SU298199A1 - Method of producing s-3-oxysulpholan-4-sulfoacid salts - Google Patents
Method of producing s-3-oxysulpholan-4-sulfoacid saltsInfo
- Publication number
- SU298199A1 SU298199A1 SU1254656A SU1254656A SU298199A1 SU 298199 A1 SU298199 A1 SU 298199A1 SU 1254656 A SU1254656 A SU 1254656A SU 1254656 A SU1254656 A SU 1254656A SU 298199 A1 SU298199 A1 SU 298199A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- salts
- producing
- oxysulpholan
- sulfoacid
- epoxysulfolane
- Prior art date
Links
- 239000011780 sodium chloride Substances 0.000 title description 3
- 150000003839 salts Chemical class 0.000 title description 2
- 238000002360 preparation method Methods 0.000 description 3
- 229910003202 NH4 Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000000875 corresponding Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- SZAIAWVGWTXVMB-UHFFFAOYSA-N 6-oxa-3$l^{6}-thiabicyclo[3.1.0]hexane 3,3-dioxide Chemical compound C1S(=O)(=O)CC2OC21 SZAIAWVGWTXVMB-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium Ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 1
- 229940001607 sodium bisulfite Drugs 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing Effects 0.000 description 1
Description
Изобретение относитс к способу получени полупродуктов синтеза поверхностно-активных веществ - солей З-оксисульфолан-4-сульфокислот общей формулыThe invention relates to a method for producing intermediates for the synthesis of surfactants - salts of 3-oxysulfolan-4-sulfonic acids of the general formula
SUjMSujm
где М-Li; Na, К, NH4.where M is Li; Na, K, NH4.
Эти соединени и способ их получени в литературе ,не описаны.These compounds and their method of preparation are not described in the literature.
Предлагаетс способ получени солей 3-оксисульфолан - 4 - сульфокислот реакцией 3,4эпоксисульфолана с насыщенным водным раствором бисульфита соответствующего металла при кип чении в течение 0,5-1 час.A method is proposed for the preparation of 3-oxysulfolan-4-sulfonic acid salts by the reaction of 3.4 epoxysulfolane with a saturated aqueous solution of a bisulfite of the corresponding metal at the boil for 0.5-1 hour.
Пример. В реактор, снабженный обратным холодильником, загружают 13,4 г 3,4эпоксисульфолана и 120 мл 40%-ного раствора бисульфита натри . Смесь кип т т в течение 30 мин. При этом вс окись сульфолаиа раствор етс . Смесь оставл ют на 15 час дл кристаллизации. Выпавщий осадок 19,3 г (81%) представл ет собой натриевую соль 3-оксисульфолан - 4 - сульфокислоты.Example. 13.4 g of 3.4 epoxysulfolane and 120 ml of 40% sodium bisulfite solution are charged to a reactor equipped with a reflux condenser. The mixture is boiled for 30 minutes. In this case, all sulfolium oxide dissolves. The mixture was allowed to crystallize for 15 hours. The precipitation of 19.3 g (81%) is the sodium salt of 3-oxysulfolane-4-sulfonic acid.
В ИК-спектре продукта присутствуют частоты , присущие ОП-грунпе при 3360 см, SOa-rpynne при 1120-1140 и 1325-1340 , ЗОг-ОМе-группе при 1200 смг, и отсутствует характеристическа частота при 980 , имеюща с в спектре исходного 3,4-эпоксисульфолана .In the IR spectrum of the product, there are frequencies inherent in the OP-ground at 3360 cm, SOa-rpynne at 1120-1140 and 1325-1340, the ЗОг-ОМe-group at 1200 cmg, and there is no characteristic frequency at 980, , 4-epoxysulfolan.
Найдено, %: С 20,76; П 3,18; S 26,20.Found,%: C 20.76; P 3.18; S 26.20.
CiHyOeSzNa.CiHyOeSzNa.
Вычислено, %: С 20,17; Н 2,96; S 26,92.Calculated,%: C 20.17; H 2.96; S 26.92.
Аналогично могут быть получены калиева , литиева и аммонийна соли.Similarly, potassium, lithium and ammonium salts can be obtained.
Предмет изобретени Subject invention
15 Способ получени солей 3-оксисульфолан4-сульфокислот общей формулы15 A process for the preparation of salts of 3-oxysulfolane-4-sulfonic acids of the general formula
2020
где М-Li; Na, К, NH4, отличающийс тем, что 3,4-эпоксисульфолан подвергают взаимодействию с насыщенным водным раствором бисульфита соответствующего металла при кип чении с последующим выделением продукта известными приемами.where M is Li; Na, K, NH4, characterized in that the 3,4-epoxysulfolane is reacted with a saturated aqueous solution of a bisulfite of the corresponding metal at the boiling point, followed by separation of the product by known methods.
Publications (1)
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SU298199A1 true SU298199A1 (en) |
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