CN109647630B

CN109647630B - Short-process purification method of graphite

Info

Publication number: CN109647630B
Application number: CN201811620694.3A
Authority: CN
Inventors: 张乾伟; 潘力; 吴建新; 石倩倩; 俞燕强; 李佩悦
Original assignee: CNBM Bengbu Design and Research Institute for Glass Industry Co Ltd
Current assignee: CNBM Bengbu Design and Research Institute for Glass Industry Co Ltd
Priority date: 2018-12-28
Filing date: 2018-12-28
Publication date: 2021-03-23
Anticipated expiration: 2038-12-28
Also published as: CN109647630A

Abstract

The invention relates to a short-process purification method of graphite, which comprises the steps of crushing, grinding and flotation and is characterized by comprising the following steps: (1) preparing graphite or carbonaceous material raw materials with the granularity of less than 1mm and the fixed carbon content of not less than 35 percent into ore pulp with the concentration of not more than 60 percent, and placing a direct-contact ultrasonic vibrator into the ore pulp, controlling the power of the ultrasonic vibrator to be not less than 1.0kW and the time to be not less than 1 min; (2) diluting the crushed and dispersed ore pulp to ore pulp with the concentration not higher than 30%, sending the ore pulp into flotation equipment, adding an inhibitor, a collecting agent and a foaming agent, performing rough concentration and fine concentration in sequence, stirring, aerating and performing flotation to obtain graphite concentrate and graphite tailings; (3) and (3) concentrating to a concentration of 30-60% or sending the mixture into a container with a direct contact type ultrasonic vibrator for crushing and dispersing, and repeating the steps (1) and (2) for 2-3 times. The invention has the beneficial effects that: the dissociation efficiency is improved, and the times of ore grinding and flotation are reduced; the method is favorable for reducing the dosage of the flotation reagent and improving the efficiency of the flotation reagent; optimizing flotation effect and improving the carbon content of the concentrate.

Description

Short-process purification method of graphite

Technical Field

The invention belongs to the technical field of graphite ore dressing and purification, and particularly relates to a short-flow purification method for graphite.

Background

Graphite is an important strategic resource and is an important composition material of conductive, fireproof, anticorrosive, lubricating, sealing and other materials in the fields of new energy, national defense and chemical industry. At present, the high-carbon graphite prepared from natural flake graphite mostly adopts a staged grinding and staged flotation process, and the main purpose is to protect the large flake graphite, but the flotation process flow is too long (such as nine times of grinding, eleven times of flotation and the like); the method for preparing high-carbon graphite from microcrystalline graphite (cryptocrystalline graphite and earthy graphite) is not only partially referred to a flake graphite beneficiation and purification method, but also adopts a one-step ore grinding and multiple flotation process, for example, Chinese patent (CN 105197920A) discloses a beneficiation and purification method for microcrystalline graphite, which adopts one-stage coarse crushing, one-stage fine crushing, one-stage or two-stage dry ultrafine crushing-grading, and combines a multi-stage fine selection and multi-stage scavenging process for processing.

Disclosure of Invention

The invention aims to solve the problems of long process and low flotation effect of the existing high-carbon graphite flotation purification process, and provides a short-process purification method of graphite.

In order to achieve the purpose, the technical scheme adopted by the invention is as follows:

a short-process purification method of graphite comprises the steps of crushing, grinding and flotation, and is characterized in that: the method comprises the following steps:

(1) crushing, grinding and floating a raw material containing graphite or carbonaceous materials to prepare a material with the granularity of less than 1mm and the fixed carbon content of not less than 35%, mixing the material with water to prepare ore pulp with the mass concentration of not more than 60%, placing a direct contact type ultrasonic vibrator in the ore pulp to perform ultrasonic crushing and dispersion, controlling the output power of a single ultrasonic wave to be not less than 1.0kW, and controlling the ultrasonic crushing and dispersion time to be not less than 1 min;

(2) diluting the ore pulp crushed and dispersed in the step (1) to ore pulp with the mass concentration not higher than 30%, sending the ore pulp into flotation equipment, adding a collecting agent (kerosene 200-;

(3) and (3) concentrating the graphite concentrate and the graphite tailings obtained in the step (2) to a mass concentration of 30-60% or directly sending the graphite concentrate and the graphite tailings into a container with a direct contact type ultrasonic vibrator for ultrasonic crushing and dispersing again, and repeating the steps (1) and (2) for 2-3 times to obtain the final high-carbon graphite concentrate.

Further, the raw materials containing graphite or carbonaceous materials in the step (1) are natural crystalline flake graphite, microcrystalline graphite, artificial graphite and carbonaceous products, and the raw materials containing carbonaceous materials are preliminarily enriched to have the fixed carbon content of not less than 30% through mineral separation processes such as crushing, grinding, flotation and the like.

Compared with the prior art, the invention has the following beneficial effects:

(1) the raw material containing graphite or carbonaceous material is crushed and dispersed by adopting direct contact ultrasonic waves to replace or partially replace an ore grinding process, so that the dissociation efficiency of the raw material containing graphite or carbonaceous material and gangue minerals is improved, the ore grinding and flotation times of high-carbon graphite preparation are reduced, and the short-process preparation of the high-carbon graphite is realized;

(2) the direct contact type ultrasonic wave combined flotation process is adopted, and in the ultrasonic crushing and dispersing circulation process for two or more times, the direct contact type ultrasonic wave has a dispersing effect on the flotation reagent, so that the coagulation of the flotation reagent in ore pulp is reduced, the use amount of the flotation reagent is favorably reduced, and the action efficiency of the flotation reagent is improved;

(3) the direct contact type ultrasonic combined flotation process is adopted, the direct contact type ultrasonic effectively cleans the surfaces of the carbon-containing raw material and the gangue minerals, the action probability of the flotation reagent and the target minerals is increased, the optimization of the flotation effect is facilitated, and the carbon content of the concentrate is improved.

Drawings

FIG. 1 is a simplified diagram of a short-run purification process for graphite;

FIG. 2 is a simplified diagram of a short process for preparing natural medium-fine flake graphite and high-carbon graphite;

FIG. 3 is a simplified diagram of a short-process preparation process of natural microcrystalline graphite high-carbon graphite.

Detailed Description

The invention is further described in detail with reference to fig. 2 and 3, and a short-flow purification method of graphite comprises the following specific implementation steps:

example 1

(1) Taking natural medium-fine flake graphite lump ore with the fixed carbon content of 10.5 percent and the particle size of less than 100mm, and sequentially adopting a cone crusher, a ball mill and a spiral classifier to carry out a closed-loop process of crushing, grinding and classifying to obtain graphite-containing ore pulp with the solid particle size of less than 0.5 mm;

(2) diluting graphite ore pulp by adding water to 40% of mass concentration, introducing the diluted graphite ore pulp into a size mixing barrel, sequentially adding kerosene (500 g/t) and pine oil (150 g/t), stirring for 2min, introducing the graphite ore pulp after size mixing into a flotation machine, aerating and scraping to obtain rough concentration concentrate foam of graphite, concentrating the rough concentration concentrate foam of graphite to 40% of mass concentration, introducing the rough concentration concentrate foam of graphite into a primary concentration flotation machine after primary sand mill grinding, aerating and scraping to obtain primary concentration graphite concentrate foam, concentrating the primary concentration graphite concentrate foam to 40% of mass concentration, introducing the fine concentration graphite concentrate foam into a secondary concentration flotation machine after secondary sand mill grinding, aerating and scraping to obtain secondary concentration graphite concentrate foam;

(3) after the secondary concentration graphite concentrate foam is concentrated to 50% ore pulp, a direct contact type ultrasonic vibrator with single output power of 2.4kW is placed in the secondary concentration graphite concentrate ore pulp, the ultrasonic action time is controlled for 10min, the ore pulp is guided to a tertiary concentration flotation machine, water is supplemented and pulp is adjusted to 15% mass concentration, and the tertiary concentration graphite concentrate is obtained through inflation and foam scraping;

(4) adding kerosene (100 g/t) and pine oil (30 g/t) into a drainage groove of the third-time concentration graphite concentrate, adding water, adjusting slurry until the mass concentration is 10%, feeding the slurry into a fourth-time concentration flotation machine, aerating, and scraping bubbles to obtain fourth-time concentration graphite concentrate, namely the final graphite concentrate.

The final graphite concentrate, middlings and tailings are concentrated, dried and dried to obtain the final product, and the indexes of the final product are shown in table 1.

TABLE 1 short-run preparation of indexes of various products from natural medium-fine flake graphite and high-carbon graphite

Product(s)	Fixed carbon content/%)	Yield/%)	Percent recovery%
				Raw ore	10.51	100.00	100.00
Graphite concentrate	94.66	9.48	85.38
				Middling	5.94	23.21	13.11
Graphite tailings	0.23	67.31	1.47

Example 2

(1) Crushing and grinding microcrystalline graphite lump ore with the fixed carbon content of 65.33% and the granularity of less than 100mm to prepare microcrystalline graphite ore powder with the granularity of less than 0.1mm, mixing the microcrystalline graphite ore powder with water to prepare ore pulp with the mass concentration of 50%, guiding the ore pulp into a roughing pulp mixing barrel, sequentially adding sodium silicate (500 g/t), kerosene (960 g/t) and pine oil (420 g/t) with the modulus of 2.8 and the mass fraction of 10%, stirring for 2min, then guiding into a roughing flotation machine, replenishing water and mixing the pulp to the mass concentration of 30%, aerating and scraping to obtain roughing microcrystalline graphite concentrate;

(2) concentrating the rough concentration microcrystalline graphite concentrate to 45% pulp, introducing the pulp into a direct contact type ultrasonic dispersion tank with a single output power of 2.8kW, controlling the action time of ultrasonic waves for 20min, then guiding the pulp into a primary concentration flotation machine, replenishing water, regulating the pulp to 20% mass concentration, inflating and scraping to obtain primary concentration microcrystalline graphite concentrate foam;

(3) concentrating the primary fine concentration microcrystalline graphite concentrate foam to 45% of pulp, introducing the pulp into a direct contact type ultrasonic dispersion tank with a single output power of 2.8kW, controlling the ultrasonic action time for 15min, then introducing the pulp into a secondary size mixing barrel, sequentially adding 2.8 modulus, 10% mass percent water glass (300 g/t), emulsified kerosene (400 g/t) and pine oil (180 g/t) into the secondary size mixing barrel, stirring for 2min, introducing into a secondary fine concentration flotation machine, replenishing water, mixing the pulp to 15% mass concentration, aerating, scraping to obtain secondary fine concentration microcrystalline graphite concentrate, connecting the secondary fine concentration microcrystalline graphite concentrate into a tertiary fine concentration flotation machine through a fine ore tank, replenishing water, mixing the pulp to 10% mass concentration, aerating, and scraping to obtain tertiary fine concentration microcrystalline graphite concentrate;

(4) and (3) introducing the microcrystalline graphite concentrate obtained by the third fine concentration into a fourth fine concentration flotation machine, replenishing water, regulating the slurry to the mass concentration of 10%, inflating and scraping to obtain fourth fine concentration microcrystalline graphite concentrate, namely the final microcrystalline graphite concentrate.

And concentrating and drying the final microcrystalline graphite concentrate, middling and tailings to obtain a final product, wherein the indexes are shown in table 2.

TABLE 2 short-run preparation of various product indexes from natural microcrystalline graphite and high-carbon graphite

Product(s)	Fixed carbon content/%)	Yield/%)	Percent recovery%
				Raw ore of microcrystalline graphite	65.33	100.00	100.00
Graphite concentrate	94.21	58.87	84.89
				Middling	34.64	20.63	10.94
Graphite tailings	13.28	20.50	4.17

The above embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and all changes in form and details may be made therein without departing from the spirit and scope of the present invention as defined in the appended claims.

Claims

1. A short-process purification method of graphite sequentially comprises the steps of crushing, ore grinding and flotation, and is characterized in that: the method comprises the following steps:

(1) the method comprises the following steps of preparing a material containing carbonaceous materials into a material with the granularity of less than 1mm and the fixed carbon content of not less than 35% after crushing, grinding and flotation in sequence, mixing the material with water to prepare an ore pulp with the mass concentration of not more than 60%, placing a direct contact type ultrasonic vibrator in the ore pulp for ultrasonic crushing and dispersion, controlling the single output power of ultrasonic waves to be not less than 1.0kW, and controlling the ultrasonic crushing and dispersion time to be not less than 1 min;

(2) diluting the ore pulp crushed and dispersed in the step (1) to ore pulp with the mass concentration not higher than 30%, sending the ore pulp into flotation equipment, adding 400g/t of collecting agent kerosene 200 and 50-250g/t of foaming agent pine oil during rough concentration, adding 0-100g/t of collecting agent kerosene and 0-150g/t of foaming agent pine oil during fine concentration, stirring and aerating, and obtaining graphite concentrate and graphite tailings by adopting a foam flotation method;

2. The short-process purification method of graphite according to claim 1, characterized in that: the carbonaceous material raw material in the step (1) is natural crystalline flake graphite, microcrystalline graphite or artificial graphite and is preliminarily enriched to the carbonaceous material raw material with the fixed carbon content of not less than 30 percent through crushing, ore grinding and flotation processes in sequence.

3. The short-process purification method of graphite according to claim 1, characterized in that: and (3) adding 0-400g/t of sodium silicate with the modulus of 2.5-3.0 and the mass fraction of 10% according to the needs during the selection in the step (2).