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A kind of preparation method of silica sol for acrylonitrile catalyst

A technology of acrylonitrile catalyst and silica sol, which is applied in the direction of silicon oxide and silicon dioxide, and can solve the problems of inability to use acrylonitrile catalyst carrier and low added value

Active Publication Date: 2017-06-23
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, most domestic silica sol products can only be used as binders in foundry and other industries, with low added value, and cannot be used as acrylonitrile catalyst carriers.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1. Ingredients: industrial sodium silicate (modulus 2.5) is mixed with water to prepare 1000 grams of a 3% aqueous solution of silicon dioxide, and industrial sulfuric acid is mixed with water to prepare a 10% aqueous solution for several standbys;

[0023] 2. Prepare sol bottom liquid: add the sodium silicate aqueous solution of step (1) into the reaction tank, keep the stirring speed at 150 rpm, at normal temperature, add the sulfuric acid aqueous solution prepared in step (1) at a speed of 500ml / min to The pH was 9.3, and the temperature was increased to 95°C for 1 hour.

[0024] 3. Regeneration of strong acid cation exchange resin: prepare hydrochloric acid into a 4% solution, soak the cation exchange resin for 4 hours, release the hydrochloric acid, and then wash it with deionized water until the conductivity is below 200μs / cm for use;

[0025] 4. Preparation of silicic acid: Add water to industrial sodium silicate (modulus 3.3) to prepare a 3% aqueous solution of ...

Embodiment 2

[0030] 1. Ingredients: industrial sodium silicate (modulus 2.5) is mixed with water to prepare 1000 grams of a 4% aqueous solution of silicon dioxide, and industrial sulfuric acid is added with water to prepare an 8% aqueous solution for several standbys;

[0031] 2. Preparation of sol bottom liquid: add the sodium silicate of step (1) into the reaction tank, keep the stirring speed at 180 rpm, at normal temperature, add the aqueous sulfuric acid solution prepared in step (1) to pH at a speed of 550ml / min is 9.5, and the temperature is raised to 95°C for 1 hour;

[0032] 3. Regeneration of strong acid cation exchange resin: prepare hydrochloric acid into a 4% solution, soak the cation exchange resin for 4 hours, release the hydrochloric acid, and then wash it with deionized water until the conductivity is below 200μs / cm for use;

[0033] 4. Preparation of silicic acid: Add water to industrial sodium silicate (modulus 3.3) to prepare a 4% aqueous solution of silicon dioxide. Wh...

Embodiment 3

[0038] 1. Ingredients: industrial sodium silicate (modulus 2.0) is mixed with water to prepare 1000 grams of a 5% aqueous solution of silicon dioxide, and industrial sulfuric acid is mixed with water to prepare a 10% aqueous solution for several standbys;

[0039] 2. Prepare sol bottom liquid: add the sodium silicate of step (1) into the reaction tank, keep stirring speed, 200 rev / min, at normal temperature, add the aqueous sulfuric acid solution prepared in step (1) to pH9 at a speed of 500ml / min .0, heat up to 90°C for 1 hour;

[0040] 3. Regeneration of strong acid cation exchange resin: prepare hydrochloric acid into a 4% solution, soak the cation exchange resin for 4 hours, release the hydrochloric acid, and then wash it with deionized water until the conductivity is below 200μs / cm for use;

[0041] 4. Preparation of silicic acid: Add water to industrial sodium silicate (modulus 3.25) to prepare a 5% aqueous solution of silicon dioxide. When preparing silicic acid, first ...

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Abstract

The invention discloses a preparation method of ludox for an acrylonitrile catalyst. The method comprises: adding sulfuric acid aqueous solution into industrial sodium silicate aqueous solution with a silicon dioxide content of 3-5 wt percent until pH is 9.0-9.5, heating up to 90-95 DEG C, and then keeping warm for 1-2 hours to form ludox base solution; adding water into industrial sodium silicate with a modulus of 3.0-3.3, preparing aqueous solution with a silicon dioxide content of 3-5 wt percent, suspending cation exchange resin by using deionized water, then adding sodium silicate and controlling outlet pH to be 2-3 after ion exchange to obtain silicic acid, adding the silicic acid into the prepared ludox base solution at a speed of 100-200ml / min, keeping pH to be 9-9.5, keeping warm for 1-2 hours under the temperature of 90-95 DEG C, and then cooling to normal temperature; performing ion exchange on a product by using strong-acidity cation exchange resin regenerated by hydrochloric acid, meanwhile keeping pH to be 1-2, and after exchange, adding ammonium hydroxide and adjusting pH to be 9-9.5; finally adding a dispersing agent into the prepared ludox, and performing ultrafiltration and concentration to obtain the ludox. The prepared ludox has the mean grain size of 20-25nm, the sodium ion content less than 0.05 percent, the concentration of 40-50 percent and the viscosity less than 20cps.

Description

technical field [0001] The present invention relates to a preparation method of silica sol, more particularly, to a preparation method of silica sol for acrylonitrile catalyst. Background technique [0002] Silica sol is a stable colloidal solution in which silica nano-colloidal particles are dispersed in water. The average particle size of silica sol is generally 8-100 nm, and its shape is approximately spherical, and the content of silica is generally 20%-30%. . [0003] Acrylonitrile is an important organic chemical raw material, which is produced by ammoxidation of propylene. In order to obtain higher activity, it is generally prepared as a fluidized bed catalyst, and acrylonitrile catalyst usually uses silica sol as a carrier. [0004] The acrylonitrile catalyst is generally composed of a metal salt and a silica sol to form a slurry with a solid content of about 50%, which is prepared into a fluidized bed catalyst by spray drying. At present, the common acrylonitrile ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/14
Inventor 胡毅于海斌周靖辉刘峰孙彦民姜雪丹季超潘月秋
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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