2-butylene-1,4-diol synthesis method

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 ...

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.