CN107602447B - Production process of tetramethyl piperidone - Google Patents

Abstract

The invention discloses a production process of tetramethyl piperidone, which comprises the following specific steps: preparing acetone with the mass concentration of 98% from 99.99% and circularly used acetone, pumping the acetone into an amination kettle, adding 0.364Kg of ammonium nitrate, adding 4.26Kg of ammonia gas, heating to 40 ℃ for reaction for 4h, heating the amination kettle to 56.5 ℃ for distillation for 4h, feeding acetone steam into a condenser pipe, rectifying the condensed acetone, and pumping the rectified acetone into a storage tank for circular use; stirring the materials in the amination kettle, standing, layering water and tetramethylpiperidone, discharging water, drying by using calcium chloride, filtering, distilling, crystallizing, centrifuging and drying the tetramethylpiperidone in the amination kettle to obtain the finished product of tetramethylpiperidone. The waste, waste water and waste gas generated by the process for producing the tetramethylpiperidone can be completely recycled, and the environmental pollution is avoided.

Description

Production process of tetramethyl piperidone

Technical Field

The invention belongs to the technical field of fine chemical engineering, and particularly relates to a production process of tetramethyl piperidone.

Background

The tetramethyl piperidone is a multipurpose chemical raw material and is a necessary production raw material for rubber, plastic, pharmacy, paint and other industries. The main raw materials for producing the tetramethylpiperidone are acetone and ammonia gas, wherein the acetone is easily soluble in water, flammable and volatile; ammonia gas is a flammable and explosive gas, has strong corrosivity, and can be poisoned after being inhaled by people. Therefore, when the tetramethylpiperidone is produced, air and water are easily polluted and harm is caused to people. In order to avoid the harm to people and environment in the production process, a green and environment-friendly process for producing tetramethylpiperidone is needed to be developed.

Disclosure of Invention

The invention solves the technical problem of providing a production process of tetramethyl piperidone, which has simple process and low cost.

The invention adopts the following technical scheme for solving the technical problems, and the production process of the tetramethylpiperidone is characterized by comprising the following specific steps of:

(1) adding 49.5Kg of acetone with the mass concentration of 99.99 percent and 45.1Kg of acetone circularly used into a liquid preparation tank to prepare acetone with the mass concentration of 98 percent, and pumping the acetone into an acetone receiving kettle for later use;

(2) pumping the prepared acetone with the mass concentration of 98% into an amination kettle, adding 0.364Kg of ammonium nitrate and then 4.26Kg of ammonia gas, and heating to 40 ℃ for reaction for 4 hours;

(3) heating the amination kettle to 56.5 ℃, distilling for 4h, introducing acetone vapor into a condensation pipe, rectifying condensed acetone, and pumping into a storage tank for recycling;

(4) stirring the materials in the amination kettle, standing, layering water and tetramethylpiperidone, discharging water, drying by using calcium chloride, storing the concentrate as a raw material for sale, and using the concentrate which cannot be absorbed by water as an additive for producing lubricating grease;

(5) and filtering, distilling, crystallizing, centrifuging and drying the tetramethylpiperidone in the amination kettle to obtain the finished product of the tetramethylpiperidone.

The invention designs a green production process to avoid harm to human and environment in the production process of tetramethyl piperidone, aiming at the problem that ammonia is not easy to recover, ammonia is not excessively introduced in the amination process to ensure complete reaction of ammonia, acetone is excessively added to ensure full reaction of ammonia, then excessive acetone is evaporated out, the evaporated acetone is condensed and rectified, and finally the acetone is recycled and reused. The acetone and ammonia react to generate water and tetramethyl piperidone, the two products can be separated, but the acetone and ammonia are dissolved in water, the water can cause harm to the environment, calcium chloride is used for adsorbing and recovering waste water, the water-containing calcium chloride can be used as a raw material for sale, and finally, a concentrate which cannot be absorbed by water can be used as an additive for producing lubricating grease.

The waste, waste water and waste gas generated by the process for producing the tetramethylpiperidone can be completely recycled, and the environmental pollution is avoided.

Detailed Description

The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.

Example 1

A production process of tetramethyl piperidone comprises the following specific steps:

(1) adding 49.5Kg of acetone with the mass concentration of 99.99 percent and 45.1Kg of acetone circularly used into a liquid preparation tank to prepare acetone with the mass concentration of 98 percent, and pumping the acetone into an acetone receiving kettle for later use;

(2) pumping the prepared acetone with the mass concentration of 98% into an amination kettle, adding 0.364Kg of ammonium nitrate and then 4.26Kg of ammonia gas, and heating to 40 ℃ for reaction for 4 hours;

(3) heating the amination kettle to 56.5 ℃, distilling for 4h, introducing acetone vapor into a condensation pipe, rectifying condensed acetone, and pumping into a storage tank for recycling;

(4) stirring the materials in the amination kettle, standing, layering water and tetramethylpiperidone, discharging water, drying by using calcium chloride, storing the concentrate as a raw material for sale, and using the concentrate which cannot be absorbed by water as an additive for producing lubricating grease;

(5) filtering, distilling, crystallizing, centrifuging and drying the tetramethylpiperidone in the amination kettle to obtain a finished product, namely the tetramethylpiperidone with the content of 97 percent and white crystal appearance.

The invention relates to an environment-friendly process for producing tetramethylpiperidone, which is mainly characterized by no discharge of waste gas, waste water and waste material, uncomplicated process equipment, easily controlled process parameters, higher recovery rate of finished products and stable product quality.

The foregoing embodiments illustrate the principles, principal features and advantages of the invention, and it will be understood by those skilled in the art that the invention is not limited to the foregoing embodiments, which are merely illustrative of the principles of the invention, and that various changes and modifications may be made therein without departing from the scope of the principles of the invention.

Claims (1)

1. A production process of tetramethyl piperidone is characterized by comprising the following specific steps:

(1) adding 49.5Kg of acetone with the mass concentration of 99.99 percent and 45.1Kg of acetone circularly used into a liquid preparation tank to prepare acetone with the mass concentration of 98 percent, and pumping the acetone into an acetone receiving kettle for later use;

(2) pumping the prepared acetone with the mass concentration of 98% into an amination kettle, adding 0.364Kg of ammonium nitrate and then 4.26Kg of ammonia gas, and heating to 40 ℃ for reaction for 4 hours;

(3) heating the amination kettle to 56.5 ℃, distilling for 4h, introducing acetone vapor into a condensation pipe, rectifying condensed acetone, and pumping into a storage tank for recycling;

(4) stirring the materials in the amination kettle, standing, layering water and tetramethylpiperidone, discharging water, drying by using calcium chloride, storing the concentrate as a raw material for sale, and using the concentrate which cannot be absorbed by water as an additive for producing lubricating grease;

(5) and filtering, distilling, crystallizing, centrifuging and drying the tetramethylpiperidone in the amination kettle to obtain the finished product of the tetramethylpiperidone.