CN1038496C - Method for directly preparing Lemery salt by using salt-cake (gypsum) type bittern or mother liquid for preparing salt (saptpetre) or mirabilite mineral bittern - Google Patents
Method for directly preparing Lemery salt by using salt-cake (gypsum) type bittern or mother liquid for preparing salt (saptpetre) or mirabilite mineral bittern Download PDFInfo
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- CN1038496C CN1038496C CN94106765A CN94106765A CN1038496C CN 1038496 C CN1038496 C CN 1038496C CN 94106765 A CN94106765 A CN 94106765A CN 94106765 A CN94106765 A CN 94106765A CN 1038496 C CN1038496 C CN 1038496C
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- bittern
- salt
- glaserite
- tartar
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Abstract
The present invention discloses a method for directly preparing potassium sulfate from sodium sulfate (calcium) type bittern, or mother liquid for preparing salt (saltpetre) or mirabilite mineral bittern. Bittern is purified to remove Ca2+ and Mg2+; the mixture of sodium sulphate decahydrate and partial sodium chloride is obtained by refrigeration; after the mixture is dissolved, potassium chloride is added to the dissolved mixture to obtain potassium sulfate after two-stage conversion. The method has the advantages of no three waste, low energy consumption and obvious economic benefit, and is very suitable for the popularization of well mineral salt enterprises.
Description
The present invention a kind ofly produces the method for vitriolate of tartar with sal prunella type bittern, particularly a kind of method of directly producing vitriolate of tartar with sodium sulfate (calcium) type bittern or salt manufacturing (nitre) mother liquor or saltcake ore deposit bittern.
Produce in sodium-chlor (salt) process at well mine salt bittern, people generally be with bittern through multiple-effect evaporation or multiple-effect vacuum-evaporation, make the sodium-chlor supersaturation and crystallize out.Because sodium sulfate (calcium) type bittern contains more SO
2- 4Do not separate out simultaneously with sodium-chlor for guaranteeing sodium sulfate with the raising of evaporation capacity, reduce the salt quality, salt making enterprises or the salt-making mother liquor of sodium sulphate content near state of saturation emitted, or the method for construction fever simultaneously carries nitre or the frozen saltpeter mention device carries out aftertreatment to salt-making mother liquor, make sodium sulfate product (thenardite), implement the sal prunella coproduction; Or before bittern carries out the multiple-effect vacuum salt, it is carried out freezing, send to salt manufacturing after sodium sulfate in the brine reduced to lower aq, to improve the quality or the output of salt.These methods or can only salt manufacturing are kept production with a large amount of discharging mother liquors, and are had a strong impact on because of a large amount of discharging mother liquors cause environment.Can only produce the thenardite of salt and low value, manufacturing enterprise's energy consumption is big, the production cost height, and product is single, and the market adaptability is strong, and this also is the relatively poor major cause of the present economic benefit of China's salt manufacturing industry.
At present, having with sulfuric acid or sodium sulfate or ammonium sulfate is that vitriolate of tartar is produced in raw material and Repone K reaction, or is that raw material and Repone K are produced vitriolate of tartar and paid production Technique of Potassium Sulphate such as product magnesium chloride with the bittern.The former production cost height, the business economic benefit is restricted.For example be that vitriolate of tartar, thenardite (Na are produced in the reaction of raw material and Repone K with sodium sulfate
2SO
4) be through freezing, the settlement separate sal glauberi of producing, sal glauberi is imitated the vapo(u)rization system evaporation at 2-3 behind hot water Hui Rong, concentrated, crystallization makes thenardite again after centrifugal, dehydration, drying, thenardite is again through dissolving, add Repone K, produce vitriolate of tartar through reaction, sedimentation, separation, centrifuge dehydration, drying again.This process complexity, the energy consumption height, investment is big.The latter is raw material with the bittern, adds Repone K, makes vitriolate of tartar and magnesium chloride etc., the method for being announced as patent CN1077434A, but this kind method only is applicable to the evaporate brine comprehensive utilization of back mother liquor of seawater.
The purpose of this invention is to provide a kind of method of producing vitriolate of tartar with sal prunella type bittern.
The object of the present invention is achieved like this: a kind ofly produce the method for vitriolate of tartar with sal prunella type bittern, it is characterized in that its technical process is: sodium sulphate type bittern or salt-making mother liquor or saltcake ore deposit bittern are passed through NaOH-Na
2CO
3Method purifies, and removes wherein Ca
2+, Mg
2+Impurity, after purified brine is frozen 10～-20 ℃, sodium sulfate reduces with temperature, its solubleness descends and separates out sal glauberi, having part sodium-chlor to follow simultaneously separates out, analysing behind the nitre bittern can send to and carry out the multiple-effect vacuum salt, rear stock solution of salt producing can return through purifying capable frozen saltpeter mention again, the sal glauberi of separating out and the mixture of small amounts of salts are sent into one section conversion reactor, return molten and add a small amount of Repone K by potassium sulfate mother liquid from two sections switching processes, get glaserite, the settlement separate back of glaserite adds two sections conversions of Repone K, gets the vitriolate of tartar solidliquid mixture, and this solid-liquid miscellany is separated, after the drying potassium product, bittern or the mother liquor contains sodium sulfate separated out behind the solid are 0.5-40g/l.The condition that sal glauberi and potassium sulfate mother liquid are converted to glaserite is: 1. temperature 10-60 ℃; 2. proportioning: sal glauberi slurry: potassium sulfate mother liquid=1: 0.5-6 (volume ratio); 3. be 0.5-10 hour switching time.The condition that vitriolate of tartar is produced in glaserite and Repone K, water conversion is: 1. temperature: 20-75 ℃; 2. proportioning: glaserite: Repone K: water=1: 0.3-1.0: 0.1-3.5 (weight ratio); 3. switching time: 0.5-10 hour.
Characteristics of the present invention are to organically combine with domestic and international salt manufacturing (nitre) process with the part technology of Repone K conversion vitriolate of tartar process, to add low-temperature receiver bittern are forced the freezing ten water nitre (Na that produce
2SO
410H
2O) and through Repone K change vitriolate of tartar, can be widely used in the well mine salt production.Direct freezing bittern no matter, still freezing salt manufacturing (nitre) mother liquor, or freezing saltcake ore deposit bittern all can be converted to the sodium sulfate after concentrating the domestic market shortage, and the vitriolate of tartar of higher-value is arranged.Both having can be salt manufacturing (nitre) or having made the alkali production process provides protosulfate high-quality raw brine (liquid salt), can produce high-quality potassium product (K again
2〉=50%).
Fig. 1 is the process flow diagram of directly producing the vitriolate of tartar method with sodium sulfate (calcium) type bittern or salt manufacturing (nitre) mother liquor or saltcake ore deposit bittern of the present invention.
Accompanying drawing number of the present invention is:
(1) sodium sulfate (calcium) type bittern;
(2) salt manufacturing (nitre) mother liquor;
(3) saltcake ore deposit bittern;
(4) purify;
(5) freezing;
(6) settling vessel;
(7) vacuum filtration;
(8) one sections conversion reactors;
(9) one sections settling vessels;
(10) centrifuge dehydration;
(11) two sections conversion reactors
(12) two sections settling vessels;
(13) centrifuge dehydration;
(14) freezing;
(15) settlement separate;
(16) ten water nitre slurries;
(17) protosulfate bittern;
(18) ten water nitre;
(19) potassium sulfate mother liquid;
(20) nitre potassium mixture;
(21) clear liquid;
(22) nitre potassium mixed slurry;
(23) glaserite mother liquor;
(24) glaserite;
(25) water;
(26) Repone K;
(27) vitriolate of tartar wet feed;
(28) fluid bed dryer;
(29) vitriolate of tartar.
Below in conjunction with accompanying drawing technological process of the present invention is elaborated.
Technological process of the present invention (referring to Fig. 1, all operations all carries out under normal pressure) is:
From sodium sulphate (calcium) the type bittern (1) of Brine of Salt Mine well extraction or bittern after salt manufacturing (nitre) mother liquor (2) or the saltcake bittern (3) of saltcake mine extraction pass through NaOH-Na2CO
3Method or Ca (OH)2-Na
2CO
3Method or Ca (OH)2-Na
2CO
3-CO
2Ca is wherein removed in method purification (4)2-、Mg
2+Impurity, force freezing (5) to uniform temperature by adding low-temperature receiver, ten water nitre are separated out (sodium sulphate content that reaches the desired bittern of user), with settler (6) ten water nitre slurry (16) sedimentations are separated with protosulfate bittern (17), protosulfate bittern is sent to salt manufacturing (nitre), ten water nitre (18) are sent into one section conversion reactor (8) and are produced glaserite after vacuum filtration (7), the purpose of filtration is to reduce the sodium chloride content in the ten water nitre slurries that enter one section conversion process.
2. ten water nitre that enter one section conversion reactor (8) and potassium sulfate mother liquid (19) reaction from two sections conversion processes, produce the glaserite mixture, in reaction, answer the vitriolate of tartar content in the visual response thing and add Repone K in right amount to adjust the concentration of resultant, make glaserite sulfur acid potassium reach 40-80%, glaserite solid-to-liquid ratio (s/l) remains on about 20%.The glaserite (24) that is obtained by centrifuge dehydration (10) after one section settling vessel (9) sedimentation is sent into two sections conversion reactors (11), glaserite mother liquor (23) through freezing (14) again to 0～-15 ℃, behind the nitre potassium mixed slurry (22) settlement separate (15), the K that separates out
2SO
4, KCl and ten water nitre mixtures (nitre, potassium mixture (20)) return one section conversion reactor (8), clear liquid (21) can mix with protosulfate bittern behind the frozen saltpeter mention, also can discharge utilization separately.
3. the glaserite (24) that enters two sections conversion reactors (11) is added less water (25), and constantly adds the slurry that Repone K (〉=90%) (26) is made into solid-to-liquid ratio about 15%, and reaction generates vitriolate of tartar.The vitriolate of tartar slurry separates through two sections settling vessels (12), and centrifuge dehydration (13) gets vitriolate of tartar wet feed (27), and the vitriolate of tartar wet feed is sent into fluid bed dryer (28) (drying temperature 80--150 ℃), makes K
2The vitriolate of tartar of O 〉=50% (29) product.The purpose that reactor adds less water is that the vitriolate of tartar resultant is washed.Potassium sulfate mother liquid (19) is sent into one section conversion reactor, dissolves ten water nitre and generates glaserite with the reaction of ten water nitre.
Embodiment 1:
For ease of explanation, we are listed in the Chemical Composition of embodiment 1 on the table 1, and used bittern is taken from the purified brine of sal prunella factory of Salt Chemical General Plant, Jianghan Petroleum administration Bureau, and proportion is 1195g/l, form to see Table 1.
With 11950 gram purified brines (T=30 ℃), put into an enamel basin and force freezing 4 hours at refrigeration chamber.Stop freezing (the crystallization this moment sal glauberi of separating out is 784.6 grams) when liquidus temperature reaches-10 ℃, and took out in 2 hours in the sedimentation of refrigeration indoor heat insulating, pour out clear liquor rapidly, and carry out solid-liquid separation, its liquid phase weight is 11165.4 grams.
The potassium sulfate mother liquid (35 ℃ of temperature) that adds the artificial preparation of 1036.8 grams in the enamel basin of clear liquor toward inclining, the nitre potassium mixture that adds the artificial preparation of 143 grams simultaneously, under agitation carry out one section conversion, temperature is 30 ℃, transform and carry out solid-liquid separation after 1.5 hours, get 716.6 gram glaserites and 1247.8 gram glaserite mother liquors.
The glaserite mother liquor is placed on forces freezing 3 hours in refrigeration chamber in another enamel basin, temperature is-10 ℃, carries out solid-liquid separation then, gets nitre potassium mixture 143.0 grams, clear liquor 1104.8 grams.
Add 318.2 gram Repone K and 35 ℃ of water of 379.6 grams in the glaserite, stirred 45 minutes down at 32 ℃, separate 376.6 gram vitriolate of tartar and 1037.8 gram potassium sulfate mother liquids.
Embodiment 2:
The Chemical Composition of the various materials of embodiment 2 is listed in the table 2, and salt-making mother liquor is from sal prunella factory of Salt Chemical General Plant, Jianghan Petroleum administration Bureau evaporation unit mother liquor that EV-304 discharges, and composition sees Table 2.
Restrain the salt mother liquor with 12200 and naturally cool to 35 ℃, stir, put into an enamel basin and force freezing 4.5 hours at refrigeration chamber, when liquidus temperature reaches-9.5 ℃, stop freezingly, be placed on freezing indoor heat insulating sedimentation and take out after 1.5 hours, pour out clear liquor rapidly, and carry out solid-liquid separation, and its liquid phase weight is 10803 grams, solid phase weight is 1397.0 grams.
The potassium sulfate mother liquid (35 ℃ of temperature) that adds the artificial preparation of 1565.0 grams in the enamel basin of clear liquor toward inclining, the nitre, the potassium mixture that add the artificial preparation of 217.9 grams simultaneously, under continuously stirring, carry out one section conversion, temperature is 30 ℃, transform and carry out solid-liquid separation after 1.5 hours, get 1325.8 gram glaserites and 1854.1 gram glaserite mother liquors.
The glaserite mother liquor is placed on forces freezing 2.5 hours in refrigeration chamber in another enamel basin, temperature is-10 ℃, carries out solid-liquid separation then, gets nitre, potassium mixture 217.9 grams, clear liquor 1636.2 grams.
Add 596.6 gram Repone K in the glaserite, 380.0 gram water stirred 1 hour down at 35 ℃, after the separation 734.9 gram vitriolate of tartar and 1567.5 gram potassium sulfate mother liquids.
Embodiment 3:
The various material Chemical Composition of embodiment 3 are listed in the table 3, and saltcake ore deposit bittern is from Jianghan Oil-field saltcake ore deposit.Form and see Table 3
With 13000 gram saltcake ore deposit bittern, put into an enamel basin and force freezing 1 hour at refrigeration chamber, when liquidus temperature reaches 10 ℃, stop freezingly, the insulation sedimentation was taken out after 0.5 hour, and inclining rapidly clear liquor and carries out solid-liquid separation.Its liquid phase weight is 7984.5 grams, and solid phase weighs 5015.5 grams.
The potassium sulfate mother liquid (35 ℃ of temperature) that adds the artificial preparation of 5600 grams in the enamel basin after the clear liquor toward inclining, add 668 gram nitre, potassium mixture simultaneously, under agitation carry out one section conversion, temperature is 30 ℃, transform and carry out solid-liquid separation after 3 hours, get 4709.3 gram glaserites and 6574.2 gram glaserite mother liquors.
The glaserite mother liquor is placed on forces freezing 4 hours in refrigeration chamber in another enamel basin, temperature is-10 ℃, carries out solid-liquid separation then, gets nitre potassium mixture 668 grams, clear liquor 5906.2 grams.
Add 2200.8 gram Repone K and 1438.9 gram water in the glaserite, stirred 2 hours down at 35 ℃, separate 2745.0 gram vitriolate of tartar and 5604.0 gram potassium sulfate mother liquids.
By embodiment 1 and embodiment 2 and embodiment 3 as can be seen, the present invention can directly make qualified vitriolate of tartar with sodium sulfate (calcium) type bittern or salt manufacturing (nitre) mother liquor or saltcake ore deposit bittern and Repone K (state quality standard of vitriolate of tartar is for containing K
2O 〉=50%).Present embodiment 1 and embodiment 2 and embodiment 3 gained vitriolate of tartar contain K
2O is respectively: 50.22%, 50.27%, 50.33%.The present invention can attached product SO in producing potassium sulfate process
2- 4The purified brine of content below 5g/l is qualified salt manufacturing (alkali) bittern.The yield of potassium reaches 94% among the embodiment 1, and the yield of potassium reaches 98.0% among the embodiment 2, and the yield of potassium reaches 99% among the embodiment 3.This produces potassium sulfate process than domestic existing bittern and is generally the 60-70% height.The present invention does not add any medicament in whole technology, product and environment are not exerted an influence, and does not have any " three wastes " discharging yet, therefore has important social benefit and economic benefit.
Various materials are formed (%/W) among table 1 embodiment 1
| The chemical constitution name of material | K + | Na + | SO 2- 4 | Cl - | H 2O | |
| Raw material | Bittern | - | 10.36 | 1.98 | 14.52 | 73.14 |
| Repone K | 52.20 | - | - | 47.30 | 0.50 | |
| Product | Vitriolate of tartar | 41.69 | - | 51.30 | - | 7.01 |
| Intermediate material | Ten water nitre | 14.25 | 24.66 | 8.28 | 52.83 | |
| Glaserite | 8.96 | 9.89 | 27.74 | 4.67 | 48.74 | |
| The glaserite mother liquor | 3.36 | 10.39 | 2.53 | 13.62 | 70.10 | |
| Nitre, potassium mixture | 22.66 | 12.38 | 20.07 | 3.50 | 41.39 | |
| Potassium sulfate mother liquid (input) | 7.10 | 6.80 | 0.55 | 17.70 | 67.85 | |
| Potassium sulfate mother liquid (output) | 7.13 | 6.81 | 0.55 | 17.73 | 67.78 | |
Various materials are formed (%/W) among table 2 embodiment 2
| The chemical ingredients name of material | K + | Na + | SO 2- 4 | Cl - | H 2O | |
| Raw material | Salt-making mother liquor | - | 11.18 | 3.49 | 14.67 | 70.66 |
| Repone K | 52.20 | - | - | 47.30 | 0.50 | |
| Product | Vitriolate of tartar | 41.69 | - | 51.36 | - | 6.95 |
| Intermediate material | Ten water nitre | - | 15.52 | 27.59 | 3.56 | 53.33 |
| Glaserite | 8.06 | 15.82 | 29.37 | 0.35 | 46.4 | |
| The glaserite mother liquor | 4.82 | 5.23 | 2.09 | 21.14 | 66.72 | |
| Nitre, potassium mixture | 38.69 | 2.94 | 15.28 | 28.04 | 15.05 | |
| Potassium sulfate mother liquid (input) | 7.18 | 8.35 | 0.617 | 18.21 | 65.65 | |
| Potassium sulfate mother liquid (output) | 7.20 | 8.36 | 0.61 | 18.24 | 65.59 | |
Various materials are formed (%/W) among table 3 embodiment 3
| The chemical ingredients name of material | K + | Na + | SO 2- 4 | Cl - | H 2O | |
| Raw material | Saltcake ore deposit bittern | - | 9.05 | 11.18 | 5.69 | 74.08 |
| Repone K | 52.20 | - | - | 47.30 | 0.50 | |
| Product | Vitriolate of tartar | 41.78 | - | 51.45 | - | 6.83 |
| Intermediate material | Ten water nitre | - | 5.04 | 28.44 | 0.37 | 66.14 |
| Glaserite | 8.00 | 16.55 | 30.89 | 5.03 | 39.53 | |
| The glaserite mother liquor | 1.41 | 5.20 | 2.12 | 18.66 | 72.61 | |
| Nitre, potassium mixture | 13.55 | 13.37 | 17.89 | 24.51 | 30.68 | |
| Potassium sulfate mother liquid (input) | 5.74 | 13.90 | 0.81 | 22.82 | 56.73 | |
| Potassium sulfate mother liquid (output) | 6.76 | 13.90 | 0.81 | 22.86 | 55.67 | |
Claims (3)
1. produce the method for vitriolate of tartar with sal prunella type bittern for one kind, it is characterized in that its technical process is: sodium sulphate type bittern or salt-making mother liquor or saltcake ore deposit bittern are passed through NaOH-Na
2CO
3Method purifies, and removes wherein Ca
2+, Mg
2+Impurity, after purified brine is frozen 10～-20 ℃, sodium sulfate reduces with temperature, its solubleness descends and separates out sal glauberi, having part sodium-chlor to follow simultaneously separates out, analysing behind the nitre bittern can send to and carry out the multiple-effect vacuum salt, rear stock solution of salt producing can return through purifying capable frozen saltpeter mention again, the sal glauberi of separating out and the mixture of small amounts of salts are sent into one section conversion reactor, return molten and add a small amount of Repone K by potassium sulfate mother liquid from two sections switching processes, get glaserite, the settlement separate back of glaserite adds two sections conversions of Repone K, gets the vitriolate of tartar solidliquid mixture, and this solid-liquid miscellany is separated, after the drying potassium product, bittern or the mother liquor contains sodium sulfate separated out behind the solid are 0.5-40g/l.
2. method according to claim 1 is characterized in that the condition that sal glauberi and potassium sulfate mother liquid are converted to glaserite is:
1. temperature 10-60 ℃; 2. proportioning: sal glauberi slurry: potassium sulfate mother liquid=1: 0.5-6; 3. be 0.5-10 hour switching time.
3. method according to claim 1 is characterized in that the conversion of glaserite and Repone K, water produces the condition of vitriolate of tartar and be:
1. temperature: 20-75 ℃; 2. proportioning: glaserite: Repone K: water=1: 0.3-1.0: 0.1-3.5; 3. switching time: 0.5-10 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94106765A CN1038496C (en) | 1994-06-18 | 1994-06-18 | Method for directly preparing Lemery salt by using salt-cake (gypsum) type bittern or mother liquid for preparing salt (saptpetre) or mirabilite mineral bittern |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94106765A CN1038496C (en) | 1994-06-18 | 1994-06-18 | Method for directly preparing Lemery salt by using salt-cake (gypsum) type bittern or mother liquid for preparing salt (saptpetre) or mirabilite mineral bittern |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1123248A CN1123248A (en) | 1996-05-29 |
| CN1038496C true CN1038496C (en) | 1998-05-27 |
Family
ID=5032651
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN94106765A Expired - Fee Related CN1038496C (en) | 1994-06-18 | 1994-06-18 | Method for directly preparing Lemery salt by using salt-cake (gypsum) type bittern or mother liquid for preparing salt (saptpetre) or mirabilite mineral bittern |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1038496C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102390847A (en) * | 2011-07-27 | 2012-03-28 | 陈海通 | Production method for preparing potassium sulfate by potassium chloride-sodium sulfate method |
| CN104261940B (en) * | 2014-09-24 | 2016-08-24 | 中国科学院青海盐湖研究所 | A kind of preparation method of potassic-magnesian fertilizer |
| CN105645440B (en) * | 2015-12-30 | 2018-02-23 | 中国中轻国际工程有限公司 | A kind of mirabilite hydrate produces sodium sulphate technique |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2573413A1 (en) * | 1984-11-21 | 1986-05-23 | Alsace Mines Potasse | Process for the preparation of potassium sulphate, which can be used especially in fertilizers, from brines containing sulphate and potassium ions |
| SU1557102A1 (en) * | 1988-05-25 | 1990-04-15 | Всесоюзный научно-исследовательский и проектный институт галургии | Method of obtaining potassium sulfate |
| CN1077434A (en) * | 1993-05-14 | 1993-10-20 | 中国石油天然气总公司工程技术研究所 | A kind of method of producing vitriolate of tartar with bittern and Repone K |
-
1994
- 1994-06-18 CN CN94106765A patent/CN1038496C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2573413A1 (en) * | 1984-11-21 | 1986-05-23 | Alsace Mines Potasse | Process for the preparation of potassium sulphate, which can be used especially in fertilizers, from brines containing sulphate and potassium ions |
| SU1557102A1 (en) * | 1988-05-25 | 1990-04-15 | Всесоюзный научно-исследовательский и проектный институт галургии | Method of obtaining potassium sulfate |
| CN1077434A (en) * | 1993-05-14 | 1993-10-20 | 中国石油天然气总公司工程技术研究所 | A kind of method of producing vitriolate of tartar with bittern and Repone K |
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|---|---|
| CN1123248A (en) | 1996-05-29 |
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