SU136387A1 - Method for isolating levoglucosane - Google Patents
Method for isolating levoglucosaneInfo
- Publication number
- SU136387A1 SU136387A1 SU663550A SU663550A SU136387A1 SU 136387 A1 SU136387 A1 SU 136387A1 SU 663550 A SU663550 A SU 663550A SU 663550 A SU663550 A SU 663550A SU 136387 A1 SU136387 A1 SU 136387A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- levoglucosane
- solution
- isolating
- soluble resin
- acetone
- Prior art date
Links
- 238000000034 method Methods 0.000 title description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- 229920005989 resin Polymers 0.000 description 7
- 239000011347 resin Substances 0.000 description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 3
- 238000001149 thermolysis Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 229920003986 novolac Polymers 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229940043430 calcium compound Drugs 0.000 description 1
- 150000001674 calcium compounds Chemical class 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- TWNIBLMWSKIRAT-VFUOTHLCSA-N levoglucosan Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@H]2CO[C@@H]1O2 TWNIBLMWSKIRAT-VFUOTHLCSA-N 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Compounds Of Unknown Constitution (AREA)
Description
Известен способ выделени левоглюкозана из растворимой смолы термолиза древесины, например, перегонкой с парами ртути, который по р ду причин в промышленности неприменим.A known method for isolating levoglucosane from a soluble resin of wood thermolysis, for example, by distillation with mercury vapor, which is not applicable in industry for a number of reasons.
В описываемом способе этот недостаток устранен, и он доступен дл применени в производственных услови х. При этом способе водорастворимую смолу экстрагируют эфиром, после удалени которого остаток обрабатывают известковым молоком, затем раствор разбавл ют ацетоном, фильтруют от выпавших в осадок солей новолаков пирокатехина и его гомологов и из фильтрата выкристаллизовывают левоглюкозан .In the method described, this disadvantage is eliminated, and it is available for use under production conditions. In this method, a water-soluble resin is extracted with ether, after removal of which the residue is treated with milk of lime, then the solution is diluted with acetone, filtered from precipitated salts of novolaks of pyrocatechin and its homologs, and left-glucosane is crystallized from the filtrate.
Процесс выделени кристаллического левоглюкозана из растворимой смолы термолиза древесины осуществл етс следующим образом.The process of separating crystalline levoglucosane from a soluble resin of wood thermolysis is carried out as follows.
Водный раствор смолы до или после извлечени ее эфиром, нейтрализуют известковым молоком до рН-12 и отдел ют раствор от нерастворимого углекислого кальци . Отделенный раствор упаривают до содержани 45-50% нелетучего остатка и разбавл ют упаренный раствор ацетоном или другим органическим растворителем. После этого отдел ют от раствора выпавшие в осадок кальциевые соединени , упаривают раствор и перекристаллизовывают сухой остаток из ацетона или другого органического растворител .The aqueous resin solution, before or after removing it with ether, is neutralized with lime milk to pH-12 and the solution is separated from insoluble calcium carbonate. The separated solution is evaporated to a content of 45-50% non-volatile residue and the stripped solution is diluted with acetone or another organic solvent. After that, the precipitated calcium compounds are separated from the solution, the solution is evaporated and the dry residue is recrystallized from acetone or another organic solvent.
Получаемый по этому способу левоглюкозан вл етс химически чистым продуктом, а его выход составл ет не менее 80% от его содержани в растворимой смоле.The levoglucosane obtained by this method is a chemically pure product, and its yield is at least 80% of its content in the soluble resin.
Выход может быть повышен дополнительной переработкой маточного раствора.The yield can be increased by additional processing of the mother liquor.
,П, изобрете и , P, invention and
Ч «vv , ;tH "vv,; t
СЖсоб SZhsob
тевоглркозана из растворимой смолы термолиза др сины/ сГ д толйи с тем, что водорастворимую смолу экстрагируют эфиром tevoglrkosan from a soluble resin of thermolysis of Dresin / cG d toli and the water-soluble resin is extracted with ether
, удалени которого . whose removal.
извест{4овым 1 | локоЯ| VaTeM; раствор разбавл ют ацетоном, фильтруют от вып авшил воСа оч солей новолаков пирокатехина н его гомологов и из фильтрэта вык)иста71лизовывают левоглюкозан.known {4th 1 | Loco | VaTeM; the solution is diluted with acetone, filtered from water from the salts of novolacs of pyrocatechol and its homologues, and levoglucosan is extracted from the filtrate.
остаток обрабатываютresidue treated
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU663550A SU136387A1 (en) | 1960-04-19 | 1960-04-19 | Method for isolating levoglucosane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU663550A SU136387A1 (en) | 1960-04-19 | 1960-04-19 | Method for isolating levoglucosane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU136387A1 true SU136387A1 (en) | 1960-11-30 |
Family
ID=48292669
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU663550A SU136387A1 (en) | 1960-04-19 | 1960-04-19 | Method for isolating levoglucosane |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU136387A1 (en) |
-
1960
- 1960-04-19 SU SU663550A patent/SU136387A1/en active
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