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Method for producing perphosphoric acid and crystal orthophosphoric acid by microwave heating

A technology of microwave heating and superphosphoric acid, which is applied in the field of phosphoric acid, can solve the problems of high impurity content, high production cost, and easy overheating of products, and achieve the effects of convenient transportation, low cost, and high thermal efficiency

Active Publication Date: 2014-02-19
WENGFU (GRP) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the two, the cost of the product produced by the wet process route is relatively low, but the product has a high impurity content, and at the same time, it is prone to overheating during concentration, and its use is limited. It is mainly used for the production of agricultural chemical fertilizers and the production of feed phosphoric acid. Salt: The product produced by the thermal process route has good quality and low impurity content, but high energy consumption, large pollution, and high production cost. It is mainly used to prepare various industrial phosphorus chemical products
But so far, there is no report on the production of superphosphoric acid and crystalline phosphoric acid by the method of concentrated phosphoric acid, and there is no related patent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take 600g of wet-process phosphoric acid purification acid with a concentration of 85% by mass and put it into a microwave reactor, raise the temperature to 320°C at a rate of 5°C / min, and keep it warm for 1h at a stirring rate of 100rpm. Then, the phosphoric acid solution after water removal was cooled down, and at a temperature of 70°C and a stirring rate of 80rpm, adding hydrogen peroxide 3g, after reacting for 50 minutes, the temperature was lowered to cool the reaction product, and a colorless transparent viscous liquid was obtained which was superphosphoric acid. After testing: P in superphosphoric acid 2 o 5 Content 81.0%.

[0022] Blend the superphosphoric acid obtained above with phosphoric acid or dilute it to orthophosphoric acid (H 3 PO 4 The mass percentage is 98.9%), under stirring, the temperature was lowered to 25°C, and 5 g of orthophosphoric acid seed crystals were added to obtain a crystalline orthophosphoric acid.

Embodiment 2

[0024] Take 600g of wet-process phosphoric acid purification acid with a concentration of 85% by mass and put it into a microwave reactor, raise the temperature to 300°C at a rate of 4°C / min, and keep it warm for 1.5h at a stirring rate of 60rpm. Then, the phosphoric acid solution after water removal was cooled down, and at a temperature of 90°C and a stirring rate of 120rpm, adding hydrogen peroxide 2 g, reacted for 30 minutes, cooled down the reaction product, and obtained a colorless transparent viscous liquid superphosphoric acid. After testing: P in superphosphoric acid 2 o 5 The content is 79.9%.

[0025] Blend the superphosphoric acid obtained above with phosphoric acid or dilute it to orthophosphoric acid (H 3 PO 4 The mass percentage is 98.2%), under stirring, the temperature was lowered to 22°C, and 9 g of orthophosphoric acid seed crystals were added to obtain a crystalline orthophosphoric acid.

Embodiment 3

[0027] Take 600g of wet-process phosphoric acid purification acid with a concentration of 80% by mass and put it into a microwave reactor, raise the temperature to 220°C at a rate of 3°C / min, and keep it warm for 2h at a stirring rate of 150rpm. Then, the phosphoric acid solution after water removal was cooled down, and at a temperature of 80°C and a stirring rate of 100rpm, adding hydrogen peroxide 0.6g, after reacting for 40 minutes, the temperature was lowered to cool the reaction product, and a colorless transparent viscous liquid was obtained which was superphosphoric acid. After testing: P in superphosphoric acid 2 o 5 The content is 75.6%.

[0028] Blend the superphosphoric acid obtained above with phosphoric acid or dilute it to orthophosphoric acid (H 3 PO 4 The mass percentage is 97.1%), under stirring, the temperature was lowered to 15°C, and 3 g of orthophosphoric acid seed crystals were added to obtain a crystalline orthophosphoric acid.

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Abstract

The invention discloses a method for producing perphosphoric acid and crystal orthophosphoric acid by microwave heating, which is characterized by comprising the following steps: placing phosphoric acid purified acid by a wet method or phosphoric acid by a hot method in a microwave reactor, performing microwave heating while stirring to the temperature of 220-320 DEG C and insulating for 1-2 hours, continuously cooling while stirring, adding hydrogen peroxide for decolouring, and reacting for 20-50 minutes and cooling the reaction product to obtain colorless transparent viscous liquid as perphosphoric acid; cooling the perphosphoric acid to the temperature of 15-25 DEG C, crystallizing while stirring, blending by phosphoric acid while crystallizing or diluting by desalinized water to obtain orthophosphoric acid, adding orthophosphoric acid seeds for inducing crystallization to obtain the crystal orthophosphoric acid. According to the invention, the liquid state phosphoric acid is changed to a solid state, thereby the phosphoric acid can be directly used by the users, perphosphoric acid or crystal orthophosphoric acid can be diluted to the required concentration by adding water, the product is convenient for transportation, the storage and logistics cost can be reduced, so that the phosphoric acid possesses substantial social benefit and economic benefit.

Description

technical field [0001] The invention relates to phosphoric acid, in particular to a method for producing superphosphoric acid and crystalline orthophosphoric acid by microwave heating. Background technique [0002] As we all know, superphosphoric acid is a kind of orthophosphoric acid (H 3 PO 4 ) and pyrophosphate (H 4 P 2 o 7 ) between the eutectic, industrially known as superphosphoric acid. it has P 2 o 5 High content, less corrosive than orthophosphoric acid, low freezing point, liquid at room temperature, significant supercooling properties, strong chelating ability for metal impurity ions, and no sludge during storage and long-distance transportation. Superphosphoric acid is not only an important chemical intermediate product, but also an important chemical product. It is widely used in the manufacture of pigments, pharmaceuticals, spices, leather, and flame retardants. It can also be used to produce liquid fertilizers or Suspended fertilizers can also be used...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B15/16C01B25/234
Inventor 刘飞解田
Owner WENGFU (GRP) CO LTD