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Preparation method of acetone oxime

A technology of acetone oxime and acetone, which is applied in the field of acetone oxime production technology, can solve the problems of complex process, long process, and environmental pollution, and achieve the effects of good solubility, improved conversion rate, and simple preparation method

Inactive Publication Date: 2019-04-09
江苏艾科维科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the industrial acetone oxime production processes mainly include hydroxylamine hydrochloride method, hydroxylamine sulfate method and sodium nitrite method. However, these processes are complicated, the process is long, and a large number of by-products are produced, polluting the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The preparation method of present embodiment acetone oxime comprises the following steps:

[0019] 1) In the reactor, 17.4g of acetone is dissolved in 45.2g of isopropanol to obtain an acetone solution, and after adding 1.2g of TS-1 molecular sieve catalyst and 33.4g of mass concentration in the acetone solution, it is after mixing evenly Obtain the pre-reaction solution.

[0020] 2) the reactor is sealed, the pre-reaction solution prepared in step 1) is heated to 50° C., slowly dripping 29 g concentration of 30% hydrogen peroxide solution with a microfeed pump, the time for adding hydrogen peroxide solution is After 2 hours, the reaction time is 5 hours at 50°C and 0.1MPa pressure to obtain the reaction solution, the reaction solution is filtered, the filtrate is rectified under normal pressure, 70-85°C is the isopropanol slip-out liquid, and the extraction agent ethyl acetate Extract three times to obtain the extract of acetone oxime, and rectify the extract under no...

Embodiment 2

[0022] The preparation method of present embodiment acetone oxime comprises the following steps:

[0023] 1) In the reactor, 17.4g acetone is dissolved in 60g hexanaphthene to make acetone solution, and 1.8gTS-1 molecular sieve catalyst, 40g mass concentration are added in the acetone solution and mixed to obtain the preliminary The reaction solution.

[0024] 2) the reactor is sealed, the pre-reaction solution prepared in step 1) is heated to 60° C., slowly dripping 35 g concentration of 30% hydrogen peroxide solution with a micro-feed pump, and the dripping time of hydrogen peroxide solution is After 3 hours, the reaction time is 7 hours at 60°C and 0.7MPa pressure to obtain the reaction solution, the reaction solution is filtered, the filtrate is rectified under normal pressure, and the cyclohexane slips out at 70-85°C, and the extraction agent dichloromethane Extract three times to obtain the extract of acetone oxime, and rectify the extract under normal pressure to obtai...

Embodiment 3

[0026] The preparation method of present embodiment acetone oxime comprises the following steps:

[0027] 1) In the reactor, 17.4g of acetone was dissolved in 74.8g of isopropanol to make an acetone solution, and after adding 2.44gTS-1 molecular sieves and 54.4g of 25% ammonia water in the acetone solution, the mass concentration was mixed. Obtain the pre-reaction solution.

[0028] 2) the reaction kettle is sealed, and the pre-reaction solution prepared by step 1) is heated to 70°C, and 52.2g concentration of 30% hydrogen peroxide solution is slowly added dropwise with a microfeed pump, and the time for adding hydrogen peroxide solution is After 4 hours, the reaction time is 9 hours at 70°C and 1MPa pressure to obtain the reaction liquid, the reaction liquid is filtered, the filtrate is rectified under normal pressure, 70-85°C is the isopropanol slip-out liquid, and extracted three times with the extractant toluene to obtain The extract of acetone oxime is rectified under no...

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Abstract

The invention relates to the technical field of acetone oxime production processes, in particular to a preparation method of acetone oxime. The preparation method of acetone oxime comprises the following steps: 1) dissolving acetone in an organic solvent to prepare an acetone solution and then adding a TS-1 molecular sieve catalyst and ammonia water into the acetone solution to be mixed to obtaina prereaction liquid; and 2) heating the prereaction liquid to 40-80 DEG C, and adding a hydrogen peroxide solution to react for 3-10 hours under the condition that the temperature is 40-80 DEG C andthe pressure is 0-1.0MPa, then carrying out filtration and rectification, extracting the solution with an extraction agent to obtain an extraction solution, and rectifying the extraction solution to obtain acetone oxime. The preparation method is simple in production process. Acetone is dissolved by isopropanol or cyclohexane, so that the solubility is good and the conversion ratio of acetone is improved. Isopropanol or cyclohexane is easily separated from a mixture of acetone oxime separately in the later period. The extraction agent is used for acetone oxime, so that the extraction rate is high, and in the whole process course, environmental pollution caused by a conventional process is avoided.

Description

technical field [0001] The invention relates to the technical field of acetone oxime production technology, in particular to a preparation method of acetone oxime. Background technique [0002] Acetone oxime is also called dimethyl ketone oxime. Acetone oxime is a kind of chemical oxygen scavenger developed in recent years. Due to its low toxicity and good oxygen scavenging effect, it is widely used as an important additive after pickling of boilers in thermal power plants. The passivation solution and running water can form a good passivation film on the inner wall of the boiler. It is a new type of boiler feed water oxygen scavenger. At present, the industrial acetone oxime production processes mainly include hydroxylamine hydrochloride method, hydroxylamine sulfate method and sodium nitrite method. However, these processes are complicated, the process is long, and a large number of by-products are produced, polluting the environment. Contents of the invention [0003] ...

Claims

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Application Information

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IPC IPC(8): C07C249/04C07C249/14C07C251/38
CPCC07C249/04C07C249/14C07C251/38
Inventor 汪俊杰刘建青李鲁祯叶茂伟
Owner 江苏艾科维科技有限公司
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