CN1006220B - Method for manufacturing scale graphite expanded at high multiplying power - Google Patents
Method for manufacturing scale graphite expanded at high multiplying power Download PDFInfo
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- CN1006220B CN1006220B CN87106070.1A CN87106070A CN1006220B CN 1006220 B CN1006220 B CN 1006220B CN 87106070 A CN87106070 A CN 87106070A CN 1006220 B CN1006220 B CN 1006220B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 84
- 239000010439 graphite Substances 0.000 title claims abstract description 84
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 26
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 13
- 238000002791 soaking Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 23
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000007654 immersion Methods 0.000 claims description 7
- 239000000138 intercalating agent Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 238000011010 flushing procedure Methods 0.000 claims description 4
- 230000003068 static effect Effects 0.000 claims description 4
- 239000007770 graphite material Substances 0.000 abstract description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 9
- 239000007800 oxidant agent Substances 0.000 abstract description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 abstract 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 abstract 2
- 230000001007 puffing effect Effects 0.000 abstract 2
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 abstract 1
- 230000008961 swelling Effects 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 6
- 239000011229 interlayer Substances 0.000 description 4
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910001507 metal halide Inorganic materials 0.000 description 3
- 150000005309 metal halides Chemical class 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 description 2
- 239000003566 sealing material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QLOKJRIVRGCVIM-UHFFFAOYSA-N 1-[(4-methylsulfanylphenyl)methyl]piperazine Chemical compound C1=CC(SC)=CC=C1CN1CCNCC1 QLOKJRIVRGCVIM-UHFFFAOYSA-N 0.000 description 1
- 206010067484 Adverse reaction Diseases 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
A method for puffing natural flake graphite with high multiplying power belongs to the field of preparation of flexible graphite materials, concentrated sulfuric acid, nitric acid and potassium permanganate are used as oxidants, ferric chloride is used as an inserting agent, ferric chloride, part of concentrated sulfuric acid and nitric acid are used for soaking graphite in the first step, potassium permanganate and a small amount of concentrated sulfuric acid and nitric acid are added in the second step, the graphite is continuously soaked in the second step, and the graphite is washed and dried and then is subjected to high-temperature swelling, so that graphite worms with the puffing multiplying power of 700-1400 times can be obtained, and a flexible graphite product with good mechanical performance can be further prepared.
Description
The invention belongs to the field of producing of flexible graphite material.
Flexible graphite material is at first succeeded in developing (United States Patent (USP) 3404061) by U.S. combinating carbide company in nineteen sixty-eight, West Germany, France, Japan also develop in succession subsequently.China has begun development work greatly before and after 1978.Flexible graphite material has excellent properties such as natural graphite is corrosion-resistant, high-low temperature resistant, self-lubricating, has flexibility, compressibility and rebound resilience again.Therefore, obtain promoting in industries such as nuclear power, oil, chemical industry, metallurgy, machineries as sealing material is very fast.
The manufacture method of flexible graphite material generally be earlier with natural flake graphite (16～50 order) through sulfuric acid, nitric acid, hydrochloric acid (H
2SO
4, HNO
3, HCl) and some oxidizer treatment obtain acidifying graphite, and then washing, drying are placed on instantaneous heating under 800～1200 ℃ of high temperature at last, promptly obtain a kind of expanded cotton-shaped graphite, claim quasiflake graphite again, its expansion multiple can reach 100～500 times.This worm graphite is suppressed according to certain procedure, promptly mentioned the flexible graphite sealing material of various types.Acidification is crucial step in the flexible graphite material manufacturing processed, and it directly influences the expansion multiple of graphite, and the expansion multiple height is an important condition that makes soft graphite.
The special public clear 44-23966 of Japanese Patent had once introduced a kind of manufacture method of flexible graphite material.This method is that the vitriol oil oxidizing solution of being formed with the nitric acid (36 Baume concentration) of unit weight 10% heat (concentration is 95～98%) that Graphite Powder 99 is put into unit weight 90% heat is carried out dip treating, after about 30 minutes, take out moistening graphite particle water flushing and dry, in 1000 ℃ of following heat treated, make it again 200～300 times of instantaneous expansion.This quasiflake graphite is promptly got flexible graphite plate through compacting.Mention spendable oxygenant in this invention and be nitric acid, Potcrate, chromic acid, potassium permanganate, potassiumchromate, potassium bichromate, perchloric acid or such as the saturated solution of nitric acid and Potcrate, chromic acid and phosphoric acid, sulfuric acid and nitric acid, perhaps as three fluoridize the strong organic acid of acetic acid and so on and in organic acid, add the mixture that the strong oxidizer etc. of solubility is formed.Can add as iron(ic) chloride (FeCl in order further to increase the distance between the carbon-coating, also to mention in the invention
3), sodium-chlor (NaCl) and Potassium Bromide (KBr) wait some metal halides, as the interlayer intercalating agent.The expansion multiple of the graphite of handling with this manufacture method generally is lower than 500 times.
In the invention of the relevant manufacturing of some of past flexible graphite material, to use oxygenant though all once mention, as H
2SO
4, HNO
3, KMnO
4(potassium permanganate) or their mixture are also mentioned and will be used metal halide, as FeCl
3Additive as the interlayer inset.But never see relevant H
2SO
4, HNO
3, KMnO
4And FeCl
3Prescription and technology that the additive of three kinds of strong oxidizers and insertion uses simultaneously, from theory and practice, these four kinds of reagent can not use simultaneously, mainly are KMnO
4And FeCl
3In acid solution with vigorous reaction, even blast on fire, the result loses the processing effect to graphite.
The objective of the invention is to study a kind of new prescription and technology, make that the expansion ratio of graphite significantly increases after the acidifying.Like this, not only can utilize 16～50 purpose crystalline flake graphites to improve the quality of expansion ratio and then raising flexible graphite material routinely, but also can utilize low price, 80 orders that the source is abundant or thinner crystalline flake graphite are made flexible graphite material, and the cost of flexible graphite material is reduced.
The present invention is a kind of method of high bulking rate expansion crystalline flake graphite.Be that 16～80 purpose natural flake graphites are raw material with granularity promptly, the first step is with iron(ic) chloride (FeCl
3Consumption is 0.5～4% parts by weight of graphite, be preferably 1～3% parts by weight) (concentration is 85～98% to be preferably 98% with the vitriol oil, consumption is 200～500% parts by weight of stone amount) and graphite put into a container, (concentration is 40～95% with nitric acid after stirring, be preferably 65～80%, consumption is 80～300% parts by weight of graphite) add in this container and stir well static then immersion 2.5～5 hours, also can soak while stirring 1～3 hour, soaking temperature is room temperature～60 ℃; Second step was with potassium permanganate (KMnO
4Consumption is 4～12% parts by weight of graphite, be preferably 5～10% parts by weight, (concentration is the same to add the vitriol oil again after stirring well in the adding container, consumption is 40～60% parts by weight of graphite) and nitric acid (concentration is the same, consumption be graphite 10～30%) parts by weight), static then immersion 5～10 hours also can be soaked 2～6 hours while stirring, and soaking temperature is room temperature～60 ℃; Graphite water flushing after the immersion is 5～7 until the pH value; Carry out drying then, water content is reduced to 30～50% parts by weight in the control graphite; Under 750～950 ℃, carry out expanded at last.
Utilization present method can make the expanded multiple of natural flake graphite reach 700～1400 times, obtains a kind of quasiflake graphite, and becoming proportion with the further moldable or rolling of this graphite is 0.8～1.7 flexible graphite article.
Crystalline flake graphite is a kind of laminated crystalline material, and the C atom has extremely strong chemical bond in layer, and interlayer then is more weak Van der Waals force, and interlamellar spacing is 3.54
, graphite layers can form the acidulants of so-called graphite under the effect of strong oxidizer, or claims graphite salt.The intercalating agent metal halide is (as FeCl
3), graphite flake layer there is stronger insertion effect, make graphite flake layer strut several times into original model ylid bloom action distance, can make some oxygenants enter graphite flake layer more like this, act on respectively with graphite and this intercalating agent, and then causing at high temperature the graphite salt and the mixture decomposition or the reaction aggravation rapidly of interlayer, the result has obtained powerful expanded graphite.
Sulfuric acid, nitric acid, potassium permanganate, iron(ic) chloride can both be entered in the middle of the graphite flake layer, must be undertaken by the step and the order of these materials of interpolation provided by the invention.It is not all right that these four kinds of materials are added in the graphite simultaneously, because meeting blast on fire is abnormally dangerous.
The measuring method of expanded multiple is as follows:
Take by weighing W(g) worm graphite, measure to such an extent that its loose volume is V(ml), try to achieve the expanded multiple E of graphite then by following formula.
E+V/W·D
D=2.3 is the theoretical proportion of graphite
Embodiment:
Example one,
Take by weighing FeCl
30.01Kg, place to add the vitriol oil (concentration 98%) 2 liters in the container, after stirring evenly, get natural flake graphite (50 orders contain C90%) 1Kg, put into same container and stir evenly, add 1 liter in nitric acid (concentration 65%) again, stirred 5 minutes, left standstill 3 hours.Can shorten time to 1 hour as continuous stirring, add KMnO again
40.05Kg, add 0.3 liter of the vitriol oil (concentration is the same) then, 0.2 liter in nitric acid (concentration is the same), left standstill after stirring 10 hours, water is flushed to pH～7, and centrifuge dehydration also is dried to not conglomeration, the expanded quasiflake graphite that obtains under 900 ℃, expansion rate is 1400 times.
Example two
Take by weighing FeCl
30.03Kg put into container, add the vitriol oil (concentration 85%) 3.0 liters and stir evenly back adding crystalline flake graphite (80 orders, contain C90%) 1Kg and continuation stirring, add nitric acid (concentration is the same) 1.5 liters, stir and left standstill 2.5 hours after 3 minutes, add potassium permanganate 0.1Kg again, after stirring evenly, 0.2 liter in 0.3 liter of the vitriol oil vitriol oil (concentration is the same) and nitric acid (concentration is the same) left standstill 8 hours, water is flushed to pH=7, centrifuge dehydration also is dried to not conglomeration, the expanded quasiflake graphite that obtains under 900 ℃, expansion rate is 1100 times.
Example three
Take by weighing FeCl
30.005Kg place in the container, add (90%) 2.0 liter of the vitriol oil and stir evenly back adding crystalline flake graphite (32 orders, contain C99%) 1Kg, stir evenly and add (50%) 1 liter in nitric acid, stir evenly and leave standstill 2.5 hours, reaction beginning temperature is 25 ℃, and solution temperature is upgraded to 40 ℃ behind the adding vitriol oil, behind the adding concentrated nitric acid temperature is controlled at 50 ℃ always and kept 1.5 hours, add KMnO
40.08Kg, 0.3 liter of the vitriol oil (concentration is the same), nitric acid (concentration is the same) stirs evenly for 0.1 liter, and temperature of reaction is by 50 ℃ of naturally cooling of beginning, and the time is 5 hours, and is expanded under 900 ℃, obtains worm graphite, and expansion multiple is 1300 times.
Comparative Examples one:
Without FeCl
3, other is with example one, and the expansion multiple of graphite is 250 times as a result.
Comparative Examples two:
Without KMnO
4, other is with example two, as a result the expansion multiple of graphite～100 times.
Comparative Examples three:
Without FeCl
3And KMnO
4, other is with example three, as a result the expansion multiple of graphite～200 times.
Claims (10)
1, the manufacture method of a kind of high magnification expansion crystalline flake graphite (16～80 order) is made oxygenant with the vitriol oil, nitric acid and is soaked graphite, it is characterized in that also using potassium permanganate as oxygenant, and iron(ic) chloride is done intercalating agent, and the first step is with iron(ic) chloride (FeCl
3Consumption is 0.5～4% parts by weight of graphite) and the vitriol oil (concentration 85%～98%, consumption is 200～500% parts by weight of graphite) and graphite put into a container, after stirring with nitric acid (concentration 40%～95%, consumption is 80～300% parts by weight of graphite) add this container for stirring, static then immersion 2.5～5 hours, soaking temperature is room temperature～60 ℃, second step was with potassium permanganate (KMnO, consumption is 4～12% parts by weight of graphite), (concentration is the same for the vitriol oil, consumption is 40%～60% parts by weight of graphite), (concentration is the same for nitric acid, consumption is 10%～30% parts by weight of graphite), static then immersion 5～10 hours, soaking temperature is room temperature～60 ℃, graphite water flushing after the immersion is 5～7 until pH, carry out drying then, water content is 30%～50% parts by weight in the control graphite, carries out expanded at last under 750 ℃～950 ℃.
2, according to the said method of claim 1, the concentration that it is characterized in that the said vitriol oil is 98%.
3,, it is characterized in that said potassium permanganate consumption is 5～10% parts by weight of graphite according to claim 1,2 said methods.
4, according to right 1,2, said method, the consumption that it is characterized in that said iron(ic) chloride is 1～3% parts by weight of graphite.
5,, it is characterized in that said concentration of nitric acid is 65～80% according to right 1,2 said methods.
6, the manufacture method of a kind of high magnification expansion crystalline flake graphite (16～80 order) is made oxygenant with the vitriol oil, nitric acid and is soaked graphite, it is characterized in that also using potassium permanganate as oxygenant, and iron(ic) chloride is done intercalating agent, and the first step is with iron(ic) chloride (FeCl
3Consumption is 0.5～4% parts by weight of graphite) and the vitriol oil (concentration 85%～98%, consumption is 200～500% parts by weight of graphite) and graphite put into a container, after stirring with nitric acid (concentration 40%～95%, consumption is 80～300% parts by weight of graphite) add this container for stirring, soaked while stirring then 1～3 hour, soaking temperature is room temperature～60 ℃, and second step was with potassium permanganate (KMnO
4Consumption is 4～12% parts by weight of graphite), (concentration is the same for the vitriol oil, consumption is 40%～60% parts by weight of graphite), (concentration is the same for nitric acid, consumption is 10%～30% parts by weight of graphite) soaked while stirring then 2～6 hours, soaking temperature is room temperature～60 ℃, and the graphite water flushing after the immersion is 5～7 until pH, carries out drying then, water content is 30%～50% parts by weight in the control graphite, carries out expanded at last under 750 ℃～950 ℃.
7, according to the said method of claim 6, the concentration that it is characterized in that the said vitriol oil is 98%.
8,, it is characterized in that said potassium permanganate consumption is 5～10% parts by weight of graphite according to claim 6,7 said methods.
9, according to claim 6,7 said methods, the consumption that it is characterized in that said iron(ic) chloride is 1～3% parts by weight of graphite.
10,, it is characterized in that said concentration of nitric acid is 65～80% according to claim 6,7, said method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN87106070.1A CN1006220B (en) | 1987-09-03 | 1987-09-03 | Method for manufacturing scale graphite expanded at high multiplying power |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN87106070.1A CN1006220B (en) | 1987-09-03 | 1987-09-03 | Method for manufacturing scale graphite expanded at high multiplying power |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1032325A CN1032325A (en) | 1989-04-12 |
| CN1006220B true CN1006220B (en) | 1989-12-27 |
Family
ID=4815561
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN87106070.1A Expired CN1006220B (en) | 1987-09-03 | 1987-09-03 | Method for manufacturing scale graphite expanded at high multiplying power |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1006220B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100378155C (en) * | 2003-06-18 | 2008-04-02 | 希尔蒂股份公司 | Use of thermally expandable graphite intercalation compounds for producing fire-protection seals and method for their production |
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| CN1098807C (en) * | 1998-06-17 | 2003-01-15 | 攀枝花大学 | Process for preparing flake-shaped expanded graphite |
| DE10162532C1 (en) | 2001-12-19 | 2003-10-09 | Hilti Ag | Expandable graphite intercalation compounds, process for their preparation and their use |
| CN101100297B (en) * | 2006-07-03 | 2010-11-03 | 哈尔滨理工大学 | Method for preparing high fire resistance property expandable graphite |
| CN102408108A (en) * | 2011-07-27 | 2012-04-11 | 攀枝花学院 | Expanding method of fine flake graphite and preparation method of expanded graphite board |
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| CN111662678B (en) * | 2020-06-12 | 2023-07-21 | 上海弘枫实业有限公司 | High-temperature antioxidant flexible graphite filler, preparation method and high-temperature antioxidant flexible graphite packing |
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-
1987
- 1987-09-03 CN CN87106070.1A patent/CN1006220B/en not_active Expired
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100378155C (en) * | 2003-06-18 | 2008-04-02 | 希尔蒂股份公司 | Use of thermally expandable graphite intercalation compounds for producing fire-protection seals and method for their production |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1032325A (en) | 1989-04-12 |
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