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Method for preparing 1,4-butynediol

A technology of butynediol and acetylene, applied in the production field of organic chemical products, can solve the problem of frequent replacement of catalysts and filter bags, achieve the effects of good mechanical strength and anti-pollution performance, avoid losses, and ensure continuous and stable operation

Active Publication Date: 2016-06-01
河北美邦工程科技股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a method for preparing 1,4-butynediol, to solve the problem of frequent replacement of catalysts and filter bags in the production process of 1,4-butynediol, and to realize continuous and stable production

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  • Method for preparing 1,4-butynediol
  • Method for preparing 1,4-butynediol

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Effect test

Embodiment 1

[0024] The preparation method of 1,4-butynediol, process flow diagram is by figure 1 shown. The preparation method steps are as follows:

[0025] (1) The catalyst is activated for the first time

[0026] A reactor with a built-in metal membrane filter was used, and it was started for the first time, and 6t of copper catalyst (CuO-Bi 2 o 3 , Cu content is about 20%, Bi content is about 3%) and 27t formaldehyde solution (mass fraction 28%), at a temperature of 80°C, 0.13MPa acetylene gas is passed through for activation. After 9h, the active component copper is converted into Copper acetylene to obtain a copper acetylene / bismuth catalyst;

[0027] (2) Continuous reaction

[0028] Control the pressure in the reactor to 0.08MPa, the temperature to 90°C, continuously feed acetylene gas into the reactor, the acetylene space velocity is 4min-1, continuously add formaldehyde solution (mass fraction 28%), in the reaction medium, acetylene copper / bismuth The catalyst content is 10...

Embodiment 2

[0036] The preparation method of 1,4-butynediol, process flow diagram is by figure 2 shown. The preparation steps are as follows:

[0037] (1) The catalyst is activated for the first time

[0038] A reactor with a built-in metal membrane filter is used, and the first start-up, 12t copper catalyst (CuO-Bi 2 o 3 , Cu content is about 20%, Bi content is about 2.5%) and 50t formaldehyde solution (mass fraction 33%), at a temperature of 70 ° C, 0.15 MPa of acetylene gas is passed through for activation. After 10 hours, the active component copper is converted into Copper acetylene to obtain a copper acetylene / bismuth catalyst;

[0039] (2) Continuous reaction

[0040] Control the pressure in the reactor to 0.10MPa, the temperature to 85°C, continuously feed acetylene gas into the reactor, the acetylene space velocity is 4.5min-1, continuously add formaldehyde solution (mass fraction 33%), in the reaction medium, copper acetylene / bismuth catalyst content is 9%, and acetylen...

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Abstract

The invention discloses a method for preparing 1,4-butynediol. The method comprises the steps that firstly, a copper catalyst is activated to obtain a copper acetylide / bismuth catalyst, acetylene and formaldehyde are subjected to a reaction under the effect of the copper acetylide / bismuth catalyst to obtain a 1,4-butynediol and copper acetylide / bismuth catalyst mixed solution, and in a reaction kettle, the mixed solution is filtered through a metal film filter to obtain a 1,4-butynediol clear solution which is fed outside the reaction kettle to be subjected to follow-up technological treatment to obtain a finished product. In the reaction process, copper acetylide / bismuth catalyst turbid liquid is extracted periodically, then, an equimolar copper acetylide / bismuth catalyst or a copper catalyst is supplemented, a clear solution obtained after the extracted copper acetylide / bismuth catalyst turbid liquid is filtered is subjected to the follow-up technological treatment to obtain a finished product finally, and copper acetylide / bismuth catalyst cakes are subjected to a regeneration procedure to be recycled; the 1,4-butynediol clear solution is adopted for performing back flushing on the metal film filter periodically. Due to periodic extraction and supplementing of the catalyst, production losses caused by frequent stopping are avoided, and the product yield and output are improved.

Description

technical field [0001] The invention relates to a method for preparing organic compounds, in particular to a method for preparing 1,4-butynediol, and belongs to the technical field of organic chemical product production. Background technique [0002] 1,4-Butynediol (C 4 h 6 o 2 ), white orthorhombic crystals, soluble in water, acid, ethanol and acetone, insoluble in benzene and ether, irritating to eye mucous membranes, skin and upper respiratory tract. It can be used to prepare a series of important organic chemical products such as butylene glycol, butanediol, n-butanol, dihydrofuran and tetrahydrofuran, and can also be used as a brightener for electroplating. In industry, the main production method of 1,4-butynediol is the Reppe method: that is, acetylene is added to a molecule of formaldehyde under the action of a copper catalyst to generate propynyl alcohol, which is then added to a formaldehyde molecule, This produces 1,4-butynediol. In the reaction process, the c...

Claims

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Application Information

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IPC IPC(8): C07C29/42C07C29/76C07C33/046B01J31/26B01J23/843B01J37/00
CPCB01J23/8437B01J31/26B01J37/00B01J2231/4205C07C29/42C07C29/76C07C33/046
Inventor 金作宏王海东
Owner 河北美邦工程科技股份有限公司
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