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Preparation method of phosphate

A technology of phosphate and dihydrogen phosphate, which is applied in the direction of phosphate, phosphorus oxyacid, etc., can solve the problems such as the report of no ether compounds, and achieve the effect of reducing the concentration and content of chloride ions

Inactive Publication Date: 2014-08-06
WUHAN INSTITUTE OF TECHNOLOGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0022] Through the review of domestic and foreign patents and published publications, no reports on the use of ether compounds for the preparation of phosphates have been found.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Mix phosphoric acid, water, and ferrous chloride, then add ethyl vinyl ether and stir at 85-95°C until the yield of phosphate is 50%, and the amount of phosphoric acid is 1mol. The phosphoric acid: ferrous chloride: ethyl The molar ratio of vinyl ether is 1:3.6 / 2:4.2, and then the resulting reaction mixture is evaporated at 90~100°C until the phosphate solution is supersaturated at the crystallization temperature, and then cooled, at a temperature of 30~40°C Crystallization, filtration, washing, and drying yielded 25 g of phosphate, and the chloride ion content was determined to be 0.18%.

Embodiment 2

[0037] Mix phosphoric acid, water, and sodium chloride, then add diphenyl ether and stir at 5-20°C until the yield of phosphate is 10%, and the amount of phosphoric acid is 1mol. The moles of phosphoric acid: sodium chloride: diphenyl ether The ratio is 1:0.13:9.4, and then the resulting reaction mixture is evaporated at 60~70°C until the phosphate solution is supersaturated at the crystallization temperature, then cooled, crystallized at 0~20°C, filtered, washed, and dried. 1 g of phosphate was obtained, and the chloride ion content was determined to be 0.01%.

Embodiment 3

[0039] Mix phosphoric acid, water, and calcium chloride, then add tert-butyl ether and stir at 170-200°C until the yield of phosphate is 90%, and the amount of phosphoric acid is 1mol. The phosphoric acid: calcium chloride: tert-butyl ether The molar ratio is 1:9.8 / 2:0.14, and then the resulting reaction mixture is evaporated at 140~150°C until the phosphate solution is supersaturated at the crystallization temperature, then cooled, crystallized at 45~59°C, filtered, After washing and drying, 5 g of phosphate was obtained, and the chloride ion content was determined to be 0.2%.

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PUM

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Abstract

The invention relates to a method for preparing phosphate. First, mix phosphoric acid, water and metal hydrochloride, then add ether compounds and stir at 5-200°C until the yield of phosphate is 10% or above, and then mix the obtained The reaction mixture is evaporated at 60-150°C until the phosphate solution is supersaturated at the crystallization temperature, then cooled, crystallized at 0-59°C, filtered, washed and dried to obtain the phosphate product. The beneficial effect of the present invention lies in that phosphoric acid, ether compounds and metal hydrochloride are used as raw materials to synthesize phosphate in aqueous solution, and hydrogen ions and chloride ions in the solution are consumed to generate phosphate. Since the chloride ion forms a more stable carbon-chloride chemical bond and separates from the water phase, the concentration of chloride ion in the solution is greatly reduced, and the content of chloride ion in the synthesized phosphate is low, realizing the use of metal hydrochloride in the production of phosphate The purpose of replacing metal oxides, carbonates or hydroxides.

Description

Technical field [0001] The present invention involves a preparation method of phosphate, which is the field of inorganic chemical industry. Background technique [0002] Phosphoric acid is very widely used due to its good chemical properties.Industrially used as a buffer, bacterial culture culture, power battery raw materials, high -temperature adhesives, etc., can also be used as raw materials for polyphonate and polarized phosphate;All types of economy crops.At present, the preparation method of phosphate is mainly to neutralize method: [0003] Neutralizing the use of metal oxides, carbonate, and hydroxide as raw materials and phosphate to react in neutral reactions. The reaction process is as follows. First of all, oxides: [0004] M 2 O 3 + 6H 3 PO 4 = 2m (h 2 PO 4 Cure 3 + 3H 2 O [0005] M, such as aluminum and three -valent iron, because the three -valent metal phosphate is a compound, the oxide and phosphate will produce a part of the incurable salt wrapped on the surfac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/26
Inventor 张勇杨三可周莹莹王景峰张英英胡宏李红林禹志宏薛绍秀
Owner WUHAN INSTITUTE OF TECHNOLOGY