A kind of treatment method of hexaphenoxycyclotriphosphazene industrial waste water

A technology of hexaphenoxycyclotriphosphazene and industrial wastewater, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problem of high treatment cost, achieve COD value reduction, significant economic benefits and environmental protection benefit effect

Active Publication Date: 2021-06-04
MIANYANG TEACHERS COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For the wastewater in the form of sodium phenate, it is necessary to add acid to convert it into phenol before extraction. After extraction, add a stripping agent to convert the phenol into sodium phenate and remove it. In addition, the more expensive special extraction agent, and procedures such as oil-water separation, etc., the treatment cost is too high high

Method used

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  • A kind of treatment method of hexaphenoxycyclotriphosphazene industrial waste water
  • A kind of treatment method of hexaphenoxycyclotriphosphazene industrial waste water
  • A kind of treatment method of hexaphenoxycyclotriphosphazene industrial waste water

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Effect test

Embodiment 1

[0028] Such as figure 1 Shown, the treatment method of hexaphenoxy cyclotriphosphazene industrial waste water of the present invention comprises the following steps:

[0029] (1) Weigh 300g of waste water and place it in a flask, transfer it to a vacuum evaporation device for evaporation and crystallization, the vacuum degree is -90KPa, and the initial heating temperature is 65°C. When the condensed water outlet speed slows down and the boiling weakens, gradually heat up to 90°C, stop heating when the waste water evaporates 80% to 90% of its total water volume, and take out the solid-liquid mixture after cooling, about 110g;

[0030] (2) add 150mL ethanol in above-mentioned solid-liquid mixture, dissolve sodium phenate, suction filtration, and wash with 50mL ethanol, obtain sodium-chlor white crystal after drying, quality is 61.4g, the SEM photograph of described sodium-chlor and energy Spectral analysis results such as figure 2 and 3 shown;

[0031] (3) The above-mention...

Embodiment 2

[0034] (1) Weigh 300g of waste water and place it in a flask, transfer it to a vacuum evaporation device for evaporation and crystallization, the vacuum degree is -80KPa, and the initial heating temperature is 65°C. When the condensed water outlet speed slows down and the boiling weakens, gradually heat up to 90°C, stop heating when the waste water evaporates 80% to 90% of its total water volume, and take out the solid-liquid mixture after cooling, about 110g;

[0035] (2) Add 150 mL of methanol to the above solid-liquid mixture, dissolve sodium phenate, filter with suction, wash with 50 mL of methanol, and obtain white crystals of sodium chloride after drying, with a quality of 60.2 g and a purity of 98%;

[0036] (3) Transfer the above-mentioned filtrate containing sodium phenate to a vacuum evaporator for evaporation and concentration. The vacuum degree is -80~-90Kpa, and the initial heating temperature is 35°C. Raise the temperature of the water bath to 90°C, and when the ...

Embodiment 3

[0039] Adopt the same steps as steps (1) to (3) in Example 1 to prepare the sodium phenate crude product, adopt ultraviolet spectrophotometry to record the mass fraction of sodium phenate in the described sodium phenate crude product at a wavelength of 290nm to be 55%, get 30g For crude sodium phenoxide, add 9 mL of deionized water, heat to 70°C to dissolve, and when the room temperature is cooled to 30-35°C, add sodium phenoxide trihydrate seed crystals, crystals begin to precipitate, and after 30 minutes, transfer to a refrigerator for crystallization at -5°C After 12 hours, a prismatic white sodium phenate crystal was obtained, which was analyzed and detected by ultraviolet spectroscopy, and the crystal composition was sodium phenate trihydrate, with a mass of 16.3 g and a purity of 97%.

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Abstract

A method for treating hexaphenoxycyclotriphosphazene industrial wastewater, comprising the following steps: heating and evaporating the hexaphenoxycyclotriphosphazene industrial wastewater to obtain a solid-liquid mixture; adding organic Sodium phenate is dissolved in a solvent, and sodium chloride crystals are obtained after solid-liquid separation, washing and drying; the solution containing sodium phenate obtained after the solid-liquid separation is heated and evaporated to obtain a sodium phenoxide concentrate; After adding deionized water or crystallization mother liquor, heating and dissolving, after cooling, crystal seeds are added for crystallization, and sodium phenoxide trihydrate crystals are obtained through separation; the crystallization mother liquor is the mother liquor after sodium phenoxide crystallization. The present invention can effectively recover sodium phenate and sodium chloride in waste water, and the obtained sodium phenate and sodium chloride have relatively high purity, can be recycled and utilized, can also significantly reduce the COD value of waste water, and have significant economic and environmental benefits .

Description

technical field [0001] The invention relates to the technical field of industrial wastewater treatment, in particular to a treatment method for hexaphenoxycyclotriphosphazene industrial wastewater. Background technique [0002] Hexaphenoxycyclotriphosphazene is a halogen-free flame retardant with excellent performance and environmental friendliness. It is widely used in PC, PC / ABS resin, PPO, nylon and other products, and is also widely used in plasticizers and lubricants. additives and auxiliaries. [0003] Hexaphenoxycyclotriphosphazene is usually prepared by the reaction of hexachlorocyclotriphosphazene and sodium phenate. In industrial production, in order to ensure the full reaction of hexachlorocyclotriphosphazene and obtain a higher yield, sodium phenate needs The excess is about 5%, and the post-treatment of the product is to adopt water washing and recrystallization to obtain relatively pure hexaphenoxycyclotriphosphazene. The wastewater generated in the productio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/235C07C37/84C01D3/14
CPCC01D3/14C07C37/84C07C39/235
Inventor 黎国兰李松陈彦君贺礼青李昭伦
Owner MIANYANG TEACHERS COLLEGE
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