A kind of hydrazine hydrate treatment method after synthesis of benzyl carbazate

A technology of benzyl carbazate and a treatment method is applied in the field of hydrazine hydrate treatment after the synthesis of benzyl carbazate, which can solve problems such as reducing environmental protection pressure, and achieve the effects of reducing environmental protection pressure, controllable degradation, and improving activity.

Active Publication Date: 2022-03-15
JINGBO AGROCHEM TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention overcomes the problem of synthetic benzyl carbazate hydrazine hydrate wastewater treatment, low-concentration hydrazine hydrate wastewater is degraded by a nickel-based catalyst, and high-concentration hydrazine hydrate is used mechanically, which reduces the pressure on environmental protection and meets the requirements of green circular economy

Method used

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  • A kind of hydrazine hydrate treatment method after synthesis of benzyl carbazate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Transfer 376g of benzyl carbazate synthesis reaction solution into a 500ml reaction bottle, cool down the system, when the temperature is ≤60°C, stop cooling, start negative pressure distillation, slowly heat up, control the vacuum of the system to 0.07-0.09MPa, and distill The end point temperature is 90°C, no distillate is separated out, and 63.5g fraction Ⅰ is obtained

[0021] (2) After Fraction I was collected, the temperature of the system continued to rise, the vacuum degree was controlled to be ≥ 0.095 MPa, the end point temperature of distillation was 120°C, no distillate was separated out, and 11.6 g of Fraction II was obtained.

[0022] (3) Add 1% Raney nickel catalyst into the reaction flask for fraction I, and react at a controlled temperature of 30° C. for 6 hours.

[0023] (4) After the reaction finishes, filter and collect the catalyst, and the catalyst can be recycled.

[0024] (5) Fraction II was added together with 1.7 g of alkali additive potass...

Embodiment 1

[0027] The reaction solution that the fraction II of Example 1 participates in the synthesis of benzyl carbazate is processed:

[0028] (1) Transfer 381g of benzyl carbazate synthesis reaction solution into a 500ml reaction bottle, cool down the system, when the temperature is ≤60°C, stop the cooling, start negative pressure distillation, slowly raise the temperature, control the vacuum degree of the system to 0.07-0.09MPa, and distill The end point temperature was 90°C, no distillate was separated out, and 57.2 g of fraction I were obtained.

[0029] (2) After Fraction I was collected, continue to heat up the system, control the vacuum degree ≥ 0.095MPa, and the distillation end point temperature was 120°C. No distillate was separated out, and 13.4g of Fraction II was obtained.

[0030] (3) Fraction I was added to the reaction flask with the recovered Raney nickel catalyst filtered after the reaction in Example 1, and the reaction was carried out at a controlled temperature o...

Embodiment 2

[0035] The reaction solution that the fraction II of embodiment 2 participates in the synthesis of benzyl carbazate is processed:

[0036] (1) Transfer 379g of synthetic benzyl carbazate reaction solution into a 500ml reaction bottle, cool down the system, when the temperature is ≤60°C, stop cooling, start negative pressure distillation, slowly heat up, control the vacuum degree of the system to be 0.07-0.09MPa, and distill The end point temperature is 90°C, no distillate is separated out, and 67.2g fraction I is obtained

[0037] (2) After Fraction I was collected, the temperature of the system continued to rise, the vacuum degree was controlled to be ≥0.095 MPa, the end point temperature of the distillation was 120°C, no distillate was detected, and 12.8 g of Fraction II was obtained.

[0038] (3) Fraction I was added to the reaction flask with the recycled Raney nickel catalyst filtered after the reaction in Example 2, and the reaction was carried out at a controlled temper...

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Abstract

The invention belongs to the field of synthesis of benzyl carbazate, in particular to a method for treating hydrazine hydrate after the synthesis of benzyl carbazate. Fraction I (hydrazine hydrate content ≤ 2%) and fraction II (hydrazine hydrate content 50-70%) are obtained by segmental negative pressure distillation, and a nickel-based catalyst is added to fraction I to destroy hydrazine hydrate and further reduce the content of hydrazine hydrate , the hydrazine hydrate in fraction II can be directly applied to the reaction of synthesizing benzyl carbazate. The invention overcomes the problem of synthetic benzyl carbazate hydrazine hydrate wastewater treatment, the low-concentration hydrazine hydrate wastewater is degraded by a nickel-based catalyst, and the high-concentration hydrazine hydrate is used mechanically, thereby reducing the pressure on environmental protection and meeting the requirements of green circular economy.

Description

technical field [0001] The invention belongs to the field of synthesis of benzyl carbazate, in particular to a method for treating hydrazine hydrate after the synthesis of benzyl carbazate. Background technique [0002] Benzyl carbazate is a key intermediate for the synthesis of the pesticide indoxacarb. The current industrial route is mainly dimethyl carbonate route, and its synthetic route is as follows: [0003] [0004] Its synthesis involves the reaction of hydrazine hydrate. After the reaction, the liquid is directly separated, resulting in the enrichment of hydrazine hydrate in the wastewater, which is difficult to use directly, and the COD discharged reaches 450,000. [0005] Wastewater rich in hydrazine hydrate will cause eutrophication of the water body, affect the quality of the water body, and endanger the survival of the human body and organisms in severe cases. Therefore, in the chemical production process, the wastewater rich in hydrazine hydrate is strict...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C281/02
CPCY02P20/584
Inventor 冯培良王平薄蕾芳刘建成王杰秀韦能春
Owner JINGBO AGROCHEM TECH CO LTD
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