Method for synthesizing 1,2,4-butanetriol

A technology of butylene glycol and mixed solution, applied in 1 field, can solve the problems of being difficult to obtain, difficult to control the reaction temperature, and high local concentration, and achieve the effects of easy control of the reaction temperature, easy industrialization, and mild operating conditions

Inactive Publication Date: 2008-12-31
SHANGHAI XUKAI SCI TECH DEV
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  • Summary
  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

However, the former uses borohydride as the original agent for chemical reduction, which requires stoichiometric or even more active hydrogen, and the raw material malate is not easy to obtain; while the atom economy of the direct hydrolysis reaction of butenol is very high, but There is a problem with bad choices
[0007] At present, there is also a synthetic method for preparing 1,2,4-butanetriol using mercury as a catalyst, which seriously pollutes the environment
[0008] In the existing industrialized production technology, in the epoxidation process of butenediol, the reagent used is hydrogen peroxide with a weight concen

Method used

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  • Method for synthesizing 1,2,4-butanetriol

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Embodiment 1

[0038] (1) With the mixed solution of 60kg butylene glycol, 400 milliliters of N-methylmorpholine and 540 grams of tungstic acid, the volume concentration is 90% oxygen-enriched gas by being arranged on the top of the reactor to be provided with the mixing of two channel nozzles After mixing in the reactor, enter the reactor to react;

[0039] The material in the reactor is sent to the mixer at the top of the reactor by a circulation pump for recycling, the reaction temperature is 25°C, the reaction time is 10 hours, and then the epoxide is collected;

[0040] The amount of oxygen-enriched gas entering the mixer of the two-channel nozzle is 1.5 times the theoretical reaction molar amount of oxygen and butylene glycol.

[0041] (2) the epoxide of 120kg step (1), 50kg volume concentration are 95% ethanol in the presence of 1.2kg catalyzer, carry out hydrogenation reaction with hydrogen, the reaction time is 1.5 hours, and temperature of reaction is 160 ℃, the reaction pressure ...

Embodiment 2

[0044] (1) With the mixed solution of 60kg butylene glycol, 400 milliliters of N-methylmorpholine and 540 grams of tungstic acid, the volume concentration is that the oxygen-enriched gas of 60% is provided with the mixing of two channel nozzles that are arranged on the top of the reactor After mixing in the reactor, enter the reactor to react;

[0045] The material in the reactor is sent to the mixer at the top of the reactor by a circulating pump for recycling, the reaction temperature is 25°C, the reaction time is 14 hours, and then the epoxide is collected;

[0046] The amount of oxygen-rich gas entering the mixer of the two-channel nozzle is 1 time of the theoretical reaction mole amount of oxygen and butylene glycol.

[0047] (2) the epoxide of 120kg step (1), 50kg volume concentration are 35% ethanol in the presence of 1kg catalyzer, carry out hydrogenation reaction with hydrogen, the reaction time is 0.5 hour, and reaction temperature is 130 ℃ , the reaction pressure i...

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Abstract

The invention provides a synthesis method for 1,2,4-tromethamine, comprising the following steps: the mixed solution of butene diol, tungsten acid and N-methyl morpholine, and epoxidizing agent are mixed through a mixer which is provided with two channel nozzles and arranged at the top part of a reactor, and then enter the reactor for reaction; the material in the reactor is sent to a nozzle at the top part of the reactor through a circulating pump for recycling use to collect epoxide; the epoxidizing agent is selected from oxygen-rich gases; in the presence of catalysts, the epoxide and ethanol go through hydrogenation reaction, then the 1,2,4-tromethamine is collected. The invention adopts oxygen-rich gas as epoxidizing agent and avoids the introduction of unnecessary media in the reaction system through the pre-mixing in a mixer provided with two channel nozzles; besides, the method of the invention has easily-controlled reaction temperature, less equipment investment and mild operating conditions, which does not use the traditional mercury catalyst and has no pollution to the environment; the reaction yield of the method can reach more than 95%, so the method is easy in industrialized implementation.

Description

technical field [0001] The invention relates to a method for synthesizing 1,2,4-butanetriol. Background technique [0002] 1,2,4-Butanetriol is an important chemical and chemical intermediate, which can replace glycerin in the military to prepare high-performance nitroglycerin explosives; in the pharmaceutical industry, butanetriol can be used to manufacture antiviral compounds and platelets Activator drugs; 1,2,4-Butanetriol also has important uses in the agrochemical industry. [0003] There are many synthetic methods for 1,2,4-butanetriol, such as the chemical reduction method of malate as raw material, the direct hydrolysis method of butenol as raw material, and the synthesis method of 2-butene-1,4-diol as raw material. Epoxidation hydrogenolysis two-step process and other processes. [0004] Among them, the epoxidation-hydrogenolysis two-step process and other processes were first reported by the German BASF company (DE264340). First, 2,3,-epoxy-1,4-diol was synthesiz...

Claims

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Application Information

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IPC IPC(8): C07C31/22C07C29/132
Inventor 顾全君陈启明杨载耀
Owner SHANGHAI XUKAI SCI TECH DEV
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