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Method for circulating utilization of reclaimed pyrolusite powder in benzoquinone manufacturing technique

A technology of pyrolusite powder and production process, which is applied in the field of recycling pyrolusite powder in the production process of p-benzoquinone, can solve the problems of high consumption of manganese powder, different particle sizes, and the impact of benzoquinone yield, etc., and achieve an increase Utilization rate, the effect of obvious economic benefits

Active Publication Date: 2007-12-05
湖北开元化工科技股份有限公司
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Problems solved by technology

[0002] In the process of using pyrolusite powder to oxidize aniline to produce p-benzoquinone, although in order to ensure the yield of p-benzoquinone, the pyrolusite powder has been excessive, and its manganese dioxide content is generally between 45-70%, which ensures the oxidant. However, due to the different particle sizes, when participating in the oxidation reaction, the particles peel off layer by layer and become small particles to participate in the oxidation reaction. At the end of the reaction, some manganese ore still did not participate in the reaction, but at this time the reducing agent aniline has Can no longer be converted (the oxidant manganese ore powder is insufficient, it is difficult to continue to oxidize aniline), the yield of p-benzoquinone is affected, other manufacturers directly discharge the waste residue containing this manganese ore powder, resulting in high consumption of manganese powder

Method used

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  • Method for circulating utilization of reclaimed pyrolusite powder in benzoquinone manufacturing technique

Examples

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Effect test

Embodiment 1

[0009] Example 1: In a 2L reactor, 600g of pyrolusite powder with a manganese dioxide content of 45%, 1350ml of 36% dilute sulfuric acid were added, and 120g of aniline was added dropwise. After the reaction was completed, p-benzoquinone was distilled out, crystallized, and dried to obtain p-benzoquinone Quinone 95g, the distillation residue is separated waste liquid and manganese slag through gravity settling, and manganese slag is about 400g, and analysis manganese dioxide content is 5%, waste liquid is processed into manganese product, obtains manganese sulfate product 320g. In another 2L reactor, add 600g of pyrolusite powder with manganese dioxide content of 45%, 400g of recovered manganese powder, 1350ml of 36% dilute sulfuric acid, and dropwise add 120g of aniline. After the reaction is completed, p-benzoquinone is distilled out, crystallized and dried. 98g of p-benzoquinone was obtained, and the distillation residue was separated by gravity sedimentation into waste liqu...

Embodiment 2

[0010] Example 2: In a 2L reactor, 600g of pyrolusite powder with a manganese dioxide content of 70%, 1350ml of 36% dilute sulfuric acid were added, and 120g of aniline was added dropwise. After the reaction was completed, p-benzoquinone was distilled out, crystallized, and dried to obtain p-benzoquinone Quinone 105g, the distillation residue is separated waste liquid and manganese slag through gravity settling, and manganese slag is about 360g, and analysis manganese dioxide content is 40%, and waste liquid is processed into manganese product, obtains manganese sulfate product 378g. In another 2L reactor, add 600g of pyrolusite powder with manganese dioxide content of 70%, 360g of recovered manganese powder, 1350ml of 36% dilute sulfuric acid, and dropwise add 120g of aniline. After the reaction is completed, p-benzoquinone is distilled out, crystallized and dried. 113g of p-benzoquinone was obtained, and the distillation residue was separated by gravity sedimentation into was...

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Abstract

The process of producing para-benzoquinone with reuse of recovered pyrolusite powder includes: throwing pyrolusite powder and 36 % concentration dilute sulfuric acid solution in the ratio of 1 g to 2-2.5 ml into one oxidizing tank, dropping aniline in the amount of 20 wt% of pyrolusite powder to react, distilling to obtain para-benzoquinone after finishing reaction, separating the residual liquid in a gravitational settler into waste liquid and manganese dioxide dreg, recovering manganese with the waste liquid, separating manganese dioxide powder from manganese dioxide dreg through gravitational settling, and returning the manganese dioxide powder to the oxidizing tank for further para-benzoquinone production. The present invention has high product yield, high pyrolusite powder utilizing rate and high economic benefit.

Description

technical field [0001] The invention relates to a method for improving the utilization rate of manganese and the yield of p-benzoquinone in the process of oxidizing aniline with pyrolusite powder to produce p-benzoquinone, in particular to a method for recycling pyrolusite powder in the production process of p-benzoquinone. Background technique [0002] In the process of using pyrolusite powder to oxidize aniline to produce p-benzoquinone, although in order to ensure the yield of p-benzoquinone, the pyrolusite powder has been excessive, and the content of manganese dioxide is generally between 45-70%, which ensures the yield of the oxidant. However, due to the different particle sizes, when participating in the oxidation reaction, the particles peel off layer by layer and become small particles to participate in the oxidation reaction. At the end of the reaction, some manganese ore still did not participate in the reaction, but at this time the reducing agent aniline has It ...

Claims

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Application Information

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IPC IPC(8): C07C50/04C07C46/02B01D21/02
Inventor 时克勤
Owner 湖北开元化工科技股份有限公司
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