Method for purifying 1,4-butanediol

A purification method and technology of butanediol, applied in 1 field, can solve the problems of complex reactor structure, increase the difficulty of factories, etc., and achieve the effects of low cost, simple composition and easy preparation

Active Publication Date: 2018-03-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] Although these methods are somewhat useful to solve the problem of 2-(4'-hydroxybutyloxy)-tetrahydrofuran in the product stream of 1,4-butanediol, there are still some deficiencies and disadvantages. Economics and efficiency of reaction methods
For example, in the method proposed by Chinese patent CN1216973A, a very large amount of stream is passed through a solid catalyst in the form of gas and liquid, but only 0.1% to 0.4% of the material is converted, and the water is in a liquid state during the reaction, which is very important for the catalyst. High requirements are placed on the performance and operating conditions of the reactor, and the complex structure of the reactor increases the difficulty of the actual operation of the plant.

Method used

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  • Method for purifying 1,4-butanediol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Take by weighing 100 grams of amino acid phosphoric acid chelating resin LSC-500 and vacuum dry at 80° C. for 2 hours. Preparation 100 milliliters concentration is the silver nitrate aqueous solution of 78.7 grams per liter, under the condition of stirring, add the LSC-500 chelate resin after 100 grams of drying at normal temperature, at 60 ℃ and under stirring aging 8 hours. Pass hydrogen into the mixture after aging to carry out reduction and activation for 4 hours, separate the mixture through reduction and activation to obtain a solid, and the gained solid is washed with water successively and vacuum-dried at 80°C for 2 hours to obtain a silver content of 5% by weight. Silver supported resin catalyst.

[0041] In the fixed-bed reactor, pack 10 grams of the silver-loaded resin catalyst prepared by the present embodiment, and at a temperature of 80° C., a pressure of 2.0 MPa, and a liquid hourly volume space velocity of 2 for crude 1,4-butanediol. Hour -1 , hydrogen...

Embodiment 2

[0043] Weigh 100 grams of iminodiacetoxy-based chelating resin D851 and dry it in vacuum at 80° C. for 2 hours. Preparation 100 milliliters of concentration is the silver nitrate aqueous solution of 78.7 grams per liter, under the condition of stirring, add 100 grams of D851 chelating resins at normal temperature, at 60 ℃ and aging 8 hours under stirring. Pass hydrogen into the mixture after aging to carry out reduction and activation for 4 hours, separate the mixture through reduction and activation to obtain a solid, and the gained solid is washed with water successively and vacuum-dried at 80°C for 2 hours to obtain a silver content of 5% by weight. Silver supported resin catalyst.

[0044] In the fixed-bed reactor, pack 10 grams of the silver-loaded resin catalyst prepared in this embodiment, and at a temperature of 80° C., a pressure of 1.0 MPa, and a liquid hourly volume space velocity of 1,4-butanediol of 2 Hour -1 1, hydrogen and crude 1,4-butanediol are treated unde...

Embodiment 3

[0046] Weighing brand is 100 grams of polystyrene-based chelating resin S-930 and dried in vacuum at 80° C. for 2 hours. Prepare 100 milliliters of concentration and be the silver nitrate aqueous solution of 15.7 grams / liter, under the condition of stirring, add 100 grams of S-930 chelate resins at normal temperature, at 60 ℃ and under stirring aging 8 hours. Pass hydrogen into the aged mixture to carry out reduction activation for 4 hours, separate the mixture through reduction activation to obtain a solid, wash the gained solid with water and vacuum dry at 80° C. for 2 hours to obtain a silver content of 1% by weight. Silver supported resin catalyst.

[0047] In the fixed-bed reactor, pack 10 grams of silver-loaded resin catalysts prepared in this embodiment, and at a temperature of 30° C., a pressure of 3.0 MPa, and a liquid hourly volume space velocity of 1,4-butanediol Hour -1 1, hydrogen and crude 1,4-butanediol are treated under the condition of 10:1 mol ratio to puri...

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Abstract

The invention discloses a method for purifying 1,4-butanediol. The method comprises the following step of enabling crude 1,4-butanediol containing aldehyde compound and/or acetal compound impurities to contact a silver-loaded resin catalyst under the hydrogen contacting condition, so as to obtain the purified 1,4-butanediol with color degree smaller than 10APHA. The method has the advantage that the crude 1,4-butanediol containing the aldehyde compound and/or acetal compound impurities can be purified, so that the color degree of the 1,4-butanediol is reduced.

Description

technical field [0001] The invention relates to a method for purifying 1,4-butanediol. Background technique [0002] 1,4-Butanediol (BDO) is an important basic organic chemical and fine chemical raw material with a wide range of uses, especially its derivatives are fine chemical products with high added value, widely used as solvents, medicines, cosmetics, Plasticizers, curing agents, pesticides, rust removers, artificial leather, fibers and engineering pigments, etc. BDO is also used in the manufacture of chemical products such as tetrahydrofuran (THF), gamma-butyrolactone (GBL) and N-methylpyrrolidone (NMP). [0003] There are about dozens of known synthesis routes for 1,4-butanediol, among which the Reppe method and the maleic anhydride hydrogenation method are the ones with relatively high industrial proportions. The Reppe method uses acetylene and formaldehyde as raw materials, and first synthesizes 1,4-butynediol from acetylene and formaldehyde under the action of a ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/74C07C29/76C07C31/20B01J31/06
CPCB01J31/06C07C29/74C07C29/76C07C31/207
Inventor 张晓昕王宣慕旭宏宗保宁
Owner CHINA PETROLEUM & CHEM CORP
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