 20mL of 1mol / L sodium hydroxide solution dropwise to the above microemulsion, continue to stir for 2h after the dropwise addition, and leave the resulting mixed solution to stand and age at room temperature for 2h to fully react to obtain a white precipitate . Centrifuge, wash once with ethanol and distilled water respectively, centrifuge again, and finally dry the obtained precipitate in an electric blast drying oven at 80°C to obtain the magnesium hydroxide flame retardant product.

Embodiment 2

[0026] First mix 8mL methyl methacrylate (MMA) and 4mL toluene in a 150mL Erlenmeyer flask, then add 4g dioctyl sodium sulfosuccinate (AOT) and 10mL of 1mol / L magnesium chloride solution in turn, and then in With stirring, 10 mL of n-amyl alcohol was added dropwise, and stirred for 30 min to obtain a clear and transparent inverse microemulsion. Under magnetic stirring, 30 mL of 1 mol / L sodium hydroxide solution was added dropwise to the above microemulsion, and then 0.15 g of azobisisobutyronitrile (AIBN) was added, stirred for 30 min, and the resulting mixture was aged at room temperature 2h to fully react, a white precipitate was obtained. Centrifuge, wash with ethanol and distilled water three times, then centrifuge again, and finally dry the obtained precipitate in an electric blast drying oven at 60°C to obtain the magnesium hydroxide flame retardant product.

Embodiment 3

[0028] First mix 10mL of isoprene and 10mL of n-hexane in a 150mL Erlenmeyer flask, then add 5g of dodecyltrimethylammonium chloride (DTAC) and 10mL of 1mol / L magnesium sulfate solution in sequence, and then With stirring, 5 mL of n-butanol and 5 mL of n-octanol were added dropwise, and stirred for 30 min to obtain a clear and transparent inverse microemulsion. Under magnetic stirring, 30 mL of 1 mol / L ammonia water was added dropwise to the above-mentioned microemulsion, and the stirring was continued for 2 h after the dropwise addition, and the obtained mixture was aged at room temperature for 4 h to fully react, and a white precipitate was obtained. Centrifuge, wash twice with ethanol and distilled water, then centrifuge again, and finally dry the resulting precipitate in an electric blast drying oven at 100°C to obtain a magnesium hydroxide flame retardant product.

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Abstract

The invention discloses a preparation and modification method of a magnesium hydroxide flame retardant. The technical steps comprise micro-emulsion blending, magnesium hydroxide synthesis, coating modification, washing separation and drying. The preparation method comprises the following steps: preparing an W / O type microemulsion by using an oil phase containing a polymer monomer, a surfactant, asoluble magnesium salt and a cosurfactant, adding an alkaline precipitant under stirring for a precipitation reaction, performing aging after the reaction, performing centrifugal separation on the obtained mixed solution, separately washing the obtained precipitate after the centrifugal separation with ethanol and distilled water, and finally performing drying to obtain the magnesium hydroxide. According to the method, the ''water core'' of the microemulsion is used as a magnesium hydroxide reactor, the polymer monomer in the microemulsion oil phase is used as a coating modifying matrix, and the preparation and the modification of magnesium hydroxide are synchronously realized. The operation is simple; the obtained magnesium hydroxide has a nano partical size, and is uniformly dispersed; the surface is oleophylic; and the magnesium hydroxide flame retardant has good application potential.

Description

technical field [0001] The invention relates to a preparation and modification method of a magnesium hydroxide flame retardant, in particular to a method for synchronously operating the preparation and modification of the magnesium hydroxide flame retardant by using a microemulsion. Background technique [0002] As an important inorganic flame retardant material, magnesium hydroxide has triple functions of filling, flame retardancy and smoke suppression, and the smoke produced is non-toxic and non-corrosive. It is an environmentally friendly green flame retardant. With the increasingly stringent environmental protection requirements and the international restrictions on the use of some brominated flame retardants, the development and use of green and environmentally friendly magnesium hydroxide flame retardants is of great significance. [0003] The preparation of magnesium hydroxide is usually made by adding magnesium salt or brine as raw material, adding alkaline precipita...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/10C08K3/22C08F112/08C08F2/32C08F120/14C08F136/08C01F5/20C01F5/22
CPCC01F5/20C01F5/22C08F2/32C08F112/08C08F120/14C08F136/08C08K3/22C08K9/08C08K9/10C08K2003/2224
Inventor 武海虹张琦赵旭马来波李涛黄西平
Owner 自然资源部天津海水淡化与综合利用研究所
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