Preparation method of 2, 5-di-tert-butyl-p-dimethoxybenzene

A technology of di-tert-butyl-p-phthalene and di-tert-butyl-hydroquinone, which is applied in the field of preparation of 2,5-di-tert-butyl-p-xylylene, can solve the problem of inconvenient operation in the production process, Long production process, many wastes, etc., to achieve the effect of low cost, less reaction steps, and less pollution

Inactive Publication Date: 2021-06-01
SHANSHAN ADVANCED MATERIALS QUZHOU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The above existing technologies exist or the production process is inconvenient to operate, the production process is long, and the cost is high; or the yield is low, there are many three wastes, and the disadvantages are not environmentally friendly.

Method used

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  • Preparation method of 2, 5-di-tert-butyl-p-dimethoxybenzene
  • Preparation method of 2, 5-di-tert-butyl-p-dimethoxybenzene
  • Preparation method of 2, 5-di-tert-butyl-p-dimethoxybenzene

Examples

Experimental program
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Effect test

Embodiment 1

[0034] (1) Preparation of 2,5-di-tert-butylhydroquinone

[0035] Take 55.0g (0.5mol) of hydroquinone, put it into a three-necked flask, add 40g of deionized water into the three-necked flask, stir and heat to 80°C, take 60g (0.81mol) of tert-butanol, and slowly drop it into the three-necked flask, Until the solid in the bottle is completely dissolved, take 163g (2.2mol) tert-butanol and 10g sulfuric acid to make a mixed solution, slowly drop it into a three-necked flask, keep the reaction temperature at 80°C, and react for 3 hours. After the reaction is completed, cool the system to room temperature. After filtering, the obtained solid was washed three times with 150 ml of water and dried to obtain 107.9 g of 2,5-di-tert-butylhydroquinone with a yield of 97%.

[0036] (2) Preparation of 2,5-di-tert-butyl-p-xylylene ether

[0037] Take 44.5g (0.2mol) of 2,5-di-tert-butylhydroquinone prepared in step (1) and dissolve in 500g DMF, add 0.46g (19mmol) sodium hydride under nitrogen...

Embodiment 2

[0039] (1) Preparation of 2,5-di-tert-butylhydroquinone:

[0040] Take 110.0g (1.0mol) of hydroquinone, put it into a three-necked flask, add 80g of deionized water into the three-necked flask, stir and heat to 70°C, take 90g (1.2mol) of tert-butanol, and slowly drop it into the three-necked flask, Until the solid in the bottle is completely dissolved, take 244.5g (3.3mol) of tert-butanol and 4g of 36.5% hydrochloric acid by mass to form a mixed solution, slowly drop it into a three-necked flask, keep the reaction temperature at 70°C, and react for 2 hours. After the completion, the system was cooled to room temperature, filtered, and the obtained solid was washed three times with 200 ml of water, and dried to obtain 2,5-di-tert-butylhydroquinone (200 g, yield 90%).

[0041] (2) Preparation of 2,5-di-tert-butyl-p-phthalyl ether:

[0042] Take 89g (0.4mol) of 2,5-di-tert-butylhydroquinone prepared in step (1) and dissolve in 500g of dimethyl carbonate, add 1.0g (25mmol) of potas...

Embodiment 3

[0044] (1) Preparation of 2,5-di-tert-butylhydroquinone:

[0045] Take 55.0g (0.5mol) of hydroquinone, put it into a three-necked flask, add 40g of deionized water into the three-necked flask, stir and heat to 90°C, take 30g (0.4mol) of tert-butanol, and slowly drop it into the three-necked flask, Until the solid in the bottle is completely dissolved, take 81.5g (1.1mol) of tert-butanol and 0.3g of sulfuric acid to form a mixed solution, slowly drop it into a three-necked flask, maintain the reaction temperature at 90°C, and react for 5h. After the reaction is completed, the system is cooled to After filtering at room temperature, the obtained solid was washed three times with 150 ml of water and dried to obtain 97.9 g of 2,5-di-tert-butylhydroquinone with a yield of 88%.

[0046] (2) Preparation of 2,5-di-tert-butyl-p-phthalyl ether:

[0047] Dissolve 89g (0.4mol) of 2,5-di-tert-butylhydroquinone prepared in step (1) in 800g THF, add 0.17g (4mmol) calcium hydride under nitro...

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Abstract

The invention discloses a preparation method of 2, 5-di-tert-butyl-p-dimethoxybenzene, which comprises the following steps: (1) reacting tert-butyl alcohol with hydroquinone in a first solvent under the action of a first catalyst, cooling and crystallizing after the reaction is finished, filtering, washing and drying to obtain 2,5-di-tert-butyl hydroquinone; and (2) reacting the 2, 5-di-tert-butyl hydroquinone obtained in the step (1) with methyl iodide in a second solvent under the action of a second catalyst, cooling to room temperature after the reaction is finished, adding brine and an organic solvent into the reaction liquid for extraction, washing the obtained organic layer, and performing vacuum drying to obtain the 2, 5-di-tert-butyl-p-dimethoxybenzene product. The method has the advantages of simple process, mild reaction conditions, environmental protection, low cost and high yield.

Description

technical field [0001] The invention relates to the technical field of batteries, in particular to a preparation method of 2,5-di-tert-butyl-p-xylylene dimethyl ether. Background technique [0002] Lithium-ion rechargeable batteries are widely used in portable electronic products and vehicles due to their advantages such as large specific capacity, high energy density, long shelf life, and no memory effect. But currently, safety concerns associated with lithium-ion batteries limit their use in many areas, such as power grids and electric vehicle applications. Among these problems, a series of consequences caused by overcharging can cause serious problems. [0003] To prevent this overcharging, commercial Li-ion batteries are often equipped with external electronics protection, which adds complexity, size, and cost to the system. An effective way to reduce costs is to add so-called redox shuttling additives directly into the electrolyte to provide intrinsic chemical protect...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/16C07C43/205
CPCC07C41/16C07C37/16C07C43/2055C07C39/08
Inventor 张晓宇吴杰曹青青钟子坊周彤
Owner SHANSHAN ADVANCED MATERIALS QUZHOU CO LTD
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