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Method for promoting hydrolysis of isooctyl isocaprylate and isooctyl formate

A technology of isooctyl ester and isooctanoic acid, which is applied in the field of recycling of by-products of fine chemical isooctyl alcohol, can solve the problem that heavy components cannot be fully utilized, and achieve the effects of low cost, high hydrolysis activity and simple preparation

Pending Publication Date: 2022-04-29
大连普莱瑞迪化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Finally, the product isooctyl alcohol is obtained through rectification separation, but there will always be heavy components produced during the reaction process at the bottom of the rectification tower during the production process that cannot be fully utilized

Method used

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  • Method for promoting hydrolysis of isooctyl isocaprylate and isooctyl formate
  • Method for promoting hydrolysis of isooctyl isocaprylate and isooctyl formate

Examples

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Effect test

Embodiment 1

[0032] The preparation of embodiment 1 catalyst

[0033] 0.5gNbCl 5 Add to 10 ml of 1mol / L ammonia water, stir and dissolve to form a colloid. Add 5.0 g CeO to the formed colloid 2 , at 50°C, after stirring for 4 hours, after suction filtration and water washing three times, drying at 100°C, the cerium oxide solid adsorbed with hydrated niobium pentoxide was obtained, and finally activated by roasting at 900°C under nitrogen atmosphere to obtain A small amount of composite oxide support of niobium pentoxide (Nb 2 o 5 @CeO 2 ).

[0034] Dissolve 0.5g of butyl stannoic acid in 5ml of acetone, and evenly add dropwise to 4.5g of the synthesized Nb 2 o 5 @CeO 2 On the carrier, dry at 60° C. for 12 hours to obtain catalyst A, and the loading amount of butyl stannoic acid is 10%.

[0035] 0.5g Ce(NO 3 ) 2 Add to 6 ml of 1mol / L aqueous oxalic acid solution, add 5.0 g of Nb to the resulting solution 2 o 5 , stirred at 40°C for 6 hours, then added 4 ml of 25% ammonia water ...

Embodiment 2

[0038] In a 1L autoclave, add isooctyl isooctanoate (274g, 1mol) and 200g of water, and add the above-mentioned catalyst A, 2.7g. The reaction kettle was stirred at 120°C, protected by nitrogen gas, and maintained at a slight positive pressure. Keeping the reaction temperature, after reacting for 8 hours, a sample was taken to analyze the composition of the product by gas chromatography. It was found that the hydrolysis conversion rate of isooctyl isooctanoate was 99%, and the hydrolyzed products were isooctanoic acid and isooctyl alcohol.

Embodiment 3

[0040] In a 1L autoclave, add isooctyl isooctanoate (274g, 1mol) and 200g of water, and add the above-mentioned catalyst B, 2.7g. The reaction kettle was stirred at 120°C, protected by nitrogen gas, and maintained at a slight positive pressure. Keeping the reaction temperature, after reacting for 8 hours, a sample was taken to analyze the composition of the product by gas chromatography. It was found that the hydrolysis conversion rate of isooctyl isooctanoate was 98%, and the hydrolyzed products were isooctanoic acid and isooctyl alcohol. After the reaction, the catalyst B was separated by filtration, the filtrate was allowed to stand for stratification, and the water was removed, and it was pickled with dilute sulfuric acid with a concentration of 9.0%, and the organic phase was collected to obtain a hydrolyzed crude product. After the catalyst B was washed with water in equal volume three times, the °C under a nitrogen atmosphere for 4 hours to obtain recovered catalyst B f...

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Abstract

The invention provides a method for promoting hydrolysis of isooctyl isooctanoate and isooctyl formate, which comprises the following steps: by taking composite oxide loaded butylstannic acid of niobium oxide and cerium oxide as a catalyst and taking isooctyl isooctanoate and / or isooctyl formate as raw materials, carrying out hydrolysis reaction in a water phase to obtain a hydrolysis crude product; the catalyst effectively promotes hydrolysis of ester, due to the special hydrophilic and oleophylic properties of the carrier, the catalyst shows excellent properties in a hydrolysis system for isooctyl alcohol ester, the conversion rates of isooctyl formate and isooctyl isooctanoate under the action of the catalytic hydrolysis system are both greater than 99%, and the catalyst is easy to separate, recycle and regenerate. In addition, the catalyst also has an excellent effect on hydrolysis reactions of other long-chain alcohol esters.

Description

technical field [0001] The invention belongs to the technical field of reuse of by-products produced by fine chemicals isooctyl alcohol, and in particular relates to a method for promoting the hydrolysis of isooctyl isooctanoate and isooctyl formate. Background technique [0002] Isooctyl alcohol, as a high value-added product downstream of the propylene industry chain, is the main raw material for the synthesis of important chemicals such as plasticizers and special functional esters, and its derivatives are used as the main plasticizer and cold-resistant auxiliary plasticizer for plastics , defoamer, dispersant, beneficiation agent and petroleum additive, also used in printing and dyeing, paint, film and so on. [0003] The main production process of iso-octanol is: propylene and synthesis gas synthesize n-butyraldehyde under the action of rhodium phosphorus catalyst; n-butyraldehyde synthesizes 2-ethylhexenal through aldol condensation dehydration; 2-ethylhexenal is added...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/125C07C29/09B01J23/20
CPCB01J23/20C07C31/125C07C29/095
Inventor 苏建龙
Owner 大连普莱瑞迪化学有限公司
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