Preparation method of grafted catalyst for continuous catalytic synthesis of isobutyl isobutyrate

A technology of isobutyl isobutyrate and catalysts, which is applied in the direction of organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, aldehyde redox preparation, etc., which can solve the large discharge of waste liquid and pollutants , poor catalyst stability, poor reusability and other problems, to achieve the effects of shortening industrial production steps, overcoming catalyst deactivation, good economy and industrial value

Active Publication Date: 2020-11-27
RUNTAI CHEM TAIXING CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The esterification reaction process has many defects. When concentrated sulfuric acid is used as a common catalyst, a large number of by-products are produced, equipment is severely corroded, and waste liquid and pollutants are discharged in large quantities; SO 2 -4 When the / MxOy type solid acid is used as a catalyst, not only the preparation of the catalyst is cumbersome, but also the stability of the catalyst is not good enough, and the catalytic activity is low; When ion exchange resin is used as a catalyst, its preparation is cumbersome and costly, and its reusability is poor

Method used

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  • Preparation method of grafted catalyst for continuous catalytic synthesis of isobutyl isobutyrate
  • Preparation method of grafted catalyst for continuous catalytic synthesis of isobutyl isobutyrate
  • Preparation method of grafted catalyst for continuous catalytic synthesis of isobutyl isobutyrate

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Experimental program
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Effect test

Embodiment 1

[0022] (1) First disperse 5.0g of NMC in 100mL of sulfuric acid washing solution (volume ratio H 2 SO 4 :H 2 o 2 =3:1), put it in an ultrasonic cleaner for 2 hours, and then stir it at 80°C for 2 hours; finally, wash the NMC repeatedly with distilled water until neutral, and dry it overnight at 60°C. The treated carrier is designated as NMC-A.

[0023] (2) Put 1.5 g of 2-hydroxy-N-methylacetamide into a container at 60° C. and heat it, protect it with nitrogen and add 2 g of elemental sodium, stir for 6 hours and filter to obtain organic sodium salt.

[0024] (3) 1.5 g of the filtered organic sodium salt and 5 g of the acidified carrier were put into ethanol and stirred for 5 hours. The catalyst was prepared by filtering and drying overnight at 60°C.

[0025] Weigh 50 grams of the catalyst, put it into a reaction tube, feed isobutyraldehyde into the fixed-bed reactor at a flow rate of 1 L / min, press 0.2 MPa, raise the temperature of the heating furnace from room temperatu...

Embodiment 2

[0027] In the step (1), the concentration of washing liquid is (H 2 SO 4 :H 2 o 2 =2:1) ​​instead of the concentration of lotion in embodiment 1 is (H 2 SO 4 :H 2 o 2 =3:1), other steps are with embodiment 1.

Embodiment 3

[0029] In the step (1), the concentration of washing liquid is (H 2 SO 4 :H 2 o 2 =4:1) instead of the concentration of lotion in embodiment 1 is (H 2 SO 4 :H 2 o 2 =3:1), other steps are with embodiment 1.

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Abstract

The invention relates to the technical field of catalysts, in particular to a preparation method of a grafted catalyst for continuous catalytic synthesis of isobutyl isobutyrate. An active center of the grafted catalyst prepared by the method belongs to a molecular form uniformly grafted on a carrier and is higher. Isobutyraldehyde is used as a reactant and reacts under the action of a grafting catalyst to prepare isobutyl isobutyrate, the reaction steps are few, byproducts are avoided, the reaction temperature is low, and the defects that the catalyst is inactivated and is difficult to separate from the product are overcome; besides, no byproducts except water are generated in the reaction process, the influence of water on the product is eliminated, and large-scale production can be achieved. The content of isobutyl isobutyrate in the prepared product is greater than 90%, and the requirements of industrial products are met.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a method for preparing a grafted catalyst for continuous catalytic synthesis of isobutyl isobutyrate. Background technique [0002] Isobutyraldehyde is not as widely used as n-butyraldehyde. The industry mainly produces isobutanol by hydrogenation. The addition reaction of isobutyraldehyde and formaldehyde produces hydroxytrimethylacetaldehyde, which is then hydrogenated to form neopentyl glycol, which is used as raw material for varnish, resin, fiber and lubricant; the fertilizer produced by the reaction of isobutyraldehyde and urea can Slowly release nitrogen; in addition, it is also used as an intermediate for amino acids, vitamins and other drugs. The oxo method can obtain n-butyraldehyde and isobutyraldehyde at the same time in proportion. The situation of consumption balance is still that the supply of isobutyraldehyde exceeds the demand, and a very large amount of isob...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07C69/24C07C67/44
CPCB01J31/0247B01J31/0254C07C67/44B01J2231/49C07C69/24
Inventor 张世元卢小松宋文国
Owner RUNTAI CHEM TAIXING CO LTD
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