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A kind of fixed-bed synthesis method of 3,3,5-trimethylcyclohexanone

A technology of trimethylcyclohexanone and its synthesis method, which is applied in the field of fixed-bed synthesis of 3,3,5-trimethylcyclohexanone, and can solve the difficulties in product separation, unfavorable large-scale production, and small processing capacity, etc. problems, to achieve the effects of filling patent gaps, being easy to implement, and increasing throughput

Active Publication Date: 2017-06-20
CHAMBROAD CHEM IND RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the C=C double bond (615kJ·mol -1 ) and C=O double bond (715kJ·mol -1 ) have similar bond energies. Under the action of general hydrogenation catalysts, not only the C=C double bond is hydrogenated, but also the C=O double bond is easily hydrogenated to form the by-product 3,3,5-tri Methylcyclohexanol, its products and by-products have similar boiling points (the boiling point of 3,3,5-trimethylcyclohexanone is 189°C, and the boiling point of 3,3,5-trimethylcyclohexanol is 191°C), Therefore, it brings great difficulties to the follow-up product separation work.
[0004] In CN102718641 B and CN201410127444.1, all propose adopting Pd or Pt catalyst in autoclave, the method for the selective hydrogenation of isophorone to prepare 3,3,5-trimethylcyclohexanone, its reaction has relatively High selectivity, but the cost is higher after the use of precious metals, and it is a batch reaction with a small amount of treatment, which is not conducive to large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Ni / γ-Al modified with cocatalyst Cu in a 5ml fixed bed reactor 2 o 3 (Molar ratio: Cu / Ni=1:2) The catalyst selectively hydrogenates isophorone to 3,3,5-trimethylcyclohexanone, the reaction temperature is 140°C, the reaction pressure is 1.0Mpa, and the space velocity is 0.5h -1 , under the condition of a hydrogen-to-oil ratio of 900:1, the conversion rate of isophorone is 93.2% and the selectivity of 3,3,5-trimethylcyclohexanone in the product is 90.0% through gas chromatography analysis.

[0029] The concrete preparation steps of the supported Ni-based catalyst of described modification are:

[0030] (1) Prepare the carrier by kneading method, place it at room temperature for 24 hours and then dry it at 120°C for 3 hours;

[0031] (2) Calcining the dried carrier at 700° C. for 4 hours in step (1);

[0032] (3) dissolving the metal salt corresponding to the cocatalyst and the active component in water in proportion to obtain a metal salt solution;

[0033] (4) Immers...

Embodiment 2

[0037] In a 5ml fixed bed reactor, Ni / γ-Al modified with cocatalyst Cr 2 o 3 (Molar ratio: Cr / Ni=1:5) The catalyst selectively hydrogenates isophorone to 3,3,5-trimethylcyclohexanone, the reaction temperature is 260°C, the reaction pressure is 2.0Mpa, and the space velocity is 3.0h -1 , under the condition of hydrogen oil ratio of 900:1, the conversion rate of isophorone is 99.3% and the selectivity of 3,3,5-trimethylcyclohexanone in the product is 97.5% through gas chromatography analysis.

[0038] The concrete preparation steps of the supported Ni-based catalyst of described modification are:

[0039] (1) Prepare the carrier by kneading method, place it at room temperature for 24 hours and then dry it at 120°C for 4 hours;

[0040] (2) Calcining the dried carrier at 800° C. for 3 hours in step (1);

[0041] (3) dissolving the metal salt corresponding to the cocatalyst and the active component in water in proportion to obtain a metal salt solution;

[0042] (4) Immersing ...

Embodiment 3

[0046] In a 5ml fixed bed reactor, Ni / γ-Al modified with cocatalyst Cr 2 o 3 + Diatomite (molar ratio: Cr / Ni=1:8) catalyst to selectively hydrogenate isophorone to 3,3,5-trimethylcyclohexanone, the reaction temperature is 300°C, the reaction pressure is 1.5Mpa, Airspeed 1.0h -1 , under the condition of a hydrogen-to-oil ratio of 800:1, the conversion rate of isophorone is 96.7% and the selectivity of 3,3,5-trimethylcyclohexanone in the product is 95.5% through gas chromatography analysis.

[0047] The concrete preparation steps of the supported Ni-based catalyst of described modification are:

[0048] (1) Prepare the carrier by kneading method, place it at room temperature for 24 hours and then dry it at 110°C for 4 hours;

[0049] (2) Calcining the dried carrier at 700° C. for 3 hours in step (1);

[0050] (3) dissolving the metal salt corresponding to the cocatalyst and the active component in water in proportion to obtain a metal salt solution;

[0051] (4) Immersing t...

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PUM

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Abstract

The present invention relates to a 3,3,5-trimethylcyclohexanone synthetic method, in particular to a fixed-bed synthetic method for 3,3,5-trimethylcyclohexanone. The synthetic method comprises: in a fixed bed reactor, under a condition that a reaction temperature is 140-300 DEG C, reaction pressure is 0.1-2.0 Mpa, space velocity is 0.5-3.0 h-1, and a hydrogen to oil ratio is 500:1 to 1500:1, isophorone is selectively hydrogenized and reduced into the 3,3,5-trimethylcyclohexanone by virtue of a modified supported Ni-based catalyst. According to the method, on the premise of guaranteeing a conversion rate of the isophorone and higher selectivity of the 3,3,5-trimethylcyclohexanone, the modified supported Ni-based catalyst is used to replace metal catalysts such as Pt or Pd and the like, thereby saving the production cost, and having higher economic significance.

Description

technical field [0001] The invention relates to a synthesis method of 3,3,5-trimethylcyclohexanone, in particular to a fixed-bed synthesis method of 3,3,5-trimethylcyclohexanone. Background technique [0002] 3,3,5-Trimethylcyclohexanone, as an important high-boiling organic solvent and pharmaceutical synthesis intermediate, is mainly used in the fields of medicine, pesticides, and fine chemicals, and its downstream products can be used as vulcanizing agents in rubber and other industries and polymerization initiators in the plastics industry. [0003] 3,3,5-Trimethylcyclohexanone is mainly prepared by hydrogenation of isophorone. The molecular structure of isophorone contains a C=C double bond and a C=O double bond, and the product 3,3,5-trimethylcyclohexanone is obtained by hydrogenating the C=C double bond. Due to the C=C double bond (615kJ·mol -1 ) and C=O double bond (715kJ·mol -1 ) have similar bond energies. Under the action of general hydrogenation catalysts, not...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/603C07C45/62B01J23/755B01J23/80B01J23/883B01J23/83
CPCB01J23/002B01J23/755B01J23/80B01J23/83B01J23/883B01J2523/00C07C45/62C07C49/603B01J2523/17B01J2523/31B01J2523/847B01J2523/28B01J2523/27B01J2523/68B01J2523/41B01J2523/3712
Inventor 赵德明郭振莲王东超徐金凤李寿丽韩立霞燕庆玲王珊珊
Owner CHAMBROAD CHEM IND RES INST CO LTD