SU259903A1 - METHOD FOR OBTAINING A FURIOUS ALCOHOL - Google Patents
METHOD FOR OBTAINING A FURIOUS ALCOHOLInfo
- Publication number
- SU259903A1 SU259903A1 SU1088840A SU1088840A SU259903A1 SU 259903 A1 SU259903 A1 SU 259903A1 SU 1088840 A SU1088840 A SU 1088840A SU 1088840 A SU1088840 A SU 1088840A SU 259903 A1 SU259903 A1 SU 259903A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- alcohol
- furfural
- solution
- furious
- obtaining
- Prior art date
Links
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title description 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N Furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 9
- 239000000243 solution Substances 0.000 description 7
- XPFVYQJUAUNWIW-UHFFFAOYSA-N Furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N acetic acid ethyl ester Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 229910000497 Amalgam Inorganic materials 0.000 description 3
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L MgCl2 Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 229910001023 sodium amalgam Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229960000583 Acetic Acid Drugs 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 1
- 239000012259 ether extract Substances 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 230000001264 neutralization Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Description
Известен способ получени фурилового спирта восстановлением амальгамой натри фурфурола в нейтральной среде ири 18 - 20°С.A known method of producing furyl alcohol is the reduction of sodium furfural with amalgam in a neutral environment of 18 to 20 ° C.
С целью повышени выхода продукта, предложено восстанавливать фурфурол в разбавленном и подкисленном водном растворе.In order to increase the yield of the product, it has been proposed to restore furfural in diluted and acidified aqueous solution.
Пример. В плоскодонную широгорлую колбу (peaiKTOp) поместили 0,3 л амальгамы натри концентрацией 3,48 г шом/л. Из фурфурола d 1,1562; Пц 1,5234 приготовили 2%-ный раствор: 17,5 мл (20 г) фурфурола и 30 мл лед ной уксусной кислоты на 1 л воды. При посто нном леремеш вании механической мешалкой раствор подавали в реактор со скоростью 15 мл/мин, что составл ет 2250 мл/час фурфурола на 1 м поверхности амальгамы. После приливани всего раствора перемешивали еще 10 мин. Затем раствор фурилового спирта отделили от амальгамы. Концентраци фурфурола оказалась равной нулю, а концентраци фурнлового спирта 1,90%, что составл ет 92,5% от теоретического на исходный фурфурол . Раствор фурилового спирта подвергли трехкратной экстракции атилацетатом. Эфирную выт жку просушили прокаленным хлористым магнием, отогнали растворитель при атмосферном давлении, а остаток в колбе - при 42 - 43°С/1,5 - 2 мм рт. ст. Получили 16,78 г фурилового спирта. В колбе осталс небольшой осадок, не растворимый в воде.Example. In a flat-bottomed shirokorly flask (peaiKTOp) was placed 0.3 l of sodium amalgam with a concentration of 3.48 g shoom / l. From furfural d 1,1562; Pts 1.5234 prepared a 2% solution: 17.5 ml (20 g) of furfural and 30 ml of glacial acetic acid per liter of water. With a constant mechanical stirring, the solution was fed into the reactor at a rate of 15 ml / min, which amounts to 2250 ml / hour of furfural per meter of amalgam surface. After the solution was added, the whole solution was stirred for another 10 minutes. Then the solution of furyl alcohol was separated from the amalgam. The furfural concentration turned out to be zero, and the concentration of furl alcohol 1.90%, which is 92.5% of the theoretical on the initial furfural. The solution of furyl alcohol was subjected to triple extraction with ethyl acetate. The ether extract was dried with calcined magnesium chloride, the solvent was distilled off at atmospheric pressure, and the residue in the flask at 42–43 ° C / 1.5–2 mm Hg. Art. Received 16.78 g of furyl alcohol. A slight precipitate remained in the flask, insoluble in water.
После экстракции этилацетатом концентраци фурилового спирта в водном растворе составила 0,11%.After extraction with ethyl acetate, the concentration of furyl alcohol in the aqueous solution was 0.11%.
Предмет изобретени Subject invention
Способ получени фурилового спирта восстановлением фурфурола .в .водном pacTiBOipe с помощью амальгамы натри при температуре 20°С, отличающийс тем, что, с целью повыщени выхода, восстановлению подвергают разбавленный водой и подкисленный раствор фурфурола.The method of producing furyl alcohol by reducing furfural in aqueous pacTiBOipe using sodium amalgam at a temperature of 20 ° C, characterized in that, in order to increase the yield, the acidized solution of furfural is reconstituted.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU259903A1 true SU259903A1 (en) |
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