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A catalyst for immobilized MPV reaction, its preparation method and its application in the production of nerol and geraniol

A catalyst and reaction technology, applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, catalytic reaction, etc., can solve the problems of poor reaction selectivity, inability to quickly and effectively separate and reuse, etc.

Active Publication Date: 2019-10-29
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The diaminoaluminum complex catalyst can be crystallized and separated, but it is still in a homogeneous state when used, and cannot be quickly and effectively separated for reuse after the reaction
[0008] Fang Wenzhong, Xiong Fang, and Jin Lin used hydrochloric acid dealumination-alkali metal and alkaline earth metal ion exchange to prepare modified BEA zeolite catalyst, and isopropanol as hydrogen so

Method used

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  • A catalyst for immobilized MPV reaction, its preparation method and its application in the production of nerol and geraniol
  • A catalyst for immobilized MPV reaction, its preparation method and its application in the production of nerol and geraniol
  • A catalyst for immobilized MPV reaction, its preparation method and its application in the production of nerol and geraniol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] 1. Free radical suspension polymerization: Weigh 160g of freshly steamed styrene and 70g of methyl vinyl ketone into a beaker, add 1.7g of azobisisobutyronitrile AIBN and stir to completely dissolve it for later use. In a four-neck flask equipped with a stirrer thermometer, dropping funnel and reflux condenser, add 200 mL of 0.1% polyvinyl alcohol-400 solution and 1 L of deionized water, and stir evenly. When the water bath is heated to 70°C, add 100g of the mixed monomer solution dissolved in AIBN, adjust the stirring speed to make the monomers evenly disperse into liquid droplets of appropriate size, slowly raise the temperature of the water bath to 90°C, and start dripping while keeping warm Add remaining mixed monomer solution. After the dropwise addition, the temperature was raised to 95° C., and the temperature was kept constant for 1 hour, and the reaction was completed. The reactant was filtered and fully washed, and air-dried at 50° C. to obtain the copolymer ...

Embodiment 2

[0052] Catalyst application

[0053] The catalyst of Example 1 is recovered, and the recovered catalyst is applied mechanically. Track the citral until the conversion rate > 99%, and the catalyst application results are shown in Table 1.

[0054] Table 1 Catalyst application

[0055] Apply times Reaction time / min selectivity / % Yield / % 1 30 99.1 93.4 2 30 99.5 91.8 3 32 99.4 95.2 4 30 99.5 94.9 5 35 99.0 92.3 6 37 99.9 93.1 7 37 99.9 93.8 8 38 99.7 92.6 9 40 99.1 93.2 10 40 99.8 91.7

[0056] The catalyst was used mechanically for 10 times, the reaction activity decreased slightly, but the selectivity and yield were basically stable.

Embodiment 3

[0058] According to the steps described in Example 1, the ratio of the PSMVK copolymer was adjusted to obtain immobilized catalysts with different monomer ratios, as shown in Table 2.

[0059] Table 2 Catalyst formula adjustment

[0060]

[0061] The obtained 1~7# catalysts were fed according to the 20% weight ratio of citral, and the reaction results are shown in Table 3.

[0062] Table 3 Catalytic activity

[0063]

[0064]

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Abstract

The invention discloses a catalyst for immobilized MPV reaction. The catalyst has a structure based on a styrene/methyl vinyl ketone copolymer skeleton, and the structure is as follows: a block representing repeated styrene-methyl vinyl ketone The copolymer structural unit, the block copolymer structural unit of styrene-methyl vinyl ketone is expressed as n=17-27, and the weight-average molecular weight of the catalyst is 3000-5000. Polystyrene-methyl vinyl ketone is obtained by copolymerization of styrene and methyl vinyl ketone, and then hydroxyl polymer is obtained under the action of sodium borohydride and other reducing agents, and finally reacted with aluminum powder to obtain immobilized aluminum alkoxide Structural Catalyst. The catalyst is applied to the selective hydrogen transfer of citral to produce nerol and geraniol, the reaction selectivity is >99%, and the yield is as high as 95%. After the reaction was completed, the catalyst was recovered by filtration, and the activity was not significantly decreased after being recycled for 10 times.

Description

technical field [0001] The invention relates to a catalyst for immobilized MPV reaction, a preparation method and its application in the production of nerol and geraniol, and belongs to the technical field of catalyst synthesis. Background technique [0002] MPV reaction is the abbreviation of Meerwein-Ponndorf-Verley reduction reaction (Meerwein-Ponndorf-Verleyreduction), which is one of the most commonly used reactions in organic synthesis. It is used for the reduction of selective carbonyl groups through the hydrogen transfer mechanism. Aldehydes and ketones can be selectively reduced to corresponding primary and secondary alcohols by MPV reaction. [0003] Due to the high chemoselectivity of the MPV reaction, mild reaction conditions, simple and safe operation, and low cost and low toxicity, the reaction has been widely used in the synthesis of intermediates for pharmaceuticals and fragrances. De Graauw CF, Peters J A, Bekkum Hvan, et al.Meerwein-Ponndorf-Verley Reducti...

Claims

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Application Information

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IPC IPC(8): B01J31/06B01J37/16B01J37/08C07C33/02C07C29/14
CPCB01J31/06B01J37/08B01J37/16B01J2231/643C07C29/14C07C33/02Y02P20/584
Inventor 信勇谢硕张永振于学丽李康
Owner WANHUA CHEM GRP CO LTD
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