SU213782A1 - METHOD FOR CLEANING CHLOROUS METHYL - Google Patents
METHOD FOR CLEANING CHLOROUS METHYLInfo
- Publication number
- SU213782A1 SU213782A1 SU1158935A SU1158935A SU213782A1 SU 213782 A1 SU213782 A1 SU 213782A1 SU 1158935 A SU1158935 A SU 1158935A SU 1158935 A SU1158935 A SU 1158935A SU 213782 A1 SU213782 A1 SU 213782A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- chloride
- methyl
- cleaning
- methyl chloride
- activated carbon
- Prior art date
Links
- 238000004140 cleaning Methods 0.000 title description 6
- -1 METHYL Chemical class 0.000 title 1
- NEHMKBQYUWJMIP-UHFFFAOYSA-N Chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims description 15
- 229940050176 Methyl Chloride Drugs 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- JIAARYAFYJHUJI-UHFFFAOYSA-L Zinc chloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 7
- 239000011592 zinc chloride Substances 0.000 claims description 7
- 235000005074 zinc chloride Nutrition 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 6
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 6
- AIYUHDOJVYHVIT-UHFFFAOYSA-M Caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 claims description 5
- 229940098124 cesium chloride Drugs 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N oxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 description 7
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 238000000746 purification Methods 0.000 description 2
- 206010008415 Chediak-Higashi syndrome Diseases 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L cacl2 Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 150000001805 chlorine compounds Chemical group 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- 238000000079 presaturation Methods 0.000 description 1
- 229910052904 quartz Inorganic materials 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Description
Известен способ очистки хлористого метила от кислородсодержащих соединений и непредельных углеводородов, заключающийс в том, что загр зненный хлористый метил подвергают обработке водородом При 50-150°С на катализаторе-хлористом палладии на носи геле.A known method for the purification of methyl chloride from oxygen-containing compounds and unsaturated hydrocarbons, is that contaminated methyl chloride is treated with hydrogen at 50-150 ° C on a palladium chloride catalyst on a nosi gel.
Предложенный способ отличаетс от известного тем, что загр зненный хлористый метил гидрохлорируют при 195-205°С на активированном угле, пропитанном хлористым цинком, или на активированном угле, пропитанном хлористым цинком и лромотированном хлористым цезием в количестве, например 0,05-0,5о/о от веса хлористого цинка.The proposed method differs from that in that the contaminated methyl chloride is hydrochlorinated at 195-205 ° C on activated carbon impregnated with zinc chloride or activated carbon impregnated with zinc chloride and liquefied with cesium chloride in an amount of, for example, 0.05-0.5o / o from the weight of zinc chloride.
Ведение процесса предложенным способом увеличивает выход хлористого метила за счет превращени примесей хлористого метила в хлористый метил.Conducting the process by the proposed method increases the yield of methyl chloride by converting methyl chloride impurities to methyl chloride.
Пример 1. В кварцевый реактор диаметром 50 мм с наружным электрообогревом и двухточечной термопарой загружают 1 л активированного угл марки АР-3, пропитанного хлористым цинком (35 вес. о/о)После предварительного насыщени угл хлористым водородом в течение 1 час через реактор пропускают за 2,5 час смесь хлористого водорода и хлористого метила в соотношении 0,5:1. Объемна скорость 70 час. Температура 200-205°С. Избыточный хлористый водород отмывают водой, после чего хлористый метил сушат хлористым кальцием, Состав смеси до очистки, об. %:Example 1. In a quartz reactor with a diameter of 50 mm with an external electrical heating and a two-point thermocouple, 1 liter of activated carbon of the brand AP-3, impregnated with zinc chloride (35% v / v) is loaded. After pre-saturation with hydrogen chloride for 1 hour, the reactor is passed through 2.5 hours a mixture of hydrogen chloride and methyl chloride in the ratio of 0.5: 1. Volume speed is 70 hours. Temperature 200-205 ° C. Excess hydrogen chloride is washed with water, then methyl chloride is dried with calcium chloride. Composition of the mixture before purification, vol. %:
85,9885.98
СНзС CHSS
13,3 (СНз)20 0,02 СПзОН СОг 0,7.13.3 (CH3) 20 0.02 SPZON CO2 0.7.
Средний состав хлористого The average composition of chloride
метила после очистки, об. о/о: methyl after cleaning, about. o / o:
99,624 CHsCl 0,07 99.624 CHsCl 0.07
(СНз)20 0,006 (CHS) 20 0.006
СНзОН 0,3. 5СОгSNZON 0.3. 5COg
Пример 2. В тот же реактор загружают 1 л активированного угл , пропитанного ZnCla и CsCl, в количествах 25 вес. о/о и 0,1 вес. о/о соответственно.Example 2. In the same reactor load 1 liter of activated carbon, impregnated with ZnCla and CsCl, in quantities of 25 weight. o / o and 0.1 wt. o / o, respectively.
При температуре 195-205°С в реактор подают хлористый водород и хлористый метил в течение 2 час при соотношении 0,5: 1. Объемна скорость 140 .At a temperature of 195-205 ° C hydrogen chloride and methyl chloride are fed to the reactor for 2 hours at a ratio of 0.5: 1. A volumetric rate of 140.
Состав хлористого метила до очистки, об. O/Q;The composition of methyl chloride to clean, about. O / Q;
Состав хлористогометила после очистки, об. %:The composition of chlorogram after cleaning, about. %:
CHgCI100CHgCI100
(СНз)2ООтсутствует(SNS) 2O is absent
СНзОНОтсутствуетNO CHANGE
СОа0,3.SO0,3.
При подаче на тот же контакт и в том же соотношении хлористого водорода и хлористого метила при температуре 200°С, но при объемной скорости 360 состав хлористого метила до очистки следующий, об. о/,,:When applying to the same contact and in the same ratio of hydrogen chloride and methyl chloride at a temperature of 200 ° C, but with a space velocity of 360, the composition of methyl chloride before cleaning is the following, vol. about/,,:
СНзС CHSS
85,84 (СНз)20 14,0 СНзОН 85.84 (СНз) 20 14.0 СНзОН
0,1 СОз0.1 Soz
0,06.0.06.
осле очистки, об. о/оСНзС After cleaning, about. o / osnzs
99,36 (СНз)20 0,6 СО, 0,04.99.36 (CH3) 20 0.6 CO, 0.04.
Анализы исходного и очищенного хлористого метила провод т на одном и том же хроматографе .Analyzes of the starting and purified methyl chloride are carried out on the same chromatograph.
Предмет изобретени Subject invention
Claims (2)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU213782A1 true SU213782A1 (en) |
Family
ID=
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4794204A (en) * | 1986-06-14 | 1988-12-27 | Hoechst Aktiengesellschaft | Process for the removal of dimethyl ether in methyl chloride |
| US4935565A (en) * | 1988-08-24 | 1990-06-19 | The Dow Chemical Company | Process and catalyst for hydrochlorination of hydrocarbons |
| US5041406A (en) * | 1988-08-24 | 1991-08-20 | The Dow Chemical Company | Catalyst for hydrochlorination of hydrocarbons |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4794204A (en) * | 1986-06-14 | 1988-12-27 | Hoechst Aktiengesellschaft | Process for the removal of dimethyl ether in methyl chloride |
| US4935565A (en) * | 1988-08-24 | 1990-06-19 | The Dow Chemical Company | Process and catalyst for hydrochlorination of hydrocarbons |
| US5041406A (en) * | 1988-08-24 | 1991-08-20 | The Dow Chemical Company | Catalyst for hydrochlorination of hydrocarbons |
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