SU256780A1 - METHOD OF DRYING DIOXANE - Google Patents
METHOD OF DRYING DIOXANEInfo
- Publication number
- SU256780A1 SU256780A1 SU1261545A SU1261545A SU256780A1 SU 256780 A1 SU256780 A1 SU 256780A1 SU 1261545 A SU1261545 A SU 1261545A SU 1261545 A SU1261545 A SU 1261545A SU 256780 A1 SU256780 A1 SU 256780A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- dioxane
- water
- benzene
- azeotrope
- drying
- Prior art date
Links
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 title description 16
- 238000001035 drying Methods 0.000 title description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N acetic acid ethyl ester Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 238000010992 reflux Methods 0.000 description 3
- RNHDAKUGFHSZEV-UHFFFAOYSA-N 1,4-dioxane;hydrate Chemical compound O.C1COCCO1 RNHDAKUGFHSZEV-UHFFFAOYSA-N 0.000 description 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N Diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 2
- 238000010533 azeotropic distillation Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- -1 for example Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000002194 synthesizing Effects 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- LZLOFGMGFADIKQ-UHFFFAOYSA-N benzene;1,4-dioxane Chemical compound C1COCCO1.C1=CC=CC=C1 LZLOFGMGFADIKQ-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000002012 dioxanes Chemical class 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Description
Известен способ осушки диоксана, заключающийс в том, что полученный пз диэтиленгликол обводненный дноксан обрабатывают хлоридами металлов и раздел ют жидкие фазы , образующиес при высаливании в три фракции: диоксан, азеотроп и вода с возвращением азеотрона в процесс.The known method of drying dioxane, which consists in the fact that the obtained diethyleneglycol hydrated dnoxane is treated with metal chlorides and the liquid phases formed during the salting out in three fractions: dioxane, azeotrope and water are separated and the azeotron is returned to the process.
С целью упрощени процесса и получени продукта высокой степени чистоты, предлагаетс способ осушки диоксана, заключающийс в том, что полученный в процессе синтеза обводненный диоксан подвергают азеотропной ректификации с органическим веществом , например, бензолом, образующим расслаивающийс азеотроп с водой, имеющий температуру кипени ниже температуры кипени азеотропа диоксан - вода, и не образующий азеотропа с диоксаном и тройного азеотропа с диоксаном и водой.In order to simplify the process and produce a product of high purity, a method of drying dioxane is proposed, which consists in that the watered dioxane obtained in the synthesis process is subjected to azeotropic distillation with organic matter, for example, benzene, which forms a stratifying azeotrope with water, having a boiling point below boiling point Azeotrope dioxane - water, and not forming an azeotrope with dioxane and a triple azeotrope with dioxane and water.
Пример 1. На непрерывно действующую колонну с числом теоретических тарелок 11 подают 714 г обводненного диоксана (30 вес. % воды) и 2212 г бензола. Разгонку ведут в следующем режиме:Example 1. On a continuously operating column with the number of theoretical plates 11, 714 g of watered dioxane (30 wt.% Of water) and 2212 g of benzene are fed. Distillation is carried out in the following mode:
ДавлениеАтмосферноеPressure Atmospheric
Флегмовое число3Reflux number3
Температура, °С:Temperature, ° С:
Получено 2380 г дистиллата состава, %:Received 2380 g of distillate composition,%:
2 8,62 8.6
диоксанdioxane
водаwater
бензол benzene
89,489.4
%: Получено 490%: Received 490
диоксана состава.dioxane composition.
99,8 99.8
диоксан 0,1 dioxane 0.1
водаwater
бензол 0,1benzene 0,1
Пример 2. На непрерывную колонну подают 2500 с обводненного диоксана (0,56 вес. % воды) и 145 г бензола. Релчим разгонки: Example 2. On a continuous column serves 2500 with water-saturated dioxane (0.56 wt.% Water) and 145 g of benzene. We wish to disperse:
Атмосферное ДавлениеAtmosphere pressure
Флегмовое число 3 Температура, °С:Reflux number 3 Temperature, ° C:
69 69
верха колонны 100column top 100
низа колонныbottom of the column
74 74
сырь дистиллата состава, %: Получено 155raw distillate composition,%: Received 155
водаwater
91,291.2
бензол диоксан benzene dioxane
отсутствует Получено 2475not received 2475
г кубового остатка состава .g VAT residue composition.
5five
водаwater
следы traces
бензол 0,147 99,853benzene 0.147 99.853
диоксан 3 Режим разгонки следующий: Давление Атмосферное Флегмовое число .3 Температура, °С: верха колонны 705 низа колонны 100 сырь 50 Получено 132 г дистиллата состава, %: вода 7,9 этилацетат 92,110 диоксан отсутствует Получено 2508 г кубового остатка состава , %: вода 0,017 4 диоксан 99,983 этилацетат отсутствует п Предмет изобретени Способ осушки диоксана путем азеотропной ректификации полученного в процессе синтеза обводненного диоксана, отличающийс тем, что, с целью упрощени процесса и получени целевого продукта высокой степени чистоты, в качестве азеотропного агента примен ют вещество , например, бензол, образующее расслаивающийс азеотроп с водой с температурой кипени , чем температура кипени азеотропа диоксан - вода.dioxane 3 Acceleration mode is as follows: Pressure Atmospheric Reflux Number .3 Temperature, ° С: top of column 705 and bottom of column 100 of raw material 50 132 g of distillate of composition were obtained,%: water 7.9 ethyl acetate 92.110 dioxane is absent 2508 g of vat residue is obtained,%: water 0.017 4 dioxane 99.983 ethyl acetate is absent p. Object of the Invention A method of drying dioxane by azeotropic distillation of the water-cooled dioxane obtained in the synthesis process, characterized in that, in order to simplify the process and to obtain the target product of high purity, Azeotropic agent is used substance, for example, benzene, forming a stratifying azeotrope with water with a boiling point than the boiling point of azeotrope dioxane - water.
-rV, ./ Jj-rV, ./jj
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU256780A1 true SU256780A1 (en) |
Family
ID=
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5817910A (en) * | 1996-06-28 | 1998-10-06 | Wellman, Inc. | Destroying 1,4-dioxane in byproduct streams formed during polyester synthesis |
| US6031065A (en) * | 1996-06-28 | 2000-02-29 | Wellman, Inc. | Polyester copolymers from naphthalate and related esters |
| US20130220935A1 (en) * | 2012-02-29 | 2013-08-29 | Eric G. Isacoff | Removal of 1,4-dioxane from water using carbonaceous adsorbents |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5817910A (en) * | 1996-06-28 | 1998-10-06 | Wellman, Inc. | Destroying 1,4-dioxane in byproduct streams formed during polyester synthesis |
| US6031065A (en) * | 1996-06-28 | 2000-02-29 | Wellman, Inc. | Polyester copolymers from naphthalate and related esters |
| US20130220935A1 (en) * | 2012-02-29 | 2013-08-29 | Eric G. Isacoff | Removal of 1,4-dioxane from water using carbonaceous adsorbents |
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