Integrated synergistic recovery method for sodium sulfate and methanol in pirimiphos-methyl production wastewater

A technology for producing pirimiphos-methyl and waste water, which is applied in chemical instruments and methods, separation/purification of hydroxyl compounds, alkali metal sulfite/sulfite, etc., which can solve waste of water resources, sulfate by-products, and environmental impact Large scale, waste water generation and other problems, to achieve the effect of improving salt efficiency, improving the environment and reducing production costs

Pending Publication Date: 2022-04-01
HUNAN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, rectification and recovery of methanol requires high energy consumption and waste water; a large amount of sodium sulfate enters the waste water, which has a great impact on the environment, wasting water resources and recyclable sulfate by-products

Method used

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  • Integrated synergistic recovery method for sodium sulfate and methanol in pirimiphos-methyl production wastewater
  • Integrated synergistic recovery method for sodium sulfate and methanol in pirimiphos-methyl production wastewater

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] An integrated synergistic recovery method of sodium sulfate and methanol in pirimiphos-methyl production wastewater, such as figure 1 shown, including the following steps:

[0046] Get 2 liters of high-concentration sodium sulfate waste water produced by the pyrimidinol production workshop. After analysis, the sodium sulfate content in the waste water is 25%; get 1 kg of hydrous methanol collected in the pyrimidinol production process, and the analyzed moisture content is 2%. The process of recovering sodium sulfate from the wastewater and realizing wastewater reuse and methanol dehydration is as follows:

[0047] (1) Under stirring conditions, the high-concentration sodium sulfate wastewater was cooled to 2°C, crystallized for 60min, and filtered at a temperature of 20°C to obtain 1593g of wet solids (sodium sulfate decahydrate) and 829g of filtrate (filtrate I ).

[0048] (2) with 42g (5% of filtrate quality) the filtrate (filtrate I) that obtains in xylene extracti...

Embodiment 2

[0054] An integrated synergistic recovery method of sodium sulfate and methanol in pirimiphos-methyl production wastewater, such as figure 1 shown, including the following steps:

[0055] Get the high-concentration sodium sulfate waste water that 2 liters of pyrimidinol production workshops produce, sodium sulfate content is 15% through analysis waste water, and mix with the 457g filtrate II that obtains in embodiment 1 step (4); Get 1kg pyrimidinol production process The collected aqueous methanol was analyzed to have a moisture content of 1.8%.

[0056] (1) High-concentration sodium sulfate wastewater (containing the 457g filtrate II obtained in step (4) of Example 1) was stirred and cooled to -5°C, crystallized for 30min, and filtered at a temperature of 15°C to obtain 1275g of wet solids (sodium sulfate decahydrate) and 1275 g of the filtrate (filtrate I).

[0057] (2) with 102g (8% of filtrate quality) the filtrate (filtrate I) that obtains in xylene extraction step (1)...

Embodiment 3

[0063] An integrated synergistic recovery method of sodium sulfate and methanol in pirimiphos-methyl production wastewater, such as figure 1 shown, including the following steps:

[0064] Get 2 liters of high-concentration sodium sulfate wastewater produced by the pyrimidinol production workshop, and the sodium sulfate content in the waste water is analyzed to be 24%; get 1 kg of hydrous methanol collected in the pyrimidinol production process, and the analyzed moisture content is 2.1%.

[0065] (1) High-concentration sodium sulfate wastewater was stirred and cooled to 10°C, crystallized for 120 minutes, and filtered at a temperature of 10°C to obtain 1588g of wet solid (sodium sulfate decahydrate) and 878g of filtrate (filtrate I).

[0066] (2) Heat the wet solid (sodium sulfate decahydrate) obtained in step (1) to 100°C, carry out distillation and concentration, stop heating when steaming 715g of water, and the gained concentrate is naturally cooled to 36°C at room temperatu...

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Abstract

The invention discloses an integrated synergistic recovery method of sodium sulfate and methanol in pirimiphos-methyl production wastewater, which comprises the following steps: cooling sodium sulfate wastewater to-5-10 DEG C for crystallization, carrying out solid-liquid separation at the temperature of less than or equal to 20 DEG C, and carrying out heating, distillation concentration and centrifugal treatment on obtained sodium sulfate decahydrate to obtain sodium sulfate decahydrate; and leaching the obtained anhydrous sodium sulfate crude product with a sodium sulfate solution, carrying out centrifugal treatment, drying to obtain a sodium sulfate solid, and purifying water-containing methanol by using the sodium sulfate solid to obtain anhydrous methanol. According to the integrated synergetic recovery method for sodium sulfate and methanol in pirimiphos-methyl production wastewater, through combined treatment of cooling crystallization, low-temperature filtration, distillation concentration and leaching filtration, zero discharge of wastewater can be realized, the environment can be improved, energy can be saved, consumption can be reduced, byproducts (sodium sulfate, methanol, xylene and water) can be synergistically recovered, and the method is suitable for industrial production. And the economic benefits of enterprises are improved.

Description

technical field [0001] The invention belongs to the technical field of resource utilization of industrial by-products and zero discharge of waste water, and relates to an integrated synergistic recovery method of sodium sulfate and methanol in pirimiphos-methyl production waste water. Background technique [0002] Pirimiphos-methyl (alias Andre, PP511) is a pyrimidine insecticide, which is recommended by the World Health Organization (WHO) and the United Nations Food and Agriculture Organization (FAO) as a safe pesticide variety for grain storage and household hygiene pest control . Compared with highly toxic aluminum phosphide, pirimiphos-methyl has a broad insecticidal spectrum, rapid action, and a drug effect of up to 45-70 weeks. It has gradually become an excellent substitute for highly toxic organophosphorus pesticides. Pyrimidinol is a key intermediate synthesized in the production process of pirimiphos-methyl, and has high economic value. The synthetic route is as f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/10C01D5/00C07C29/76C07C31/04
Inventor 曹金艳王胜得陈灿尤瑶瑶吴曼
Owner HUNAN CHEM RES INST
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