CN103373723A

CN103373723A - High-purity crystalline graphite purifying process

Info

Publication number: CN103373723A
Application number: CN201210110737XA
Authority: CN
Inventors: 夏华松
Original assignee: Individual
Current assignee: Individual
Priority date: 2012-04-17
Filing date: 2012-04-17
Publication date: 2013-10-30

Abstract

The invention relates to a high-purity crystalline graphite purifying process comprising the following steps of: with crystalline graphite with the carbon content of larger than 90% as a raw material, adding the crystalline graphite and a hydrofluoric acid, nitric acid and sulfuric acid solution into a reaction kettle, heating water vapor to 80-90 DEG C, meanwhile, stirring the mixture, dipping and reacting for 2-3h; then, separating the solution and the graphite to prepare acid-contained graphite, washing the acid-contained graphite by using water until the pH value of the solution is 6.5-6.8, and then, settling the graphite; and finally, carrying out filter pressing, and drying to obtain microcrystalline graphite with the carbon content of 99%. By using the purifying process, the microcrystalline graphite with the carbon content of 90% can be purified to form high-purity graphite with the carbon content of not smaller than 99%, the water content of not larger than 0.2% and the ash content of not larger than 0.7%, the technical content of the microcrystalline graphite is greatly increased, the application range of the microcrystalline graphite is greatly widened, and particularly, a colorcast graphite latex product can be produced by using the high-purity graphite.

Description

High purity Scaly graphite purifying technique

Technical field

The present invention relates to the purifying technique of a high Scaly graphite, particularly a kind of purifying technique that extracts high purity graphite take Scaly graphite as raw material.

Background technology

Graphite is a kind of important nonmetallic mineral material, high-carbon, high-purity, ultra-fine be the intermediary material that graphite material is used widely in high-tech sector.Scaly graphite is that the method for purification of raw material comprises: (1) molten alkaline process take solid members solid NaOH as auxiliary material; (2) the normal pressure method of purification take liquid NaOH as auxiliary material; (3) with HF-HCL system method of purification; (4) with HF-chloroazotic acid system method of purification.The carbon content of the method for these several purifications between 92-97.5%, do not reach the requirement of 99% purity, thereby range of application is restricted usually.

Summary of the invention

Purpose of the present invention is exactly the low defective of purification degree that exists for prior art, and a kind of purifying technique of high purity Scaly graphite is provided.

Its technical scheme comprises the steps:

(1) take carbon content greater than 90% Graphite Powder 99 as raw material, add in the reactor with hydrofluoric acid, nitric acid powder and sulphuric acid soln, water vapour is warmed to 80-90 ℃, stirs simultaneously, impregnation 2-3 hour, simultaneously combustion gas; (2) with whizzer reacted acid solution is separated with graphite, the acid solution after the separation is recycled; (3) graphite that contains acid is washed, and reaches pH value at 6.0-6.5; (4) carry out settlement separately, acid solution after the separation is recycled; (5) discharge with pressure filter Re-isolation solution and with solution, obtain Graphite Cake; (6) Graphite Cake is dried rear pulverizing, make high purity finished product Graphite Powder 99.The weight proportion of graphite and hydrofluoric acid, nitric acid-sulfuric acid solution is respectively: 30%-35%, 15%-20%, 20%-45%, hydrofluoric acid are concentration 40%, density 1.13, and nitric acid is concentration 98%, and proportion is 1.50; Sulfuric acid is concentration 98%, density 1.84.

Purifying technique can be purified to the micro crystal graphite of carbon content 90% carbon content and be not less than 99%, and moisture content is not more than 0.3%, and the ash content of coal is not more than 0.7% high purity graphite, has greatly promoted technology content and the range of application of micro crystal graphite.

Description of drawings

Accompanying drawing is the process flow sheet of one embodiment of the present invention.

Embodiment

Referring to accompanying drawing, concrete grammar is: (1) adds three successively in the interconnective feed reservoir, with the hydrofluoric acid solution of 960 kilograms of concentration 40%, density 1.13 with the microlite ink powder of 1280 kilograms carbon content 80%; 500 kilograms of concentration of nitric acid 96%, in the sulphuric acid soln amount acid tank of density 1.5 and 1180 kilograms of vitriol oil concentration 98%, density 1.84, add reactor, with 100 ℃ steam reactor is heated to 90 ℃, stir simultaneously, impregnation 2 hours, Exhaust Gas carries out environmental protection treatment.(2) with whizzer reacted acid solution is separated with graphite, recycle in the acid solution amount of the returning to acid tank after the separation or the feed reservoir.(3) disperse to deliver to water wash column through the Graphite Cake of disperseing the pond will contain acid and wash, pH value is controlled at 6.2.(4) put into settling bowl and precipitate, the acid solution after the separation returns in the feed reservoir to be recycled.(5) recycle as the washing water in the step (3) after the environmental protection treatment with pressure filter Re-isolation solution and with carrying out after the solution discharge, and obtain Graphite Cake.(6) Graphite Cake put into dryer dry after, carry out pulverizer and pulverize, make high purity finished product Graphite Powder 99, measure at last, pack.

This purifying technology is in time cleared up the fluorochemical that chemical reaction produces in the purification process, and the fluoro-gas that produces when clearing up is constantly escaped, and has guaranteed that reaction channel is unblocked, and the chemical reaction of graphite purification can be carried out thoroughly.Adopt this technique, can be that 90% micro crystal graphite is purified as carbon content is not less than 99%, ash is not more than 0.7%, moisture is not more than 0.3% high-carbon graphite with carbon containing, make micro crystal graphite raw ore increment decades of times, can create significant economic benefit and social benefit.

Claims

1. high purity Scaly graphite purifying technique, it is characterized in that: this technique comprises the steps---(1) take carbon content greater than 90% Graphite Powder 99 as raw material, add in the reactor with hydrofluoric acid and nitric acid and sulphuric acid soln, water vapour is warmed to 80-90 ℃.Stir simultaneously, impregnation 2-3 hour, simultaneously combustion gas; (2) with whizzer reacted acid solution is separated with graphite, the acid solution after the separation is recycled; (3) graphite that contains acid is washed, and reaches pH value at 6.5-6.8; (4) carry out settlement separately, acid solution after the separation is recycled; (5) discharge with pressure filter Re-isolation solution and with solution, obtain Graphite Cake; (6) Graphite Cake is dried rear pulverizing, support high purity finished product graphite.

2. high purity graphite purfying process according to claim 1, it is characterized in that: the weight proportion of graphite and hydrofluoric acid, nitric acid and sulphuric acid soln is respectively 30%-35%, 15%-20%, 20%-45%, described hydrofluoric acid is concentration 40%, density 1.13, and sulfuric acid is concentration 98%, density 1.84; Nitric acid is concentration 96%, density 1.50..