CN110217787A - A method of micro crystal graphite is purified using industrial waste acid - Google Patents
A method of micro crystal graphite is purified using industrial waste acid Download PDFInfo
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- CN110217787A CN110217787A CN201910485299.7A CN201910485299A CN110217787A CN 110217787 A CN110217787 A CN 110217787A CN 201910485299 A CN201910485299 A CN 201910485299A CN 110217787 A CN110217787 A CN 110217787A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/215—Purification; Recovery or purification of graphite formed in iron making, e.g. kish graphite
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Abstract
The invention discloses a kind of methods using industrial waste acid purification micro crystal graphite, micro crystal graphite raw material is uniformly mixed with industrial waste acid, steam heating carries out acidleach twice, filtering, the micro crystal graphite of high-purity obtained by drying, the present invention is by waste acid recycling, micro crystal graphite is purified with factory's mixing spent acid, production cost and cost of sewage disposal is greatly reduced, solves high-performance, high safety, the bottleneck of the lithium ion battery negative material production of low cost, it realizes and produces lithium ion battery negative material industrialization using micro crystal graphite, micro crystal graphite purity produced is greater than 96%, substantially increase micro crystal graphite use value.
Description
Technical field
The present invention relates to a kind of methods using industrial waste acid purification micro crystal graphite, belong to micro crystal graphite purification field.
Background technique
Micro crystal graphite is called amorphous graphite powder, amorphous graphite powder , ?lead powder, belong to aphanitic graphite.Mainly contain in
Hebei, Inner Mongol, northeast, Hunan, the ground such as Xinjiang.It is repeatedly explored through geology department, existing 2,000,000,000 tons of amorphous graphite of China is the world
Reserves first.The micro crystal graphite overwhelming majority is graphitic carbon, and color is just grey, there is metallic luster, and matter is soft, not color hardness 1-2, specific gravity 2-
2.24, chemical property is stablized, and is not influenced by strong acid-base, and objectionable impurities is few, and iron, sulphur, phosphorus, nitrogen, molybdenum, hydrogen content is low, has resistance to height
The features such as temperature, heat transfer, conductive, lubrication and plasticity, was widely used in casting, smearing, battery, carbon product, pencil, pigment, resistance to
Fiery material, smelting, carburant, casting covering slag etc..
But for a long time, people mostly pay attention to the exploitation and processing of Scaly graphite, ignore and occupy a greater part of reserves
The development and utilization of microcrystalline graphite, deep process technology level and the lower problem of deep processing ability are not solved effectively for a long time
Certainly.At present mainly based on raw ore and rough-wrought product application, resource is not fully utilized, or even blindly exports, and causes mine
Produce being largely lost and wasting for resource.Therefore, the chemical purification research work of microcrystalline graphite, developing low-cost high-carbon stone are carried out
Black production technology, has important practical significance.
The purification of microcrystalline graphite at present mostly be use for reference Scaly graphite technology, common method of purification include floatation,
High temperature method, alkali acid system, hydrogen fluoride, chlorinating roasting etc., floatation are chiefly used in the preliminary purification of Scaly graphite, graphite products product
Position is not high, and the rate of recovery is very low, the method for the non-chemical purification graphite of alkali acid system, hydrogen fluoride, chlorinating roasting, wherein alkali
Acid system purifies the shortcomings that graphite and is to need high-temperature calcination, and energy consumption is big, and the reaction time purified is long, and the method is to setting
Standby corrosion is more serious, and is not achieved 99.9% by the graphite purity that the method obtains, although high temperature method refining effect
Preferably, but its cost is excessively high, capital invested needed for industrialization is huge, and hydrogen fluoride purifies that graphite is high-efficient, low energy consumption, but hydrogen
The dosage of fluoric acid is huge and has severe toxicity and strong corrosive, leads to production equipment and environmentally friendly higher cost.
Summary of the invention
Limited for prior art chemical purification effect, extracted micro crystal graphite purity is low, and the present invention provides one kind
Using the method for industrial waste acid purification micro crystal graphite, following scheme is specifically used:
Utilize the method for industrial waste acid purification micro crystal graphite, comprising the following steps:
1) industrial waste acid is added into the micro crystal graphite raw material that phosphorus content is 70%-75%, after mixing 80-90 DEG C of steaming
Vapour hot acid-leaching 10-12h, is obtained by filtration micro crystal graphite crude product；
2) industrial waste acid is added into micro crystal graphite crude product, 80-90 DEG C of steam heats secondary pickling 8- after mixing
10h, filtering, micro crystal graphite obtained by drying.
The present invention purifies micro crystal graphite by waste acid recycling, with factory's mixing spent acid, and production cost and dirt is greatly reduced
Cost of water treatment solves the bottleneck of the lithium ion battery negative material production of high-performance, high safety, low cost, realizes and utilize
Micro crystal graphite produces lithium ion battery negative material industrialization, and micro crystal graphite purity produced is greater than 96%, substantially increases
Micro crystal graphite use value.
Further, above-mentioned industrial waste acid be concentration be 8%-10% hydrochloric acid, nitric acid, any one or more of hydrofluoric acid
Mixed acid.
In the industrial production, spent acid or nitrification, esterification, sulfonation, alkylation, catalysis and the gas dry of organic matter are resulted from
Etc. processes, or result from the processes such as titanium white production, pickling iron and steel and gas dry, concentration is generally relatively low, and containing a large amount of
Organic matter, utilization is more difficult, and cost recovery is higher, and the present invention carries out micro crystal graphite purification using industrial waste acid, substantially drops
Low production cost and cost of sewage disposal.
Further, the solid-to-liquid ratio of industrial waste acid and micro crystal graphite raw material is 2-2.5: 1, preferably 2: 1 in step 1)；Step
2) solid-to-liquid ratio of industrial waste acid and micro crystal graphite raw material is 1.5-2: 1, preferably 2: 1 in.
Detailed description of the invention
Fig. 1 is the method and process flow chart that the present invention purifies micro crystal graphite using industrial waste acid.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
Utilize the method for industrial waste acid purification micro crystal graphite, comprising the following steps:
1) industrial waste acid is added with solid-to-liquid ratio 2: 1 in the micro crystal graphite raw material for being 70% to phosphorus content, after mixing 90
DEG C steam hot acid-leaching 12h, is obtained by filtration micro crystal graphite crude product；
2) industrial waste acid is added with solid-to-liquid ratio 2: 1 into micro crystal graphite crude product, 80 DEG C of steam heating are secondary after mixing
Acidleach 10h, filtering, micro crystal graphite obtained by drying.
Industrial waste acid selects the mixed acid for the hydrochloric acid and nitric acid that concentration is 10%.
Products therefrom is detected according to the detection method of micro crystal graphite purity in GB/T 3519-2008, purity is
98.8%.
Embodiment 2
Utilize the method for industrial waste acid purification micro crystal graphite, comprising the following steps:
1) industrial waste acid is added with solid-to-liquid ratio 2: 1 in the micro crystal graphite raw material for being 75% to phosphorus content, after mixing 80
DEG C steam hot acid-leaching 12h, is obtained by filtration micro crystal graphite crude product；
2) industrial waste acid is added with solid-to-liquid ratio 1.5: 1 into micro crystal graphite crude product, after mixing 90 DEG C of steam heating two
Secondary acidleach 10h, filtering, micro crystal graphite obtained by drying.
It is 8% hydrochloric acid that industrial waste acid, which selects concentration,.
Products therefrom is detected according to the detection method of micro crystal graphite purity in GB/T 3519-2008, purity is
96.4%.
Embodiment 3
Utilize the method for industrial waste acid purification micro crystal graphite, comprising the following steps:
1) industrial waste acid is added with solid-to-liquid ratio 2.5: 1 in the micro crystal graphite raw material for being 75% to phosphorus content, after mixing
90 DEG C of steam hot acid-leaching 12h, are obtained by filtration micro crystal graphite crude product；
2) industrial waste acid is added with solid-to-liquid ratio 2: 1 into micro crystal graphite crude product, 90 DEG C of steam heating are secondary after mixing
Acidleach 10h, filtering, micro crystal graphite obtained by drying.
It is 9% hydrofluoric acid that industrial waste acid, which selects concentration,.
Products therefrom is detected according to the detection method of micro crystal graphite purity in GB/T 3519-2008, purity is
97.5%.
Embodiment 4
Utilize the method for industrial waste acid purification micro crystal graphite, comprising the following steps:
1) industrial waste acid is added with solid-to-liquid ratio 2: 1 in the micro crystal graphite raw material for being 70% to phosphorus content, after mixing 85
DEG C steam hot acid-leaching 10h, is obtained by filtration micro crystal graphite crude product；
2) industrial waste acid is added with solid-to-liquid ratio 2: 1 into micro crystal graphite crude product, 85 DEG C of steam heating are secondary after mixing
Acidleach 10h, filtering, micro crystal graphite obtained by drying.
Industrial waste acid selects the hydrochloric acid that concentration is 10%, the mixed acid of nitric acid and hydrofluoric acid.
Products therefrom is detected according to the detection method of micro crystal graphite purity in GB/T 3519-2008, purity is
98.2%.
Embodiment 5
Utilize the method for industrial waste acid purification micro crystal graphite, comprising the following steps:
1) industrial waste acid is added with solid-to-liquid ratio 2: 1 in the micro crystal graphite raw material for being 70% to phosphorus content, after mixing 80
DEG C steam hot acid-leaching 10h, is obtained by filtration micro crystal graphite crude product；
2) industrial waste acid is added with solid-to-liquid ratio 2: 1 into micro crystal graphite crude product, 90 DEG C of steam heating are secondary after mixing
Acidleach 8h, filtering, micro crystal graphite obtained by drying.
It is 10% hydrofluoric acid that industrial waste acid, which selects concentration,.
Products therefrom is detected according to the detection method of micro crystal graphite purity in GB/T 3519-2008, purity is
97.6%.
Claims (6)
1. a kind of method using industrial waste acid purification micro crystal graphite, which comprises the following steps:
1) industrial waste acid is added into micro crystal graphite raw material, after mixing hot acid-leaching 10-12h, micro crystal graphite is obtained by filtration
Crude product；
2) industrial waste acid is added into micro crystal graphite crude product, heats secondary pickling 8-10h after mixing, filtering is obtained by drying
The micro crystal graphite.
2. a kind of method using industrial waste acid purification micro crystal graphite according to claim 1, which is characterized in that the work
Industry spent acid be concentration be 8%-10% hydrochloric acid, nitric acid, any one or more of hydrofluoric acid mixed acid.
3. a kind of method using industrial waste acid purification micro crystal graphite according to claim 1, which is characterized in that described micro-
The phosphorus content of brilliant graphite raw material is 70%-75%.
4. a kind of method using industrial waste acid purification micro crystal graphite according to claim 1, which is characterized in that step 1)
And/or the operation of heating described in step 2) is 80-90 DEG C of steam heating.
5. a kind of method using industrial waste acid purification micro crystal graphite according to claim 1, which is characterized in that step 1)
Described in the solid-to-liquid ratio of industrial waste acid and micro crystal graphite raw material be 2-2.5: 1.
6. a kind of method using industrial waste acid purification micro crystal graphite according to claim 1, which is characterized in that step 2)
Described in the solid-to-liquid ratio of industrial waste acid and micro crystal graphite raw material be 1.5-2: 1.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101683979A (en) * | 2009-08-17 | 2010-03-31 | 福建省富友石墨科技有限公司 | New process for purifying and manufacturing microcrystalline graphite product |
| CN106882805A (en) * | 2017-04-28 | 2017-06-23 | 福建凯昱微晶石墨有限公司 | A kind of micro crystal graphite purifies preparation technology |
| CN106966389A (en) * | 2017-04-28 | 2017-07-21 | 福建凯昱微晶石墨有限公司 | A kind of method of purification of micro crystal graphite |
| CN107555428A (en) * | 2017-10-31 | 2018-01-09 | 湖南国盛石墨科技有限公司 | A kind of micro crystal graphite secondary pickling method of purification and its high-purity micro crystal graphite |
| WO2019099225A1 (en) * | 2017-11-20 | 2019-05-23 | Nanotek Instruments, Inc. | Continuous process and apparatus for producing graphene |
-
2019
- 2019-05-27 CN CN201910485299.7A patent/CN110217787A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101683979A (en) * | 2009-08-17 | 2010-03-31 | 福建省富友石墨科技有限公司 | New process for purifying and manufacturing microcrystalline graphite product |
| CN106882805A (en) * | 2017-04-28 | 2017-06-23 | 福建凯昱微晶石墨有限公司 | A kind of micro crystal graphite purifies preparation technology |
| CN106966389A (en) * | 2017-04-28 | 2017-07-21 | 福建凯昱微晶石墨有限公司 | A kind of method of purification of micro crystal graphite |
| CN107555428A (en) * | 2017-10-31 | 2018-01-09 | 湖南国盛石墨科技有限公司 | A kind of micro crystal graphite secondary pickling method of purification and its high-purity micro crystal graphite |
| WO2019099225A1 (en) * | 2017-11-20 | 2019-05-23 | Nanotek Instruments, Inc. | Continuous process and apparatus for producing graphene |
Non-Patent Citations (1)
| Title |
|---|
| 边炳鑫 等: "《石墨加工与石墨材料》", 31 May 2014, 中国矿业大学出版社 * |
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Effective date of registration: 20210720 Address after: 012000 xingwangjiao Industrial Park, Xinghe County, Wulanchabu City, Inner Mongolia Autonomous Region Applicant after: Inner Mongolia Rui Sein carbon new Mstar Technology Ltd. Address before: 013650 Xingwang Industrial Park, Xinghe County, Wulanchabu, the Inner Mongolia Autonomous Region Applicant before: INNER MONGOLIA RISING NEW ENERGY Co.,Ltd. |
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