Phosphine and sodium trimetaphosphate preparation method

A technology of sodium trimetaphosphate and phosphine, applied in chemical instruments and methods, phosphine, phosphorus compounds, etc., can solve the problems of low phosphine yield, consumption of large element phosphorus, environmental pollution, etc. Reduce the production of long-chain high molecular weight chemicals, increase the content, and ensure the effect of purity

Inactive Publication Date: 2013-08-21
江苏先锋生物基技术研究中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of phosphine in traditional industrial production is not high, it needs to consume a large amount of elemental phosphorus, and the purity is also low, which often requires further purification, and it is easy to cause environmental pollution

Method used

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  • Phosphine and sodium trimetaphosphate preparation method
  • Phosphine and sodium trimetaphosphate preparation method
  • Phosphine and sodium trimetaphosphate preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A mixture of sodium phosphite and sodium phosphate prepared from 25 g of phosphorous acid, 26 g of phosphoric acid (85.7%) and 21 g of sodium hydroxide (96%) was evaporated to dryness under reduced pressure at 70°C to constant weight to obtain the theoretical amount of trivalent phosphorus sodium salt and pentavalent phosphorus sodium salt anhydrous mixture 55.8g, the P of the mixed salt III / P V Calculated value is 1.34, and the sodium-phosphorus ratio calculated value is 0.947, and the pH value of the solution of 1% is 3.34 with the concentration that this mixed salt is made, and this mixed salt 30g is placed in the there-necked flask that nitrogen inlet and outlet are housed, with Replace the air in the flask with nitrogen. After half an hour, keep the nitrogen flow, the pressure is slightly higher than the standard atmospheric pressure, and then raise the temperature of the mixed salt to 400oC. In the absorption bottle of mercury solution (2-3%), the released phosp...

Embodiment 2

[0027] Sodium phosphite and sodium phosphate salt mixture (P III / P V=1.001) evaporated to dryness under reduced pressure at 70°C to constant weight to obtain 54.3 grams of theoretical anhydrous mixed salt. The calculated value of the sodium-phosphorus ratio of the mixed salt is 0.950. The pH value of solution is 3.48, and this mixed salt 10g is placed in the there-necked flask that nitrogen inlet and outlet are housed, replaces air in the flask with nitrogen, after half an hour, keeps nitrogen flow, and pressure is slightly greater than standard atmospheric pressure, then mixture is heated up to 350°C, the material melts and bubbles at this temperature, the released phosphine is brought into the absorption bottle filled with mercury chloride solution (2-3%) by nitrogen, and the released phosphine is dried by the precipitate in the absorption liquid The final weight and the amount of mercury ion loss in the solution are determined. After the bubbling ends, continue heating at...

Embodiment 3

[0029] Sodium phosphite and sodium phosphate salt mixture (P III / P V =1.000) evaporated to dryness under reduced pressure at 70°C to constant weight to obtain 90.2 grams of theoretical anhydrous mixed salt. The calculated value of the sodium-phosphorus ratio of the mixed salt is 0.990. The pH value of solution is 3.51, and this mixed salt 20g is placed in the there-necked flask that nitrogen inlet and outlet are housed, replaces air in the flask with nitrogen, after half an hour, keeps nitrogen flow, and pressure is slightly greater than standard atmospheric pressure, then mixture is heated up to 310°C, the material melts and bubbles at this temperature, and the released phosphine is brought into the absorption bottle filled with mercuric chloride solution (2-3%) by nitrogen gas, and the released phosphine is dried by the precipitate in the absorption liquid The final weight and the amount of mercury ion loss in the solution are determined. After the bubbling ends, continue ...

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Abstract

The invention discloses a phosphine and sodium trimetaphosphate preparation method, wherein a mixture of a sodium salt of trivalent phosphate and a sodium salt of pentavalent phosphate is heated to a temperature of 300-400 DEG C to be subjected to a disproportionation and condensation reaction under nitrogen protection so as to obtain phosphine and sodium trimetaphosphate, wherein a sodium-phosphorus ratio of the mixture is 0.93-0.99, and a ratio (P<III>/P<V>) of trivalent phosphorus atoms to pentavalent phosphorus atoms of the mixture is 1-1.34. With the method, decomposition and oxidation of an intermediate product phosphine produced from the reaction are avoided, the important chemical industry material phosphine is collected, the condensation reaction for sodium trimetaphosphate production is promoted in the presence of the phosphine, the high purity sodium trimetaphosphate is obtained, long chain high molecule weight substance production is avoided, the sodium trimetaphosphate process is shortened, environmental pollution is reduced, production energy consumption is reduced, production cost is reduced, the whole production process and the final product meet food industry requirements, and comprehensive utilization is achieved.

Description

technical field [0001] The invention relates to a method for preparing phosphine and sodium trimetaphosphate from a mixture of trivalent phosphorus sodium salt and pentavalent phosphorus sodium salt. Background technique [0002] Sodium trimetaphosphate and phosphine are important materials in the chemical industry. Sodium trimetaphosphate is widely used in industry, especially in the process of starch esterification, the field of fine chemical industry needs high-purity sodium trimetaphosphate, the water insoluble matter is less than 0.5%, does not contain or contains a small amount of phosphate. The traditional preparation of sodium trimetaphosphate is to pass sodium orthophosphate at 500 degrees through an intermediate product, mainly disodium dihydrogen pyrophosphate (acid pyrophosphate), to generate a reactant containing trimetaphosphate. This reactant Often mixed with water-insoluble polyphosphate (Maddrell's salt). When the raw material is heated slowly, a large...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/06C01B25/445
Inventor 周跃辉施春锦徐霞
Owner 江苏先锋生物基技术研究中心有限公司
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