Method for separating and purifying byproduct isopropyl hydrazine produced in preparation of hydrazine hydrate from ketazine

Abstract

The invention discloses a method for separating and purifying the byproduct isopropyl hydrazine produced in the preparation of hydrazine hydrate from ketazine. The method comprises the following steps: distilling the byproduct, namely isopropyl hydrazine waste liquid separated in the production process of hydrazine hydrate via a ketazine method, controlling the temperature of a distillation kettleto be 100-108 DEG C and a distillation temperature to be 95-100 DEG C, and distilling off low-boiling-point substances to obtain a concentrated isopropyl hydrazine solution at the bottom of the kettle; subjecting the kettle-bottom isopropyl hydrazine solution obtained after distillation to standing and layering, removing a water phase, then extracting an oil phase containing isopropyl hydrazine,distilling an extract, controlling a distillation temperature to be 106-108 DEG C after an extracting agent is distilled out, and collecting a fraction to obtain isopropyl hydrazine. According to themethod, the byproduct isopropyl hydrazine waste liquid containing isopropyl produced in the preparation of hydrazine hydrate from ketazine is separated and purified through the four steps consisting of distillation, standing and layering, extraction and distillation, so the low-value isopropyl hydrazine organic waste liquid is converted into high-quality medical raw materials and intermediates, and thus, problems in treatment of the organic waste liquid produced in the preparation of hydrazine hydrate from ketazine are solved.

Description

technical field

[0001] The invention relates to a method for separating and purifying a by-product of ketazine hydrazine hydrate, in particular to a method for separating and purifying isopropylhydrazine, a by-product of ketazine hydrazine hydrate. Background technique

[0002] Hydrazine hydrate, also known as: hydrazine hydrate, chemical formula is N 2 h 4 ·H 2 O, a strong reducing agent, is an important chemical raw material, and is also a raw material for medicine, pesticides, dyes, foaming agents, developers, and antioxidants; it is used for deoxidizing boiler water, producing high-purity metals, and synthesizing and reducing organic compounds. , separation of rare elements, and also used in the manufacture of rocket fuel and explosives. With the advancement of technology and the development of society, the application fields of hydrazine hydrate are constantly expanding in recent years. The production methods of hydrazine hydrate mainly include Raschig method, urea m...

Examples

Embodiment 1

[0029] Add 500 kg of a solution containing 10.30% isopropylhydrazine into the distillation still, heat to carry out distillation, control the temperature of the still still at 100-105°C, control the distillation temperature at 95-98°C, and the concentration of isopropylhydrazine after distillation is 78.25% , standing for stratification, standing for 0.5h, there is an obvious phase interface, the stratification is over, add the oil phase to the extraction kettle, add 300kg ether for extraction three times each time, combine the extracts into the distillation kettle, distill out the ether, and collect at 750mmHg 49.95kg of isopropylhydrazine was obtained from the fraction at 106-108°C, the content of which was analyzed to be 95.52%, and the calculated yield was 92.64%.

Embodiment 2

[0031]Add 500 kg of a solution containing 10.05% isopropylhydrazine into the still, heat to carry out distillation, control the temperature of the still still at 100-108°C, control the distillation temperature at 95-100°C, and the concentration of isopropylhydrazine after distillation is 80.5% , standing for stratification, standing for 1h, there is an obvious phase interface, the stratification is over, add the oil phase to the extraction kettle, add 350kg ether for extraction three times each time, combine the extracts into the distillation kettle, distill out the ether, and collect at 750mmHg 46.96kg of isopropylhydrazine was obtained from the fraction at 106-108°C, the content of which was analyzed to be 98.84%, and the calculated yield was 94.55%.

Embodiment 3

[0033] Add 500 kg of a solution containing 11.3% isopropylhydrazine into the distillation still, heat to carry out distillation, control the temperature of the still still at 101-108°C, control the distillation temperature at 95-100°C, and the concentration of isopropylhydrazine after distillation is 81.62% , standing for stratification, standing for 0.5h, there is an obvious phase interface, the stratification is over, add the oil phase to the extraction kettle, add 300kg ether for extraction three times each time, combine the extracts into the distillation kettle, distill out the ether, and collect at 750mmHg 53.0kg of isopropylhydrazine was obtained from the fraction at 106-108°C, the content of which was analyzed to be 98.50%, and the calculated yield was 92.39%.

technical field

[0001] The invention relates to a method for separating and purifying a by-product of ketazine hydrazine hydrate, in particular to a method for separating and purifying isopropylhydrazine, a by-product of ketazine hydrazine hydrate. Background technique

[0002] Hydrazine hydrate, also known as: hydrazine hydrate, chemical formula is N 2 h 4 ·H 2 O, a strong reducing agent, is an important chemical raw material, and is also a raw material for medicine, pesticides, dyes, foaming agents, developers, and antioxidants; it is used for deoxidizing boiler water, producing high-purity metals, and synthesizing and reducing organic compounds. , separation of rare elements, and also used in the manufacture of rocket fuel and explosives. With the advancement of technology and the development of society, the application fields of hydrazine hydrate are constantly expanding in recent years. The production methods of hydrazine hydrate mainly include Raschig method, urea m...

Examples

Embodiment 1

[0029] Add 500 kg of a solution containing 10.30% isopropylhydrazine into the distillation still, heat to carry out distillation, control the temperature of the still still at 100-105°C, control the distillation temperature at 95-98°C, and the concentration of isopropylhydrazine after distillation is 78.25% , standing for stratification, standing for 0.5h, there is an obvious phase interface, the stratification is over, add the oil phase to the extraction kettle, add 300kg ether for extraction three times each time, combine the extracts into the distillation kettle, distill out the ether, and collect at 750mmHg 49.95kg of isopropylhydrazine was obtained from the fraction at 106-108°C, the content of which was analyzed to be 95.52%, and the calculated yield was 92.64%.

Embodiment 2

[0031]Add 500 kg of a solution containing 10.05% isopropylhydrazine into the still, heat to carry out distillation, control the temperature of the still still at 100-108°C, control the distillation temperature at 95-100°C, and the concentration of isopropylhydrazine after distillation is 80.5% , standing for stratification, standing for 1h, there is an obvious phase interface, the stratification is over, add the oil phase to the extraction kettle, add 350kg ether for extraction three times each time, combine the extracts into the distillation kettle, distill out the ether, and collect at 750mmHg 46.96kg of isopropylhydrazine was obtained from the fraction at 106-108°C, the content of which was analyzed to be 98.84%, and the calculated yield was 94.55%.

Embodiment 3

[0033] Add 500 kg of a solution containing 11.3% isopropylhydrazine into the distillation still, heat to carry out distillation, control the temperature of the still still at 101-108°C, control the distillation temperature at 95-100°C, and the concentration of isopropylhydrazine after distillation is 81.62% , standing for stratification, standing for 0.5h, there is an obvious phase interface, the stratification is over, add the oil phase to the extraction kettle, add 300kg ether for extraction three times each time, combine the extracts into the distillation kettle, distill out the ether, and collect at 750mmHg 53.0kg of isopropylhydrazine was obtained from the fraction at 106-108°C, the content of which was analyzed to be 98.50%, and the calculated yield was 92.39%.

Images