SU172295A1 - METHOD OF OBTAINING CLEAN BUTANDIOL-1,4 - Google Patents
METHOD OF OBTAINING CLEAN BUTANDIOL-1,4Info
- Publication number
- SU172295A1 SU172295A1 SU909268A SU909268A SU172295A1 SU 172295 A1 SU172295 A1 SU 172295A1 SU 909268 A SU909268 A SU 909268A SU 909268 A SU909268 A SU 909268A SU 172295 A1 SU172295 A1 SU 172295A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- butandiol
- obtaining clean
- pure
- product
- hydrogen peroxide
- Prior art date
Links
- MHAJPDPJQMAIIY-UHFFFAOYSA-N hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- WERYXYBDKMZEQL-UHFFFAOYSA-N 1,4-Butanediol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- CSNNHWWHGAXBCP-UHFFFAOYSA-L mgso4 Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- -1 1-butylboron cyclopentane Chemical compound 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative Effects 0.000 description 1
- 229940072033 potash Drugs 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Description
Изобретение касаетс способа получени 1истого бутандиола-1,4 окислением борациклонентаиа или его производных.The invention concerns a process for the preparation of a pure butanediol-1,4 by oxidation of boracyclonenthenium or its derivatives.
Известен способ получени бутапдиола-1,4 гидрированием бутаидиола-1,4. Процесс осуществл ют при температуре и давлении 4 ат. Выход продукта с т. пл. 19,9°С 85 /оПредложенный способ отличаетс от известного тем, что бутаидиол-1,4 получают окислением борациклопентана или его производных перекисью водорода в щелочной среде при температуре от -5 до . Получают хроматографически чистый продукт с выходом 82-85о/о.A known method for producing butadiol-1.4 is by hydrogenation of butadiol-1.4. The process is carried out at a temperature and pressure of 4 at. The product yield with so pl. 19.9 ° C 85 / about. The proposed method differs from the well-known one in that butaidiol-1,4 is produced by oxidizing borocyclopentane or its derivatives with hydrogen peroxide in an alkaline medium at a temperature of from -5 to. A chromatographically pure product is obtained with a yield of 82-85 ° / o.
Способ позвол ет выделить более чистый продукт по сравнению с продуктом, получаемым известным методом.The method makes it possible to isolate a more pure product in comparison with the product obtained by a known method.
Пример 1. В четырехгорлую колбу, снабжепную мешалкой, термометром, капельной воронкой и обратным холодильником, предварительно продутую азотом, помещают 18,1 г 1-метоксиборациклонентана. При перемешивании в колбу приливают 66 мл 3 М раствор едкого натра, а затем 48 мл ЗОэ/о-ной перекиси водорода, поддержива при этом температуру реакционной среды от -5 до -|-5°С. Затем смесь оставл ют на 15 час нри комнатной температуре дл окончани реакции. Дл Example 1. In a four-necked flask, supplied with a stirrer, thermometer, addition funnel and reflux condenser, previously purged with nitrogen, 18.1 g of 1-methoxy-cyclocyclonentane are placed. While stirring, 66 ml of 3 M sodium hydroxide solution is poured into the flask, and then 48 ml of SOE / o-th hydrogen peroxide, while maintaining the temperature of the reaction medium from -5 to -5 ° C. The mixture is then allowed to stand at room temperature for 15 hours at the end of the reaction. For
выделени диолов смесь насыщают поташом и экстрагируют тетрагидрофураном (3 раза но 50 .ил). Экстракт сушат безводным сернокислым магнием, растворитель отгон ют, а бутандиол-1,4 перегон ют.the selection of diols is saturated with potash and extracted with tetrahydrofuran (3 times but 50.il). The extract is dried with anhydrous magnesium sulphate, the solvent is distilled off, and 1.4-butanediol is distilled.
Получают 13,7 г (85i/o) бутандиола-1,4 с т. кип. 87-88 С (2 .ил рт. ст.). По данным хроматографического анализа продукт представл ет собой ЧИСТЫ бутандиол-1,4.13.7 g (85i / o) of 1.4-butanediol are obtained with a t. Bale. 87-88 C (2 .yl. Hg. Art.). According to the chromatographic analysis, the product is PURE butanediol-1,4.
Пример 2. Из 16 г 1-хлорборациклопентана , 100 мл 3 М раствора едкого натра и 37 мл 308/o-Hoii перекиси водорода по вышеописанной методике получают 11,5 г (82-Vo) чистого бутандиола-1,4.Example 2. From 16 g of 1-chloro-cyclocyclopentane, 100 ml of 3 M sodium hydroxide solution and 37 ml of 308 / o-Hoii hydrogen peroxide using the above method, 11.5 g (82-Vo) of pure 1,4-butanedol are obtained.
Пример 3. Из 12 г 1-бутилбораииклопентана , 33 мл ЗМ раствора едкого натра и 36 мл ЗОо/о-ной перекиси водорода по вышеописанной методике получают 7,4 г () чистого бутандиола-1,4.Example 3. From 12 g of 1-butylboron cyclopentane, 33 ml of ZM caustic soda solution and 36 ml of ZOO / o-hydrogen peroxide using the procedure described above, 7.4 g () of pure 1,4-butanedol are obtained.
И р е д м е т и з о б р е т е и и And redemt and z obrete and and
Способ получени чистого бутандиола-1,4, отличающийс тем, что, с целью упрощени процесса и повышени качества продукта, борациклопентан или его производные обрабатывают перекисью водорода в щелочпой среде при температуре от -5 до .A method of obtaining pure butanediol-1,4, characterized in that, in order to simplify the process and improve the quality of the product, boracyclopentane or its derivatives are treated with hydrogen peroxide in alkaline medium at a temperature of from -5 to.
колонка строканапечатаноследует читатьthe line column is printed follow
174 ат.5 ат.174 at.5 at.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU172295A1 true SU172295A1 (en) |
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