CN1031512A - Liquid phase method for purifying national graphite - Google Patents
Liquid phase method for purifying national graphite Download PDFInfo
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- CN1031512A CN1031512A CN 87105509 CN87105509A CN1031512A CN 1031512 A CN1031512 A CN 1031512A CN 87105509 CN87105509 CN 87105509 CN 87105509 A CN87105509 A CN 87105509A CN 1031512 A CN1031512 A CN 1031512A
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Abstract
The invention relates to the processing method of liquid phase method for purifying national graphite.The present invention adopts low temperature, normal pressure, alkali circulation.The natural graphite of processing-100 orders～+ 32 purpose carbon containings 85%.Cross the low-carbon (LC) natural graphite after the present invention purifies, can reach the high-carbon graphite more than 99%.Volume particle size graphite after the present invention purifies can be used for industries such as nuclear industry, automotive industry, spationautics, metallurgy.
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.
Openly specially permit the clear 57-95077 of communique and 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 smart separately refining 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) add 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, consume 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 to neutrality filtration, dry that product 333.2 restrains product purity 99.30%, the carbon rate of recovery 98% with water.
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 filtered and recycled alkali 700 grams after the discharging, consume alkali 140 grams, filter residue washes with water and joins to the neutrality in 3% the hydrochloric acid soln, and 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 gram, 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, 44 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 463 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 324.7 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, filter then, wash, through acidolysis, drying, it is characterized in that: granularity is-100～+ 32 purposes, 85% low-carbon (LC) natural graphite, under agitation add in 50～70% the NaOH solution,, filter 180～200 ℃ of abundant stirring reactions 2～4 hours, filter cake was washed till neutral back and adds in 3～6% the hydrochloric acid, 70～90 ℃ of stirring reactions 1～2 hour.
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 true CN1031512A (en) | 1989-03-08 |
| CN1005103B 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) |
Cited By (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
Cited By (3)
| 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 |
| WO2023198472A1 (en) | 2022-04-12 | 2023-10-19 | Dorfner Anzaplan GmbH | Method for producing purified graphite |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1005103B (en) | 1989-09-06 |
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