Hydroxypropyl hydroxylamine and synthesizing method thereof

A technology of hydroxypropyl hydroxylamine and a synthesis method, which is applied to the application of styrene polymerization inhibitors, in the field of hydroxypropyl hydroxylamine, can solve the problem of low closed flash point of diisopropyl hydroxylamine, which does not conform to the styrene production process, and is flammable Risk and other problems, to achieve the effect of easy industrial continuous production, high flash point, and good polymerization inhibition effect

Inactive Publication Date: 2017-07-18
威海翔泽新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The amines used in this patent application will have certain dangers when added to the crude styrene tower at 100°C-200°C, such as: diisopropylhydroxylamine has a low closed flash point, is toxic, and is flammable Products, etc., do not meet the requirements of styrene production process

Method used

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  • Hydroxypropyl hydroxylamine and synthesizing method thereof

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[0027] One aspect of the embodiments of the present invention provides a synthetic method of hydroxypropyl hydroxylamine, comprising the following steps:

[0028] S1: add substituted hydroxylamine and solvent to the reactor, after the substituted hydroxylamine is completely dissolved, add lye to the reactor, fully stir in ice bath for 1-8 hours;

[0029] S2: Add alkylene oxide to the reactor, remove the ice bath, and fully stir for 10-36 hours to obtain a mixed product;

[0030] S3: Carry out rotary steaming on the mixed product, and extract the product after rotary steaming with an extractant, fully stir, place at 0°C-20°C for 1-10 hours, filter to obtain a clear and transparent solution; The extractant in the clear transparent solution is obtained to obtain hydroxypropyl hydroxylamine.

[0031] In the above examples, the mixed product of the pure target product can be obtained by directly using substituted hydroxylamine, solvent, lye and alkylene oxide, and then the target ...

Embodiment 1

[0046] (1) Add 1 part of diethylhydroxylamine and 1 part of ethanol to the reactor, stir to dissolve the diethylhydroxylamine completely, add 0.1 part of potassium hydroxide solution to the above reactor, and fully stir for 8 hours at 20°C;

[0047] (2) Add 1 part of ethylene oxide into the above reactor, and fully stir at 60° C. for 36 hours to obtain a mixed product;

[0048] (3) Carry out rotary steaming to the mixed product, and use ethanol to extract the product after rotary steaming, fully stir, place at 20° C. for 10 hours, filter to obtain a clear and transparent solution; rotary steaming again removes the clear and transparent Ethanol in the solution obtains hydroxypropyl hydroxylamine as a styrene polymerization inhibitor.

Embodiment 2

[0050] (1) Add 1 part of hydroxylamine sulfate and 10 parts of deionized water into the one-mouth bottle, stir to completely dissolve the hydroxylamine sulfate, then add 2 parts of sodium hydroxide solution into the above-mentioned one-mouth bottle, and fully stir for 2 hours at 0°C;

[0051] (2) Add 15 parts of propylene oxide to the above-mentioned single-necked bottle, and fully stir at 20°C for 10 hours to obtain a mixed product;

[0052] (3) Carry out rotary evaporation to the mixed product, and use tetrahydrofuran to extract the product after rotary evaporation, place it at 0° C. for 1 hour, filter to obtain a clear and transparent solution; The tetrahydrofuran, obtains the hydroxypropyl hydroxylamine as styrene polymerization inhibitor.

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Abstract

The invention provides hydroxypropyl hydroxylamine and a synthesizing method thereof, and belongs to the technical field of organic synthesis. The hydroxypropyl hydroxylamine synthesized by the synthesizing method can be used as a styrene polymerization inhibitor, and can be effectively used for inhibiting generation of polystyrene and blockage of polystyrene on pipelines and equipment in the process of producing styrene. According to the technical scheme, the method comprises the following steps: (1) adding substituted hydroxylamine and a solvent in a reactor, adding an alkali liquor into the reactor after the substituted hydroxylamine is completely dissolved, sufficiently stirring for 1-8 hours under ice bath; (2) adding alkylene oxide into the reactor, removing the ice bath, and sufficiently stirring for 10-36 hours to obtain a mixed product; and (3) performing rotary evaporation on the mixed product, extracting the rotary-evaporated product by utilizing an extracting agent, sufficiently stirring, standing at 0-20 DEG C for 1-10 hours, and filtering to obtain a clear transparent solution, and removing the extracting agent in the clear transparent solution to obtain the hydroxypropyl hydroxylamine. The hydroxypropyl hydroxylamine can be applied to continuous production of styrene.

Description

[0001] Related literature cross reference [0002] The present invention claims the priority of the application number 201610185241.7 submitted on March 29, 2016, entitled "Synthesis of a styrene polymerization inhibitor", the entire content of which is incorporated herein by reference. technical field [0003] The invention belongs to the technical field of organic synthesis, and in particular relates to a kind of hydroxypropyl hydroxylamine, its synthesis method and its application as a styrene polymerization inhibitor. Background technique [0004] As a widely used chemical raw material, styrene has developed rapidly in China in recent years. Since the extracyclic double bonds of styrene are very active, during the rectification process, free radical polymerization is initiated by heat to form a high polymer, which not only consumes styrene monomer, affects product quality, but also seriously threatens the continuous production process. . In order to reduce the self-pol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C239/12C07C7/20C07C15/46
CPCC07C239/12C07C7/20C07C15/46
Inventor 王俊谕程晓婷李洪社
Owner 威海翔泽新材料科技有限公司
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