CN110156006A - A kind of purification process technique of graphite - Google Patents
A kind of purification process technique of graphite Download PDFInfo
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- CN110156006A CN110156006A CN201910617566.1A CN201910617566A CN110156006A CN 110156006 A CN110156006 A CN 110156006A CN 201910617566 A CN201910617566 A CN 201910617566A CN 110156006 A CN110156006 A CN 110156006A
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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
It include: Step 1: graphite ingredient the present invention relates to a kind of purification process technique of graphite;Step 2: reaction dissolvent ingredient;Step 3: primary first-order equation;Step 4: a filters pressing;Step 5: secondary response;Step 6: secondary filters pressing;Step 7: third-order reaction;Step 8: graphite washs;Step 9: graphite is dried;Step 10: graphite combination cooling;Step 11: graphite magnetic separation is classified;Step 12: graphite is packed.The present invention has the purification mass effect that can guarantee graphite.
Description
Technical field
The present invention relates to the technical fields of graphite purification, more particularly, to a kind of purification process technique of graphite.
Background technique
Graphite is a kind of high energy crystal carbon data, because its structure and conductive, thermally conductive, smooth, high temperature resistant, chemical functional are stable
Etc. characteristics, make its in high function data have higher use value, be widely used in metallurgy, machinery, environmental protection, chemical industry, fire resisting,
The scopes such as electronics, medicine, military project and aerospace.With new technology, the continuous development of new process, common high purity graphite material
Be no longer satisfied the demand of many industries, the height of graphite purification quality decides the use characteristic of graphite material and comprehensive
Can, graphite purity is higher, and application value is higher.
Because providing one kind can guarantee that the purifying technique of graphite purification quality is particularly important.
Summary of the invention
The object of the present invention is to provide a kind of purification process techniques of graphite, have the purification quality that can guarantee graphite.
Foregoing invention purpose of the invention has the technical scheme that
A kind of purification process technique of graphite, comprising the following steps:
Step 1: graphite ingredient: graphite former material being delivered to graphite raw material storehouse by powder conveying apparatus, then by graphite raw material
Graphite in storehouse send spare to graphite measuring chute;
Step 2: reaction dissolvent ingredient: taking hydrofluoric acid, hydrochloric acid, nitric acid to send respectively and mixed into agitator tank;
Step 3: primary first-order equation: will mixing complete hydrofluoric acid, hydrochloric acid, nitric acid, with graphite and add purified water input once it is anti-
Answer in tank and be stirred, graphite, hydrofluoric acid, hydrochloric acid, nitric acid, purified water mass fraction ratio are as follows: 1:0.9:1.5:1:2, adjust
Saving temperature in primary first-order equation tank is 100-150 DEG C, is reacted 15-22 hours;
Step 4: a filters pressing: the graphite solution for reacting completion in step 3 in primary first-order equation tank is transported in a filter press,
Filters pressing is carried out, the waste liquid that filters pressing generates is drained into waste liquid tank;
Step 5: secondary response: the graphite after filters pressing in step 4 is drained into secondary response tank, and again by hydrofluoric acid, hydrochloric acid,
It is stirred in nitric acid and purified water input reactor tank, the mass fraction ratio of graphite, hydrofluoric acid, hydrochloric acid, nitric acid and purified water
Are as follows: 1:0.1:1:0.5:2.5, adjusting temperature in secondary response tank is 50-100 DEG C, and the reaction time is 10-18 hours;
Step 6: secondary filters pressing: the graphite solution for reacting completion in step 5 in secondary response tank is delivered to secondary filter press
It is interior, filters pressing is carried out, the waste liquid that filters pressing generates is drained into waste liquid tank;
Step 7: diluting reaction: the graphite after filters pressing in step 6 being drained into diluting reaction tank, and purified water is input to dilution
Mixing stirring is carried out in reactor tank, adjusting temperature in diluting reaction tank is 60-85 DEG C, and the reaction time is 5-8 hours;
Step 8: graphite washs: the graphite solution in step 7 being sent to centrifuge, centrifugal dehydration, dehydration to moisture are carried out
Lower than 20%;
Step 9: graphite is dried: the graphite in step 6 being delivered to flash dryer and carries out breaing up drying;
Step 10: graphite combination cooling: the graphite powder that completion is dried in step 9 is thrown to carrying out mixing in spiral mixer, and
Lead to cooling water in the barrel of spiral mixer to be cooled to room temperature graphite;
Step 11: graphite magnetic separation is classified: graphite after cooling being delivered to feed bin, and the graphite powder in feed bin is uniformly defeated
It send to graphite magnetic separator, the waste material that magnetic separation generates is delivered in waste product storehouse, and the graphite that magnetic separation is completed is delivered in screening machine and carries out
Sieving and grading is simultaneously sent to feed bins at different levels, while the waste material that screening generates is delivered to graphite waste storehouse;
Step 12: graphite is packed: the graphite in feed bins at different levels is sent respectively to carrying out packing packaging in packing machine.
By using above-mentioned technical proposal, graphite raw material can be completed and expect purification drying again to the whole of screening packaging from down
A process can effectively ensure that the purification quality of graphite.
The present invention is further arranged to: the step three, in the reaction process of the primary first-order equation tank, by graphite, hydrogen
Fluoric acid, nitric acid, hydrochloric acid and purified water stir into paste, then primary every stirring in 30 minutes, primary stirring 8-10 minutes.
By using above-mentioned technical proposal, it can guarantee graphite in primary first-order equation tank, hydrofluoric acid, nitric acid, hydrochloric acid and pure
Change being sufficiently stirred for water, to guarantee the abundant reaction of primary first-order equation tank inner melt.
The present invention is further arranged to: the step five, in the reaction process of the secondary response tank, by graphite, hydrogen
Fluoric acid, nitric acid, hydrochloric acid and purified water stir into paste, then primary every stirring in 1 hour, primary stirring 5-7 minutes.
By using above-mentioned technical proposal, it can guarantee graphite in secondary response tank, hydrofluoric acid, nitric acid, hydrochloric acid and pure
Change being sufficiently stirred for water, to guarantee the abundant reaction of secondary response tank inner melt.
The present invention is further arranged to: the step seven, in the reaction process of the diluting reaction tank, by graphite with it is pure
Change water and is carried out continuously stirring until reaction terminates.
By using above-mentioned technical proposal, it can guarantee being sufficiently stirred for purified water and graphite in diluting reaction tank, thus
Convenient for completing the abundant washing of graphite.
The present invention is further arranged to: the step nine, and the drying temperature of the flash dryer is 200-400 DEG C.
By using above-mentioned technical proposal, by using drying temperature be 200-400 DEG C, can be realized the abundant of graphite
Drying, convenient for the moisture in removal graphite.
The present invention is further arranged to: the step one, and graphite former material uses the graphite of purity 60%-80%, and graphite is defeated
It is screened out before entering graphite raw material storehouse and lives together reason.
It can be convenient for graphite by carrying out removal of impurities processing before the purifying of graphite former material by using above-mentioned technical proposal
Purification process.
The present invention is further arranged to: the step three, and graphite, hydrofluoric acid, nitric acid, hydrochloric acid and purified water are put into
20-30 minutes are continuously stirred first to paste after primary first-order equation tank.
By using above-mentioned technical proposal: graphite, hydrofluoric acid, nitric acid, hydrochloric acid and purified water are put into primary first-order equation
It is stirred 20-30 minutes after tank, graphite, hydrofluoric acid, nitric acid, hydrochloric acid and purified water can be made adequately to mix, be convenient for subsequent stone
The purifying reaction of ink.
The present invention is further arranged to: the step ten, and the temperature of the cooling water is 10-15 DEG C.
By using above-mentioned technical proposal: when the graphite by drying enters progress mixing in spiral mixer, by logical
10-15 DEG C of the cooling water entered can complete being fully cooled for graphite.
In conclusion advantageous effects of the invention are as follows:
1. can complete graphite raw material expects that purification drying again to the whole process of screening packaging, can effectively ensure that stone from down
The purification quality of ink completes the graphite purification that purity is 99% or more;
2. by using drying temperature be 200-400 DEG C, can be realized the abundant drying of graphite, convenient for removal graphite in water
Point;
3. being stirred 20-30 minutes after graphite, hydrofluoric acid, nitric acid, hydrochloric acid and purified water are put into primary first-order equation tank, can make
Graphite, hydrofluoric acid, nitric acid, hydrochloric acid and purified water adequately mix, and react convenient for the purifying of subsequent graphite.
Detailed description of the invention
Fig. 1 is process flow diagram of the invention.
Specific embodiment
Below in conjunction with attached drawing, invention is further described in detail.
It referring to Fig.1, is a kind of purification process technique of graphite disclosed by the invention, comprising the following steps:
Step 1: graphite ingredient: the graphite former material that purity is 60%-80% being cleaned by screening, then passes through powder carry and fills
It sets and is delivered to graphite raw material storehouse, then send the graphite in graphite raw material storehouse spare to graphite measuring chute;
Step 2: reaction dissolvent ingredient: taking hydrofluoric acid, hydrochloric acid, nitric acid to send respectively and mixed into agitator tank;
Step 3: primary first-order equation: will mixing complete hydrofluoric acid, hydrochloric acid, nitric acid, with graphite and add purified water input once it is anti-
Answer in tank and be stirred, graphite, hydrofluoric acid, hydrochloric acid, nitric acid, purified water mass fraction ratio are as follows: 1:0.9:1.5:1:2, adjust
Saving temperature in primary first-order equation tank is 100-120 DEG C, is put by graphite, hydrofluoric acid, nitric acid, hydrochloric acid and purified water to primary anti-
It answers tank to continuously stir stirring in 20-30 minutes first later and then once every stirring in 30 minutes once stirs 8- to paste
10 minutes, total coreaction 15-22 hours;
Step 4: a filters pressing: the graphite solution for reacting completion in step 3 in primary first-order equation tank is transported in a filter press,
Filters pressing is carried out, the waste liquid that filters pressing generates is drained into waste liquid tank;
Step 5: secondary response: draining into secondary response tank for the graphite after filters pressing in step 4, and again by hydrofluoric acid, hydrochloric acid,
It is stirred in nitric acid and purified water input reactor tank, the mass fraction ratio of graphite, hydrofluoric acid, hydrochloric acid, nitric acid and purified water
Are as follows: 1:0.1:1:0.5:2.5, adjust secondary response tank in temperature be 80-100 DEG C, by graphite, hydrofluoric acid, nitric acid, hydrochloric acid with
And purified water puts into primary first-order equation tank and continuously stirs stirring in 20-30 minutes first later to paste, then stirs every 1 hour
Once, primary stirring 5-7 minutes, the reaction time is 10-18 hours in total;
Step 6: the graphite solution for reacting completion in step 5 in secondary response tank secondary filters pressing: is delivered to secondary filter press
It is interior, filters pressing is carried out, the waste liquid that filters pressing generates is drained into waste liquid tank;
Step 7: diluting reaction: the graphite after filters pressing in step 6 is drained into diluting reaction tank, and purified water is input to dilution
Mixing stirring is carried out in reactor tank, adjusting temperature in diluting reaction tank is 60-85 DEG C, and the reaction time is 5-8 hours, then this phase
Between, graphite is carried out continuously stirring until reacting terminates with purified water;
Step 8: graphite washing: the graphite solution in step 7 is sent to centrifuge, carries out centrifugal dehydration, dehydration to moisture
Lower than 20%;
Step 9: graphite drying: being delivered to flash dryer for the graphite in step 6 and carry out breaing up drying, flash dryer
Drying temperature is kept for 200-400 DEG C;
Step 10: graphite combination cooling: the graphite powder that completion is dried in step 9 is thrown to carrying out mixing in spiral mixer, and
10-15 DEG C of cooling water is passed through in the barrel of spiral mixer to be cooled to room temperature graphite;
Step 11: graphite magnetic separation classification: graphite after cooling is delivered to feed bin, and the graphite powder in feed bin is uniformly defeated
It send to graphite magnetic separator, the waste material that magnetic separation generates is delivered in waste product storehouse, and the graphite that magnetic separation is completed is delivered in screening machine and carries out
Sieving and grading is simultaneously sent to feed bins at different levels, while the waste material that screening generates is delivered to graphite waste storehouse;
Step 12: graphite packaging: the graphite in feed bins at different levels is sent respectively to carrying out packing packaging in packing machine.
It can be realized graphite raw material by using above-mentioned technique and expect that purification is dried, again to the entire mistake of screening packaging from down
Journey completes the graphite purification that purity is 99% or more, guarantees the purification quality of graphite.
The embodiment of present embodiment is presently preferred embodiments of the present invention, not limits protection of the invention according to this
Range, therefore: the equivalence changes that all structures under this invention, shape, principle are done, should all be covered by protection scope of the present invention it
It is interior.
Claims (8)
1. a kind of purification process technique of graphite, which comprises the following steps:
Step 1: graphite ingredient: graphite former material being delivered to graphite raw material storehouse by powder conveying apparatus, then by graphite raw material
Graphite in storehouse send spare to graphite measuring chute;
Step 2: reaction dissolvent ingredient: taking hydrofluoric acid, hydrochloric acid, nitric acid to send respectively and mixed into agitator tank;
Step 3: primary first-order equation: will mixing complete hydrofluoric acid, hydrochloric acid, nitric acid, with graphite and add purified water input once it is anti-
Answer in tank and be stirred, graphite, hydrofluoric acid, hydrochloric acid, nitric acid, purified water mass fraction ratio are as follows: 1:0.9:1.5:1:2, adjust
Saving temperature in primary first-order equation tank is 100-120 DEG C, is reacted 15-22 hours;
Step 4: a filters pressing: the graphite solution for reacting completion in step 3 in primary first-order equation tank is transported in a filter press,
Filters pressing is carried out, the waste liquid that filters pressing generates is drained into waste liquid tank;
Step 5: secondary response: the graphite after filters pressing in step 4 is drained into secondary response tank, and again by hydrofluoric acid, hydrochloric acid,
It is stirred in nitric acid and purified water input reactor tank, the mass fraction ratio of graphite, hydrofluoric acid, hydrochloric acid, nitric acid and purified water
Are as follows: 1:0.1:1:0.5:2.5, adjusting temperature in secondary response tank is 80-100 DEG C, and the reaction time is 10-18 hours;
Step 6: secondary filters pressing: the graphite solution for reacting completion in step 5 in secondary response tank is delivered to secondary filter press
It is interior, filters pressing is carried out, the waste liquid that filters pressing generates is drained into waste liquid tank;
Step 7: diluting reaction: the graphite after filters pressing in step 6 being drained into diluting reaction tank, and purified water is input to dilution
Mixing stirring is carried out in reactor tank, adjusting temperature in diluting reaction tank is 60-85 DEG C, and the reaction time is 5-8 hours;
Step 8: graphite washs: the graphite solution in step 7 being sent to centrifuge, centrifugal dehydration, dehydration to moisture are carried out
Lower than 20%;
Step 9: graphite is dried: the graphite in step 6 being delivered to flash dryer and carries out breaing up drying;
Step 10: graphite combination cooling: the graphite powder that completion is dried in step 9 is thrown to carrying out mixing in spiral mixer, and
Lead to cooling water in the barrel of spiral mixer to be cooled to room temperature graphite;
Step 11: graphite magnetic separation is classified: graphite after cooling being delivered to feed bin, and the graphite powder in feed bin is uniformly defeated
It send to graphite magnetic separator, the waste material that magnetic separation generates is delivered in waste product storehouse, and the graphite that magnetic separation is completed is delivered in screening machine and carries out
Sieving and grading is simultaneously sent to feed bins at different levels, while the waste material that screening generates is delivered to graphite waste storehouse;
Step 12: graphite is packed: the graphite in feed bins at different levels is sent respectively to carrying out packing packaging in packing machine.
2. a kind of purification process technique of graphite according to claim 1, it is characterised in that: the step three, it is described
In the reaction process of primary first-order equation tank, graphite, hydrofluoric acid, nitric acid, hydrochloric acid and purified water are stirred into paste, then every 30
Minute stirring is primary, primary stirring 8-10 minutes.
3. a kind of purification process technique of graphite according to claim 1, it is characterised in that: the step five, it is described
In the reaction process of secondary response tank, graphite, hydrofluoric acid, nitric acid, hydrochloric acid and purified water are stirred into paste, then every 1
Hour stirring is primary, primary stirring 5-7 minutes.
4. a kind of purification process technique of graphite according to claim 1, it is characterised in that: the step seven, it is described
In the reaction process of diluting reaction tank, graphite is carried out continuously stirring until reacting terminates with purified water.
5. a kind of purification process technique of graphite according to claim 1, it is characterised in that: the step nine, it is described
The drying temperature of flash dryer is 200-400 DEG C.
6. a kind of purification process technique of graphite according to claim 1, it is characterised in that: the step one, graphite
Former material uses the graphite of purity 60%-80%, is screened out before graphite input graphite raw material storehouse and lives together reason.
7. a kind of purification process technique of graphite according to claim 1, it is characterised in that: the step three, by stone
20-30 minutes are continuously stirred first to paste after ink, hydrofluoric acid, nitric acid, hydrochloric acid and purified water investment primary first-order equation tank.
8. a kind of purification process technique of graphite according to claim 1, it is characterised in that: the step ten, it is described
The temperature of cooling water is 10-15 DEG C.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112723352A (en) * | 2020-12-29 | 2021-04-30 | 青岛洛唯新材料有限公司 | high-pH-value graphite processing technology |
CN113149001A (en) * | 2021-03-05 | 2021-07-23 | 大同氢都驰拓新能源有限公司 | Automatic high-yield method for preparing and purifying spherical graphite |
CN113753885A (en) * | 2021-09-03 | 2021-12-07 | 黑龙江省宝泉岭农垦溢祥石墨有限公司 | Chemical purification and wastewater treatment process for natural spherical graphite |
CN115285988A (en) * | 2022-08-31 | 2022-11-04 | 浙江碳一新能源有限责任公司 | Flash evaporation drying device, purification process for improving pH value of spherical graphite and spherical graphite |
CN115849369A (en) * | 2023-02-24 | 2023-03-28 | 潍坊新翰泽能源科技有限公司 | Energy-saving environment-friendly high-purity graphite deep processing production line and control method |
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CN105776191A (en) * | 2016-02-19 | 2016-07-20 | 青岛田庄恒源石墨有限公司 | Spherical graphite production process |
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 |
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CN110171825A (en) * | 2019-07-10 | 2019-08-27 | 青岛洛唯新材料有限公司 | A kind of high purity graphite purifying technique |
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CN1052463A (en) * | 1990-11-30 | 1991-06-26 | 中国科学院西安光学精密机械研究所 | Purification of graphite |
CN105776191A (en) * | 2016-02-19 | 2016-07-20 | 青岛田庄恒源石墨有限公司 | Spherical graphite production process |
WO2018088636A1 (en) * | 2016-11-11 | 2018-05-17 | 주식회사 카보랩 | Method for recycling waste graphite powder and graphite powder manufactured by the same |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112723352A (en) * | 2020-12-29 | 2021-04-30 | 青岛洛唯新材料有限公司 | high-pH-value graphite processing technology |
CN113149001A (en) * | 2021-03-05 | 2021-07-23 | 大同氢都驰拓新能源有限公司 | Automatic high-yield method for preparing and purifying spherical graphite |
CN113753885A (en) * | 2021-09-03 | 2021-12-07 | 黑龙江省宝泉岭农垦溢祥石墨有限公司 | Chemical purification and wastewater treatment process for natural spherical graphite |
CN115285988A (en) * | 2022-08-31 | 2022-11-04 | 浙江碳一新能源有限责任公司 | Flash evaporation drying device, purification process for improving pH value of spherical graphite and spherical graphite |
CN115285988B (en) * | 2022-08-31 | 2023-11-10 | 碳一新能源集团有限责任公司 | Flash evaporation drying device, purification process for improving pH value of spherical graphite and spherical graphite |
CN115849369A (en) * | 2023-02-24 | 2023-03-28 | 潍坊新翰泽能源科技有限公司 | Energy-saving environment-friendly high-purity graphite deep processing production line and control method |
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Inventor after: Li Yanxiong Inventor after: Liu Junde Inventor after: Li Qingquan Inventor before: Li Yanxiong Inventor before: Liu Junde Inventor before: Li Qingquan |
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Application publication date: 20190823 |