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Catalyst for preparing isononanoic acid through catalytic oxidation of isononyl alcohol as well as preparation method and application thereof

A technology of catalytic oxidation and isononanol, applied in catalyst activation/preparation, preparation of organic compounds, metal/metal oxide/metal hydroxide catalyst, etc., can solve the problems of poor thermal stability, acid and alkali resistance, etc., Achieving the effect of simple preparation method and good catalyst performance

Active Publication Date: 2021-04-16
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is a phenomenon of dehydration or decarbonylation of a small part of the product in this process, resulting in a small amount of diisobutene in the product
At the same time, the existing production process needs to add a homogeneous catalyst to decompose the peroxide produced in the reaction process, and bring various potential problems and risks to the subsequent separation and purification process
The cost of the raw material isononanal used in the patent CN 108047027 A is much higher than that of isononanol. At the same time, the metal-organic framework catalyst used in this patent has the problems of poor thermal stability and resistance to acid and alkali, which greatly improves the instability and stability of the production process. cost

Method used

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  • Catalyst for preparing isononanoic acid through catalytic oxidation of isononyl alcohol as well as preparation method and application thereof
  • Catalyst for preparing isononanoic acid through catalytic oxidation of isononyl alcohol as well as preparation method and application thereof
  • Catalyst for preparing isononanoic acid through catalytic oxidation of isononyl alcohol as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Vector pretreatment

[0037] Weigh 5g of activated carbon, disperse in 100ml of 8wt% nitric acid solution, place in 90°C oil bath, stir, condense and reflux for 3h. Then use deionized water to centrifuge and wash several times until the supernatant is neutral in acidity and alkalinity. Finally, under the condition of 55° C., vacuum drying was performed for 12 hours to obtain a pretreated modified activated carbon carrier.

Embodiment 2

[0039] Preparation of Pd-Co / C

[0040] Weigh 8.2mg of palladium chloride, add a small amount of concentrated hydrochloric acid dropwise until completely dissolved; weigh 6.8mg of cobalt chloride hexahydrate, dissolve in a small amount of deionized water, then add chloropalladium acid solution, mix well and add deionized water Dilute to 20ml. Weigh 0.1 g of modified activated carbon, add it to the above solution, and stir at room temperature for 3 h. The pH value of the solution was adjusted to 9-10 with saturated sodium carbonate solution, followed by stirring for 1 h. Weigh 25mg of sodium borohydride, add 10ml of water to dissolve, quickly drop into the above solution, and continue to stir for 3h. Filter the above system through a filter and wash it several times until the filtrate is neutral in acidity and alkalinity, put it in a drying oven at 40°C, and dry it in vacuum for 12 hours to obtain the catalyst Pd-Co / C.

[0041] figure 1 It is the XRD spectrum of the prepared...

Embodiment 3

[0043] Preparation of Pd-Cu / C

[0044] Weigh 8.2mg of palladium chloride, add a small amount of concentrated hydrochloric acid dropwise until completely dissolved; weigh 4.8mg of copper chloride dihydrate, dissolve it in a small amount of deionized water, then add it to the chloropalladium acid solution, mix well and then add deionized Dilute to 20ml with water. Weigh 0.1 g of modified activated carbon, add it to the above solution, and stir at room temperature for 3 h. The pH value of the solution was adjusted to 9-10 with saturated sodium carbonate solution, followed by stirring for 1 h. Weigh 25mg of sodium borohydride, add 10ml of water to dissolve, quickly drop into the above solution, and continue to stir for 3h. Filter the above system through a filter and wash it several times until the filtrate is neutral in acidity and alkalinity, put it in a 40°C drying oven, and dry it in vacuum for 12 hours to obtain the catalyst Pd-Cu / C.

[0045] figure 2It is the XRD spectr...

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Abstract

The invention discloses a catalyst for preparing isononanoic acid through catalytic oxidation of isononyl alcohol as well as a preparation method and application of the catalyst. The preparation method comprises the following steps: (1) uniformly dispersing carrier activated carbon in dilute nitric acid, and carrying out pretreatment modification; (2) dissolving an active metal salt palladium chloride in concentrated hydrochloric acid to prepare a chloropalladic acid solution; preparing an active additive into an aqueous solution, and mixing the aqueous solution with the chloropalladic acid solution to obtain an impregnation solution; adding the pretreated carrier activated carbon into the impregnation solution, and stirring and impregnating; and (3) adjusting the pH value of the system by using an alkaline solution to pre-disperse the active components. And (4) carrying out wet reduction on the active component, separating and drying to obtain the target composite catalyst. Meanwhile, the route for preparing isononanoic acid by oxidizing isononyl alcohol disclosed by the invention is relatively high in isononyl alcohol conversion rate and high in isononanoic acid selectivity, the energy consumption and investment of a separation section can be effectively reduced, and the reaction route for obtaining isononanoic acid by directly oxidizing isononyl alcohol is more friendly to raw material transportation conditions and has a good application prospect.

Description

technical field [0001] The invention relates to the field of heterogeneous catalysis, in particular to a catalyst for catalyzing and oxidizing isononanol to produce isononanoic acid, a preparation method and application thereof. Background technique [0002] Isononanoic acid (3,5,5-trimethylhexanoic acid), the structure is as follows As a fine chemical intermediate with a wide range of uses, it can be used as an upstream raw material for coatings, lubricants, plasticizers, and is also suitable for alkyd resin modification , and can also be used to produce various isononanoic acid esters, which are used in the field of cosmetics. [0003] [0004] The preparation of isononanoic acid by aldehyde oxidation is the main production process at present. The raw material is isononanal (3,5,5-trimethylhexanal) or isononanol (3,5,5-trimethylhexanol). Reaction temperature above 300°C and alkali fusion under 2MPa reaction pressure to obtain the corresponding acid. There is a phenome...

Claims

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Application Information

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IPC IPC(8): B01J23/89B01J37/02B01J37/16C07C53/126C07C51/215
Inventor 李映伟杨弈涛
Owner SOUTH CHINA UNIV OF TECH
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