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A method for recycling pyrolusite powder in p-benzoquinone production process

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 different particle sizes, high consumption of manganese powder, and the influence of benzoquinone yield, and achieve obvious Economic benefits and the effect of improving utilization

Active Publication Date: 2012-02-01
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

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  • A method for recycling pyrolusite powder in p-benzoquinone production process
  • A method for recycling pyrolusite powder in p-benzoquinone production process

Examples

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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 liqui...

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

A method for recycling pyrolusite powder in the p-benzoquinone production process. The pyrolusite powder and dilute sulfuric acid with a concentration of 36% are put into the oxidation tank according to 1g: 2ml-2.5ml, and then aniline is added dropwise to react, aniline The dripping amount is 20% of the pyrolusite powder amount. After the reaction is over, p-benzoquinone is distilled out, and the raffinate enters the gravity settler to separate the waste liquid and manganese slag. The waste liquid is used for recycling manganese products, and the manganese slag is passed through The manganese powder is separated by gravity sedimentation, and the manganese powder is put into the oxidation tank for the next production of p-benzoquinone as a raw material. The present invention increases the concentration of reactants by adding excessive manganese powder, thereby increasing the yield of products and improving the utilization rate of manganese in pyrolusite. The invention can produce obvious economic benefits.

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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Patent Type & Authority Patents(China)
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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