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Preparing process of catalyst for cyclopropanizing reaction of 2,5-dimethyl-2,4-hexadiene

A hexadiene cyclopropane, catalyst technology, applied in catalyst activation/preparation, physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, etc. Influence of activity and product yield, small catalyst surface area, etc.

Inactive Publication Date: 2004-12-22
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With this method, the catalyst and the product are easily separated, the yield is high, and it has industrial application value; but because the catalyst is prepared by a simple mechanical mixing method, the surface area of ​​the catalyst is small, and the grain size of the active component is large. The uneven distribution of the components has a great influence on the activity of the catalyst and the product yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: Preparation and activity of catalyst A

[0018] Weigh 12.6 grams of dry activated alumina powder (20-40 mesh), soak it with 50 ml of an aqueous solution containing 0.35 grams of KOH for 24 hours, and measure the pH=9 of the modified solution; the filtered solid is dried at 120 ° C; after 350 After calcination and cooling at ℃, impregnate with a mixed aqueous solution containing polyvinyl alcohol, cobalt, copper, iron and other active components for 20 hours, dry at 110 ℃, and calcine at 450 ℃ for 2 hours; the obtained solid contains 0.75 gram of hydrogen Immerse in an aqueous solution of potassium oxide for 20 hours, dry at 110°C, and bake at 400°C for 2 hours. The amount of active components added in the obtained catalyst A is 70% of the total mass of the catalyst (calculated as oxides). The composition and specific surface area of ​​Catalyst A are listed in Table 1.

[0019] In a 250ml three-necked flask, add 0.10 grams of catalyst A, then add 20 grams...

Embodiment 2

[0020] Embodiment 2: the preparation and activity of catalyst B, C, D

[0021] Weigh 37.8 grams of dry activated alumina powder, soak it with 150 ml of an aqueous solution containing 1.05 grams of KOH for 24 hours, and measure the pH of the modification solution=9; the filtered solid is dried at 120° C.; roasted at 350° C. for 2 hours. The obtained modified carrier was divided into 3 parts on average, soaked in the aqueous solution of the mixture with the same citric acid content and different inorganic salt active component content for 20 hours, dried at 110°C, and calcined at 450°C for 2 hours; the obtained solid was used for 40 The gram contains 0.75 gram of potassium hydroxide to obtain the aqueous solution impregnation 20 hours, oven dry at 110 ℃, roast 2 hours at 400 ℃. The obtained catalysts were B, C and D, respectively. The catalyst composition and specific surface area and other properties are listed in Table 1.

[0022] Cyclopropanation reaction except catalyst is...

Embodiment 3

[0024] Embodiment 3: Catalyst E 1 -E 5 Preparation and activity

[0025] Take by weighing 12.6 grams of dry active alumina powder each time, with 50ml containing the aqueous solution of 0.35 grams of KOH and impregnate after 24 hours, record the pH=9 of modification solution; The operation procedure of reactivity evaluation is the same as that of Example 1. Catalyst composition and product yield (%) are listed in Table 2.

[0026] catalyst

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PUM

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Abstract

A carried catalyst used for cyclopropanizing 2,5-dimethyl-2,4-hexadiene contains the active component (20-90%) chosen from Fe, Ca, Ni, Ca, Zn, Cr, Mo or Ti, the assistant (0.1-5%) chosen from L, Na or K, and the carrier chosen from alumina silica gel and activated carbon. It is prepared through premodifying carrier, and immersing while adding active component and the organic compound containing hydroxy or carboxyl group and oxygen. Its advantages are low dosage, high output rate, little coking and easy separation.

Description

technical field [0001] The invention relates to a supported catalyst, in particular to a preparation method of the supported catalyst for 2,5-dimethyl-2,4-hexadiene cyclopropanation reaction. In the presence of the catalyst, the cyclopropanation reaction of olefin and diazoacetate is carried out to prepare the first methyl chrysanthemate, the first ethyl chrysanthemate and the like. The process has the characteristics of high reaction yield, less coking, less catalyst consumption, and easy separation of catalyst and reaction system. technical background [0002] Catalytic cyclopropanation of olefins is an important method for the synthesis of a class of organic intermediates, and is widely used in the synthesis of pharmaceutical and pesticide industries, such as the synthesis of the first methyl chrysanthemum acid, the first ethyl chrysanthemum acid, and permethrin Methyl ester, ethyl permethrin, etc. Most of the synthetic methods currently used are synthesized by homogene...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/06B01J23/26B01J23/34B01J23/70B01J23/72B01J37/02B01J37/08C07C67/30C07C69/743
Inventor 徐杰胡信全
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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