CS224932B1 - The 2-hydroxy-chlorinepropyl-trialkylammonium alkylsulphates and their preparation - Google Patents
The 2-hydroxy-chlorinepropyl-trialkylammonium alkylsulphates and their preparation Download PDFInfo
- Publication number
- CS224932B1 CS224932B1 CS411682A CS411682A CS224932B1 CS 224932 B1 CS224932 B1 CS 224932B1 CS 411682 A CS411682 A CS 411682A CS 411682 A CS411682 A CS 411682A CS 224932 B1 CS224932 B1 CS 224932B1
- Authority
- CS
- Czechoslovakia
- Prior art keywords
- hydroxy
- temperature
- chloropropyl
- preparation
- trialkylammonium
- Prior art date
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- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 3
- -1 2-hydroxy-3-chloropropyl Chemical group 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 2
- 125000004178 (C1-C4) alkyl group Chemical group 0.000 claims 1
- 125000000217 alkyl group Chemical group 0.000 claims 1
- 150000008051 alkyl sulfates Chemical class 0.000 claims 1
- 150000001412 amines Chemical class 0.000 claims 1
- 125000004432 carbon atom Chemical group C* 0.000 claims 1
- 125000005265 dialkylamine group Chemical group 0.000 claims 1
- DENRZWYUOJLTMF-UHFFFAOYSA-N diethyl sulfate Chemical compound CCOS(=O)(=O)OCC DENRZWYUOJLTMF-UHFFFAOYSA-N 0.000 claims 1
- 229940008406 diethyl sulfate Drugs 0.000 claims 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims 1
- 238000005956 quaternization reaction Methods 0.000 claims 1
- 239000000376 reactant Substances 0.000 claims 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims 1
- VAYGXNSJCAHWJZ-UHFFFAOYSA-N dimethyl sulfate Chemical compound COS(=O)(=O)OC VAYGXNSJCAHWJZ-UHFFFAOYSA-N 0.000 description 5
- 238000001816 cooling Methods 0.000 description 3
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 238000006277 sulfonation reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 240000008790 Musa x paradisiaca Species 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Do 1 1 tříhrdlé sulfonační banky opatřené míchadlem , vnitřním teploměrem, zpětným chladičem a kapací nálevkou se předloží 139 g vodného roztoku dimetylaminu (32,4 % hm). Přidá se 170,4 g vody a za ohlazení solankou se podchladí na cca 0 °C. Za intenzivního s139 g of an aqueous solution of dimethylamine (32.4% by weight) was charged to a 1 L three-necked sulfonation flask equipped with a stirrer, an internal thermometer, a reflux condenser and a dropping funnel. 170.4 g of water are added and cooled to about 0 ° C with cooling with brine. For intense p
ohlazení a míchání se z kapačky regulovaně dávkuje epichlorhydrin tak, aby reakční teplota v banoe se držela pod +5 °C (5 °C maximum), Vydávkování 92*5 g epichlorhydrinu trvá cca 1 hod. Od konce přídavku posledního množství epichlorhydrinu se míchá dalších 10 minut, načež se z kapačky během 2 hodin nadávkuje 121 g dimetylsulfátu. Teplota se během přidávkování dimety lsuftlátu udržuje v rozmezí 0 až 10 °C (+10 °C maximum). Po vydávkování dimety lsulfátu se teplota zvýší na 50 °C a při zmíněné teplotě se doreaguje další 1 hod. Výtěžek činí 522 g vodného neutrálního roztoku (pH 6) s 50% obsahem účinné látky, tj. 2-hydroxy-3-chlorpropy1-trimetylamoniumme t o sulfátu.epichlorohydrin is controlled in a controlled manner from the dropper, so that the reaction temperature in the banane is kept below + 5 ° C (5 ° C maximum), dispensing 92 * 5 g of epichlorohydrin takes about 1 hour. After 10 minutes, 121 g of dimethyl sulfate was metered from the dropper over 2 hours. The temperature is maintained between 0 and 10 ° C (+ 10 ° C maximum) during the addition of the dimethisulfate dimer. After dispensing of dimethyl sulphate, the temperature is raised to 50 ° C and reacted at this temperature for an additional 1 hour. The yield is 522 g of an aqueous neutral solution (pH 6) with 50% active substance, ie 2-hydroxy-3-chloropropyl to sulfate.
Příklad 2Example 2
Do 0,5 1 sulfonační banky opatřené KPG míchadlem, kapačkou a teploměrem se předloží 36,5 S dieiylaminu, zředí l46 ml vody.A 0.5 L sulfonation flask equipped with a KPG stirrer, dropper and thermometer was charged with 36.5 S of dieiylamine, diluted with 146 mL of water.
Za stálého míchání a mírného chlazení se během l/2 hodiny přikape 46,25 g epichlorhydrinu tak, aby teplota se držela v rozmezí 10 až 20 °C. Od ukončení přídavku epichlorhydrinu se při stejné teplotě míchá dalších 10 minut, načež se započne dávkovat dimety1sulfát. Teplota během dávkování dimetylsulfátu se udržuje za mírného přichlazování v rozmezí 10 až 20 °C, Vydávkování 62 g dimetylsulfátu trvá oca 1 hodinu. Teplota se zvedne na 50 °C, načež se při zmíněné teplotě doreaguje další 1 hodinu. Výtěžek činí 290 g čirého světlého nažloutlého roztoku s 5θ$ obsahem akt.l., pHs6.While stirring and gentle cooling, 46.25 g of epichlorohydrin are added dropwise over 1/2 hours, maintaining the temperature between 10 and 20 ° C. After the addition of epichlorohydrin was complete, the mixture was stirred at the same temperature for a further 10 minutes, and then dimethyl sulfate was started. The temperature during the dimethylsulfate dosing is maintained under moderate cooling in the range of 10-20 ° C. The dispensing of 62 g of dimethylsulfate lasts for 1 hour. The temperature is raised to 50 ° C and then reacted at this temperature for a further 1 hour. The yield was 290 g of a clear, light yellowish solution having an active substance content of 5%, pH6.
Claims (3)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS411682A CS224932B1 (en) | 1982-06-03 | 1982-06-03 | The 2-hydroxy-chlorinepropyl-trialkylammonium alkylsulphates and their preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS411682A CS224932B1 (en) | 1982-06-03 | 1982-06-03 | The 2-hydroxy-chlorinepropyl-trialkylammonium alkylsulphates and their preparation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS224932B1 true CS224932B1 (en) | 1984-02-13 |
Family
ID=5383194
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS411682A CS224932B1 (en) | 1982-06-03 | 1982-06-03 | The 2-hydroxy-chlorinepropyl-trialkylammonium alkylsulphates and their preparation |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS224932B1 (en) |
-
1982
- 1982-06-03 CS CS411682A patent/CS224932B1/en unknown
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