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Preparation method of synergistic flame retardant nanometer zinc borate

A technology of nano-zinc borate and synergistic flame retardant, which is applied in the direction of borate, nanotechnology, boron oxide, etc., can solve the problems of crystallization and agglomeration, and cannot meet the needs of nano-zinc borate preparation, and achieves small particle size, The effect of low requirements on conditions and high yield

Inactive Publication Date: 2012-08-15
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In these synthetic methods, it is necessary to remove certain impurities, and there are crystallization and agglomeration problems in solvent evaporation and drying, which cannot meet the needs of the preparation of nano-zinc borate.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1) Weigh 0.9g (0.0056mol) zinc sulfate powder, add 40ml distilled water, 50ml ethanol, (6.2*10 -2 mol / L) was stirred to dissolve; the solution was set aside.

[0022] 2) Weigh 4.4g (0.0115mol) borax (Na 2 B 4 o 7 .10H 2 O), add 80ml distilled water, 100ml ethanol, (6.4*10 -2 mol / L) was stirred to dissolve it. The solution is ready for use. (zinc sulfate: borax = 1:2)

[0023] 3) Put the solution prepared in 2 into the water bath, start to heat up, the temperature rises from room temperature to 70°C, and keep stirring to make the borax dissolve as much as possible. Put the solution prepared in 1 into an acid burette, and add it dropwise to the solution prepared in 2 under high-speed magnetic stirring. The dropwise addition can be completed within 0.5 hour.

[0024] 4) After the dropwise addition, continue to react for 0.5h, then stop heating, take out the product after cooling to room temperature, filter with suction, wash with deionized water and absolute ethan...

Embodiment 2

[0026] 1) Weigh 1.8g (0.0112mol) zinc sulfate powder, add 50ml distilled water, 80ml ethanol, (8.6*10 -2 mol / L) was stirred to dissolve; the solution was set aside.

[0027] 2) Weigh 4.4g (0.0115mol) borax (Na 2 B 4 o 7 .H 2 O), add 80ml distilled water, 100ml ethanol, (6.4*10 -2 mol / L) was stirred to dissolve it. The solution is ready for use. (zinc sulfate: borax = 1:1)

[0028] 3) Put the solution prepared in 2 into the water bath, start to heat up, the temperature rises from room temperature to 75°C, and keep stirring to dissolve the borax as much as possible. Put the solution prepared in 1 into an acid burette, and add it dropwise to the solution prepared in 2 during stirring. The dropwise addition can be completed within 1 hour.

[0029] 4) After the dropwise addition, continue to react for 0.5h, then stop heating, take out the product after cooling to room temperature, filter with suction, wash with deionized water and absolute ethanol three times each, take it...

Embodiment 3

[0031] 1) Weigh 3.6g (0.0223mol) zinc sulfate powder, add 80ml distilled water, 100ml ethanol, (1.24*10 -1 mol / L) was stirred to dissolve; the solution was set aside.

[0032] 2) Weigh 4.4g (0.0115mol) borax (Na 2 B 4 o 7 .10H 2 O), add 80ml distilled water, 100ml ethanol, (6.4*10 -2 mol / L) was stirred to dissolve it. The solution is ready for use. (zinc sulfate: borax = 2:1)

[0033] 3) Put the solution prepared in 2 into the water bath, start to heat up, the temperature rises from room temperature to 80°C, and keep stirring to make the borax dissolve as much as possible. Put the solution prepared in 1 into an acid burette, and add it dropwise to the solution prepared in 2 during stirring. The dropwise addition can be completed within 2 hours.

[0034] 4) After the dropwise addition, continue to react for 0.5h, then stop heating, take out the product after cooling to room temperature, filter with suction, wash with deionized water and absolute ethanol three times eac...

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Abstract

The invention relates to the preparation of synergistic flame retardant nanometer zinc borate. A halogen-free flame retardant is characterized by having a good flame retardant effect and not generating toxic gas in combustion; and a nanometer zinc borate particle is an inorganic synergistic flame retardant, has the advantages of good heat stability, small granularity, small specific gravity, easiness in dispersing, non-toxicity and the like, and has excellent synergisti effects when being used as flame-retarding additives for plastic, rubber, chemical industry and other organic macromolecule composite materials. The invention relates to a preparation method of nanometer zinc borate, and the method has the advantages of simplicity in operation, low cost, single products, high yield and uniform particle size distribution, and does not generate innoxious products in a reaction process and the like. The optimal conditions obtained by the experiment is that the mixing ratio of zinc salt to borax is 0.1-12:1, the reaction temperature is 50-90 DEG C, and the dripping rate is controlled within 100-200 ml / h. The technical method has the advantages of simple technology, short reaction period, and high utilization ratio of raw materials.

Description

technical field [0001] The invention relates to the field of manufacturing inorganic nanoparticles, in particular to a method for preparing a synergistic flame retardant nano-zinc borate. Background technique [0002] At present, most domestic flame retardants use halogen and phosphorus as the center flame retardant elements. However, halogen-containing flame retardants produce a large amount of corrosive gas during combustion, which is extremely harmful to the human body and the environment. Halogen-free flame retardants It has the advantages of high efficiency, non-toxicity, and no pollution to the environment, so it gradually replaces halogen-containing flame retardants and becomes a new research hotspot. When using a halogen-free flame retardant, it is necessary to add a large amount to meet the flame retardant requirements, but a large amount of flame retardant additives will affect the mechanical properties and processing properties of the material. In the actual flame...

Claims

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Application Information

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IPC IPC(8): C01B35/12B82Y40/00
Inventor 黄定海王迪陈帮烈
Owner TIANJIN UNIV
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