Method for extracting urotropine from oxadiazine wastewater

A technology for urotropine and oxadiazine, which is applied in the field of extracting urotropine, can solve problems such as difficulty in separating ammonium sulfate and urotropine, and achieve the effect of accelerating dissolution

Pending Publication Date: 2022-08-09
NINGXIA DONGWU AGROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a kind of solution that solves the problem that ammonium sulfate and urotropine are difficult to separate in the oxadiazine waste wate

Method used

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  • Method for extracting urotropine from oxadiazine wastewater
  • Method for extracting urotropine from oxadiazine wastewater
  • Method for extracting urotropine from oxadiazine wastewater

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0041] Example 1,

[0042] Add 1000g of evil twozine wastewater to the single-mouth pear bottle for heating and decompression and dehydration. The negative pressure is -0.08 ~ -0.09MPa, and the dehydration temperature is 60 to 80 ℃. The water bath cools to 30 ° C, and then use ice water to cool down to 10 ° C.

[0043] Filter the lower salt pump to dry. The main ingredient of the filter cake is ammonium sulfate. The main components of the filter liquid are Ulot, ammonium sulfate, and water. Continue heating and decompression dehydration, adjust the negative pressure to -0.08 ~ -0.09MPa, dehydrate temperature of 60-90 ℃, until the moisture is basically removed, and the methanol is added, and the temperature is stirred at about 60 ° C for 1h.

[0044] Filter the ammonium sulfate in the methanol solution while it is hot. The ulot product is dissolved in methanol. The Ulotne methanol solution is added to the single-port pear-shaped bottle for heating and decompression of the methanol....

Example Embodiment

[0046] Example 2,

[0047] Add 2000g of evil twozine wastewater to the single-mouth pear-shaped bottle for heating and decompression and dehydration, adjust the negative pressure to -0.08 ~ -0.09MPa, dehydrate temperature of 60 to 80 ℃, until a large amount of salt stops from the water, and the precipted salt will be salt. Stir in the water bath to cool to 30 ° C, then use ice water to cool down to 10 ° C.

[0048] Filter the lower salt to dry to dry. The main ingredient of the filter cake is ammonium sulfate; the main component of the filter liquid is Ulot, ammonium sulfate, and water, and then add Ulot, ammonium sulfate, and water to a single -mouth pear -shaped bottle Continue heating and decompression dehydration, adjust the negative pressure to -0.08 ~ -0.09MPa, dewater temperature of 60-90 ℃, until the water is basically removed, 600g of methanol, and the temperature is stirred at about 60 ° C for 1h.

[0049] Filter the ammonium sulfate in the methanol solution while it is ...

Example Embodiment

[0051] Example 3,

[0052] Add 3000g of wicked azine wastewater to the single-mouth pear-shaped bottle for heating and decompression dehydration, adjust the negative pressure to -0.08 ~ -0.09MPa, dewater temperature of 60 to 80 ℃ until a large amount of salt stops from the water, and the precipted salt will be salt. Stir in the water bath to cool to 30 ° C, then use ice water to cool down to 10 ° C.

[0053] Filter the lower temperature material to dry. The main component of the filter cake is ammonium sulfate. The main components of the filter liquid are Ulot, ammonium sulfate, and water. Heating and decompression dehydration, adjustment of negative pressure -0.08 ~ -0.09MPa, dehydration temperature of 60-90 ℃, until the water is basically removed, and 900g of methanol is added to keep the temperature stir at about 60 ° C for 1h.

[0054] Filter the ammonium sulfate in the methanol solution while it is hot. The ulot product is dissolved in methanol. The Ulotne methanol solution i...

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Abstract

The invention discloses a method for extracting urotropin from oxadiazine wastewater, which comprises the following steps of: adding oxadiazine wastewater into a single-opening pear-shaped bottle, heating, decompressing and dehydrating until a large amount of salt is separated out from water, stirring, cooling to 30 DEG C in a water bath, cooling to 10 DEG C by using ice water, carrying out suction filtration on the cooled material until the material is dry, and filtering to obtain the urotropin. Adding the prepared material into a single-opening pear-shaped bottle, continuously heating and dehydrating under reduced pressure until moisture is basically removed, adding methanol, keeping the temperature at about 60 DEG C, stirring for 1 hour, filtering out ammonium sulfate in a methanol solution while the solution is hot, dissolving urotropine in methanol, adding the urotropine methanol solution into the single-opening pear-shaped bottle, heating and dehydrating under reduced pressure to remove methanol, and filtering to obtain a urotropine-methanol solution; according to the technical scheme, ammonium sulfate in the oxadiazine wastewater is taken as a raw material to obtain viscous urotropine which cannot be subjected to suction filtration, 5%-20% of ammonia water is added into the viscous urotropine, stirring is performed for 30 min, and then a large amount of urotropine solid is separated out at the normal temperature, the problem that ammonium sulfate in the oxadiazine wastewater is difficult to separate from urotropine is solved, and the urotropine with very high purity is obtained.

Description

Technical field [0001] The invention involves the field of pesticide intermediate synthesis technology, which is a method for extracting Ulot products from evil diezine wastewater. Background technique [0002] Ulotopine, also known as Symnaphorethramine, is C6H12N4, which is an organic compound. [0003] Ulot, white humidity crystal powder or colorless and luster diamond crystals, combustible. The melting point is 263 ℃. If you exceed this melting point, sublimate and decompose, but do not melt. When the temperature is increased to 300 ° C, the hydrogen cyanide is released. When the temperature rises again, it is decomposed to methane, hydrogen and nitrogen. Relative density 1.331 (20 / 4 ℃). Flash point 50 ° C. Almost odorless, sweet and bitter. Soluble in water, methanol and chlorine. It is difficulty in carbon chloride, acetone, benzene, and ether, and insoluble in petroleum ether. [0004] Evilzide wastewater discharge not only pollutes the environment, but also causes waste o...

Claims

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Application Information

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IPC IPC(8): C07D487/18C02F9/10C02F101/38
CPCC07D487/18C02F9/00C02F1/04C02F1/001C02F2001/007C02F2101/38Y02A50/30
Inventor 吴根龙杨亚民方慧慧吴建明郭鹏梁佳梅胡卫东
Owner NINGXIA DONGWU AGROCHEM
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