CN109574003A - A kind of method of ultrasonic wave auxiliary alkali acid system purification graphite - Google Patents

Abstract

The present invention relates to a kind of methods of ultrasonic wave auxiliary alkali acid system purification graphite, it is characterized by: 1) 94% or more high-carbon graphite of purity and 15 ~ 30%NaOH ultrasound of 1:1 in mass ratio ~ 2 stir evenly 5 ~ 30min, control power is not less than 18000Hz not less than 3kW, frequency；2) is dried to moisture 20% hereinafter, going to 400 ~ 450 DEG C of Muffle furnaces 10 ~ 60min of roasting, is washed till neutrality after cooling, filters；3) is gone in 15 ~ 25% hydrochloric acid, adjusts pulp density 30 ~ 60%, ultrasonic 5 ~ 30min of acidleach, and control power is not less than 18000Hz not less than 3kW, frequency；4) ore pulp is filtered, is washed till neutral, 100 ~ 150 DEG C of 30 ~ 90min of drying.The utility model has the advantages that 1. purity are up to 99.90% or more；2. soda acid usage amount, alkali melt, leaching time is reduced；3. production capacity increases, salkali waste, waste acid quantity are reduced.

Description

A kind of method of ultrasonic wave auxiliary alkali acid system purification graphite

Technical field

The invention belongs to nonmetallic mineral manufacture fields, are related to a kind of method of ultrasonic wave auxiliary alkali acid system purification graphite.

Background technique

High purity graphite material is that the industries such as sealing material, lithium cell cathode material, diamond, aquadag lubricant are used Main raw material(s), raw ore one of of the crystalline flake graphite as high purity graphite material, using traditional means be only capable of making grade improve to 90 ~ 96%, it is difficult to meet the requirement of downstream client, it need to be through the methods of hydrogen fluoride, high temperature method, chlorinating roasting, alkali acid system Further purification.

Hydrogen fluoride can be but high to equipment acidproof requirement by graphite purification to 99.9%, and hydrofluoric acid wastewater processing difficulty Greatly, the country is phased out；High temperature method can be by graphite purification to 99.99%, but equipment is disposably put into greatly, and operating cost pole High, industrial production is difficult to stablize；Chlorinating roasting can only improve purity to 98 ~ 99%, domestic seldom to use；Alkali acid technological process Simply, disposably less investment, operating cost is low, and application potential is big, but purity can only generally be improved to 99.5%, how into one Step improves product purity, is urgent problem.

Summary of the invention

The problem of purifying graphite purity not high (99.5%) the purpose of the present invention is to solve existing acid-base method, provides one The method of kind ultrasonic wave auxiliary alkali acid system purification graphite.

To achieve the goals above, The technical solution adopted by the invention is as follows:

A kind of method of ultrasonic wave auxiliary alkali acid system purification graphite, it is characterised in that comprise the steps of:

A. it prepares alkali and melts graphite

1) uses the high-carbon graphite of preliminary purification to 94% or more for raw material, by the NaOH of high-carbon graphite and mass concentration 15 ~ 30% Solution 1:1 ~ 2 in mass ratio stir and evenly mix 5 ~ 30min under ultrasonic wave effect, obtain mixture, control supersonic generator power It is not less than 18000Hz not less than 3kW, frequency；

2) mixture be placed in baking oven be dried to moisture content 20% in advance hereinafter, transfer in 400 ~ 450 DEG C of Muffle furnaces into It goes and roasts 10 ~ 60min, roasting is completed, and is adopted after cooling and is washed with water to neutrality, and alkali is obtained after filtering and melts graphite；

B. high purity graphite is prepared

1) alkali made from step a is melted graphite and is transferred in the hydrochloric acid solution of mass concentration 15 ~ 25% by, and adjusting pulp density is 30 ~ 60%, and 5 ~ 30min of acidleach under ultrasonic wave effect, control supersonic generator power are not less than not less than 3kW, frequency 18000Hz；

2) ore pulp after acidleach is using filter, distillation water washing to neutral, 100 ~ 150 DEG C of 30 ~ 90min of drying up to high purity graphite (99.90% or more purity, moisture≤0.1%).

It selects the flaky graphite through preliminary purification to 99.4% as raw material, energy is melted using ultrasonic wave auxiliary mixing, enhancing alkali Power makes NaOH solution break through graphite crack and inter-laminar tension under the action of ultrasonic wave, sufficiently reacts with impurity under roasting condition, Sodium metasilicate, meta-aluminate and hydroxide precipitating are generated, wherein the soluble-salts such as sodium metasilicate, meta-aluminate are through being filtered, washed It removes, obtained alkali melts rear graphite；Alkali melts rear graphite and is handled by the acid leaching process that ultrasonic wave assists, and keeps hydroxide sufficiently anti-with acid Reaction generates soluble-salt, then through quickly diffusing in solution, and washed, filtering removal is finally prepared purity and is up to 99.90% graphite.

Beneficial effects of the present invention: 1. use this method of purification, and graphite purity can reach 99.90% or more；2.NaOH dosage 60 ~ 70% are reduced, hydrochloric acid dosage reduces 40 ~ 50%, and alkali melts time reduction 50 ~ 70%, and leaching time reduces 70 ~ 80%；3. effectively increasing Add production capacity, salkali waste, spent acid yield is greatly decreased, reduces sewage treatment difficulty, be conducive to environmental protection.

Detailed description of the invention

A kind of process flow diagram of ultrasonic wave auxiliary alkali acid system purification graphite of Fig. 1.

Specific embodiment

In conjunction with Fig. 1, the invention will be further described:

A kind of method of ultrasonic wave auxiliary alkali acid system purification graphite, specific implementation step are as follows:

Embodiment 1

High-carbon graphite of the sample from Kai Sheng graphitic carbon material Co., Ltd, main component are graphite, quartz, mica, are also contained A small amount of feldspar, chlorite, allochite, bloodstone etc..

A. it prepares alkali and melts graphite

1) the NaOH solution 1:2 in mass ratio of high-carbon graphite (94% or more purity) and mass concentration 20% occurs in ultrasonic wave 10min is stirred and evenly mixed in device, obtains mixture, controls supersonic generator power 3kW, frequency 20000Hz；

2) mixture is placed in baking oven is dried to surface without obvious moisture in advance, transfers in Muffle furnace, is to slowly warm up to 450 DEG C, heat preservation 0.5h reacts impurity sufficiently with NaOH, and roasting is completed, and adopts after cooling and is washed with distilled water to neutrality, after filtering It obtains alkali and melts graphite；

B. high purity graphite is prepared

1) alkali made from step a is melted graphite and is added in the hydrochloric acid of mass concentration 20% by, and is leached in supersonic generator The ore pulp of concentration 50% is made in 10min, controls supersonic generator power 3kW, frequency 20000Hz；

2) ore pulp after acidleach is using drying 60min at a temperature of filter, distillation water washing to neutrality, 105 DEG C up to high purity graphite (99.90% or more purity).

Comparing result such as the following table 1 of front and back graphite content content is purified using this method.

The purification of table 1 front and back graphite content content balance table

The result shows that: sealing material, lithium cell cathode material, artificial gold have been reached by high purity graphite index prepared by this method The quality requirement of the industries such as hard rock, aquadag lubricant.

The above described is only a preferred embodiment of the present invention, being not intended to limit the present invention in any form.This The technical staff in field carries out possible changes and modifications using the methods and technical content of the disclosure above, or is revised as equivalent change The equivalent embodiment of change still falls within technical solution of the present invention protection scope.

Claims (1)

1. a kind of method of ultrasonic wave auxiliary alkali acid system purification graphite, it is characterised in that comprise the steps of:

A. it prepares alkali and melts graphite

1) uses the high-carbon graphite of preliminary purification to 94% or more for raw material, by the NaOH of high-carbon graphite and mass concentration 15 ~ 30% Solution 1:1 ~ 2 in mass ratio stir and evenly mix 5 ~ 30min under ultrasonic wave effect, obtain mixture, control supersonic generator power It is not less than 18000Hz not less than 3kW, frequency；

2) mixture be placed in baking oven be dried to moisture content 20% in advance hereinafter, transfer in 400 ~ 450 DEG C of Muffle furnaces into It goes and roasts 10 ~ 60min, roasting is completed, and is adopted after cooling and is washed with water to neutrality, and alkali is obtained after filtering and melts graphite；

B. high purity graphite is prepared

1) alkali made from step a is melted graphite and is transferred in the hydrochloric acid solution of mass concentration 15 ~ 25% by, and adjusting pulp density is 30 ~ 60%, and 5 ~ 30min of acidleach under ultrasonic wave effect, control supersonic generator power are not less than not less than 3kW, frequency 18000Hz；

2) ore pulp after acidleach is using filter, distillation water washing to neutral, 100 ~ 150 DEG C of 30 ~ 90min of drying up to high-purity stone Ink.