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Preparation method of nano SiO2

A nano-silica and silicate technology, applied in the direction of silica, silicon oxide, nanotechnology, etc., can solve the problems of consumption of inorganic acids, environmental pollution, and the inability to recycle or recycle waste water containing salt and acid, and achieve The effect of reducing loss

Inactive Publication Date: 2012-08-15
ZHEJIANG YUDA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Therefore, although the above-mentioned process has solved the problem of replacing expensive raw materials with cheap materials, it has brought about the need to consume a large amount of inorganic acid, produce a large amount of salty and acidic waste water that cannot be recycled or recycled, and simultaneously cause problems such as environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Take a sodium silicate with a Baume degree of 37°Be' (20°C, the same below), add 4 times the amount (weight, the same below) of water to dilute, filter, and measure the diluent containing SiO 2 %=5.0%, Na 2 O% = 1.4%, its modulus n = 3.7, weigh 600g of the dilute solution, mix it with 600g of 1.8% NH under stirring 4 HCO 3 The solution is mixed (the reaction molar ratio is 1:1.0), until there is basically no SiO in the test liquid phase 2 , continue to stir for about 15 minutes, filter, wash the precipitate with water until the washing water is nearly neutral, drain, wash the precipitate with ethanol, drain, dry in an oven, and then pulverize to obtain about 27.5g of nano-silica finished product .

[0041] In the preceding filtration, the hydrated SiO 2 After precipitation, obtain filtrate about 900g, pass CO 2 Reaction, test for NH 4 HCO 3 and NaHCO 3 The mixed solution, detect the NH 4 HCO 3 Content is 0.9%, NaHCO 3 The content is 1.9%. while 1.9% NaHCO 3...

Embodiment 2

[0043] Take a sodium silicate with a Baume degree of 40°Be', add 3 times the amount of water to dilute, filter, and measure that the diluted solution contains SiO 2 % = 6.5%, Na 2 O%=2.1%, its modulus n=3.2, weighs 600g of this dilute sodium silicate solution, mixes with 700g containing 2.4% NH under stirring 4 HCO 3 The solution is mixed (the reaction molar ratio is 1:1.05), until there is basically no SiO in the test liquid phase 2 , continue to stir for about 15 minutes, filter, and use 0.5% NH 4 HCO 3 Wash the precipitate with tap water for 3 times, then wash with clean water until the washing water is nearly neutral, drain, then wash the precipitate with isopropanol several times, drain, dry in an oven, and then pulverize to obtain a finished nano-silica product of about 35g.

[0044] In the preceding filtration, the hydrated SiO 2 After precipitation, obtain filtrate about 900g, pass CO 2 Reaction, test for NH 4 HCO 3 and NaHCO 3 The mixed solution, detect the ...

Embodiment 3

[0046] Take a sodium silicate with a Baume degree of 46°Be', add 3.5 times the amount of water to dilute, filter, and measure that the diluted solution contains SiO 2 %=5.8%, Na 2 O%=2.2%, its modulus n=2.7, weigh 600g of this dilute sodium silicate solution, mix it with 700g containing 2.6% NH under stirring 4 HCO 3 The solution is mixed (reaction molar ratio is 1:1.08), until there is basically no SiO in the test liquid phase 2 , continue to stir for about 15 minutes, filter, and use 0.3% NH 4 HCO 3 The precipitate was washed 3 times with tap water and washed with 0.02M dilute H 2 SO 4 Wash the precipitate 3 times, then wash it with water until the washing water is nearly neutral, drain it, add it to n-butanol, remove the water contained in the filter cake by azeotropic distillation, stop heating after the distillation is completed, cool to room temperature and wash it with a cloth filter through a funnel, and put the filter cake in an oven to dry. After drying, a loos...

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Abstract

The invention discloses a preparation method of nano SiO2. The preparation method is characterized by taking soluble silicate M2O.nSiO2 and NH4HCO3 as raw materials to react to obtain hydrate SiO2 through precipitation, separating out filtrate through filtration, then washing the filter cake, displacing the filter cake with an organic solvent and drying the product to obtain the nano SiO2 product, wherein the filtrate mainly contains carbonate M2CO3 and NH3 and also contains little NH4HCO3; and M is an alkali metal Na or K. The preparation method has the following beneficial effects: the filtrate mainly contains M2CO3 and NH3 which can generate MHCO3 and NH4HCO3 through reaction with CO2, and MHCO3 can react with M2O.nSiO2 to obtain the hydrate SiO2 through precipitation, i.e. several components in the filtrate can regenerate the required reaction raw materials through reaction with CO2, so the materials can be recycled, thus the preparation cost of precipitated SiO2 is reduced, simultaneously fewer resources are consumed and emission is reduced.

Description

technical field [0001] The invention relates to a method for preparing nano silicon dioxide, which belongs to the technical field of new chemical materials. Background technique [0002] Nano silicon dioxide (nm-SiO 2 ) is an amorphous silica product with a particle size of nanoscale (generally 1 to 100nm). Its appearance is white powder. It is a non-toxic, odorless and non-polluting non-metallic oxide material. The quasi-granule spherical structure, because of its small size, large specific surface area, high surface energy, high interface energy in contact with polymers, and superior stability, reinforcement, thickening and thixotropy, is used in many It has a very wide range of applications, especially in rubber, special coatings, textile industry, resin-based composite material modification and other application fields, which are increasingly showing its irreplaceable role. [0003] At present, nm-SiO is produced 2 There are mainly two kinds of methods: dry method and...

Claims

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Application Information

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IPC IPC(8): C01B33/12B82Y40/00
CPCY02P20/141
Inventor 章浩龙
Owner ZHEJIANG YUDA CHEM IND
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