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Preparation of Magnesium Hydrogen Phosphate Trihydrate in Non-aqueous System

A magnesium hydrogen phosphate trihydrate system technology, applied in the field of fine chemicals, can solve the problems that the final product is significantly affected by temperature, the pH of the system is greatly affected, and the system requires a high temperature, achieving good application prospects, high product purity, and uniform size Effect

Inactive Publication Date: 2019-04-30
OCEAN UNIV OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The neutralization method to prepare magnesium hydrogen phosphate trihydrate is to prepare MgHPO by reacting magnesium oxide with phosphoric acid under the condition that the reaction temperature is higher than 36°C. 4 ∙3H 2 O, this method has shortcomings such as being greatly affected by the activity of magnesium oxide, the final product is significantly affected by temperature, and the reaction process is long.
Phosphate metathesis method uses potassium hydrogen phosphate or sodium hydrogen phosphate to react with magnesium chloride at a temperature higher than 65°C to prepare MgHPO 4 ∙3H 2 O, this method has defects such as being greatly affected by the pH of the system and requiring a high temperature for the system
In the non-aqueous system, on the basis of in-depth research on the solubility of magnesium salts in organic systems, the reaction of using common magnesium salts, phosphoric acid, and inorganic bases as reaction materials to directly prepare micron-structured magnesium hydrogen phosphate trihydrate under constant temperature conditions No report

Method used

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  • Preparation of Magnesium Hydrogen Phosphate Trihydrate in Non-aqueous System

Examples

Experimental program
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Effect test

Embodiment approach 1

[0017] Take MgCl with a concentration of 0.2mol / L 2 ∙6H 2 O / C 2 h 5 OH solution 125ml, 4.32g concentration of 85% phosphoric acid solution was added to MgCl 2 ∙6H 2 O / C 2 h 5 OH solution, stirred in a beaker for 10 minutes to mix evenly, and then placed the beaker in an ice-water bath at 0°C. After the temperature of the mixed solution reaches 40°C, add NaOH / C with a concentration of 2.5mol / L to the system at a feed rate of 5ml / min through a peristaltic pump. 2 h 5 20ml of OH solution, stirred at a stirring rate of 200r / min, continued to stir for 30 minutes after the NaOH feeding was completed, and then stopped stirring, and placed the beaker in an ice-water bath at 0°C for 24 hours. Take out the beaker, use vacuum filtration to separate the product, use it again after distilling and purifying the organic solvent, and wash the solid product with deionized water and ethanol until there is no Cl - After detection, the solid product was placed in an oven at 60°C and drie...

Embodiment approach 2

[0019] Take MgCl with a concentration of 0.4mol / L 2 ∙6H 2 O / C 2 h 5 125ml of OH solution, 8.54g concentration of 85% phosphoric acid solution was added to MgCl 2 ∙6H 2 O / C 2 h 5 OH solution, stirred and mixed evenly in a beaker for 15 minutes, and then placed the beaker in a water bath at 20°C. After the temperature of the mixed solution reaches 20°C, add KOH / C with a concentration of 1mol / L to the system at a feed rate of 10ml / min through a peristaltic pump. 2 h 5 100ml of OH solution, stirred at a stirring rate of 300r / min, continued to stir for 30 minutes after the KOH feeding was completed, and then stopped stirring, and placed the beaker in a water bath at 20°C for 24 hours. Take out the beaker, use vacuum filtration to separate the product, use it again after distilling and purifying the organic solvent, and wash the solid product with deionized water and ethanol until there is no Cl - After detection, the solid product was placed in an oven at 60°C and dried fo...

Embodiment approach 3

[0021] Take MgCl with a concentration of 0.6mol / L 2 ∙6H 2 O / C 2 h 5 125ml of OH solution, 12.97g concentration of 85% phosphoric acid solution was added to MgCl 2 ∙6H 2 O / C 2 h 5 OH solution, stirred and mixed evenly in a beaker for 20 minutes, and then placed the beaker in a water bath at 40°C. After the temperature of the mixed solution reaches 40°C, add NaOH / C with a concentration of 0.5mol / L to the system at a feed rate of 5ml / min through a peristaltic pump. 2 h 5 300ml of OH solution, stirred at a stirring rate of 250r / min, continued to stir for 60 minutes after the NaOH feeding was completed, and then stopped stirring, and placed the beaker in a water bath at 40°C for 12 hours. Take out the beaker, use vacuum filtration to separate the product, use it again after distilling and purifying the organic solvent, and wash the solid product with deionized water and ethanol until there is no Cl - After detection, the solid product was placed in an oven at 60°C and drie...

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Abstract

The invention relates to a method of preparing magnesium hydrogen phosphate trihydrate in a non-water system and belongs to the field of fine chemicals. The method particularly comprises the following steps of: in the non-water system, preparing an organic mixed solution of magnesium salt and phosphoric acid, wherein the molar ratio of magnesium salt to phosphoric acid is 10: 1 to 1: 10; taking inorganic alkali as an alkali source, wherein the molar ratio of magnesium salt to inorganic alkali is 5: 1 to 1: 5, and the concentration of an organic solution of the inorganic alkali is 0.01-3mol / L; performing a constant temperature water bath reaction for 1-72h; and after reaction, performing suction filtration and washing of a product, and drying the product in vacuum at a certain temperature to obtain magnesium hydrogen phosphate trihydrate which is good in shape. The magnesium hydrogen phosphate trihydrate prepared by the method provided by the invention is of a fusiform crystallized micro structure, the lengths of the crystals are 15-30 microns, and the thicknesses of the crystals are 5-15 microns. The method provided by the invention is simple in preparation process and convenient to operate, has no need of complicated expensive equipment, and is expected to realize industrial production.

Description

technical field [0001] The invention relates to a method for preparing magnesium hydrogen phosphate trihydrate in a non-aqueous system, belonging to the field of fine chemicals. It specifically relates to the development of an economical and efficient method for preparing magnesium hydrogen phosphate trihydrate with regular morphology in a non-aqueous system. Background technique [0002] Magnesium hydrogen phosphate trihydrate is widely used in various fields. It is commonly used in the food industry for nutritional supplements, pH regulators, anti-caking agents, and stabilizers. Plasticizer for packaging materials, stabilizer for fertilizer ammonium bicarbonate, etc. [0003] At present, the commonly used methods for preparing magnesium hydrogen phosphate trihydrate include neutralization method and phosphate double decomposition method. The neutralization method to prepare magnesium hydrogen phosphate trihydrate is to prepare MgHPO by reacting magnesium oxide with phosp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/34
CPCC01B25/34C01P2004/61C01P2006/80
Inventor 刘丹毛丽莉王海增
Owner OCEAN UNIV OF CHINA
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