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The preparation method of n-isopropyl hydroxylamine

A technology of isopropyl hydroxylamine and isopropylamine, applied in the field of preparation of N-isopropyl hydroxylamine, can solve the problems of harsh catalyst synthesis conditions, troublesome carbon dioxide metering, difficulty in process amplification, etc., achieves good market space, and has low technical requirements for equipment , the effect of less dosage

Active Publication Date: 2017-06-16
山东丰汇泽化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The raw material of this method is easy to obtain, and the yield is also high, but there are disadvantages such as troublesome carbon dioxide metering, harsh catalyst synthesis conditions, cumbersome steps, and certain difficulties in process scale-up.

Method used

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  • The preparation method of n-isopropyl hydroxylamine
  • The preparation method of n-isopropyl hydroxylamine
  • The preparation method of n-isopropyl hydroxylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Pour 1 kg of isopropylamine and 2 kg of deionized water into the tank reactor equipped with 0.05 kg of titanium-silicon molecular sieve catalyst, start to feed cooling water into the reflux condenser of the reactor, stir and raise the temperature to 35°C under normal pressure, Start to drop 2.0Kg of 30% hydrogen peroxide into the reaction kettle, and control the dropping time at 2hr. After the hydrogen peroxide dripping is completed, continue the insulation reaction for 2hr, and the reaction ends. The reaction solution was sampled, and the components of the reaction solution were analyzed by gas chromatography. The molecular sieve catalyst in the reaction liquid is filtered out with a microfilter, and the obtained filtrate is sent to a rectification tower. Collect fractions at 33-45°C by rectification under normal pressure to recover the aqueous solution of isopropylamine, and then collect the aqueous solution of acetone oxime at 50-80°C under vacuum condition of 0.03MP...

Embodiment 2

[0037] Put the measured 1kg of isopropylamine and 2kg of deionized water into the tank reactor equipped with 0.21kg of titanium-silicon molecular sieve TS-1 catalyst, and start to feed cooling water into the reflux condenser of the reactor, and stir and heat up to At 90°C, start to drop 0.9Kg of 30% hydrogen peroxide into the reaction kettle, and the dropping time is controlled at 4hr. After the hydrogen peroxide drop is completed, continue to keep warm for 2hr, and the reaction ends. The reaction kettle was sampled, and the components of the reaction solution were analyzed by gas chromatography. The molecular sieve catalyst in the reaction liquid is filtered out with a microfilter, and the obtained filtrate is sent to a rectification tower. Collect fractions at 33-45°C by rectification under normal pressure to recover the aqueous solution of isopropylamine, and then collect the aqueous solution of acetone oxime at 50-80°C under vacuum condition of 0.03MPa. The still liquid a...

Embodiment 3

[0040] 9.8Kg of 30% hydrogen peroxide was added dropwise into the reaction kettle, the dropping time was controlled at 4hr, the addition amount of the titanium silicon molecular sieve catalyst was 0.49Kg, the reaction temperature was controlled at 55°C, and the rest were the same as in Example 2. The results of gas chromatography analysis are shown in Table 1.

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Abstract

The invention relates to a preparation method of N-isopropylhydroxylamine oxalate. Isopropylamine serves as raw materials, deionized water serves as a solvent, a titanium silicate molecular sieve serves as a catalyst, hydrogen peroxide serves as an oxidant for reaction, and the N-isopropylhydroxylamine oxalate is prepared. Preferentially, the titanium silicate molecular sieve TS-1 or TS-2 serves as the catalyst. The isopropylamine which is low in price and easy to obtain is adopted as raw materials, the high-directivity titanium silicate molecular sieve TS-1 or TS-2 serves as the catalyst, the technology is simple and easy to operate, the catalyst TS-1 or TS-2 can be directly filtered through a filter, separation is easy, the technological requirement for equipment is low, and industrialized production can be achieved easily.

Description

technical field [0001] The invention relates to a preparation method of N-isopropylhydroxylamine. Background technique [0002] N-isopropyl hydroxylamine, usually abbreviated as IPHA, belongs to the secondary alkyl hydroxylamines. Because of its performance as a polymerization inhibitor and terminal polymerization inhibitor, it is mainly used as a polymerization inhibitor and terminal polymerization inhibitor in the production of styrene-butadiene rubber and nitrile rubber. It is also used as an oxygen scavenger for dissolving and removing oxygen in the water supply system of thermal power generation. In addition, it has good volatility and strong reducibility. The oxidation product acetone oxime after N-isopropyl hydroxylamine is oxidized can still continue to react with oxygen, so it is often used as an oxygen scavenger for boiler scale and a protective agent for furnace walls. [0003] The traditional preparation method of N-isopropylhydroxylamine is 2-nitropropane hig...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C239/08C07C249/04C07C251/38B01J29/89
Inventor 石振解全诚王敏崔晓坤宋伟斌
Owner 山东丰汇泽化工股份有限公司
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