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Micron-sized iron-doped silicon dioxide as well as preparation method and application thereof

A silicon dioxide, micron-scale technology, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, inorganic chemistry, etc., can solve problems such as iron ion precipitation, shutdown and maintenance that cannot be completely solved, and achieve Easy access to raw materials, reduced operating costs, and high activity

Pending Publication Date: 2021-03-19
冷水江三Ａ新材料科技有限公司
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  • Summary
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  • Description
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  • Application Information

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Problems solved by technology

However, the blockage of the liquid-phase desulfurizer due to salting out is also inevitable, resulting in downtime for maintenance
[0005] For the above-mentioned technical problems, those skilled in the art have also invented many chelating agents that reduce iron ion precipitation, but can not completely solve the problem of iron ion precipitation

Method used

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  • Micron-sized iron-doped silicon dioxide as well as preparation method and application thereof

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preparation example Construction

[0026] As an example, the preparation method of micron-scale iron-doped silicon dioxide is characterized in that: comprising the following steps:

[0027] S1: Prepare sodium silicate aqueous solution and ferric acetate aqueous solution; the silicon dioxide content of the sodium silicate aqueous solution is 3-5%wt, and the iron oxide content of the ferric acetate aqueous solution is 1-2%wt.

[0028] S2: Add EDTA to the aqueous sodium silicate solution in step S1 at 25-30°C and stir for 20-30 minutes, heat up to 40-50°C and add iron acetate aqueous solution at a rate of 100-200ml / min to pH8-9. The amount of EDTA added is 1-3%wt of silicon dioxide.

[0029] S3: add hydrogen peroxide to the material in step S2 at 80-90° C. and keep it warm for 40-60 minutes.

[0030] The amount of hydrogen peroxide added is 5-10% of the silicon dioxide mass.

[0031] S4: washing the material in step S3 with water until the water resistivity is below 1000Ω / cm.

[0032] S5: Add the materials in s...

Embodiment 1

[0035] S1: Prepare 1000 g of an aqueous sodium silicate solution with a silicon dioxide content of 3%wt, and prepare an aqueous solution of iron oxide with a 2%wt iron oxide content for later use;

[0036] S2: Add 0.9 g of EDTA to the aqueous solution of sodium silicate in step S1 at 25°C and stir for 30 minutes, raise the temperature to 48°C and add iron acetate at a rate of 100ml / min to pH 8.2;

[0037] S3: Warm up the material in step S2 to 80°C, add 3g of hydrogen peroxide and keep it warm for 40 minutes;

[0038] S4: washing the material in step S3 until the water resistivity is below 1000Ω / cm;

[0039] S5: Add the materials in step S4 to the reaction kettle, add water to adjust the carbon dioxide content to 10%, add 0.9g of polycarboxylate water reducer, heat up to 100°C, stir and beat for 40 minutes; stir and keep warm for 2-4 hours.

[0040] S6: Step S5 is dried and pulverized to obtain micron-sized iron-doped silica.

Embodiment 2

[0042] S1: Prepare 1000 g of sodium silicate aqueous solution with a silicon dioxide content of 4%wt, and prepare an aqueous solution of iron oxide with a 1.5%wt iron oxide content for later use;

[0043] S2: Add 0.8 g of EDTA to the aqueous solution of sodium silicate in step S1 at 28°C and stir for 25 minutes, raise the temperature to 40°C and add iron acetate at a rate of 150ml / min to pH 8.5;

[0044] S3: Warm up the material in step S2 to 90°C, add 3.2g of hydrogen peroxide and keep it warm for 50 minutes;

[0045] S4: washing the material in step S3 until the water resistivity is below 1000Ω / cm;

[0046] S5: Add the materials in step S4 to the reactor, add water to adjust the carbon dioxide content to 8%, add 0.8g of polycarboxylate water reducer, heat up to 95°C, stir and beat for 35 minutes; stir and keep warm for 2-4 hours.

[0047] S6: Step S5 is dried and pulverized to obtain micron-sized iron-doped silica.

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Abstract

The invention provides micron-sized iron-doped silicon dioxide as well as a preparation method and application thereof. The preparation method comprises the following steps: preparing a sodium silicate aqueous solution and an iron acetate aqueous solution; mixing the solutions, adjusting the pH value, keeping the temperature, washing the solutions with water, adding the materials into a reaction kettle, adding water to prepare carbon dioxide with the content of 5-10%, adding a water reducing agent, stirring and pulping the mixture for 30-40 minutes, and heating the mixture to 90-100 DEG C; stirring the mixture with heat perservation for 2-4 hours; and drying and crushing the mixture to obtain the micron-sized iron-doped silicon dioxide. According to the invention, sodium silicate and ferric acetate are used as raw materials, so that the method has the advantages of easily available raw materials, low cost and facilitation of industrial production. The micron-sized iron-doped silicon dioxide serving as a desulfurization catalyst has the advantages that the suspension property in water is good, iron loss is avoided, the operation cost is reduced and the like. Because the surface of the silicon dioxide has a large number of surface hydroxyl groups and has natural adsorption performance on metal ions, in the liquid-phase desulfurization process of the iron-doped silicon dioxide, due to the action of the surface hydroxyl groups, the iron ions always keep relatively high activity.

Description

technical field [0001] The invention relates to the technical field of silicon dioxide preparation methods, in particular to micron-sized iron-doped silicon dioxide and its preparation method and application. Background technique [0002] Sulfur element widely exists in fossil fuels, and the acid gas pollutants in the petrochemical process come from the production of natural gas excavation, coal chemical industry, refining chemical industry and so on. It will affect the subsequent production process, such as catalyst poisoning, pipeline corrosion, so it is necessary to control the sulfur content in process materials and products. [0003] The removal and treatment of hydrogen sulfide is an important process in petrochemical production. As the country's environmental protection requirements become increasingly strict, petrochemical tail gas treatment is a problem that must be solved. In petrochemical production, the treatment methods for removing hydrogen sulfide include liq...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/193B01J23/745
CPCC01B33/193B01J23/745C01P2006/14C01P2006/12
Inventor 胡颖妮
Owner 冷水江三Ａ新材料科技有限公司
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