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Method for preparing propargyl alcohol from 1,4-butynediol

A technology of butynediol and propynyl alcohol, which is applied in the field of preparing propynyl alcohol by pyrolysis of BYD, can solve the problems of high preparation cost, low yield of propynyl alcohol, and hidden dangers, and achieve the goal of reducing costs and overcoming safety hazards Effect

Inactive Publication Date: 2018-09-07
SINOPEC CHANGCHENG ENERGY CHEM NINGXIA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above-mentioned propynyl alcohol preparation technology is to synthesize acetylene and formaldehyde to co-produce propynyl alcohol and BYD under a certain pressure. There are safety and environmental protection risks in the preparation process, and the preparation cost is high, and the yield of propynyl alcohol is low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The unsupported catalyst catalyzes the decomposition of BYD to produce propynyl alcohol, adding 56.0g of BYD solid, 110.29g of solvent γ-butyrolactone, and 34.51g of catalyst, bubbling acetylene gas under normal pressure, and reacting at 140-155°C After 4 hours, the obtained product contained 36.2% propynyl alcohol, and the yield of propynyl alcohol was 22.68%.

Embodiment 2

[0029] Magnesium silicate-loaded acetylene copper catalyzes the decomposition of BYD to produce propynyl alcohol. Add 27.29g of BYD solid, 54.26g of solvent γ-butyrolactone, and 16.32g of catalyst. Acetylene gas is bubbled in under normal pressure. After reacting for 4 hours under ambient conditions, the obtained product contained 31.3% propynyl alcohol, and the yield of propynyl alcohol was 33.3%.

Embodiment 3

[0031] Continuous experiment of magnesium silicate supported acetylene copper catalyzed BYD decomposition to produce propynyl alcohol, reaction temperature 140-155°C, acetylene gas bubbling, normal pressure operation, no rectification device, solvent ethylene glycol / BYD mass ratio of 1 , The initial concentration of the catalyst is 10% and it is added regularly. After 24 hours of reaction, the product contains 53.8% of propynyl alcohol, and the yield of propynyl alcohol is 23.68%.

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PUM

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Abstract

The invention discloses a method for preparing propargyl alcohol from 1,4-butynediol. The method comprises the steps: carrying out distillation concentration on a 1,4-butynediol BYD aqueous solution by using a rotary evaporator, starting a vacuum pump at a certain temperature, gradually increasing the vacuum degree until a distillate accounts for 40% or above of the undistilled BYD aqueous solution and a liquid in a kettle is not boiled, stopping a rotary evaporation device, and taking out BYD for later use; and adding the refined BYD, a solvent and a catalyst according to a proportion, carrying out heating to a certain temperature, then, starting to time, controlling the temperature constant, carrying out a reaction for a period of time, carrying out water analysis and chromatographic analysis on a distilled product, calculating the yield and concentration of propargyl alcohol, and keeping the intermittent reaction period at 4h. By using the method, potential safety hazards existing in co-production of BYD and propargyl alcohol in a high-pressure acetylene system are overcome, and the relevant operation expense is reduced.

Description

technical field [0001] The invention belongs to the field of methods for preparing propynyl alcohol in the chemical industry, in particular to a method for preparing propynyl alcohol by pyrolysis of BYD. Background technique [0002] Proynyl alcohol is an important intermediate in organic synthesis in industry. In the pharmaceutical industry, propynyl alcohol is an important intermediate for the synthesis of fosfomycin sodium, fosfomycin calcium, and sulfadiazine, and is also used in the production of allyl alcohol, acrolein, vitamin A and other pharmaceutical products. In the pesticide industry, it is used for the synthesis of decantide pesticide; it is also used as a brightener in the electroplating industry; it is also an important rust remover; it can also be used in oil extraction, and is widely used in oil and gas wells under high temperature, high pressure, and high concentration hydrochloric acid. The key effective components of high-efficiency acidification corrosi...

Claims

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Application Information

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IPC IPC(8): C07C29/00C07C33/042
CPCC07C29/00C07C33/042
Inventor 周代红唐宇虹唐元宋锋刘新文
Owner SINOPEC CHANGCHENG ENERGY CHEM NINGXIA CO LTD
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