Method for preparing monohydric alcohol or dihydric alcohol through organic acid hydrogenation

An organic acid and monohydric alcohol technology, applied in the preparation of organic compounds, organic chemistry, chemical instruments and methods, etc., can solve the problems of difficult product separation and high reaction temperature

Active Publication Date: 2013-09-11
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because this reaction adopts homogeneous catalysis method, product separation difficulty, and reaction temperature is higher, so also there is certain defective (Frank M.A.Geilen, BarthelEngendahl, Andreas Harwardt, Wolfgang Marquardt, JürgenKlankermayer, Walter Leitner.Angew.Chem.Int.Ed. 2010, 49, 5510);

Method used

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  • Method for preparing monohydric alcohol or dihydric alcohol through organic acid hydrogenation
  • Method for preparing monohydric alcohol or dihydric alcohol through organic acid hydrogenation
  • Method for preparing monohydric alcohol or dihydric alcohol through organic acid hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-8

[0021] Preparation of Catalyst by Impregnation Method

[0022] A 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, and then dried in an oven at 120°C for 12 hours; then according to a certain B / A molar ratio Weigh the soluble salt solution of component B, add it to the above-mentioned carrier impregnated with component A, age at room temperature for 12 hours, then dry at 120°C for 12 hours, and bake in air at 500°C for 3 hours; the catalyst Before use, it needs to be reduced under hydrogen, the reduction temperature is 200°C, H 2 The pressure is 6MPa, H 2 The flow rate was 160 mL / min, and the catalyst was reduced for 2 hours under this condition to obtain a supported A-B / X catalyst. The composition of catalyst in each embodiment, the kind of starting material of component A, B is shown in Table 1.

[0023] Table 1. The composition of each catalyst ...

Embodiment 9-11

[0028] Catalyst activity evaluation

[0029]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 before the reaction, and the reaction temperature is lowered to the reaction temperature after the reduction, and the H 2 The flow rate is 60mL / min, the flow rate of the organic acid liquid is 0.04mL / min, and the reaction pressure is 6MPa. After 6 hours of reaction, sampling and analysis are carried out.

Embodiment 9

[0031] Activity Evaluation of Acetic Acid Hydrogenation to Ethanol

[0032] 1) The influence of reaction temperature on the hydrogenation activity of acetic acid, the activity evaluation results are shown in Table 2.

[0033] Table 2. Effect of reaction temperature on acetic acid hydrogenation activity

[0034]

[0035] Note:

[0036] 4%Ir-MoO x / SiO 2 (Mo / Ir=0.13, x=0~3) Catalyst, 10% acetic acid solution (mass concentration), gas phase products methane, ethane and a small amount of acetaldehyde are represented by "other".

[0037] As can be seen from Table 2, 4% Ir-MoO x / SiO 2 (Mo / Ir=0.13, x=0~3) the catalyst has good low-temperature activity, and when the reaction temperature is 100°C, the yield of ethanol is the highest (47.2%).

[0038] 2) Comparison of the hydrogenation activity of different additives to acetic acid, the activity evaluation results are shown in Table 3.

[0039] Table 3. Effect of different additives on the hydrogenation activity of acetic aci...

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Abstract

The invention relates to a method for preparing monohydric alcohol or dihydric alcohol through organic acid hydrogenation. According to the method, any one of acetic acid, propionic acid, valeric acid, stearic acid, oleic acid, palmitic acid, levulinic acid, lactic acid, succinic acid, 3-hydracrylic acid and other organic acids is taken as a reactant, and an A-B/X supported catalyst is adopted, wherein the component A is any one or more than two from Ir, Pt, Pd, Rh and Ru, the assistant B is any one or more than two from Mo, Re and W, the carrier X is any one in SiO2, activated carbon, titanium oxide, zirconium oxide, SiO2-Al2O3 (the mass content of Al2O3 accounts for 17 percent) and molecular sieves, the mass load amount of A in the catalyst is 0.5-10 percent, the molar ratio of the assistant B to A is 0.01-1.0, the reaction pressure is 2-20 MPa, and the reaction temperature is 40-180 DEG C. The catalyst has the characteristics of mild reaction conditions, high reaction activity and good selectivity, and a novel effective way for preparing monohydric alcohol or dihydric alcohol from biomass is provided.

Description

technical field [0001] The invention relates to a method for preparing monohydric alcohol or dihydric alcohol by hydrogenation of organic acid. Specifically, one of acetic acid, propionic acid, valeric acid, stearic acid, oleic acid, palmitic acid, levulinic acid, lactic acid, succinic acid, 3-hydroxypropionic acid and other organic acids is used as the reactant. The A-B / X supported catalyst is used to realize the non-petroleum and renewable preparation route of monohydric alcohol and dihydric alcohol from biomass under milder conditions. Background technique [0002] The increasing scarcity of fossil resources, the increase in oil prices, the massive emissions of greenhouse gases, and the demand for energy in society require people to look for new energy sources that can replace fossil resources. Biomass, as the only renewable organic carbon source, can be used to produce fuels, chemicals and carbon materials, and has become a hot research topic at present. [0003] Cellu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/08C07C31/10C07C31/125C07C31/20C07C29/149B01J23/652B01J23/656B01J23/89
Inventor 张涛王志强李宁王爱琴王晓东
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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