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Recycling method for waste acid generated during preparation of graphite oxide through liquid-phase chemical method

A chemical method and resource-based technology, applied in chemical instruments and methods, graphene, manganese oxide/manganese hydroxide, etc., can solve the problems of no resource-based comprehensive treatment technology, waste of resources, high acid content, etc., and achieve operating costs Low cost, saving production cost, simple operation effect

Active Publication Date: 2017-02-15
HARBIN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods have their own advantages and disadvantages in the actual application process, and a single process is difficult to meet the practical requirements, especially the waste acid produced in the process of preparing graphene oxide by liquid phase chemical method, which not only contains high acid content, but also Contains a large amount of metal ions, if it is not properly treated comprehensively, it will not only cause serious environmental pollution, but also cause a great waste of resources
For the waste acid produced by the preparation of graphene oxide by liquid-phase chemical method, there is still no effective resource comprehensive treatment technology, which is still blank in our country

Method used

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  • Recycling method for waste acid generated during preparation of graphite oxide through liquid-phase chemical method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Use an acid-resistant pump to inject the waste acid into the homogenization tank for homogenization. The homogenized waste acid is pumped to the reaction sedimentation tank A, and the amount of precipitant CaO and Ca(OH)2 is added according to the molar amount of sulfate ions in the waste acid. The mixture is stirred and reacted to form raw gypsum (CaSO4 2H2O). After precipitation, the supernatant is pumped to the reaction sedimentation tank B, and the sediment is pumped to the filtration equipment. Solid-liquid separation, the filtrate is discharged into the reaction sedimentation tank B, and the filter cake is raw gypsum. Add KOH to the reaction sedimentation tank B, adjust the pH value to 9, stir to form Mn(OH)4, then add potassium permanganate, react to form Mn3O4, after precipitation, the supernatant is pumped to the next process, and the sediment Pump to filtration equipment. Solid-liquid separation, the filtrate is sent to the next process, and the filter cake i...

Embodiment 2

[0033] Use an acid-resistant pump to inject the waste acid into the homogenization tank for homogenization. The homogenized waste acid is pumped to the reaction sedimentation tank A, and the precipitant CaO is added according to the molar amount of sulfate ions in the waste acid, and the reaction is stirred to form raw gypsum (CaSO4 2H2O), the supernatant after precipitation is pumped to the reaction sedimentation tank B, and the sediment is pumped to the filtration equipment. Solid-liquid separation, the filtrate is discharged into the reaction sedimentation tank B, and the filter cake is raw gypsum. Add NaOH to the reaction sedimentation tank B, adjust the pH value to 10, stir to form Mn(OH)2, then add potassium permanganate, and react to form MnO. After precipitation, the supernatant is pumped to the next process, and the sediment Pump to filtration equipment. Solid-liquid separation, the filtrate is sent to the next process, and the filter cake is dried to obtain MnO. Th...

Embodiment 3

[0035] Use an acid-resistant pump to inject the waste acid into the homogenization tank for homogenization. The homogenized waste acid is pumped to the reaction sedimentation tank A, and the amount of precipitant CaO and Ca(OH)2 is added according to the molar amount of sulfate ions in the waste acid. The mixture is stirred and reacted to form raw gypsum (CaSO4 2H2O). After precipitation, the supernatant is pumped to the reaction sedimentation tank B, and the sediment is pumped to the filtration equipment. Solid-liquid separation, the filtrate is discharged into the reaction sedimentation tank B, and the filter cake is raw gypsum. Add KOH and NaOH to the reaction sedimentation tank B, adjust the pH value to 9.5, stir to form Mn(OH)2, then add sodium hypochlorite and potassium permanganate, react to form MnO2, and pump the supernatant to the next channel after precipitation In the process, the sediment is pumped to the filter equipment. Solid-liquid separation, the filtrate is...

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Abstract

The invention provides a recycling method for waste acid generated during the preparation of graphite oxide through the liquid-phase chemical method. The method comprises the steps of homogenizing the waste acid: pumping the waste acid into a homogenization tank by an acid-resistant pump to homogenize the waste acid; recycling sulfate: adding a precipitant in the homogenization tank according to the molar weight of sulfate ions in the waste acid, conducting the stirring reaction and recycling gypsum (CaSO4*2H2O); recycling manganese ions: adding an inorganic base to adjust the pH value so as to form a manganese hydroxide, then adding an oxidant to react with the manganese hydroxide so as to form a manganese oxide, recycling the manganese hydroxide / manganese oxide or the mixture of the manganese hydroxide and the manganese oxide; conducting the separation and purification operation; recycling chloride ions; and recycling the water. Conventional methods for preparing graphene are mainly divided into physical methods and chemical methods. The physical methods are composed of a micro-mechanical stripping method, a high-energy ball milling method and the like. The above methods are low in yield and are not suitable for large scale production. The method of the present invention is applied to the clean production of graphite oxide and the comprehensive utilization of waste acid resources.

Description

[0001] Technical field: [0002] The invention relates to a resource recovery method for waste acid produced by preparing graphene oxide by a liquid-phase chemical method. [0003] Background technique: [0004] Graphene is a carbon nanomaterial with a two-dimensional planar structure. Because of its special monoatomic layer structure, it exhibits many unique physical and chemical properties, and has been widely used in energy, environment, electronics, biology, medicine, chemistry and other fields. The basic and applied research on graphene has become one of the current hot frontier topics. The preparation methods of graphene are mainly divided into physical methods and chemical methods. Physical methods mainly include micromechanical exfoliation method, high-energy ball milling method, etc. This method has low yield and is not suitable for large-scale production. Chemical methods mainly include chemical vapor deposition, crystal epitaxial growth, and oxidation-reduction meth...

Claims

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Application Information

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IPC IPC(8): C02F9/10C01B32/184C01F11/46C01G45/02
CPCC01F11/46C01G45/02C02F1/001C02F1/04C02F1/441C02F1/442C02F1/444C02F1/4693C02F1/5236C02F9/00C02F2301/08
Inventor 胥焕岩
Owner HARBIN UNIV OF SCI & TECH
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