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Preparation method of polymer catalyst for acetone condensation

A catalyst and polymer technology, applied in the field of polymer catalyst preparation, can solve the problems of poor thermal stability, low specific surface area, low strength, etc.

Active Publication Date: 2016-07-06
NANJING UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The inventive method actually divides the reaction into 2 to 3 sections, and a device for removing water is added in the middle of each section to break the reaction balance and improve the conversion rate of acetone, but the catalyst used is γ-Al 2 o 3 The solid base catalyst of loaded calcium or barium has poor thermal stability, low strength and low specific surface area, which limits its application

Method used

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  • Preparation method of polymer catalyst for acetone condensation
  • Preparation method of polymer catalyst for acetone condensation
  • Preparation method of polymer catalyst for acetone condensation

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Add 1.6988 g of N-methylol acrylamide, 0.2985 g of 2-methyl-2-acrylic acid-4-L-proline methyl ester, and 2-methyl-2-acrylic acid-4- Piperidine methyl ester 0.0855g, initiator BPO0.0460g and solvent DMSO10mL, stirred to dissolve and deoxygenated. The reaction was carried out in an oil bath at 75°C for 12 hours. After the reaction, the product was precipitated with 100 mL of anhydrous tetrahydrofuran as a precipitant, centrifuged, and the precipitate was placed in a vacuum oven at 50°C to dry for 12 hours to obtain catalyst PNL-I1.3795g. 66.23%, where a:b:c=36:3:1.

Embodiment 2

[0037] Add 1.3213 g of N-methylol acrylamide, 0.2985 g of 2-methyl-2-acrylic acid-4-L-proline methyl ester, and 2-methyl-2-acrylic acid-4- 0.0855 g of piperidine methyl ester, 0.0368 g of initiator BPO and 15 mL of solvent MA were stirred and dissolved, and oxygen was removed. The reaction was carried out in an oil bath at 65°C for 10 hours. After the reaction, the product was precipitated with 150 mL of anhydrous tetrahydrofuran as a precipitant, centrifuged, and the precipitate was placed in a vacuum oven at 50°C for 12 hours to dry to obtain 1.2686g of catalyst PNL-II. The preparation yield 74.39%, where a:b:c=28:3:1.

Embodiment 3

[0039] Add 0.9438 g of N-methylol acrylamide, 0.2985 g of 2-methyl-2-acrylic acid-4-L-proline methyl ester, and 2-methyl-2-acrylic acid-4-methyl ester into the pressure-resistant reaction flask. 0.0855 g of piperidine methyl ester, 0.0276 g of initiator BPO and 20 mL of solvent MA were stirred and dissolved, and oxygen was removed. The reaction was carried out in an oil bath at 55°C for 12 hours. After the reaction was completed, the product was precipitated with 200 mL of anhydrous tetrahydrofuran as a precipitant, centrifuged, and the precipitate was placed in a vacuum oven at 50°C to dry for 12 hours to obtain a catalyst PNL-III 0.9438 g, with a preparation yield 71.08%, where a:b:c=20:3:1.

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Abstract

The invention relates to a preparation method and applications of a polymer catalyst. The catalyst is applied to acetone condensation and dehydration for preparing mesityl oxide and is capable of improving the conversion rate of acetone. The preparation method comprises the following steps: adding N-hydroxymethyl acrylamide, 2-methyl-2-acrylic acid-4-L-methyl proline ester, 2-methyl-2-acrylic acid-4-methyl piperidine ester, an initiator namely benzoperoxide (BPO), and a solvent into a pressure resistant reaction flask in sequence, wherein the solvent can be methanol (MA), N,N-dimethyl formamide (DMF), dimethyl sulfoxide (DMSO), or N,N-dimethyl acetamide (DMA), stirring to dissolve the components mentioned above, removing oxygen; carrying out reactions at a certain polymerization temperature, after reaction, precipitating the reaction product, subjecting the reaction production to centrifugation, and drying the reaction product to obtain the catalyst (PNL).

Description

Technical field [0001] The invention relates to a method for preparing a polymer catalyst and its application. The catalyst can increase the conversion rate of acetone when it is used in the reaction of acetone condensation dehydration to prepare mesityl oxide. Background technique [0002] Mesityl oxide (4-methyl-3-penten-2-one, Mesityloxide, MO for short) is a colorless, transparent, volatile, and medium boiling point solvent. It is an important raw material for chemical products such as drugs and pesticides. It is mainly used to prepare methyl isobutyl ketone, methyl isobutyl alcohol, phorone and isophorone; it is also used in the manufacture of coatings, polyvinyl chloride, high Molecular polymer resins, dyes, solvents for dewaxing in the oil refining industry, diluents, cleaning agents, extraction agents and mineral flotation agents. [0003] Acetone catalyzes the condensation of acetone to produce diacetone alcohol (DAA). The catalyst used is usually alkali metal hydroxide o...

Claims

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Application Information

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IPC IPC(8): B01J31/06C07C45/74C07C49/203C08F220/58C08F220/36
CPCC07C45/74C08F220/58B01J31/06B01J2231/34C07C49/203C08F220/36C08F220/365Y02P20/584
Inventor 徐林黄杰军范以宁丁克鸿顾克军
Owner NANJING UNIV
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