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2-butylene-1,4-diol synthesis method

A diol and selectivity technology, applied in hydrogenation preparation and other directions, can solve the problems such as the lack of a method for separating products and recovering catalysts, poor selectivity of 1,4-butene diol, corrosion separation, etc., and the production process is mature. , the effect of improved operating conditions and low production costs

Inactive Publication Date: 2007-05-23
上海中远化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In this synthetic method, first, these reactions not only have poor selectivity for the desired 1,4-butenediol, but also require 50 hours for the reaction to be completely
Second, it does not provide a method for isolating the product and recovering the catalyst from the reaction mixture
[0007] In this synthetic method, not only the yield is low, but also there are corrosion problems and separation problems due to the use of hydroiodic acid containing water.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Weigh 300g of butynediol aqueous solution and the Pd-C catalyst poisoned with lead, and put them into a 0.5L stainless steel autoclave. The amount of catalyst in the reactor is 1g (accounting for 0.3322% of the mass of the total reaction material), wherein the content of Pd is 0.0166%, and the content of Pb is 0.0100%. Replace the air in the kettle with nitrogen, then replace the nitrogen with hydrogen, and then raise the temperature to 35-45°C while stirring at a low speed (450-550 rpm). The reaction pressure is increased and maintained at 0.6-1.5 MPa, and the reaction is started. The reaction time is 330-390 minutes. After the reaction, the stirring was stopped, the hydrogen gas was stopped, the temperature was rapidly lowered, and the pressure was released. After replacing the unreacted hydrogen in the still with nitrogen, open the still and pour out the product, remove the catalyst by filtration and take a sample for analysis. The finally obtained raw material bu...

Embodiment 2

[0024] Except catalyst consumption 2g (accounting for 0.6623% of total reaction mass), wherein the content of Pd is 0.0331%, the content of Pb is 0.0199%, and the reaction time is 200-230 minutes, all the other process steps, material proportioning and reaction parameters are all the same In Example 1, when the concentration of butynediol in the final raw material is zero, the concentration of butynediol is too high. The product yield is 93.4-94.8%, and the raw material selectivity is 93.9-95.6%.

Embodiment 3

[0026] Except catalyst consumption 3 grams (accounting for 0.9901% of total reaction mass), wherein the content of Pd is 0.0495%, the content of Pb is 0.0297%, and the reaction time is 150-180 minutes, all the other process steps, material proportioning and reaction parameters are all Same as Example 1, when the butynediol concentration of the raw material finally obtained is zero, the butanediol concentration is relatively low. The product yield is 93.4-94.3%, and the raw material selectivity is 93.4-94.7%.

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PUM

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Abstract

The invention relates to a synthesis method for 2-butene-1, 4-diol through selective hydrogenation of 2-butyne-1, 4-diol. The method includes placing butynediol aqueous solution and lead poisoned catalyst of Pd-C in an autoclave, replacing air with nitrogen and then replacing nitrogen with hydrogen, heating to 35 ~ 45degreeC with stirring, increasing pressure and maintaining under 0.6-1.7 MPa, reacting for 60 ~ 390 min, stopping stirring and providing hydrogen, cooling rapidly and venting, replacing unreacted hydrogen with nitrogen , and obtaining the final product for sampling analysis after filtering to remove catalyst. The quality content of catalyst is 5 wt.% Pd-C, which is poisoned by 1 -3 wt.% lead poisoning catalyst. The amount of the catalyst is 0.33 ~ 0.99 wt.% of the total reaction products. The products of this invention is a multifunctional compound, which can be formed oxygenated heterocycle after closing loop and used as the intermediates for vitamin B6 and furan ring-containing drug. Therefore, butynediol production has good market prospects.

Description

technical field [0001] The invention relates to a method for selectively hydrogenating 2-butene-1,4-diol to synthesize 2-butene-1,4-diol. Background technique [0002] In the presence of a palladium metal catalyst, 2-butyne-1,4-diol can be added with hydrogen to generate alkenes or alkanes, and this hydrogenation reaction is carried out on the surface of the catalyst. The catalyst can chemically adsorb hydrogen and alkynes. If the conditions can be properly controlled to make the reaction stay in this stage (ie, the semi-hydrogenation stage), 2-butene-1,4-diol will be released from the surface of the catalyst. Otherwise, the resulting 2-butene-1,4-diol is hydrogenated again to form alkanes. [0003] 2-butene-1,4-diol is a light yellow liquid, and most of the synthetic products are cis-structure isomers. It can be used as an intermediate to produce n-(iso)propyl heptacyclic ring, which is used in the production of vitamin B6 and is the most upstream raw material of vitamin ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/17C07C33/035
Inventor 王维维
Owner 上海中远化工有限公司
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