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Process for producing easily dispersable duoparental nano-silicon dioxide

A nano-silica, silicon dioxide technology, applied in the direction of silica, silicon oxide, etc., can solve the problems of complex process, larger particle size, particle agglomeration, etc., and achieve good powder dispersion, reduced particle agglomeration, The effect of good parental performance

Inactive Publication Date: 2009-05-13
SHANDONG HINA HI TECH MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Different nano-silica preparation methods have their own characteristics, and some have different degrees of problems such as unsuitable for industrialization, complicated process, high equipment investment, and high production cost.
More importantly, the particle size of some products is too large, and the product particles are seriously agglomerated. It is difficult for users to open them with ordinary dispersion and mixing methods. In actual use, the desired effect of nano-products cannot be achieved. The main reason for these problems is that Nanoparticles have a large specific surface area and high surface energy, and are prone to particle agglomeration during preparation and use, forming secondary particles and making the particle size larger
In addition, most nano-silica does not undergo surface modification, so it is difficult to be directly used in organic systems. It does not have amphiphilic properties, which increases the difficulty of application and greatly limits the application fields of products.

Method used

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  • Process for producing easily dispersable duoparental nano-silicon dioxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Add 600g of 25wt% sodium silicate aqueous solution into a 1000ml three-necked flask, and control the temperature at 52±2°C. Add 12 g of bis(dioctyl pyrophosphate) glycolate titanate, keep the temperature and stir for 1 h.

[0023] (2) One-step reaction: Slowly and uniformly drop 12% (wt) hydrochloric acid (dropped within 40 minutes), adjust the pH value of the reaction solution to 8, stop adding acid, and stir at constant temperature for 1 hour.

[0024] (3) Two-step reaction: continue to heat up to 75±2°C, add 6g of bis(dioctylpyrophosphate) glycolate titanate, stir for 30min, and then slowly and uniformly drop in 12% (wt) dilute hydrochloric acid , until the pH value of the reaction system was adjusted to 6, stop adding acid. Maintain constant temperature and stir for 1h.

[0025] (4) The reaction liquid is filtered and washed.

[0026] (5) Heat the washed precipitated silica to 180°C in a vacuum drying oven and dry for 4 hours to obtain easily dispersible amph...

Embodiment 2

[0028] (1) Add 600g of 30% (wt) sodium silicate aqueous solution into a 1000ml three-necked flask, and control the temperature at 55±2°C. Add 20 g of bis(dioctyloxypyrophosphate) ethylene titanate, keep the temperature and stir for 1 h.

[0029] (2) One-step reaction: Slowly and uniformly drop 15% (wt) hydrochloric acid (dropped within 20 minutes), adjust the pH value of the reaction solution to 8, stop adding acid, and stir at constant temperature for 1 hour.

[0030] (3) Two-step reaction: continue to heat up to 75±2°C, add 10 g of bis(dioctyloxypyrophosphate)ethylene titanate, stir for 30 minutes, and then slowly and uniformly drop in 15% dilute hydrochloric acid until the reaction system When the pH value is adjusted to 6.5, stop adding acid. Maintain constant temperature and stir for 1h.

[0031] (4) The reaction liquid is filtered and washed.

[0032] (5) Heat the washed precipitated silica to 160°C in a vacuum drying oven and dry for 6 hours to obtain easily dispersi...

Embodiment 3

[0034](1) Add 600g of 25% (wt) sodium silicate aqueous solution into a 1000ml three-necked flask, and control the temperature at 58±2°C. Add 20g of chelated phosphate titanium coupling agent quaternary ammonium salt, keep the temperature and stir for 1h.

[0035] (2) One-step reaction: Slowly and uniformly drop 12% (wt) hydrochloric acid (dropped within 50 minutes), when the pH value of the reaction solution is adjusted to 8.5, stop adding acid, and stir at constant temperature for 1 hour.

[0036] (3) Two-step reaction: continue to heat up to 78±2°C, add 10g of chelated phosphate titanium coupling agent quaternary ammonium salt, stir for 30min, then slowly and uniformly drop in 12% dilute hydrochloric acid again until the pH value of the reaction system is adjusted At 6 o'clock, stop adding acid. Maintain constant temperature and stir for 1h.

[0037] (4) The reaction liquid is filtered and washed.

[0038] (5) Dry the washed precipitated silica in a microwave drying oven ...

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Abstract

A method for preparing amphiphilic nano silicon dioxide with good dispersity has main technical characteristics that a sodium silicate water solution with silicon dioxide weight content being 25-30% is heated to 50-60 DEG C, a titanic acid ester coupling agent is added, and stirring is performed evenly at a constant temperature; then dilute hydrochloric acid is slowly added at an even speed until the pH value reaches 8-9, and stirring is performed for 1 h; the temperature is risen to 70-80 DEG C, the titanic acid ester coupling agent is added according to 50% of the first adding amount, stirring is performed for 30 minutes, dilute hydrochloric acid is slowly added at an even speed again until the pH value of the reaction system reaches 6-7, the temperature is kept, and stirring is performed for 1 h; and the amphiphilic nano silicon dioxide powder with good dispersity can be obtained after the reaction solution is filtered, washed, heated and dried. The product has good amphiphilic performance, so as to be well compatible with organic matters in the added system, and have good hydrophilicity. The product only needs common dispersing or grinding equipment to disperse well in the nano state in the added system.

Description

technical field [0001] The invention relates to a preparation method of easily dispersible amphiphilic nano silicon dioxide. Background technique [0002] Nano-silica is commonly known as "ultrafine silica", because of its volume effect and surface effect, it exhibits specific properties in terms of magnetism, electricity, catalytic performance, adsorption performance, light absorption, thermal resistance, etc., and is widely used in catalysts. Petrochemicals, decolorizers, matting agents, rubber reinforcing agents, plastic fillers, ink thickeners, metal soft polishing agents, insulating fillers, advanced daily cosmetic fillers and spraying materials, etc. In recent years, people have paid more and more attention to its application fields and development potential, and enjoy the reputation of "industrial monosodium glutamate" and "the origin of material science". Due to the large specific surface area and high surface energy of nanoparticles, particle agglomeration is very ...

Claims

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Application Information

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IPC IPC(8): C01B33/18
Inventor 王海平董振民杨若峰于新生
Owner SHANDONG HINA HI TECH MATERIAL
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