Method for resource utilization of graphene waste acid

A graphene and resource-based technology, applied in chemical instruments and methods, manganese sulfate, fluorosilicic acid, etc., can solve the problems of resource utilization of metal ions, inability to effectively reduce production costs, and high energy consumption of corrosion-resistant equipment. Achieve the effect of green environmental protection in the process, improve the quality score and reduce the production cost

Active Publication Date: 2019-07-12
NANJING GUANSHAN CHEM TECH +1
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  • Application Information

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Problems solved by technology

If it is not treated effectively, it will not only cause serious environmental pollution, but also cause a great waste of resources.
[0004] Chinese patent CN104085861B discloses a device for recovering sulfuric acid from graphene acid-containing wastewater and its corresponding process, purifying sulfuric acid from graphene wastewater to achieve the purpose of resource recycling, using its device and process to account for the recovery rate of acid liquid Reach 92%-95%, but require corrosion-resistant equipment and higher energy consumption
[0005] Chinese patent CN103696015A discloses a treatment method for waste sulfuric acid in the production process of graphene, which is characterized in that the waste sulfuric acid is collected, filtered and settled to obtain transparent waste sulfuric acid, and then the dilute sulfuric acid solution prepared by diluting the waste sulfuric acid with water is used Calcium sulfate whiskers are synthesized with dilute sulfuric acid. The beneficial effect of this invention is that waste sulfuric acid is used to produce calcium sulfate whiskers in the graphene production process, which eliminates pollution and improves environmental quality. However, sulfuric acid cannot be recycled to graphite due to the introduction of calcium precipitants. In the production of alkene, the production cost cannot be effectively reduced, and it does not involve the resource utilization of metal ions in waste acid
Concentrate the waste water, combine multi-effect evaporation to obtain potassium sulfate by-products and deionized water. This invention only recycles manganese and potassium, and mainly uses chemical conversion to process graphene waste acid, resulting in waste of sulfuric acid resources.

Method used

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  • Method for resource utilization of graphene waste acid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Get graphene waste acid 500g, wherein the massfraction of sulfuric acid is 43.79%, the massfraction of potassium sulfate is 3.14%, and the massfraction of manganese sulfate is 2.72%.

[0034] Pretreatment of waste acid: Add 400g of water to the waste acid to dilute it until the mass fraction of sulfuric acid is less than 25%. The diluted waste acid is removed by ultrafiltration to remove suspended particles and macromolecular impurities;

[0035] Membrane filtration: the pretreated waste acid is treated with aromatic polyamide nanofiltration membrane to obtain concentrate and permeate. The mass fraction of manganese sulfate in the permeate is analyzed and detected to be 0.036%. After the concentrate is collected, it is concentrated and crystallized to obtain manganese sulfate ;

[0036] Precipitation treatment: add fluorosilicic acid to the above permeated liquid according to the molar ratio of potassium sulfate to fluorosilicic acid of 1:1, carry out precipitation reac...

Embodiment 2

[0039] Get graphene waste acid 500g, wherein the massfraction of sulfuric acid is 42.18%, potassium sulfate concentration is 3.56%, and manganese sulfate concentration is 2.38%.

[0040] Pretreatment of waste acid: add 400g of water to the waste acid to dilute it until the mass fraction of sulfuric acid is less than 25%. The diluted waste acid is removed by a combination of coarse filtration and ultrafiltration to remove suspended particles and macromolecular impurities;

[0041] Membrane filtration: the pretreated waste acid is treated with aromatic polyamide nanofiltration membrane to obtain concentrated liquid and permeate, and the mass fraction of manganese sulfate in the permeate is analyzed and detected to be 0.025%. After the concentrated liquid is collected, it is concentrated and crystallized to obtain manganese sulfate ;

[0042] Precipitation treatment: add fluorosilicic acid to the above permeated liquid according to the molar ratio of potassium sulfate to fluorosi...

Embodiment 3

[0045] Get graphene waste acid 500g, wherein the massfraction of sulfuric acid is 24.11%, potassium sulfate concentration is 4.27%, and manganese sulfate concentration is 5.61%.

[0046] Pretreatment of waste acid: use a combination of coarse filtration and ultrafiltration to remove suspended particles and macromolecular impurities in waste acid;

[0047] Membrane filtration: the pretreated waste acid is treated with aromatic polyamide nanofiltration membrane to obtain concentrated liquid and permeate. The mass fraction of manganese sulfate in the permeate is analyzed and detected to be 0.048%. After the concentrated liquid is collected, it is concentrated and crystallized to obtain manganese sulfate ;

[0048] Precipitation treatment: add fluorosilicic acid to the above-mentioned permeated liquid according to the molar ratio of potassium sulfate to fluorosilicic acid of 1:1, carry out precipitation reaction under the conditions of stirring, reaction temperature 65°C, and reac...

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Abstract

The invention belongs to the technical field of graphene waste acid treatment, and particularly relates to a method for resource utilization of graphene waste acid. The method comprises the followingsteps: a) pre-treatment: adjusting the content of sulfuric acid in waste acid and removing suspended particles and macromolecular impurities in the waste acid; b) membrane filtration: treating the pre-treated waste acid by an aromatic polyamine nanofiltration membrane to obtain a concentrated liquor and a permeable liquid; c) precipitating treatment: adding silicofluoric acid into the permeable liquid and filtering the mixture to obtain a filter cake and a filtrate; and d) vacuum concentration: concentrating the filtrate in a vacuum condition to obtain sulfuric acid, of which the mass fraction is greater than 95%. Sulfuric acid is recycled and metal ions are recovered in a graphene production process, so that the industrial value is improved, and the industrial production cost of grapheneis lowered. The method has an obvious economical benefit. In addition, the environmental pollution is also eliminated, the environmental quality is improved favorably and the method has a good socialbenefit.

Description

technical field [0001] The invention belongs to the technical field of graphene waste acid treatment, in particular to a method for resource utilization of graphene waste acid. Background technique [0002] At present, domestic and foreign methods for treating waste acid mainly include waste acid cracking, concentration, solvent extraction, ion exchange, membrane separation and chemical conversion. These methods have their own advantages and disadvantages in practical application, and a single process is very difficult It is difficult to meet the target requirements. [0003] The preparation of graphene by the Hummer redox method usually treats the raw graphite with an inorganic strong protonic acid (such as concentrated sulfuric acid, concentrated nitric acid, or a mixture thereof), inserts small molecules of the strong acid between the graphite layers, and then uses a strong oxidant (such as potassium permanganate , potassium perchlorate, etc.) to oxidize it. During the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/10C01G45/10C01B33/10
CPCC01B33/103C01G45/10C02F1/046C02F1/442C02F1/5236C02F9/00
Inventor 华军伍俊何育苗张慧丽
Owner NANJING GUANSHAN CHEM TECH
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