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Preparation method of aluminum hydroxide/expandable graphite composite material

A technology of expanded graphite and composite materials, applied in the field of materials, can solve the problems of difficult recovery of chloroform and unsaturated compounds, deterioration of mechanical properties of high polymers, hindering industrial production, etc., and achieves simple and feasible process, low cost and low cost. Effect

Active Publication Date: 2019-07-05
NORTHEASTERN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, the development and utilization of composite flame retardants are the focus of current flame retardant research work; patent CN1844311A has obtained aluminum hydroxide and magnesium hydroxide composite flame retardants with sodium aluminate, magnesium salt and caustic alkali as raw materials. The heat-resistant decomposition temperature of the prepared composite flame retardant is significantly increased, reaching above 250 ° C, and the particle size and dispersion are improved; The deterioration of mechanical properties has not been greatly improved; patent CN 103193227A discloses a preparation method of highly flame-retardant expandable graphite, which uses chloroform, unsaturated compounds, acyl melamine chloride, etc. as raw materials, and is synthesized by gamma ray irradiation and other technical means High flame retardant expandable graphite has been developed, which greatly improves the compatibility between expandable graphite and polymers, but its synthesis process is complicated, and the recovery of chloroform and unsaturated compounds remaining in the reaction is difficult, which seriously hinders its industrial production

Method used

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  • Preparation method of aluminum hydroxide/expandable graphite composite material
  • Preparation method of aluminum hydroxide/expandable graphite composite material
  • Preparation method of aluminum hydroxide/expandable graphite composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Process such as figure 1 shown;

[0037] Aluminum chloride is added with water to make a mass concentration of 10% aluminum chloride solution;

[0038] Mix perchloric acid solution and glacial acetic acid solution and then dilute with water to prepare an acid solution with a mass fraction of 80%, wherein the volume ratio of perchloric acid solution and glacial acetic acid solution is 1:1; the perchloric acid solution The mass concentration of the glacial acetic acid solution is 70%, and the mass concentration of the glacial acetic acid solution is 98%; the flake graphite, aluminum chloride solution and acid solution with a particle size of 50 to 200 meshes are mixed in a mass ratio of 1:1:10, and then ultrasonically dispersed. Time 100min, made suspension;

[0039] The suspension is introduced into the reaction tank; the reaction tank is provided with a diaphragm, and the inside of the reaction tank is divided into a cathode area and an anode area, and the cathode are...

Embodiment 2

[0045] Method is with embodiment 1, and difference is:

[0046] (1) aluminum chloride solution mass concentration 20%;

[0047] (2) The mass fraction of acid solution is 30%, and the volume ratio of perchloric acid solution and glacial acetic acid solution is 10:1; the flake graphite, aluminum chloride solution and acid solution are mixed in a mass ratio of 1:10:50, and ultrasonically dispersed 10min;

[0048] (3) Electrochemical intercalation temperature 30°C, current density 1.0A / cm 2 , replace the positive and negative poles every 20 minutes; the time is 60 minutes;

[0049] (4) Mix the solid phase with the ammoniacal liquor of pH value 8.0, and the mixing ratio is 1:2 by making the mass ratio of the solid phase and the ammoniacal liquor;

[0050] (5) The second ultrasonic dispersion treatment time is 2h, then stand still for 20min;

[0051] (6) The secondary solid phase was dried at 200°C for 60 minutes, and the expansion volume of the aluminum hydroxide / expandable gra...

Embodiment 3

[0053] Method is with embodiment 1, and difference is:

[0054] (1) aluminum chloride solution mass concentration 30%;

[0055] (2) The mass fraction of acid solution is 50%, and the volume ratio of perchloric acid solution and glacial acetic acid solution is 5:1; the flake graphite, aluminum chloride solution and acid solution are mixed in a mass ratio of 1:5:30, and ultrasonically dispersed 50min;

[0056] (3) Electrochemical intercalation temperature 5°C, current density 0.5A / cm 2 , replace the positive and negative electrodes every 40 minutes; the time is 160 minutes;

[0057] (4) The solid phase is mixed evenly with the ammoniacal liquor of pH value 8.5, and the mixing ratio is 1:5 by making the mass ratio of the solid phase and the ammoniacal liquor;

[0058] (5) The second ultrasonic dispersion treatment time is 6h, then stand still for 30min;

[0059] (6) The secondary solid phase was dried at 100°C for 100 minutes, and the expansion volume of the aluminum hydroxid...

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Abstract

A preparation method of an aluminum hydroxide / expandable graphite composite material comprises following steps: (1) adding water into aluminum salts to prepare an aluminum salt solution; (2) mixing aperchloric acid solution and a glacial acetic acid solution, adding water, and mixing the mixed solution with flake graphite and the aluminum salt solution to prepare a turbid liquid; (3) introducingthe turbid liquid into a reactor, and carrying out electrochemical intercalation through a periodical direction changing method; (4) filtering the materials, and washing the materials by water to obtain a solid phase; (5) evenly mixing the solid phase with ammonia water or a water solution of ammonium bicarbonate; (6) carrying out a secondary ultrasonic dispersing treatment, carrying out separation to remove the upper-layer supernate, filtering, and performing water washing; and (7) performing drying to obtain the aluminum hydroxide / expandable graphite composite material. The raw materials aresimple, easily available and cheap; through an electrochemical intercalation method, the using amount of an oxidizing agent is reduced; the acid solution can be recovered and repeatedly used, the environmental pollution is small, the cost is low, and the technical process is simple and feasible.

Description

technical field [0001] The invention belongs to the field of material technology, in particular to a preparation method of aluminum hydroxide / expandable graphite composite material. Background technique [0002] Expandable graphite is a graphite interlayer compound obtained by oxidation of natural flake graphite. The graphite layer of expandable graphite will be pushed away at a certain temperature so that the graphite layer exhibits high expansion in the c-axis direction. A new worm-like substance, exfoliated graphite, is formed. Expandable graphite is non-toxic, smoke-suppressing, corrosion-resistant, and has excellent thermal insulation properties. It will not affect the mechanical properties of the polymer itself when used in polymers; in addition, expandable graphite also has the functions of absorbing waves, resisting radiation, and lubricating. Expanded graphite has a wide range of applications including sealing materials, battery materials, environmental protection ...

Claims

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Application Information

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IPC IPC(8): C25B1/00C25B9/08C09K21/02C01B32/22C25B9/19
CPCC25B1/00C09K21/02C01B32/22C01P2004/03C01P2002/82C01P2002/85C25B9/19
Inventor 崔智春狄跃忠王耀武彭建平马广超冯乃祥
Owner NORTHEASTERN UNIV
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