CN114380662A - Method for preparing absolute ethanol from ethanol-water azeotrope by adopting dissolved salt extraction rectification mode - Google Patents
Method for preparing absolute ethanol from ethanol-water azeotrope by adopting dissolved salt extraction rectification mode Download PDFInfo
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- CN114380662A CN114380662A CN202011129310.5A CN202011129310A CN114380662A CN 114380662 A CN114380662 A CN 114380662A CN 202011129310 A CN202011129310 A CN 202011129310A CN 114380662 A CN114380662 A CN 114380662A
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- ethanol
- ethyl alcohol
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- extracting
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 238000000605 extraction Methods 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 16
- 150000003839 salts Chemical class 0.000 title claims abstract description 11
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 title claims abstract description 9
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 claims abstract description 38
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 21
- 235000019441 ethanol Nutrition 0.000 claims abstract description 20
- 235000011056 potassium acetate Nutrition 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 238000010992 reflux Methods 0.000 claims abstract description 6
- 238000000895 extractive distillation Methods 0.000 claims abstract description 5
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims 1
- 229910001220 stainless steel Inorganic materials 0.000 claims 1
- 238000000926 separation method Methods 0.000 abstract description 14
- 239000002994 raw material Substances 0.000 abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract 1
- 230000018044 dehydration Effects 0.000 abstract 1
- 238000006297 dehydration reaction Methods 0.000 abstract 1
- 229910052700 potassium Inorganic materials 0.000 abstract 1
- 239000011591 potassium Substances 0.000 abstract 1
- 238000004821 distillation Methods 0.000 description 5
- 238000004817 gas chromatography Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 230000036571 hydration Effects 0.000 description 4
- 238000006703 hydration reaction Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000000855 fermentation Methods 0.000 description 3
- 230000004151 fermentation Effects 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000002572 peristaltic effect Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 244000151018 Maranta arundinacea Species 0.000 description 1
- 235000010804 Maranta arundinacea Nutrition 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 235000012419 Thalia geniculata Nutrition 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 238000010533 azeotropic distillation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 description 1
- 239000001639 calcium acetate Substances 0.000 description 1
- 235000011092 calcium acetate Nutrition 0.000 description 1
- 229960005147 calcium acetate Drugs 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 235000019439 ethyl acetate Nutrition 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000002816 fuel additive Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
- C07C29/84—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation
Abstract
The invention belongs to the field of separation engineering of acetic acid preparation from synthesis gas and absolute ethyl alcohol preparation from hydrogenation, and relates to a method for separating an ethyl alcohol-water azeotrope in a hydrogenation product by a dissolved salt extraction rectification method. The rectifying tower for extractive distillation and separation consists of three sections, namely a rectifying section, an extracting section and a stripping section. An extractant feeding hole is arranged between the rectifying section and the extracting section; a raw material feeding hole is arranged between the extraction section and the stripping section. The raw material feeding composition of the tower is a solution (ethanol content is 95% by weight) formed by ethanol-water azeotropy, and the extracting agent feeding composition is (5-20% by weight) potassium acetate- (90-95% by weight) ethanol. When the feeding amount of the extracting agent is 12mL/min, the volume ratio of the extracting agent to the raw material is 1: 1-3: 1, and the reflux ratio is 1: 1-1: 3, more than 99.8 wt% of absolute ethyl alcohol can be extracted from the top of the tower, and the extraction amount is about 20 mL/min; the tower bottom is a potassium acetate solution diluted by separating residual water, and the potassium acetate solution can be recycled after negative pressure dehydration. The method for extracting and rectifying the dissolved salt realizes the separation of the ethanol-water near azeotrope system to obtain the absolute ethanol, simplifies the separation process of the system, reduces the separation difficulty, and saves the equipment investment and the operation cost.
Description
Technical Field
The invention belongs to the field of separation engineering for preparing absolute ethyl alcohol by separating hydrous ethyl alcohol, and relates to a refining separation method for preparing a mixed product for producing ethyl alcohol by acetic acid hydrogenation by using synthesis gas.
Background
The fuel ethanol is a clean fuel additive which is widely popularized in China at the present stage. The main production routes of ethanol at home and abroad are divided into three routes, namely a biological fermentation route, an ethylene hydration route and a synthesis gas route. The raw materials of the biological fermentation route mainly comprise crops such as corn, arrowroot and wheat, and are sometimes restricted by a series of non-resistant factors, and if the yield of grains is reduced due to weather factors, the raw material supply is inevitably impacted, and the problem of competing for grains with people is very easily caused. The ethylene hydration route is divided into an indirect hydration method and a direct hydration method, and is suitable for countries or regions with rich petroleum resources. The synthetic gas route comprises a novel synthetic gas fermentation method, a method for preparing ethanol by hydrogenating acetic acid or acetic ester from synthetic gas, a method for preparing ethanol by hydrogenating the synthetic gas through methanol, dimethyl ether and methyl acetate, a method for directly preparing the ethanol from the synthetic gas, and the like, wherein the method for preparing the ethanol from the synthetic gas through hydrogenating the acetic acid meets the energy framework of 'rich coal and less oil' in China, can meet the market demand of fuel ethanol, and is also beneficial to relieving the current situation of surplus acetic acid production capacity in China.
The main products of ethanol preparation by acetic acid hydrogenation are ethanol and water, and a binary azeotrope of 4.4 wt% water and 95.6 wt% ethanol (normal pressure boiling point 78.17 ℃) exists between the ethanol and the water. The ordinary distillation operation can not separate azeotrope, the extraction distillation and azeotropic distillation separation azeotrope system is usually adopted in industry, the salt-dissolving extraction distillation is a novel special distillation separation mode, the salt substance is added into the system to change the relative volatility among the components and eliminate the azeotropic point, the solvent ratio is low, the energy consumption is low, the salt can not be mixed into the light component on the top of the tower, the dissolved salt is widely adopted as a green environment-friendly extractant in recent years, and the research value in the azeotrope separation aspect is very high. Regarding the rectification separation of the dissolved salt of the alcohol-water system, the soluble salt extracting agents such as sodium chloride, calcium chloride, magnesium chloride, potassium acetate and the like are usually selected, and in consideration of the corrosion problem of chloride ions in calcium chloride and the like to equipment, the invention selects potassium acetate, sodium acetate, calcium acetate and the like as the extracting agents to separate and refine the absolute ethyl alcohol.
Disclosure of Invention
The invention adopts a set of glass material extractive distillation tower which is designed and processed by self to separate the ethanol-water azeotrope. The rectifying tower has an inner diameter of 30mm and an outer diameter of 45mm, belongs to a packed tower, is internally provided with a Fenske packing, is a triangular spiral formed by winding a metal wire, has the specification of phi 1.5 multiplied by 1.5, is divided into a rectifying section, an extracting section and a stripping section, has effective heights of 0.75m, is provided with a condensing head of an electromagnetic valve reflux ratio controller at the top of the tower, and adopts a four-mouth flask with the volume of 1000mL as a tower kettle. An extractant feeding hole with a temperature measuring port is arranged between the rectifying section and the extracting section; a raw material feeding hole with a temperature measuring hole is arranged between the extraction section and the stripping section. The method adopts absolute ethyl alcohol with potassium acetate as an extracting agent, feeds the material from a feed inlet of the extracting agent, obtains the absolute ethyl alcohol at the top of an extraction rectifying tower, and simultaneously recovers the potassium acetate at a tower kettle.
Drawings
Figure 1 ethanol-water azeotrope salt-dissolving extraction rectification separation tower
In FIG. 1, 6-Mercury thermometer; 2 glass condenser with electromagnetic valve reflux ratio control; 3-a glass packed column; 4. 5-a feed pump; 7, a storage tank; 8-four-neck flask; 9-glass condenser; 10-an electric heating jacket; a-an extractant feed port; b, a raw material feeding hole; c, a tower top extraction port; d, a tower kettle extraction outlet.
The technical solution of the invention is as follows:
dissolving potassium acetate in absolute ethyl alcohol to serve as a salt-dissolving extracting agent (the mass concentration of the potassium acetate is 5-20 wt.%), storing the salt-dissolving extracting agent in a feeding bottle, metering the salt-dissolving extracting agent by a metering pump (4), pumping the salt-dissolving extracting agent to the feeding side of an extraction rectifying tower, and feeding the salt-dissolving extracting agent from a tower section position (A) of the feeding tower; 95 wt% azeotropic ethanol-water is used as a raw material and stored in a feeding bottle, and is metered by a metering pump (5) and then pumped to the feeding side of the extractive distillation tower, and enters from the tower section position (B) of the feeding tower.
Discharging absolute ethyl alcohol (normal pressure boiling point is 78.2 ℃) from the tower top (C), and recycling a part of products as an entrainer of potassium acetate for circular feeding; the discharge of the tower bottom (D) is diluted potassium acetate aqueous solution.
And thirdly, refining and separating the absolute ethyl alcohol in the extraction rectifying tower through the treatment of the first step and the treatment of the second step.
The invention is characterized in that:
the dissolved salt extractive distillation takes the absolute ethyl alcohol as an entrainer of the potassium acetate, other vapor-liquid phase components are not introduced, and the potassium acetate is difficult to be mixed into light components on the top of the tower through distillation, so that the separation difficulty is reduced, the equipment investment and the operation cost are saved, and the separation and refining cost of the absolute ethyl alcohol is reduced.
Detailed Description
Example 1
500mL of 95% wt. ethanol is added into a tower kettle (8), a small amount of zeolite is added to prevent bumping in the experimental process, 5L of an extracting agent (10% wt. potassium acetate in absolute ethanol) and 5L of a raw material (95% wt. ethanol) are respectively prepared and put into two sealed polytetrafluoroethylene barrels, and are respectively connected with an extracting agent feeding port (A) and a raw material feeding port (B) in the graph 1 through peristaltic pumps (4, 5). And opening the freezing thermostatic bath and the advection pump, and enabling the ethylene glycol refrigerating fluid to circularly flow in the upper and lower condensers (2,9) of the rectifying tower, wherein the temperature of the freezing thermostatic bath is set to be 1 ℃ so as to ensure the refrigerating effect. And opening the electric heating sleeve (10), starting the peristaltic pumps (4,5) after the tower top has reflux, feeding the extracting agent feed port (A) and the raw material feed port (B) according to the feeding ratio of 1:1, wherein the feeding flow of the extracting agent is 12 mL/min. Opening a top discharge electromagnetic valve switch, setting a reflux ratio to be 1:1, discharging from a top extraction outlet (C), and performing gas chromatography analysis to obtain 99.82 wt% of absolute ethyl alcohol from the top of the tower, wherein the extraction flow is about 20mL/min, and meanwhile, recycling part of the absolute ethyl alcohol (about 50% of volume) as an entrainer of the potassium acetate.
Example 2
Experimental setup and operating conditions example 1 was carried out, except that the extractant was replaced with a 15% wt. solution of potassium acetate in anhydrous ethanol, and gas chromatography: the content of absolute ethyl alcohol extracted from the tower top is 99.81 wt.%.
Example 3
Experimental setup and operating conditions as in example 1, except that the extractant was replaced with a 20% wt. solution of potassium acetate in anhydrous ethanol, gas chromatography analysis showed: the content of absolute ethyl alcohol extracted from the tower top is 99.80 percent by weight.
Example 4
Experimental setup and operating conditions example 1 was carried out, except that the extractant was replaced with a 5% wt. solution of potassium acetate in anhydrous ethanol, and gas chromatography: the content of absolute ethyl alcohol extracted from the tower top is 99.14 percent by weight.
Claims (3)
1. The invention belongs to the field of engineering for preparing absolute ethyl alcohol from hydrous ethyl alcohol, and relates to a method for preparing absolute ethyl alcohol by using synthetic gas to prepare a mixed product of ethyl alcohol produced by acetic acid hydrogenation, namely an azeotrope formed by ethyl alcohol and water, using potassium acetate as an extracting agent, and separating the mixed product by adopting a dissolved salt extraction rectification method.
2. The salt-dissolving extractant of claim 1 which is an aqueous solution of 5 to 20% by weight potassium acetate and 95 to 99.5% by weight ethanol.
3. The extractive distillation column of claim 1, which comprises a rectifying section, an extracting section and a stripping section, wherein the column is filled with a Fenske stainless steel wire triangular spiral high-efficiency filler, an extractant feeding port is arranged between the rectifying section and the extracting section, and an ethanol-water azeotrope feeding port is arranged between the stripping section and the extracting section; the operation conditions of the tower are that the volume ratio of the feeding of the extracting agent to the feeding of the azeotropic material is 1: 1-3: 1, when the reflux ratio is 1: 1-1: 3, more than 99.8 wt% of absolute ethyl alcohol can be extracted from the top of the tower, and the extraction amount is 50% of the feeding amount; the operation is carried out under the condition, and the content of the discharged material at the top of the tower is 99.82 percent by weight of absolute ethyl alcohol measured by a gas chromatograph.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011129310.5A CN114380662A (en) | 2020-10-21 | 2020-10-21 | Method for preparing absolute ethanol from ethanol-water azeotrope by adopting dissolved salt extraction rectification mode |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011129310.5A CN114380662A (en) | 2020-10-21 | 2020-10-21 | Method for preparing absolute ethanol from ethanol-water azeotrope by adopting dissolved salt extraction rectification mode |
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| Publication Number | Publication Date |
|---|---|
| CN114380662A true CN114380662A (en) | 2022-04-22 |
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| CN202011129310.5A Pending CN114380662A (en) | 2020-10-21 | 2020-10-21 | Method for preparing absolute ethanol from ethanol-water azeotrope by adopting dissolved salt extraction rectification mode |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1887834A (en) * | 2006-07-19 | 2007-01-03 | 江苏工业学院 | Bulkhead rectifying tower method and apparatus for extracting, rectifying and separating tert-butyl alcohol from water |
| JP2007332077A (en) * | 2006-06-15 | 2007-12-27 | Chuo Kakoki Kk | Method for distilling ethanol |
| CN102633597A (en) * | 2012-03-22 | 2012-08-15 | 河北工业大学 | Process of recovering ethanol, propyl alcohol and isobutyl alcohol from polyalcohol-water mixture |
| CN103613485A (en) * | 2013-12-09 | 2014-03-05 | 北京化工大学 | Method for extracting, distilling and separating alcohol-water solution through ethylene glycol and ionic liquid |
-
2020
- 2020-10-21 CN CN202011129310.5A patent/CN114380662A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007332077A (en) * | 2006-06-15 | 2007-12-27 | Chuo Kakoki Kk | Method for distilling ethanol |
| CN1887834A (en) * | 2006-07-19 | 2007-01-03 | 江苏工业学院 | Bulkhead rectifying tower method and apparatus for extracting, rectifying and separating tert-butyl alcohol from water |
| CN102633597A (en) * | 2012-03-22 | 2012-08-15 | 河北工业大学 | Process of recovering ethanol, propyl alcohol and isobutyl alcohol from polyalcohol-water mixture |
| CN103613485A (en) * | 2013-12-09 | 2014-03-05 | 北京化工大学 | Method for extracting, distilling and separating alcohol-water solution through ethylene glycol and ionic liquid |
Non-Patent Citations (5)
| Title |
|---|
| ROGER A. COOK等: "Extractive Distillation Employing a Dissolved Salt as Separating Agent", THE CANADIAN JOURNAL OF CHEMICAL ENGINEERING, vol. 46, pages 119 - 123 * |
| 方凯等: "利用溶盐精馏法分离乙醇-水体系的研究", 河南化工, vol. 30, no. 10, pages 24 - 26 * |
| 杨亚鸣等: "加盐萃取精馏分离乙醇-水体系的研究进展", 河南化工, vol. 31, no. 10, pages 21 - 23 * |
| 王成林等: "工业化制备无水乙醇的研究进展", 河南化工, vol. 30, no. 2, pages 21 - 23 * |
| 王洪海等: "加盐萃取精馏制取无水乙醇过程的模拟", 石油化工, vol. 37, no. 3, pages 258 - 261 * |
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