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A method for extracting tetrahydro-2-ethylanthraquinone from working solution for producing hydrogen peroxide by anthraquinone method

A technology of ethyl anthraquinone and hydrogen peroxide, applied in quinone separation/purification, organic chemistry and other directions, can solve the problems of increasing cost and time, complicated steps, etc., and achieve the effect of improving hydrogenation efficiency, low cost and reducing anthraquinone degradation reaction

Active Publication Date: 2018-04-06
CHINA TIANCHEN ENG +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, a variety of new organic solvents are introduced in the preparation process of this method, and the target product with high purity needs to be obtained through repeated processes such as dissolution and crystallization, and the steps are cumbersome and increase the cost and time.

Method used

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  • A method for extracting tetrahydro-2-ethylanthraquinone from working solution for producing hydrogen peroxide by anthraquinone method
  • A method for extracting tetrahydro-2-ethylanthraquinone from working solution for producing hydrogen peroxide by anthraquinone method

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Take 300mL of the circulating working solution in a rotary evaporator, distill at -0.1MPa, 110°C for 2h, put the residual liquid in an oven at 110°C, and cool it down to 15°C after 1.5h, at this time, a large number of crystals are precipitated at the bottom. Suction filter the distillate, wash the filter cake 3 times with ethanol, and then dry it at 60°C. The obtained crystals were placed in a Buchner funnel with filter paper, and heavy aromatic hydrocarbons were added dropwise at -0.1 MPa until the needle crystals disappeared and a large number of flaky crystals appeared on the filter paper. The filtrate was collected and evaporated to dryness in a rotary evaporator to obtain needle-like crystals.

Embodiment 2

[0030] Take 300mL of the circulating working solution in a rotary evaporator, distill at -0.05MPa, 120°C for 1.5h, then put it in an oven at 120°C, and cool it down to 15°C after 2h, when a large amount of crystals are precipitated at the bottom. Suction filter the distillate, wash the filter cake 3 times with ethanol, and then dry it at 70°C. The obtained crystals were placed in a Buchner funnel with filter paper, and pseudocumene was added dropwise at -0.05 MPa until the needle crystals disappeared and a large number of flaky crystals appeared on the filter paper. The filtrate was collected and evaporated to dryness in a rotary evaporator to obtain needle-like crystals.

Embodiment 3

[0032]Take 300mL of the circulating working solution in a rotary evaporator, distill at -0.03MPa, 130°C for 4.5h, put it in an oven at 130°C, and cool it down to 15°C after 3h, when a large amount of crystals are precipitated at the bottom. Suction filter the distillate, wash the filter cake 3 times with ethanol, and then dry it at 55°C. The obtained crystals were placed in a Buchner funnel with filter paper, and 1,3,5-trimethylbenzene was added dropwise at -0.03 MPa until the needle-like crystals disappeared and a large number of flaky crystals appeared on the filter paper. The filtrate was collected and evaporated to dryness in a rotary evaporator to obtain needle-like crystals.

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Abstract

The invention creatively provides a method for extracting tetrahydro-2-ethylanthraquinone from a working solution for producing hydrogen peroxide with an anthraquinone method. The method comprises the following steps: S1: taking a circulating working solution for producing the hydrogen peroxide with the anthraquinone method; steaming out a component at 110 DEG C to 140 DEG C; slowly cooling steamed residual liquid to be lower than 25 DEG C until crystals are formed in the steamed residual liquid; S2: filtering the cooled steamed residual liquid to obtain a filter cake; washing the filter cake with ethanol and drying to obtain a dried material; S3: washing the dried material by utilizing an organic solvent under a suction filtration condition so as to reduce or eliminate needle-shaped crystals and show or remain sheet-shaped crystals; taking filtrate and evaporating to obtain the tetrahydro-2-ethylanthraquinone. The method provided by the invention is simple to operate and relatively high in efficiency.

Description

technical field [0001] The invention belongs to the technical field of hydrogen peroxide production, and in particular relates to a simple method for extracting tetrahydro-2-ethylanthraquinone from a circulating working solution for producing hydrogen peroxide by an anthraquinone method. Background technique [0002] Hydrogen peroxide is known as a clean chemical raw material because its complete decomposition products are water and oxygen, and does not produce gas, solid and liquid waste. It has been widely used in the fields of papermaking, textiles, electronics, medicine and chemical industry, and its demand continues to grow . In addition, with the rapid development of the green chemical synthesis process, hydrogen peroxide has been rapidly promoted in this field, especially in the preparation of propylene oxide (HPPO) by epoxidation of propylene hydrogen peroxide and the synthesis of green caprolactam. my country's hydrogen peroxide industry has put forward higher requi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C50/16C07C46/10
CPCC07C46/10C07C50/16
Inventor 曹立杨克俭郑仁史文涛姚立东王志文刘香云袁海朋金宗良杜小宝姚立德吕睿王绍伟李大为王聪刘晶张二涛
Owner CHINA TIANCHEN ENG
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