A kind of preparation method of carboxylic acid

A carboxylic acid and step method technology, applied in the field of carboxylic acid preparation, can solve the problems of large investment and complex composition of reaction solution, and achieve the effects of high selectivity, easy control and operation, and simple preparation process

Active Publication Date: 2019-09-13
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the complex composition of the reaction solution, special measures need to be taken for separation and purification, the investment is large, and the disadvantages are obvious.

Method used

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  • A kind of preparation method of carboxylic acid
  • A kind of preparation method of carboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Activated alumina powder (purchased from Aluminum Corporation of China Shandong Branch) was placed in a muffle furnace and calcined at 500°C for 3 hours under static or flowing air with a heating rate of 5°C / min to obtain calcined alumina powder . Weigh 0.8-1.2 g of calcined activated alumina, press into tablets, grind, and take 40-60 mesh particles as the catalyst.

[0029] The prepared Al 2 o 3 The catalyst is installed in the middle of a tubular reactor with a diameter of 8 mm and a length of 45 cm, and the upper and lower parts of the catalyst are filled with 40-60 mesh quartz sand. Then place the tubular reactor filled with catalyst in the heating furnace, open the carrier gas (N 2 ) and feed, the feed flow rate is 20ml / min, open the heating device, make the temperature reach 300°C in the mode of temperature program (3-5°C / min), constant temperature, feed 10wt% lactic acid aqueous solution, feed flow rate Be 0.5ml / min, begin to collect product and carry out pro...

Embodiment 2

[0031] The activated silica powder was placed in a muffle furnace and calcined at 500° C. for 3 hours under static or flowing air with a heating rate of 5° C. / min to obtain calcined silica powder. Weigh 0.8-1.2 g of the calcined silicon dioxide, press into tablets, grind, and take 40-60 mesh particles as the catalyst.

[0032] The prepared silicon dioxide catalyst was placed in the middle of a tubular reactor with a diameter of 8 mm and a length of 45 cm, and the upper and lower parts of the catalyst were filled with 40-60 mesh quartz sand. Then place the tubular reactor filled with catalyst in the heating furnace, open the carrier gas (N 2) and pass in, the flow rate is 20ml / min, the heating device is turned on, and the temperature reaches 300°C in the mode of temperature program (3-5°C / min), at a constant temperature, 10wt% lactic acid aqueous solution is passed in, and the flow rate is It was 0.5ml / min, and the product was collected and analyzed after 3 hours of reaction, ...

Embodiment 3

[0034] The activated alumina powder was placed in a muffle furnace and calcined at 500° C. for 3 hours under static or flowing air with a heating rate of 5° C. / min to obtain calcined alumina powder.

[0035] Weigh 0.2g of barium sulfate in a beaker, add 30ml of deionized water, add 1.0g of calcined alumina powder into the solution, use ultrasonic impregnation method, treat at room temperature for three hours, and then place the obtained solution in microwave Microwave treatment in the processor for 2 hours, after suction filtration / rotary evaporation filtration, the obtained catalyst was dried in a drying oven at 130°C for 4 hours, and then calcined with programmed temperature control at a heating rate of 5-10°C / min, set Set the calcination temperature at 600°C, and calcine at constant temperature for 3 hours to obtain 20wt% BaSO 4 / Al 2 o 3 Supported catalyst, where BaSO 4 Equivalent to carrier Al 2 o 3 The loading amount is 20wt%.

[0036] The obtained 20wt% BaSO 4 / A...

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Abstract

The invention discloses a preparation method of carboxylic acid. According to the preparation method, a metal carrier of activated aluminum oxide is modified, and one or more types of metallic ions are introduced to regulate the activity in an active center of the surface of the carrier to ensure that a catalyst can be efficiently and highly-selectively used for preparing the carboxylic acid, so that the carboxylic acid can be prepared continuously and efficiently, and the preparation method disclosed by the invention is simple in preparation process, is easy to control and operate, and effectively reduces the cost; and the preparation method disclosed by the invention is high in selectivity for the carboxylic acid, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a preparation method of carboxylic acid. Background technique [0002] Carboxylic acid is an important class of organic compounds, widely used in pesticides, veterinary drugs, pharmaceuticals and other industries. For example, acetic acid can be used as an acidity regulator, acidulant, pickling agent, flavor enhancer, spice, etc.; propionic acid can be used as an esterifying agent, a solvent for nitrocellulose, a plasticizer, a chemical reagent, and a food preparation, etc.; N-butyric acid is an important synthetic fragrance and raw material for other fine chemical products. [0003] The synthesis methods of carboxylic acids can be mainly divided into oxidation method and hydrolysis method. Oxidation methods can be divided into hydrocarbon oxidation, oxidation of primary alcohols and aldehydes, and oxidation of methyl ketones. Hydrolysis methods include nitrile hydrolysis, oi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/377C07C53/122C07C57/30B01J27/053B01J23/14B01J23/08B01J23/78
Inventor 牟新东李学民王喜成刘晓然徐国强
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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