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A kind of preparation method of spherical diethoxymagnesium

A technology of diethoxymagnesium and spherical shape, which is applied in the field of preparation of spherical diethoxymagnesium, can solve the problems of using precursors and being unable to be used as spherical initiators, etc., achieves stable reaction, is beneficial to control production, and has no residue of impurities Effect

Active Publication Date: 2022-03-01
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current diethoxymagnesium is prepared from metal magnesium powder by reacting with ethanol in the presence of a composite initiator. The particles of the prepared diethoxymagnesium are irregular in shape and cannot be used as a spherical initiator. precursor use of

Method used

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  • A kind of preparation method of spherical diethoxymagnesium
  • A kind of preparation method of spherical diethoxymagnesium
  • A kind of preparation method of spherical diethoxymagnesium

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Take 21g of magnesium powder, 270mL of absolute ethanol, 135mL of tetrahydrofuran, and 0.6253g of iodine;

[0035] Under the protection of an inert gas, add 0.6253g of iodine and 45mL of preheated absolute ethanol to a 500mL five-necked branch bottle at one time, stir until fully dissolved, generally 5-10min; then add 7g of magnesium powder and 45mL of preheated absolute ethanol and 45mL of tetrahydrofuran, react with stirring for 10-20min; then continue to add 7g of magnesium powder, 90mL of preheated absolute ethanol and 45mL of tetrahydrofuran, and react for 10min with stirring; add 7g of magnesium powder for the third time , 90 mL of preheated absolute ethanol and 45 mL of tetrahydrofuran.

[0036] React for about 5 hours. After the reaction until the color turns white and no hydrogen is generated in the bubbler, transfer the solution into a branch tube suction filter bottle, wash with preheated absolute ethanol for 3-5 times, and then vacuum dry for a period of tim...

Embodiment 2

[0039] Take 21g of magnesium powder, 402mL of absolute ethanol, 201mL of 1,4-dioxane, and 0.6253g of iodine;

[0040] Under the protection of an inert gas, add 0.6253g of iodine and 67mL of preheated absolute ethanol to a 750mL five-necked branch bottle at one time, stir until fully dissolved, generally 5-10min; then add 7g of magnesium powder, 67mL of preheated absolute ethanol and 67mL of dioxane, reacted for 10-20min under stirring; then continued to add 7g of magnesium powder, 134mL of preheated absolute ethanol and 67mL of dioxane, and reacted for 10min under stirring; the third time Add 7 g of magnesium powder, 134 mL of preheated absolute ethanol and 67 mL of dioxane.

[0041] React for about 5 hours. After the reaction until the color turns white and no hydrogen is generated in the bubbler, transfer the solution into a branch tube suction filter bottle, wash with preheated absolute ethanol for 3-5 times, and then vacuum dry for a period of time. , transferred to a vac...

Embodiment 3

[0044] Take 21g of magnesium powder, 402mL of absolute ethanol, and 0.6253g of initiator iodine;

[0045] Under the protection of an inert gas, add 0.6253g and 67mL of preheated absolute ethanol to a 500mL five-necked branch bottle at one time, stir until fully dissolved, generally 5-10min; then add 7g of magnesium powder and 67mL of Preheated absolute ethanol, stirred for 10-20min; then continued to add 7g magnesium powder and 134mL preheated absolute ethanol, stirred for 10min; added 7g magnesium powder and 134mL preheated absolute ethanol for the third time.

[0046] React for about 5 hours. After the reaction until the color turns white and no hydrogen is generated in the bubbler, transfer the solution into a branch tube suction filter bottle, wash with preheated absolute ethanol for 3-5 times, and then vacuum dry for a period of time. , transferred to a vacuum drying oven and vacuum-dried in the range of 40-60° C. for one night to obtain a diethoxymagnesium carrier.

[0...

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Abstract

The invention provides a method for preparing diethoxymagnesium, which comprises using metal spherical magnesium powder and absolute ethanol as raw materials, adding iodine simple substance and a cosolvent to prepare spherical diethoxymagnesium. The particle size range of the obtained spherical diethoxymagnesium is 1-200um, and the span of the particle size distribution is less than 3; by adding a co-solvent to the reaction system, the particle size of the obtained diethoxymagnesium can even reach 5um-15um, and Compared with the traditional method of adding surfactant, silicone oil or spar, the method is easier to remove the cosolvent, has no residue of impurities, and is more convenient for post-processing. The method of the present invention has lower reaction temperature, stable reaction and shorter reaction time. Short, no environmentally unfriendly substance discharge, suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of spherical diethoxymagnesium, which belongs to the technical field of metal oxide preparation. Background technique [0002] Solid diethoxymagnesium, off-white granules, can be used as composite initiator for synthetic reactions in pesticide, medicine, spices, plastics and other industries; recently, it has been found that it can be used as a precursor of olefin polymerization composite initiator. The current development direction of olefin polymerization is to synthesize spherical polymer particles, and to obtain spherical polymer particles, spherical initiators must be used. The current diethoxymagnesium is prepared from metal magnesium powder by reacting with ethanol in the presence of a composite initiator. The particles of the prepared diethoxymagnesium are irregular in shape and cannot be used as a spherical initiator. use of precursors. Contents of the invention [0003] In order to overcome th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/41C07C53/10
CPCC07C51/412C07C53/10
Inventor 李化毅王如秀李倩胡友良
Owner INST OF CHEM CHINESE ACAD OF SCI
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