A kind of water-saving and energy-saving precipitation production method of silica

Abstract

The invention discloses a water-saving and energy-saving precipitation production method of silica. In the invention, water glass is used as raw material, sulfuric acid is used as precipitating agent, silica is prepared by hydrothermal method, and silicyl groups on the surface of silica particles are subjected to metal ion silicate treatment, so as to reduce silica particles. The silanol content on the surface reduces the strong hydrogen bond adsorption of silica particles to water, thereby achieving the goal of reducing production water and drying energy consumption. By adopting the technology of the present invention to produce the filter cake of washing and filtration of silica material, the water content is reduced from more than 90% before treatment to less than 75% after alkaline earth metal ion treatment. Compared with the traditional precipitation method for producing the silicon dioxide powder material, the invention has the characteristics of simple process, less water consumption in the production process, less pollution and low energy consumption. Compared with the production of silicon dioxide by the gas phase method, the invention has the characteristics of simple equipment requirements, low cost, little pollution and low energy consumption.

Description

Technical field:

[0001] The invention belongs to the technical field of inorganic powder material preparation, and particularly relates to a water-saving and energy-saving precipitation production method of silicon dioxide. Background technique:

[0002] Inorganic fillers play an important role in materials with their unique physical and chemical properties. Generally, they can toughen and reinforce a single matrix material, improve the aging resistance and corrosion resistance of products, and can mostly reduce the performance of products. cost. Precipitated silica is an important inorganic filler. It has a wide source of raw materials, easy preparation and low price, and is widely valued.

[0003] Silica powder material, commonly known as white carbon black, is an important inorganic filler because of its high purity, low density, high specific surface area, good dispersibility, surface silanol groups (silicon hydroxyl groups) and active silane bond energy It forms hydro...

Examples

Embodiment 1

[0042](1) Take 100 mL of water glass, add water to dilute to 500 mL, and stir evenly.

[0043] (2) The water glass diluent prepared in step (1) is heated to 80° C., and the pH value is adjusted to 7.0 with 10 wt % sulfuric acid to form a dilute orthosilicic acid gel.

[0044] (3) Transfer the dilute orthosilicic acid gel into a 1000 mL high-pressure reaction kettle, the stirring speed is 200 rpm, and the reaction is heated to 170° C. for 5 hours.

[0045] (4) Using high pressure nitrogen gas, 80 mL of the solution in which 2 g of magnesium sulfate was dissolved was pressurized from the auxiliary tank to the reaction kettle, and the reaction was continued at 170° C. for 1 hour.

[0046] (5) After the reaction is completed, the temperature is lowered to below 80° C., filtered with a Buchner funnel, washed until detected by barium chloride without sulfate radicals, and dried to obtain the product. Each time the filter cake was beaten and washed with 800 mL of water, and washed t...

Embodiment 2

[0049] (1) Take 100 mL of water glass, add water to dilute to 500 mL, and stir evenly.

[0050] (2) The water glass diluent prepared in step (1) is heated to 65° C., and the pH value is adjusted to 7.0 with 10 wt % sulfuric acid to form a dilute orthosilicic acid gel.

[0051] (3) The dilute orthosilicic acid gel was transferred to a 1000 mL pressure reaction kettle, the stirring speed was 200 rpm, and the reaction was heated to 140° C. for 10 hours.

[0052] (4) 80 mL of the solution in which 2.5 g of calcium nitrate was dissolved was pressurized from the auxiliary tank to the reaction kettle with high-pressure nitrogen, and the reaction was continued at 140° C. for 1 hour.

[0053] (5) After the reaction is completed, the temperature is lowered to below 80° C., filtered with a Buchner funnel, washed until the barium chloride does not contain sulfate radicals, and dried to obtain the product. Each time the filter cake was beaten and washed with 800 mL of water, and washed 4 ...

Embodiment 3

[0056] (1) Take 100 mL of water glass, add water to dilute to 500 mL, and stir evenly.

[0057] (2) The water glass diluent prepared in step (1) is heated to 85° C., and the pH value is adjusted to 7.0 with 10 wt % sulfuric acid to form a dilute orthosilicic acid gel.

[0058] (3) Transfer the dilute orthosilicic acid gel into a 1000 mL pressure reaction kettle, and the stirring speed is 200 rpm, and the reaction is heated to 200° C. for 4 hours.

[0059] (4) The temperature of the reaction kettle was lowered to 160° C., and 80 mL of a solution containing 3 g of magnesium sulfate was dissolved in the reaction kettle from the auxiliary tank, and the reaction was continued for 1 hour.

[0060] (5) After the reaction is completed, the temperature is lowered to below 80° C., filtered with a Buchner funnel, washed until the mother liquor does not contain sulfate radicals as detected by barium chloride, and dried to obtain the product. The amount of water for each washing was 800 m...

Technical field:

[0001] The invention belongs to the technical field of inorganic powder material preparation, and particularly relates to a water-saving and energy-saving precipitation production method of silicon dioxide. Background technique:

[0002] Inorganic fillers play an important role in materials with their unique physical and chemical properties. Generally, they can toughen and reinforce a single matrix material, improve the aging resistance and corrosion resistance of products, and can mostly reduce the performance of products. cost. Precipitated silica is an important inorganic filler. It has a wide source of raw materials, easy preparation and low price, and is widely valued.

[0003] Silica powder material, commonly known as white carbon black, is an important inorganic filler because of its high purity, low density, high specific surface area, good dispersibility, surface silanol groups (silicon hydroxyl groups) and active silane bond energy It forms hydro...

Examples

Embodiment 1

[0042](1) Take 100 mL of water glass, add water to dilute to 500 mL, and stir evenly.

[0043] (2) The water glass diluent prepared in step (1) is heated to 80° C., and the pH value is adjusted to 7.0 with 10 wt % sulfuric acid to form a dilute orthosilicic acid gel.

[0044] (3) Transfer the dilute orthosilicic acid gel into a 1000 mL high-pressure reaction kettle, the stirring speed is 200 rpm, and the reaction is heated to 170° C. for 5 hours.

[0045] (4) Using high pressure nitrogen gas, 80 mL of the solution in which 2 g of magnesium sulfate was dissolved was pressurized from the auxiliary tank to the reaction kettle, and the reaction was continued at 170° C. for 1 hour.

[0046] (5) After the reaction is completed, the temperature is lowered to below 80° C., filtered with a Buchner funnel, washed until detected by barium chloride without sulfate radicals, and dried to obtain the product. Each time the filter cake was beaten and washed with 800 mL of water, and washed t...

Embodiment 2

[0049] (1) Take 100 mL of water glass, add water to dilute to 500 mL, and stir evenly.

[0050] (2) The water glass diluent prepared in step (1) is heated to 65° C., and the pH value is adjusted to 7.0 with 10 wt % sulfuric acid to form a dilute orthosilicic acid gel.

[0051] (3) The dilute orthosilicic acid gel was transferred to a 1000 mL pressure reaction kettle, the stirring speed was 200 rpm, and the reaction was heated to 140° C. for 10 hours.

[0052] (4) 80 mL of the solution in which 2.5 g of calcium nitrate was dissolved was pressurized from the auxiliary tank to the reaction kettle with high-pressure nitrogen, and the reaction was continued at 140° C. for 1 hour.

[0053] (5) After the reaction is completed, the temperature is lowered to below 80° C., filtered with a Buchner funnel, washed until the barium chloride does not contain sulfate radicals, and dried to obtain the product. Each time the filter cake was beaten and washed with 800 mL of water, and washed 4 ...

Embodiment 3

[0056] (1) Take 100 mL of water glass, add water to dilute to 500 mL, and stir evenly.

[0057] (2) The water glass diluent prepared in step (1) is heated to 85° C., and the pH value is adjusted to 7.0 with 10 wt % sulfuric acid to form a dilute orthosilicic acid gel.

[0058] (3) Transfer the dilute orthosilicic acid gel into a 1000 mL pressure reaction kettle, and the stirring speed is 200 rpm, and the reaction is heated to 200° C. for 4 hours.

[0059] (4) The temperature of the reaction kettle was lowered to 160° C., and 80 mL of a solution containing 3 g of magnesium sulfate was dissolved in the reaction kettle from the auxiliary tank, and the reaction was continued for 1 hour.

[0060] (5) After the reaction is completed, the temperature is lowered to below 80° C., filtered with a Buchner funnel, washed until the mother liquor does not contain sulfate radicals as detected by barium chloride, and dried to obtain the product. The amount of water for each washing was 800 m...

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