Method for synthesizing hydroxylamine hydrochloride from nitromethane and hydrochloric acid through phase transfer

A technology of nitromethane and hydroxylamine hydrochloride, applied in chemical instruments and methods, hydroxylamine, nitrogen and non-metallic compounds, etc., can solve the problems of low conversion rate and long reaction time, and achieve low production cost, fast reaction speed, and yield high rate effect

Active Publication Date: 2017-07-14
BEIJING CHEM REACTION ENG SCI & TECH CO LTD
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Problems solved by technology

[0005] Aiming at the problems of long reaction time and low conversion rate in the existing nitromethane method, the present invention provides a method for synthesizing hydroxylamine hydrochloride by phase transfer from nitromethane and hydrochloric acid

Method used

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  • Method for synthesizing hydroxylamine hydrochloride from nitromethane and hydrochloric acid through phase transfer

Examples

Experimental program
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Effect test

Embodiment 1

[0034] like figure 1 As shown, nitromethane and hydrochloric acid are added in the synthesis reactor 1 in a molar ratio of 1:1.5, stirred and mixed, and the extractant n-octanol is added, and the molar ratio of nitromethane and n-octanol is 1:1, and the temperature is raised to 130 After reacting at ℃ for 36 hours, the heating is stopped, and the reaction product is sent to the phase separator 2. After phase separation, the oil phase enters the rectification tower 3. After rectification, formic acid is a by-product, and nitromethane and octanol are recovered and recycled. The aqueous phase coming out of the phase separator 2 enters the concentration tower 4, and the concentration adopts vacuum distillation, and the distillation pressure is － 0.1MPa (G), concentrated distilled water and hydrochloric acid are recycled, the concentrated solution enters the crystallizer 5 to crystallize, then enters the filter 6 to filter out the solid, washes with anhydrous ether for 3 times, and...

Embodiment 2

[0040] like figure 1 As shown, nitromethane and hydrochloric acid are added in the synthesis reactor 1 in a molar ratio of 1:3, stirred and mixed, and the extractant n-hexanol is added, and the molar ratio of nitromethane and n-hexanol is 1:1, and the temperature is raised to 130 ℃ reaction 36h. In addition, the same method as in Example 1 was used to obtain hydroxylamine hydrochloride crystals with a yield of 76.22%.

Embodiment 3

[0046] like figure 1 As shown, nitromethane and hydrochloric acid are added in the synthetic reactor 1 in molar ratio 1:2, stir and mix, add extraction agent trioctylamine, the mol ratio of nitromethane and trioctylamine is 1:1, heat up to The temperature was 130°C for 36h. In addition, the same method as in Example 1 was used to obtain hydroxylamine hydrochloride crystals with a yield of 74.12%.

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Abstract

The invention relates to a method for synthesizing hydroxylamine hydrochloride from nitromethane and hydrochloric acid through phase transfer. The method comprises the following steps: 1, carrying out a synthesis reaction: adding raw materials which are nitromethane, hydrochloric acid and water into a batch reactor with a stirrer, stirring and mixing the raw materials, adding an extractant, heating the reactor to a reaction temperature, and carrying out the reaction for a period of time to obtain a reaction product; and 2, separating the product: standing the reaction product to layer the reaction product, conveying the obtained water phase to a concentration tower, carrying out crystallizing, filtering, washing and drying on the obtained concentrate to obtain the hydroxylamine hydrochloride, recycling hydrochloric acid and water obtained in the concentration tower, conveying the obtained oil phase to a rectifying tower, and carrying out separation to obtain the extract and nitromethane which can be recycled and formic acid as a byproduct.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and relates to a method for synthesizing hydroxylamine hydrochloride by phase transfer from nitromethane and hydrochloric acid. Background technique [0002] Hydroxylamine hydrochloride is a widely used organic chemical raw material and organic synthesis intermediate. It is used in the preparation of oximes in organic synthesis, and is also used as a raw material for the synthesis of anticancer drugs (such as hydroxyurea), sulfonamides (such as sulfamethoxazole) and pesticides (such as methomyl); used as a depolarizer in electroanalysis; In the synthetic rubber industry, it is used as a non-coloring short-term stopper; in the synthetic fuel industry, it is used to prepare isatin intermediates; in the oil industry, it is used as an anti-aging agent and antioxidant for fatty acids and soaps; in analytical chemistry, it is used to analyze formaldehyde, furfural, and camphor And the reducing ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/14
CPCC01B21/1409
Inventor 王金福唐强任立军廖玉会丰秀珍靳辉
Owner BEIJING CHEM REACTION ENG SCI & TECH CO LTD
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