Preparation method of LDHs (Layered Double Hydroxides) composite flame retardant

A composite flame retardant and coupling agent technology, which is applied in the field of inorganic flame retardants, can solve the problems of reducing the flame retardant efficiency of flame retardants, difficult to meet thermal stability, and limiting the scope of use, etc., to achieve droplet suppression performance, good Application prospect, excellent effect of thermal stability

Active Publication Date: 2014-06-25
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, APP itself has strong hygroscopicity, is easy to precipitate on the surface of the material, and its thermal stability is difficult to meet the processing requirements of some plastics, which reduces the flame retardant efficiency of this type of flame retardant to a certain extent and limits its application range.

Method used

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  • Preparation method of LDHs (Layered Double Hydroxides) composite flame retardant
  • Preparation method of LDHs (Layered Double Hydroxides) composite flame retardant
  • Preparation method of LDHs (Layered Double Hydroxides) composite flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1. Weigh 46.2g of magnesium nitrate and 22.6g of aluminum nitrate and dissolve in 300mL of water to form a metal salt solution; another weigh 24g of sodium hydroxide and dissolve in 500mL of water to form lye; at 25°C, slowly dissolve the prepared lye adding the metal salt solution to adjust the pH value of the metal salt solution to 10 to prepare a precursor slurry.

[0032] 2. Add 3.5g of APP with a degree of polymerization of 200 to 500mL of the above precursor slurry, stir and react at 25°C for 3 hours, then let stand for 12 hours, filter, wash and dry to obtain APP-LDHs powder.

[0033] 3. Weigh 40 parts of APP-LDHs powder prepared in step 2, and weigh 8 parts of monopentaerythritol, 1 part of γ-aminopropyltriethoxysilane, 20 parts of absolute ethanol, 80 parts of grinding balls, and put In the ball mill tank, ball mill at a ball mill speed of 250 rpm for 8 hours and then dry to obtain a composite flame retardant.

[0034] figure 1 It is the XRD pattern of the pr...

Embodiment 2

[0037] 1. Dissolve 20.5g of magnesium chloride and 24.8g of aluminum sulfate in 300mL of water to form a metal salt solution; take another 22g of sodium hydroxide and 17g of sodium carbonate and dissolve in 500mL of water to form a lye; The lye is slowly added into the metal salt solution, and the pH value of the metal salt solution is adjusted to 11 to prepare a precursor slurry.

[0038] 2. Add 5.0 g of APP with a degree of polymerization of 400 to 500 mL of the above precursor slurry, stir and react at 35°C for 2.5 hours, then let stand for 11.5 hours, filter, wash and dry to obtain APP-LDHs powder.

[0039] 3. Weigh 39 parts of APP-LDHs powder prepared in step 2, and weigh 9 parts of dipentaerythritol, 0.5 parts of γ-aminopropyltriethoxysilane, 22 parts of absolute ethanol, 85 parts of grinding balls, and put In the ball milling tank, the ball milling speed is 300 rpm for 6 hours and then dried to obtain the composite flame retardant.

[0040] Mix the composite flame reta...

Embodiment 3

[0042] 1. Weigh 35.7g of zinc nitrate, 30.2g of magnesium nitrate and 44.2g of aluminum nitrate and dissolve in 500mL of water to form a metal salt solution; another weigh 30g of sodium hydroxide and dissolve in 500mL of water, add 200mL of ammonia water (mass concentration 28%) as lye; at 45°C, slowly add the prepared lye into the metal salt solution, adjust the pH of the metal salt solution to 11, and prepare the precursor slurry.

[0043] 2. Add 8g of APP with a polymerization degree of 100 to 500mL of the above precursor slurry, stir and react at 45°C for 2.5 hours, then let stand for 24 hours, filter, wash and dry to obtain APP-LDHs powder.

[0044] 3. Weigh 65 parts of APP-LDHs powder prepared in step 2, and weigh 10 parts of β-cyclodextrin, 0.8 parts of isopropyl tris(dioctyl pyrophosphate acyloxy) titanate, 30 parts of industrial alcohol Parts, 150 parts of balls, put into a ball mill jar, mill at a milling speed of 520 rpm for 5 hours and then dry to obtain a composit...

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Abstract

The invention discloses a preparation method of a LDHs (Layered Double Hydroxides) composite flame retardant. The preparation method comprises the following steps of: synthesizing LDHs in the regulation and control of ammonium polyphosphate (APP) to prepare APP-LDHs, and then carrying out ball-milling and blending APP-LDHs with a coupling agent and a carbon-forming agent so as to prepare the LDHs composite flame retardant. The composite flame retardant is good in heat stability and has good performances of carbon-forming, smoke suppression and molten drop suppression. The composite flame retardant is not precipitated after being blended with high polymer materials, and has little influence to the mechanical property of materials, so that the composite flame retardant is especially applicable to processing the high polymer materials which have high temperature and generate molten drop when combusting. The method is simple in operation technology and low in production cost, and can realize industrial production, so that the method has a good application prospect.

Description

1. Technical field [0001] The invention relates to a preparation method of a flame retardant, in particular to a preparation method of an LDHs type composite flame retardant, and belongs to the technical field of inorganic flame retardants. 2. Background technology [0002] Traditional halogen-containing flame retardants have the advantages of good flame retardant effect, less addition amount, and little impact on the mechanical properties of organic matter, and are widely used in the flame retardant of polymer materials. However, due to the fact that most of the halogen-containing flame retardants are toxic and carcinogenic, and release a large amount of smoke and toxic gases such as hydrogen halides during combustion, secondary pollution occurs, and the adverse effects on the environment and human life are becoming more and more significant. The use of halogenated flame retardants has proposed restrictive measures. Therefore, the development of new halogen-free and enviro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/10C08K7/00C08K3/22C08K3/32C08L23/12C09C1/42C09C1/00C09C3/04C09C3/08C09C3/12
Inventor 杨保俊薛中华王百年张先龙李茜
Owner HEFEI UNIV OF TECH
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