Method and system for recycling graphene waste sulfuric acid

A technology of waste sulfuric acid and graphene, applied in the field of resources and environment, can solve the problems of no resource utilization, etc., and achieve the effect of low cost, less investment and simple process

Pending Publication Date: 2019-08-06
YI KELI TIANJIN ENVIRONMENTAL PROTECTION TECH DEV CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, graphene waste sulfuric acid is mainly neutralized by calcium method, which has not been fully utilized as a resource

Method used

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  • Method and system for recycling graphene waste sulfuric acid
  • Method and system for recycling graphene waste sulfuric acid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] (1) open reactor and stir, adding sulfuric acid mass content by sulfuric acid metering tank is 40% graphene waste sulfuric acid 1000kg and 90% light-burning magnesium oxide 182kg, until pH value reaches 7, temperature of reaction keeps 30 minutes at 90 DEG C;

[0081] (2) the solution of step (1) adds the hydrogen peroxide of 6.5kg mass concentration 30%, oxidizes divalent manganese ion (waste manganese ion content is 0.3%), generates manganese dioxide precipitation; After 1 hour of reaction, add 1kg polysulfuric acid Aluminum flocculant, filtering and separating manganese dioxide precipitate, and drying the precipitate to obtain 5kg of manganese fertilizer (manganese mass content is 60%);

[0082] (3) the filtrate from step (2) is mainly magnesium sulfate and a small amount of potassium sulfate solution (waste acid contains potassium ion 0.4%), through circulating concentration and cooling crystallization, obtain 950kg of magnesium sulfate that meets HG / T 2680-2017 tech...

Embodiment 2

[0086] (1) open reactor and stir, adding sulfuric acid mass content by sulfuric acid metering tank is 50% graphene waste sulfuric acid 1000kg and 90% light-burning magnesium oxide 227kg, until pH value reaches 6, and temperature of reaction keeps 30 minutes at 90 DEG C;

[0087] (2) the solution of step (1) adds 7.2kg of sodium hypochlorite, oxidizes divalent manganese ions (the content of waste manganese ions is 0.5%), and generates manganese dioxide precipitation; after 1 hour of reaction, 1.2kg of polyaluminum sulfate flocculant is added, Filter and separate manganese dioxide precipitate, and the precipitate is dried to obtain 8kg of manganese fertilizer (manganese content is 60%);

[0088] (3) the filtrate from step (2) is mainly magnesium sulfate and a small amount of potassium sulfate solution (waste acid contains potassium ion 0.2%), through cyclic concentration and cooling crystallization, obtain 1225kg of magnesium sulfate that meets the technical requirements of HG / T ...

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Abstract

The invention provides a method and a system for recycling graphene waste sulfuric acid, and relates to the technical field of resource environments. The method comprises the following steps: carryingout a neutralizing reaction on the graphene waste sulfuric acid and magnesium oxide, oxidizing the obtained reaction product with an oxidant, and carrying out flocculation treatment to obtain a precipitate and a filtrate; carrying out cyclic concentration, crystallization and separation on the filtrate until the mass concentration of potassium sulfate in a separation liquid obtained after separation is equal to or more than 10%, using the separation liquid with the potassium sulfate mass concentration of 10% or more as a first mother liquor, and separating a solid obtained after the separation to obtain magnesium sulfate; and sequentially co-crystallizing and separating the first mother liquor to obtain potassium magnesium sulfate co-crystals and a second mother liquor, and returning thesecond mother liquor to the cyclic concentration and crystallization step. The graphene waste sulfuric acid is neutralized with the magnesium oxide to obtain magnesium sulfate and potassium magnesiumsulfate, so the recovery of sulfuric acid and potassium ions is achieved; and manganese ions in the graphene waste acid are recovered by an oxidation process. The method and the system have the advantages of simple process, recycling of all the elements of the graphene waste sulfuric acid, and significant economic and social benefits.

Description

technical field [0001] The invention relates to the technical field of resources and environment, in particular to a method and system for recycling waste sulfuric acid of graphene. Background technique [0002] Graphene is an emerging material with very broad application prospects; the main production process of graphene at present is the redox method, in which the oxidation process mainly adopts the improved Hummers method. There are two commonly used methods: 1. Potassium permanganate is used as a strong The oxidant is intercalated with sulfuric acid; ② the graphite powder is pre-oxidized with potassium persulfate and phosphorus pentoxide, and then potassium permanganate is used as a strong oxidant and sulfuric acid is intercalated. [0003] The oxidation process will produce a large amount of waste sulfuric acid, of which the sulfuric acid content is about 30% to 59% (wt%), the manganese ion content is about 0.2% to 2% (wt%), and the potassium ion content is about 0.2% t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D5/06C01F5/40C05D5/00C05D9/02
CPCC01F5/40C01D5/06C05D5/00C05D9/02
Inventor 李梅彤袁文蛟周晶张柯范文浩
Owner YI KELI TIANJIN ENVIRONMENTAL PROTECTION TECH DEV CO LTD
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