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Method for preparing calcium-magnesia phosphate fertilizer by using waste water generated in synthetic process of 2, 4, 6-trichloropyrimidine

A technology of calcium magnesium phosphate fertilizer and trichloropyrimidine, which is applied in the field of waste water treatment and recycling, can solve environmental pollution and other problems, achieve high economic value, no damage and pollution, and protect the environment

Inactive Publication Date: 2010-01-06
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using barbituric acid as raw material, phosphorus oxychloride as chlorination agent, under the catalysis of QD composite catalyst (N, N-diethylaniline, N, N-dimethylaniline, quinoline), The waste liquid produced in the process of synthesizing 2,4,6-trichloropyrimidine contains a large amount of phosphorus (the content of phosphorus is 3.52-3.72g / L, existing in the form of phosphoric acid) and organic catalysts. If it is discharged directly, will cause serious pollution to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Recovery of catalyst

[0029] Take 500 mL of waste water generated during the synthesis of 2,4,6-trichloropyrimidine in a 1000 mL beaker, add 40 mL of distilled water, add 15.5 mL of NaOH solution with a mass concentration of 20%, and adjust the pH to 8.50. The solution is divided into two layers, the upper layer is a khaki emulsion and the lower layer is a colorless liquid. Use a separatory funnel to separate and collect the khaki-yellow emulsion in the upper layer; add 40 mL of water to the collected khaki-yellow emulsion to wash, stir, let stand, and then use a separatory funnel to separate, and the lower layer is the same as the lower layer obtained last time. liquid merger. Add 40 mL of distilled water to the upper layer of the khaki emulsion (organic phase), then distill out the organic phase by steam distillation under reduced pressure, cool for 60 min, the leaching liquid is divided into two layers, the upper layer of yellow oil is the catalyst, use a separ...

Embodiment 2

[0035] (1) Recovery of catalyst

[0036] Take 500 mL of waste water generated during the synthesis of 2,4,6-trichloropyrimidine in a 1000 mL beaker, add 40 mL of distilled water, add 15.0 mL of NaOH solution with a mass concentration of 20%, and adjust the pH to 8.00. The solution is divided into two layers, the upper layer is a khaki emulsion and the lower layer is a colorless liquid. Use a separatory funnel to separate and collect the khaki-yellow emulsion; add 40 mL of water to the khaki-yellow emulsion to wash, stir, let stand, and then use a separatory funnel to separate, and the lower layer liquid is combined with the previous lower layer liquid. Add 40 mL of distilled water to the upper layer of the khaki emulsion (organic phase), then distill out the organic phase by steam distillation under reduced pressure, cool for 60 min, the leaching liquid is divided into two layers, the upper layer of yellow oil is the catalyst, use a separatory funnel The upper khaki oily liqu...

Embodiment 3

[0042] (1) Recovery of catalyst

[0043] Take 500 mL of waste water generated during the synthesis of 2,4,6-trichloropyrimidine in a 1000 mL beaker, add 40 mL of distilled water, add 15.2 mL of NaOH solution with a mass concentration of 20%, and adjust the pH to 8.40. The solution is divided into two layers, the upper layer is a khaki emulsion and the lower layer is a colorless liquid. Use a separatory funnel to separate and collect the khaki-yellow emulsion; add 40 mL of water to the khaki-yellow emulsion to wash, stir, let stand, and then use a separatory funnel to separate, and the lower layer liquid is combined with the previous lower layer liquid. Add 40 mL of distilled water to the upper layer of the khaki emulsion (organic phase), then distill the organic phase with steam under reduced pressure, cool for 60 min, the leaching liquid is divided into two layers, and the upper layer of yellow oil is the catalyst, which is separated by liquid separation. The funnel separate...

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Abstract

The invention provides a method for preparing calcium-magnesia phosphate fertilizer by using the waste water generated in the synthetic process of 2, 4, 6-trichloropyrimidine, which comprises the following steps: separating out a catalyst in a waste liquid by a reduced pressure distillation method, and acquiring calcium phosphate by the methods of deposition and the like; then uniformly mixing the calcium phosphate and talcum powders in a mass ratio of 1.00:0.82-1.00-0.84, burning for 2-3 hours at the temperature of 800-1200 DEG C, grinding after cooling, and sieving through a 250 micrometers standard sieve to acquire the calcium-magnesia phosphate fertilizer. The prepared finished product of the calcium-magnesia phosphate fertilizer has high contents of available phosphorus, low mass fractions of free moisture and high mass fractions of alkali components, soluble silica and available magnesium; each technical index is superior to the requirement of high-class products in the Chemical Industry Standard of the People's Republic of China (GB 20413-2006). The phosphorus in the waste liquid generated in the production process of 2, 4, 6-trichloropyrimidine can be recycled (the recovery ratio of the phosphorus in the waste liquid reaches 99.77-99.86 percent, and the recovery ratio of the catalyst reaches 81-89 percent), waste is changed into valuables, and the method has good social meanings and high economic value.

Description

technical field [0001] The invention belongs to the technical field of wastewater treatment and recycling, and relates to a recycling technology for phosphorus and catalysts in wastewater generated during the synthesis of 2,4,6-trichloropyrimidine, in particular to a recycling technology for 2,4,6-trichloropyrimidine A method for preparing calcium-magnesium-phosphate fertilizer from waste water produced during pyrimidine synthesis. Background technique [0002] As one of the members of the phosphate fertilizer family, calcium magnesium phosphate fertilizer is widely used in agricultural production. Calcium magnesium phosphate fertilizer, in addition to phosphorus, also contains calcium, magnesium, silicon and other active ingredients that can be absorbed by crops. [0003] Among them, phosphorus is a component of nucleic acids and nucleotides, and is the main component of protoplasm and nucleus. Almost many important organic compounds in plants contain phosphorus. Phosphor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C05G1/00C02F9/10B01J31/02C02F1/04C02F1/66C02F103/36
Inventor 秦淑琪刘颖王建明徐延渭
Owner NORTHWEST NORMAL UNIVERSITY