CN1005103B - Liquid phase method for purifying natural graphite - Google Patents
Liquid phase method for purifying natural graphite Download PDFInfo
- Publication number
- CN1005103B CN1005103B CN87105509.0A CN87105509A CN1005103B CN 1005103 B CN1005103 B CN 1005103B CN 87105509 A CN87105509 A CN 87105509A CN 1005103 B CN1005103 B CN 1005103B
- Authority
- CN
- China
- Prior art keywords
- graphite
- carbon
- natural graphite
- liquid phase
- grams
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 238000000034 method Methods 0.000 title claims abstract description 16
- 229910021382 natural graphite Inorganic materials 0.000 title claims abstract description 12
- 239000007791 liquid phase Substances 0.000 title claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 25
- 239000010439 graphite Substances 0.000 claims abstract description 25
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 7
- 239000012065 filter cake Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- 238000003672 processing method Methods 0.000 claims description 2
- 239000003513 alkali Substances 0.000 abstract description 16
- 239000002245 particle Substances 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 238000005904 alkaline hydrolysis reaction Methods 0.000 description 9
- 239000000047 product Substances 0.000 description 7
- 238000011084 recovery Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- -1 8.82% Inorganic materials 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a process method for purifying natural graphite by a liquid phase method. The invention adopts low temperature, normal pressure and alkali circulation. Processing natural graphite containing 85% of carbon with-100 meshes to + 32 meshes. The low-carbon natural graphite purified by the method can reach over 99 percent of high-carbon graphite. The graphite with large particle size purified by the method can be used in the industries such as atomic energy industry, automobile industry, aerospace technology, metallurgy and the like.
Description
The invention relates to the processing method of liquid phase method for purifying national graphite.
In some special industries, must use carbon content as industry such as nuclear industry, automotive industry, spationautics, metallurgy is 99% high-carbon graphite.Natural graphite (referring to the graphite after ore dressing) carbon content can reach 85%, far can not satisfy the requirement of using the high-carbon graphite industry.For this reason, must purify to natural graphite.
The clear 57-95077 of day disclosure special permission communique has introduced a kind of method of purification.This method heats powdered graphite in strong base solution, roasting, dry to remove impurity.But this method at first will be processed as natural graphite the medium-carbon graphite of carbon content 95%, secondly graphite particle size requires less than 200 orders, certainly will to pulverize the difficulty that fine grinding And and fine powder will increase filtration washing like this, its three this method only can be removed metallic impurity such as Sb, As, Mo, Fe, Cu, Ni, the requirement that does not still reach high-carbon graphite.In addition, this method has been used KOH, the also corresponding raising of cost.
At the shortcoming of above-mentioned technology, the present invention proposes a kind of purifying technique, directly uses-100 orders～+ 32 purpose volume particle sizes, low-carbon (LC) (85%) natural graphite, through operations such as normal pressure alkaline hydrolysis, washing, acidolysis, makes the finished product become high-carbon level graphite.
The present invention under agitation adds natural graphite in the strong base solution, the intensification stirring reaction, through filtering, filtrate is added alkali and is recycled, and adds acid-respons after the filter cake washing, and then after filtration, washing, dry, obtain 99% high-carbon level graphite.
Alkaline hydrolysis is an important procedure of the present invention.The present invention uses soda lye, considers big-100 orders of direct use low-carbon (LC) natural graphite processing size range～+ 32 orders, has therefore selected higher alkali concn for use, and its span is good 50～70%.The alkaline hydrolysis temperature will influence alkaline hydrolysis speed, it is considered herein that temperature of reaction is advisable at 180～200 ℃, high again alkaline hydrolysis temperature, though also can accelerate alkaline hydrolysis speed again, not obvious.Stirring fully, increased the contact surface of graphite granule and alkali lye, is very favourable to alkaline hydrolysis.The alkaline hydrolysis time generally was controlled at 2～4 hours.
Filtration washing, filter cake must be washed till neutrality, reacts the impurity that transfers solubility to guarantee to remove through alkaline hydrolysis.
Carry out acidolysis in the neutral filter cake adding dilute hydrochloric acid solution.Concentration of hydrochloric acid is advisable 3～6%, 70～90 ℃ of temperature.Stirring reaction 1～2 hour.
Its granularity of natural graphite that the present invention uses is-100 orders～+ 32 orders, and carbon content 85%, one step purification is 99% high-carbon graphite, and does not need the refining separately industry that requires high-carbon graphite that promptly can be used for resemble the nuclear industry again.The present invention is suitable for processing-100 orders～all kinds of graphite of+32 purposes.
Example 1
Get emerging river graphite ore natural flake graphite 400 grams, sample carbon containing 85%, foreign matter content SiO
2, 8.82%, Fe
2O
32.17%, Al
2O
31.96%, MgO1.05% adds solid NaOH480 gram, water 320 grams, 180 ℃ of alkali concn 60% temperature of reaction, 4 hours time, dilute filtration reclaims alkali 350.2 grams after the discharging, consumes alkali 129.8 grams, filter residue washes with water to neutrality, join in 5% the hydrochloric acid soln, the ratio of hydrochloric acid soln amount and filter residue amount be 3: 1 80 ℃ of reactions 1 hour down, filter, wash with water to neutrality, filtration, dry that product 333.2 restrains product purity 99.30%, the carbon rate of recovery 98%
Example 2
Get southern villa graphite ore natural flake graphite 400 grams, sample carbon containing 85%, foreign matter content SiO
25.53%, Fe
2O
33.05%, Al
2O
31.78%, MgO1.93%, CaO1.64% add solid NaOH840 gram, water 360 grams, alkali concn 70%, 180 ℃ of temperature of reaction, 2 hours time, dilute after the discharging, filtered and recycled alkali 700 gram consumes alkali 140 grams, and filter residue washes with water and joins to the neutrality in 3% the hydrochloric acid soln, the hydrochloric acid soln amount is 3: 1 with the ratio of wet filter residue, 90 ℃ down reaction filtered in 2 hours, wash with water to neutral filtration drying and get product 323 grams, product purity 99.40, the carbon rate of recovery 95%.
Example 3
Get graphite sample 400 grams in used emerging river in the example 1, add solid sodium hydroxide 660 grams, water 540 grams, 200 ℃ of alkali concn 55% temperature of reaction, 4 hours time, dilute filtration reclaims alkali 525 grams, consume alkali 135 grams, filter residue washes with water to neutrality, joins in 6% the hydrochloric acid soln, and hydrochloric acid soln is 3: 1 with the wet slag ratio, reacting filtration in 1 hour down at 70 ℃ washes with water to neutrality, filtration, dry that product 326.4 restrains, purity is 99.6, the carbon rate of recovery is 96%.
Example 4
Get graphite ore sample 400 grams in used southern villa in the example 2, add solid NaOH600 gram, water 600 grams, alkali concn is 50%, reacted 2 hours down at 200 ℃, reclaim alkali 400 grams behind the dilute filtration, consume alkali 137 grams, filter residue washes with water and joins to the neutrality in 3% the hydrochloric acid soln, the hydrochloric acid soln amount is 3: 1 with the wet slag ratio, 90 ℃ of reaction filtrations in 2 hours down, washes with water to neutrality filtration, dry product 3247 grams that get, purity is 99.80%, the carbon rate of recovery 95.50%.
Claims (1)
1, a kind of processing method of liquid phase method purification graphite, be graphite to be added in the strong base solution react, then the washing, drying, it is characterized in that: granularity is-100～+ 32 purposes, 85% low-carbon (LC) natural graphite, under agitation adds in 50～70% the NaOH solution, 180～200 ℃ of reactions 2～4 hours, filter, filter cake is washed till neutral back and adds in 3～6% the hydrochloric acid, 70～90 ℃ of stirring reactions 1～2 hour, and washing, drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN87105509.0A CN1005103B (en) | 1987-08-10 | 1987-08-10 | Liquid phase method for purifying natural graphite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN87105509.0A CN1005103B (en) | 1987-08-10 | 1987-08-10 | Liquid phase method for purifying natural graphite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1031512A CN1031512A (en) | 1989-03-08 |
| CN1005103B true CN1005103B (en) | 1989-09-06 |
Family
ID=4815350
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN87105509.0A Expired CN1005103B (en) | 1987-08-10 | 1987-08-10 | Liquid phase method for purifying natural graphite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1005103B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102616773A (en) * | 2012-04-10 | 2012-08-01 | 中国地质大学（武汉） | Method for purifying medium-carbon flake graphite to obtain high-purity graphite |
| DE102022108846A1 (en) | 2022-04-12 | 2023-10-12 | Dorfner Anzaplan GmbH | Process for producing purified graphite |
-
1987
- 1987-08-10 CN CN87105509.0A patent/CN1005103B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN1031512A (en) | 1989-03-08 |
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| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| C13 | Decision | ||
| C14 | Grant of patent or utility model | ||
| C19 | Lapse of patent right due to non-payment of the annual fee |