Process for production of hydrazine hydrate

Patent metadata

Field	Value
Publication number	US-11225413-B2
Application number	US-201716335225-A
Country	US
Kind code	B2
Filing date	Sep 28, 2017
Priority date	Oct 3, 2016
Publication date	Jan 18, 2022
Grant date	Jan 18, 2022

Abstract

A process for the production of concentrated aqueous solutions of hydrazine hydrate includes preparation of hydrazine hydrate by a ketazine method using 50-70% hydrogen peroxide, recyclable solid acetamide and ammonium acetate activator for ketazine formation, and catalyst-free hydrolysis of ketazine to provide aqueous solutions of hydrazine hydrate in an energy efficient manner.

First claim

The invention claimed is:

1. A process for preparation of concentrated aqueous solutions of a hydrazine hydrate, the process consisting of:
(a) reacting a hydrogen peroxide solution, ammonia, and methyl ethyl ketone in the presence of an activator to form a mixture, wherein the activator comprises acetamide and ammonium acetate, and wherein the hydrogen peroxide solution, methyl ethyl ketone, and ammonia are present in a molar ratio of 1:4:3;
(b) separating the mixture from step (a) into a ketazine layer and an aqueous solution layer;
(c) concentrating the ketazine layer to obtain ketazine and recovering the methyl ethyl ketone by evaporation;
(d) purifying the ketazine by vacuum distillation to obtain a purity of more than 95%;
(e) recovering the acetamide from the aqueous solution layer by dehydration;
(f) recycling the recovered methyl ethyl ketone and the recovered acetamide to step (a);
(g) hydrolyzing the ketazine with water in a volume ratio of 1.5:1 to obtain the hydrazine hydrate and regenerating the methyl ethyl ketone;
(h) recycling the methyl ethyl ketone to the step (a), and
(i) purifying and concentrating the hydrazine hydrate obtained in step (g) to obtain 80% concentrated hydrazine hydrate in one cycle, and wherein the hydrolysis is catalyst free.

2. The process according to claim 1 , wherein the acetamide used in step (a) is a crystalline solid.

3. A process for preparation of concentrated aqueous solutions of a hydrazine hydrate, the process consisting of:
(a) reacting a hydrogen peroxide solution, ammonia, and methyl ethyl ketone in the presence of an activator to form a mixture, wherein the activator comprises acetamide and ammonium acetate, and wherein the hydrogen peroxide solution, methyl ethyl ketone, and ammonia are present in a molar ratio of 1:4:3;
(b) separating the mixture from step (a) into a ketazine layer and an aqueous solution layer;
(c) concentrating the ketazine layer to obtain ketazine and recovering the methyl ethyl ketone by evaporation;
(d) purifying the ketazine by vacuum distillation to obtain a purity of more than 95%;
(e) recovering the acetamide from the aqueous solution layer by dehydration;
(f) recycling the recovered methyl ethyl ketone and the recovered acetamide to step (a);
(g) hydrolyzing the ketazine with water in a volume ratio of 1.5:1 to obtain the hydrazine hydrate and regenerating the methyl ethyl ketone;
(h) recycling the methyl ethyl ketone to the step (a), and
(i) purifying and concentrating the hydrazine hydrate obtained in step (g) to obtain 80% concentrated hydrazine hydrate in one cycle, and wherein the hydrolysis is catalyst free;
wherein the acetamide recovered from dehydration step (e) is further purified by centrifugation or filtration under vacuum to get crystalline solid before being recycled in step (f).

4. The process according to claim 1 , wherein the hydrogen peroxide solution is a 50 to 70 weight % H 2 O 2 solution.

5. The process according to claim 4 , wherein step (a) is carried out at temperatures ranging from 0 to 60° C.

6. The process according to claim 4 , wherein step (c) evaporation is carried out at temperatures ranging from 85 to 110° C.

7. The process according to claim 4 , wherein step (d) vacuum distillation is carried out at temperatures ranging from 75 to 100° C.

8. The process according to claim 4 , wherein the hydrolysis step (g) is carried out under a pressure ranging from 2 to 20 bars, and at a temperature ranging from 150 to 200° C.

9. The process according to claim 4 , wherein step (d) vacuum distillation is carried out at temperatures ranging from 80-90° C.

10. The process according to claim 4 , wherein the hydrolysis step (g) is carried out under a pressure ranging from 8 to 12 bars.

11. The process according to claim 4 , wherein the hydrolysis step (g) is carried out at a temperature ranging from 175 to 200° C.

Assignees

• Council Scient Ind Res
• Gujarat Alkalies And Chemicals Ltd

Inventors

• Mamidpelliwar Pradeep Kumar
• Kajjam Ravindranath
• Madabhushi Radhakrishna
• Ugle Ashutosh
• Pathak Shobha Rajendra
• Murthy Vijaya Garikapati
• Srinivasan Thyagarajan
• Veeraiah Gannoji
• Mamilla Shyam Sunder
• Sarma Vanka Uma Maheshwara
• Yellamraju Parthasaradhy
• Sinha Sunil
• Shah Manish Babulal
• Shah Nikhilkumar Navinchandra
• Patel Shailesh Ashabhai
• Patel Gautam Punjabhai

Classifications

• C01B21/16 Primary

  Hydrazine; Salts thereof · CPC title

• C07C249/16

  of hydrazones · CPC title

• Y02P20/582

  Recycling of unreacted starting or intermediate materials · CPC title

• C07C251/88

  having also the other nitrogen atom doubly-bound to a carbon atom, e.g. azines · CPC title

• Y02P20/10

  Process efficiency · CPC title