Method for preparation of monohydric alcohol or dihydric alcohol by low temperature selective hydrogenation of organic acid water phase

An organic acid and selective technology, applied in the preparation of organic compounds, organic chemistry, chemical instruments and methods, etc., can solve problems such as high reaction temperature and pressure

Inactive Publication Date: 2014-10-29
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Hydrogenation of organic acids has broad application prospects, but due to the special structure of organic acid molecules and highly polarized C=O bonds, the conditions for direct hydrogenation become strict, and generally require higher reaction temperatures and larger pressure

Method used

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  • Method for preparation of monohydric alcohol or dihydric alcohol by low temperature selective hydrogenation of organic acid water phase
  • Method for preparation of monohydric alcohol or dihydric alcohol by low temperature selective hydrogenation of organic acid water phase
  • Method for preparation of monohydric alcohol or dihydric alcohol by low temperature selective hydrogenation of organic acid water phase

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-7

[0013] Preparation of Catalyst by Impregnation

[0014] The soluble salt solution containing 10% (mass fraction) of A is added to the carrier for impregnation according to a certain metering ratio, aged at room temperature for 12 hours, then dried in an oven at 60°C for 6 hours, and then transferred to an oven at 120°C for 6 hours; Then weigh the soluble salt solution of component B according to a certain molar ratio of B / A, add it to the above-mentioned carrier impregnated with component A, age at room temperature for 12 hours, and then dry it in an oven at 60°C for 6 hours and then transfer it to 120°C Dry in an oven for 6 hours, and bake in air at 500° C. for 3 hours to obtain a supported A-B / S catalyst. The composition of catalyst in each embodiment, the kind of starting material of component A, B is shown in Table 1.

[0015] Table 1. The composition of each catalyst

[0016] Example

[0017] Note: in each embodiment, the mass loading of A is 4%, the molar rat...

Embodiment 8-9

[0019] Catalyst activity evaluation

[0020] The catalyst evaluation of the present invention is carried out in a fixed-bed mobile phase reactor, which is a stainless steel tube with an outer diameter of 6 mm and a length of 360 mm. The experimental process is as follows: 2g of catalyst is loaded into the reaction tube, the catalyst is reduced in situ at 300°C before the reaction, and after the reduction is completed, it is lowered to the reaction temperature, and the H 2 The flow rate is 60mL / min, the flow rate of the organic acid liquid is 0.08mL / min, and the reaction pressure is 6MPa. After 6 hours of reaction, samples are taken for analysis.

Embodiment 8

[0022] Activity Evaluation of Levulinic Acid Hydrogenation to 1,4-Pentanediol

[0023] 1) Accelerator V for Rh / SiO 2 Effect on levulinic acid hydrogenation activity

[0024] Table 2. Accelerator V for Rh / SiO 2 Influence on the hydrogenation activity of levulinic acid

[0025]

[0026]

[0027] Note: For 10% levulinic acid solution, the gas phase products are methane and pentane, etc., expressed by "other". The mass loading of Rh in a is 4%, V / Rh=0.13, and the V species in the catalyst can be either a simple substance or an oxide, so x=0-3. The reaction temperature is 80 °C.

[0028] It can be seen from Table 2 that the addition of V can significantly improve the Rh / SiO 2 The hydrogenation activity also shows that there is a synergistic effect between V and Rh so that Rh-VO x / SiO 2 It has good catalytic hydrogenation performance.

[0029] 2) The effect of catalyst V / Rh ratio on the hydrogenation activity of levulinic acid.

[0030] Table 3. Effect of V / Rh ratio o...

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Abstract

The invention relates to a method for preparation of monohydric alcohol or dihydric alcohol by selective catalytic hydrogenation of an organic acid water phase under a mild condition. The reactant is any one of a mixture of over two of organic acids. The catalyst is an A-B / S loaded catalyst, wherein the component A is any one or more than two of Ir, Pt, Pd, Rh and Ru; the assistant B is a simple substance or oxide of any one or more than two of Nb, Ta and V; and the carrier S is any one of or a mixture of over two of silicon oxide, alumina, activated carbon, titanium oxide, zirconia and a molecular sieve. The mass loading capacity of A in the catalyst is 0.5-10%, the mole ratio of the assistant B to A is 0.01-2.0, the reaction pressure is 1-20MPa, and the reaction temperature is 40-180DEG C. The catalyst provided by the invention has the characteristics of mild reaction condition, high reaction activity and good alcohol product selectivity.

Description

technical field [0001] The invention relates to a method for preparing monohydric alcohol or dihydric alcohol by selective catalytic hydrogenation of organic acid aqueous phase under mild conditions. Specifically, acetic acid, propionic acid, butyric acid, valeric acid, stearic acid (oleic acid), lauric acid, palmitic acid, levulinic acid, lactic acid, oxalic acid, succinic acid, malonic acid (3- Hydroxypropionic acid) and one or two or more of other organic acids are reactants, and the A-B / S supported catalyst is used to realize the hydrogenation of organic acids to prepare monohydric alcohols under milder conditions. Background technique [0002] As the source of power for economic development and the basic conditions for the survival of human society, energy and the environment are two hot topics that attract the attention of the public in today's society. In recent years, the importance of energy has become more and more obvious as the world's fossil energy reserves are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/648C07C29/149C07C31/20C07C31/08C07C31/10C07C31/12C07C31/125
Inventor 张涛李孟夏李宁王爱琴王晓东
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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