SU162523A1 - - Google Patents
Info
- Publication number
- SU162523A1 SU162523A1 SU784590A SU784590A SU162523A1 SU 162523 A1 SU162523 A1 SU 162523A1 SU 784590 A SU784590 A SU 784590A SU 784590 A SU784590 A SU 784590A SU 162523 A1 SU162523 A1 SU 162523A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- ethylene glycol
- dimethyl
- sulfate
- glycol
- flask
- Prior art date
Links
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Substances OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N methylene dichloride Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- VAYGXNSJCAHWJZ-UHFFFAOYSA-N Dimethyl sulfate Chemical compound COS(=O)(=O)OC VAYGXNSJCAHWJZ-UHFFFAOYSA-N 0.000 description 3
- -1 dimethyl sulfate sodium glycolate Chemical compound 0.000 description 2
- JZMJDSHXVKJFKW-UHFFFAOYSA-M methyl sulfate(1-) Chemical compound COS([O-])(=O)=O JZMJDSHXVKJFKW-UHFFFAOYSA-M 0.000 description 2
- 239000012429 reaction media Substances 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- XTHFKEDIFFGKHM-UHFFFAOYSA-N dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- QACCCIVMWADWMN-UHFFFAOYSA-N ethane-1,2-diol;methoxymethane Chemical compound COC.OCCO QACCCIVMWADWMN-UHFFFAOYSA-N 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000004922 lacquer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L na2so4 Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
Description
Диметиловый эфир этиленгликол в последние годы примен ют в качестве растворителей лаков и красок.Ethylene glycol dimethyl ether in recent years has been used as a solvent for varnishes and paints.
Известен способ получени дпметилового ыфира этиленгликол иутем 1 заимодейетви диметилсульфата гликол том натри в среде этилового спирта. Однако при таком способе получени процесс сопр жен с огиевзрывоопасиостью .A known method of producing ethylene glycol dimethyl acid and by means of 1 lender dimethyl sulfate sodium glycolate in ethyl alcohol. However, with this method of production, the process is associated with high explosiveness.
Предложенным сиособом диметидор.ьп эфир этилеигликол получают путем взаимодействи дн.мстилсульфата с гликол том патри в водно-пделочно среде при рМ 7-8.The proposed dimetidor ester is an ethylene glycol ester obtained by reacting one day of methyl sulfate with pathoxide glycol in a water-plating medium at pM 7-8.
Способ заключаетс в том, что пронесс ведут в колбе, спабженной .мешалкой, термометром , обратны.м холодильником и дву.м капельны .мн воронкамн. В колбу помещают раствор этиленгликол и SOo/o-Hbiii водно-щелочiioii раствор едкого натра и при 30-35 С постепенно добавл ют диметилсульфат, иоддержива рН реакционной Среды в предела.х 7 - 8.The method consists in the fact that the lead is carried in a flask, filled with a stirrer, a thermometer, a reciprocal of a refrigerator and a double drop of microscopic funnels. A solution of ethylene glycol and a water-alkali solution of ethylene glycol and SOo / o-Hbiii caustic soda is placed in a flask and dimethyl sulfate is gradually added at 30-35 ° C, keeping the pH of the reaction medium in the limit. 7-8.
Пример. В колбу, снабженную меи,1алкой , термометро.м, обратным холодильником и двум капельны.ми вороиками, по.мещаюг pacTiiOp 62 г эти.тенгликол (1 моль в 30 лг. ЗОэ/с-ного водного раствора едкого натра и при 30-35 С постепенно добавл ют 189 г диметилсульфата (1,5 моль), поддержива рП реакииониой среды 7 - - 8-иорциопиым прибавлением ЗОо/о-ного раствора щелочи (по 5 - 7 мл каждый раз).Example. In a flask equipped with mealy, lacquer, a thermometer, a reflux condenser, and two droplets, add a pacTiiOp of 62 g of eth. Tetra glycol (1 mole in 30 lg ZOe / s-aqueous solution of caustic soda and at 30 35 C, 189 g of dimethyl sulfate (1.5 mol) are gradually added, maintaining the RP of the reaction medium with 7- to 8-orthio-pyonium by the addition of 30% alkaline solution (5-7 ml each time).
Е5сего расходуют около 200 мл плелочиого раствора. После прибаг лени ди.метилеульфата с.месь раз.мепшвают при Toii же температуре еще в течеипе 30 мин, затем на1ревают .то слабого кииени и выдерживают в течение 5 час.About 200 ml of pond bleach are consumed. After the addition of dimethyl sulphate, the mixture is stirred at Toii at the same temperature for another 30 minutes, then it is heated weakly and kept for 5 hours.
Охлажденную до комнатно те.мпературы реакииоииую массу фильтруют и фильтрат экстрагируют в иесколько прпемов 500 мл хлористого метилена. Метиленхлоридный экстракт сущат над безводным сульфатом натри (15-20 г), фильтруют, отгон ют растворитель (при 39-43 С), а остаток фракционируют с елочным дефлег.матором (М 50 см), собира чистый диметиловьи эфир этиленгликол нри 82-84-С. Выход 35-37 г (-ЮУо от теоретического).Cooled to room temperature, the reaction mass is filtered and the filtrate is extracted into several solutions with 500 ml of methylene chloride. Methylene chloride extract is dissolved over anhydrous sodium sulfate (15-20 g), filtered, the solvent is distilled off (at 39-43 ° C), and the residue is fractionated with a fir-tree reflux condenser (M 50 cm), collecting pure dimethyl ether ethylene glycol 82-84 -WITH. Output 35-37 g (-UUo from theoretical).
Предмет изобретен и The subject is invented and
Сиособ получени диметилово1о эфира эти .ленгликол путем взаимо.1,ейетв 1 .тиметилсульфата с гликол том иатри , отличаюИ1 , и ii с тем, что, с пелью упрощеии те.хиологического пронееса и уменьпгенн его взр воогиеопаспости , пропесс ведут в водно-щелочной среде при рН 7 - 8.The method of obtaining dimethyl ether of these glycol by means of mutual. 1, it is in 1. Methyl sulfate with glycolite and sodium, which differs from I., and ii. at pH 7 - 8.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU162523A1 true SU162523A1 (en) |
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