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Method for synthesizing citricacide-titatnium chelate by microwave chelation process by using new metatitanic acid precipitate

A technology of titanium citrate and metatitanic acid, applied in the preparation of carboxylate and other directions, can solve the problem of not finding metatitanic acid, and achieve the effects of high purity, simple process and stable performance

Inactive Publication Date: 2013-12-11
福建超大现代农业集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] After retrieving published patent documents and academic papers related to metatitanic acid, it was not found that using an ice solution in ice water to neutralize titanium salts with alkali to prepare metatitanic acid soluble in citric acid, and to newly precipitate metatitanic acid As a report on the synthesis of titanium citrate as a titanium source, there is no report on the synthesis of titanium citrate by microwave hot-melt chelation process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] (1) Preparation of metatitanic acid:

[0046] a. Add 1000ml of ice water at 0°C~5°C to a 1500ml beaker, and add 10ml of hydrochloric acid and 20ml of titanium tetrachloride dropwise under the stirring of an electric stirrer to generate a titanium tetrachloride hydrochloric acid solution. The sodium hydroxide solution neutralizes the titanium tetrachloride hydrochloric acid solution, the temperature of the solution is controlled at ≤5°C, and the pH value is 7.0~8.0, so that metatitanic acid is precipitated in cold water at ≤5°C;

[0047] B, the newly precipitated metatitanic acid is washed with distilled water to remove chloride ions;

[0048] c. After the metatitanic acid that has been washed to remove chloride ions is removed by a centrifuge to remove part of the adsorbed water, it can be used for acid-soluble chelation.

[0049] (2) Preparation of titanium citrate chelate:

[0050] a. Preparation of citric acid-metatitanic acid suspension mixture:

[0051]The tit...

Embodiment 2

[0057] (1) Preparation of metatitanic acid:

[0058] a. Add 1000ml of ice water at 0°C~5°C to a 1500ml beaker, and add 10ml of hydrochloric acid and 20ml of titanium tetrachloride dropwise under the stirring of an electric stirrer to generate a titanium tetrachloride hydrochloric acid solution. The sodium hydroxide solution neutralizes the titanium tetrachloride hydrochloric acid solution, the temperature of the solution is controlled at ≤5°C, and the pH value is 7.0~8.0, so that metatitanic acid is precipitated in cold water at ≤5°C;

[0059] B, the newly precipitated metatitanic acid is washed with distilled water to remove chloride ions;

[0060] c. After the metatitanic acid that has been washed to remove chloride ions is removed by a centrifuge to remove part of the adsorbed water, it can be used for acid-soluble chelation.

[0061] (2) Preparation of titanium citrate chelate:

[0062] a. Preparation of citric acid-metatitanic acid suspension mixture:

[0063] The ti...

Embodiment 3

[0069] (1) Preparation of metatitanic acid:

[0070] a. Add 1000ml of ice water at 0°C~5°C to a 1500ml beaker, and add 10ml of hydrochloric acid and 20ml of titanium tetrachloride dropwise under the stirring of an electric stirrer to generate a titanium tetrachloride hydrochloric acid solution. The sodium hydroxide solution neutralizes the titanium tetrachloride hydrochloric acid solution, the temperature of the solution is controlled at ≤5°C, and the pH value is 7.0~8.0, so that metatitanic acid is precipitated in cold water at ≤5°C;

[0071] B, the newly precipitated metatitanic acid is washed with distilled water to remove chloride ions;

[0072] c. After the metatitanic acid that has been washed to remove chloride ions is removed by a centrifuge to remove part of the adsorbed water, it can be used for acid-soluble chelation.

[0073] (2) Preparation of titanium citrate chelate:

[0074] a. Preparation of citric acid-metatitanic acid suspension mixture:

[0075] The ti...

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Abstract

The invention relates to a method for synthesizing citricacide-titatnium chelate by a microwave chelation process by using new metatitanic acid precipitate. The method is characterized in that: the new metatitanic acid precipitate is prepared by neutralizing an iced solution of titanium salt by using alkali; the new metatitanic acid precipitate replacing titanium chloride and sulfate is used as raw materials for synthesizing the citricacide-titatnium chelate; and the citricacide-titatnium chelate is synthesized by a microwave hot melting chelation process by using the new metatitanic acid precipitate as a titanium source and citric acid as an acid solvent and chelant. The synthesized citricacide-titatnium chelate is high in purity, does not contain foreign ions such as chlorine ions or sulfur ions, is stable in performance, and can be placed for a long time; titanium gel precipitate is not separated out after the citricacide-titatnium chelate is diluted; and the citricacide-titatnium chelate can be compounded with multiple kinds to metal ions and organic matter, can be reacted with peroxide to form titanium peroxide complex, and can also be compounded into various functional materials. A process is simple and is easy to control.

Description

technical field [0001] The invention belongs to a new technology for the preparation of titanium citrate, specifically relates to the use of new precipitated metatitanic acid soluble in citric acid as a titanium source, citric acid as an acid solvent and a chelating agent, and microwave heat melting A new method for synthesizing titanium citrate without chlorine and sulfide ions by chelation reaction process. Background technique [0002] Titanium citric acid has wide application prospects, such as titanium citrate has been popularized and applied as a new crop growth regulator and functional micro-fertilizer; It has been promoted and applied; titanium citrate has also been proven to have anti-tumor drug efficacy. [0003] At the same time, titanium citrate is also a precursor for preparing titanium-based functional materials such as photocatalytic self-cleaning materials, air purification materials, antibacterial materials, anti-fog materials, special electrode materials,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C59/265C07C51/41
Inventor 徐福乐翁莹冰张美娟林秀翁仁发
Owner 福建超大现代农业集团有限公司
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