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    • 专利摘要:

    公开号:SU906364A3
    申请号:SU792719751
    申请日:1979-02-07
    公开日:1982-02-15
    发明作者:Кейнен Альфред；Коссвиг Курт；Хентщель Бернхард；Цибарт Юрген
    申请人:Хемище Верке Хюльс Аг (Фирма)；
    IPC主号:
    专利说明:

    3 N-dodecyl-M-ethylaniline, M-dodecyl-M-hexyl aniline, H, M-dihexyl-p-toluidine, N, M-di-2-ethylbutyl-p-toluidine N, N-diheptyl-p-toluidine , N, N-dioct-p-toluidine, N, N-di-2-ethylhexyl-p-toluidine, p-isooctylaniline, Organic liquids are used as a solvent, which are inert to water under the conditions of treatment, hydrogen chloride and amine and the boiling point of which is above 120 ° C. The upper limit of the boiling point of the solvent is determined by physical characteristics such as, for example, a bond or melting point. Suitable inert solvents are, for example, unbranched or branched, aliphatic or cycloaliphatic, aromatic or araliphatic hydrocarbons, mixtures or appropriate petroleum fractions, for example, decane, tetralin, decalin, tetradecane, xylene, durol, isobutyl benzene, tantyl benzole, isobutyl benzene, tetradecane, xylene, durol, isobutyl benzene, a mixture of or corresponding petroleum fractions, for example, decane, tetralin, hydrocarbons, aromatic or araliphatic hydrocarbons. also cyclic ethers or straight chain ethers, for example dibutyl ether, diisobutyl ether, hexyl methyl ether, anisole, diphenyl ether ether, derivatives of tetrahydrofuran and tetrahydropyran and dioxane, and also d-branched (non-condensable) ketones or cyclic ketones, such as diisopropyl ketone or 2,6-dimethylcyclohexanone, and benzene derivatives, n-example chlorobenzene, dichlorobenzene, nitrobenzene, nitro, nitro, nitrile, nitro, nitro, nitro, nitro, nitrile, nitro, nitrile, nitro, nitro, nitrile, nitro, nitrile, nitro, nitro, nitrile, nitro, nitro, nitrile, nitro, nitro, nitrile, nitro, nitrile, nitro, nitrile, nitroxylene, nitrochloride, nitrochloride, nitroxybenzene, and The partial pressure of hydrogen chloride over the amine hydrochloride increases with increasing solvent concentration. This effect is quite unexpected. The thermolysis solution of the amine hydrochloride must not contain water, since water prevents the removal of hydrogen chloride. If necessary, the water should be removed before the thermosil, for example, by distillation using a suitable ablation agent. The solvent should have a possible low partial pressure and its boiling point should exceed the process temperature at least by so as to maintain the possibility of a low degree of entrainment of the solvent in the form of steam by an inert gas flow. The solvent and amine hydrochloride are taken, as a rule, in a ratio of 9: 1-1: 9, preferably t: 1-1: i. The thermolysis-exposed amine hydrochloride solution is preferably obtained by extracting amine with dilute hydrochloric acid. But according to the method, it is also possible to use an amine hydrochloride solution, which is obtained in a different way. For example, a tertiary aliphatic amine hydrochloride obtained by reacting alkyl chloride with an amine is also suitable as a raw material. Argon, nitrogen, methane, ethane, propane, ethylene, propylene can be used as an inert gas. The amount of inert gas required to release a certain amount of hydrogen chloride depends on the partial pressure that is set above the amine hydrochloride solution, depending on the temperature and amount of solvent. The proposed method can be carried out periodically and continuously. In continuity, the inert gas is fed in countercurrent to the solution. In this case, a high degree of enrichment of hydrogen chloride in an inert gas is achieved. So, it is possible to achieve a concentration of loric hydrogen more than 50%. Hydrogen chloride is easily removed from the inert gas stream, for example, by adsorption. But separation of the mixture of inert gas with hydrogen chloride is not always necessary. So, if ethylene is used as an inert gas, then the resulting gas mixture can be used directly for the synthesis of chloroethanes. The proposed method also releases the free amine, which is suitable for direct use. However, it is not always necessary to separate the amine from the solvent used, since the mixture of amine and solvent can be directly used for various purposes, for example for the extraction of dilute hydrochloric acid. Example 1 A reactor made in the form of a cylindrical glass container is used to cleave the hydrochloride amine solution. equipped with a casing, which reaches up to the upper edge, through which oil circulates as a heat carrier, and also three branch pipes located in the upper part. An amine hydrochloride stock solution is fed through the middle nozzle. This pack is closed in the process of thermolysis. A tube that goes to the bottom of the tank passes through the second pipe. An inert gas is introduced into the liquid through the tube. Gases are withdrawn through the third inlet, and hydrogen chloride is absorbed in the sodium hydroxide solution. 26.7 g of a solution (5.3 g of tri- (2-ethylhexyl) -amine hydrochloride in 21, A g of octadecane) are fed to the reactor, which is heated to 140 ° C. Through the solution, kj l of nitrogen is passed hourly. The original solution contains 0.51 g of hydrogen chloride. At the same time, after 7 minutes, the degree of evolution of gaseous hydrogen chloride is 57%, after 15 minutes 88, and after 35 minutes 9b%.
    Example 2. Example 1 is repeated with the difference that a solution of 7.2 g of tri- (2-ethylhexyl) -amine hydrochloride in 28.9 g of octadecane is used. At 170 ° C, 170 l / h of nitrogen is passed through the solution. The original solution contains 0,69 g of hydrogen chloride. Moreover, after 3 minutes, the degree of release of gaseous hydrogen chloride is kQ%, after 6 minutes 83, and after 10 minutes 9b
    Example-1 Repeat Example 1, with the difference that 29.6 g of a solution of 5.9 g of tri (2-ethylhexyl) -amine hydrochloride in 23.7 g of tetradecane are used. The solution is heated to and A7 L / h of ethylene is passed through it. The original solution contains 0.55 g of hydrogen chloride. Moreover, after 7 minutes, the degree of release of gaseous hydrogen chloride 51, after 15 minutes 78, and after 29 minutes 96.
    An example. An example is repeated with the difference that a solution of 5.8 g of trioxylamine hydrochloride in 23.0 g of octadecane is used, which is heated to 207 ° C. Through the solution hourly pass 7 liters of nitrogen. The original solution contains 5 g of hydrogen chloride. In this case, after 15 minutes, the degree of evolution of gaseous hydrogen chloride is 9
    thirty
    35
    Example 7. The rate of cleavage of hydrogen chloride increases as the inert gas transmission rate increases through the amine hydrochloride solution.
    Analogously to example 1, through a solution of 20 wt D of tri- (2-methylhexyl) -amine hydrochloride in 80 wt.% Tetradecane with a temperature of 142 ° C, nitrogen is passed at a different rate. After 10 minutes, hydrogen chloride in the following amount,% of the theoretical
    权利要求:
    Claims (1)
    [1]
    0.5 l of nitrogen / 10 min 36 1.3 l of ethylene / 10 min 63 3.2 l of nitrogen / 10 min 88. After 30 minutes, the amount of hydrogen chloride that can be removed is (at 0.3 liter of nitrogen). it6, after 50 minutes 81, and after 70 minutes 92. Example 5. Example k is repeated with the difference that the process is carried out at .. In this case, after 15 minutes, the degree of release of gaseous hydrogen chloride is 71%, after 25 min 87, and after 50 min 96%. Example 6. In order to detect the rate of cleavage of tri- (2-ethylhexyl) -amine hydrochloride, depending on the solvent, a series of experiments was carried out in the reactor of Example 1.8. calculation of 0.3 liters of nitrogen and 1 g of tri- (2-ethylhexyl) -amine hydrochloride. In all experiments, a solution of 20 parts of tri (2-ethylhexyl) -amine hydrochloride in 80 parts of solvent was used. (at 1.3 liters of ethylene) and 99.8% (at 3.2 liters of nitrogen). Example 8: Example 1 is repeated, with the difference that the 7.2 g hydrochloride solution of f M-dibutyl-N-hexylamine in 28.8 g dodecane is treated at 183 ° C in a nitrogen atmosphere supplied in a quantity of 20 l / h. after 10 minutes, the release of gaseous hydrogen chloride is 30%, after 20 minutes 55%, and after 65 minutes 100%. The remaining solvent contains all the original amount of amine. Example 9. The example is repeated with the difference that a solution of 6.5 g of trihexylamine hydrochloride of 23.5 octadecane is treated under an atmosphere of nitrogen supplied in an amount of 48 l / h. Moreover, after 10 minutes, the degree of release of gaseous hydrogen chloride is 3%, after 30 minutes 85%, and after 55 minutes 100%. The remaining solvent contains all the original amount of amine. Example 10. Example 1 is repeated, with the difference that a solution of 5.3 g of tridodecylamine hydrochloride in 23 g of cannon tetrads is treated at 203 C under a nitrogen atmosphere in the amount of 20. l / h. In this case, after 5 minutes, the degree of excretion of gaseous hydrogen chloride is 36%, after 10 minutes 70%, and after 20 minutes 100%. The solvent left contains the total amount of amine. Example 11. Example 1 is repeated, with the difference that a solution of 8.3 g of hydrochloride (Hjg) NC CJ, H 2 in 33 g of tetradecane is processed under an atmosphere of nitrogen, given in an amount of 22 l / h. At the same time, the degree of evolution of a gas of shaped hydrogen chloride was 35% over the course of 5 minutes, 61% after 10 minutes, 88.5% after 20 minutes, and 100% after 30 minutes. The remaining solvent contains all the initial amount of amine. Example 12. Example 1 is repeated, with the difference that a solution of 5.8 g of M, M-dipentadecyl-N-hexylamine hydrochloride in 23.1 g of octadecane is treated under an atmosphere of nitrogen supplied in an amount of 20 l / h. At the same time, after 5 minutes, the degree of release of gaseous water of the genus is 57%, after 10 minutes 48 and after 15 minutes MOO /. The remaining solvent contains all the original amount of amine. Example 13. Example 1 is repeated, with the difference that a solution of 6.2 g of diddecylamine hydrochloride in 25.8 g of tetradecane under a nitrogen atmosphere is supplied in an amount of 22 l / h. Moreover, after 5 minutes, the degree of release of gaseous hydrogen chloride is 43%, and after 10 minutes 63% over a period of 20 minutes 91, and after 30 minutes 100%. The remaining solvent contains all the original amount of amine. Example 14. Example 1 is repeated with the difference that a solution of 7.2 g of M, M-diisoheptyldecyl-N-methylamine hydrochloride solution is treated at 180 ° C. under a nitrogen atmosphere fed in an amount of 22 l / h. Moreover, after 10 minutes, the degree of release of gaseous hydrogen chloride is 42%, after 20 minutes 63%, and after 60 minutes 100%. The remaining solvent contains all the original amount of amine. Example 15. Example 1 is repeated, with the difference that a solution of 6.4 g of tri- {2-ethyl-hexyl) -amine hydrochloride in 23.7 g of decane is treated at 100 ° C under a nitrogen atmosphere of 47 liters / h Moreover, after 30 minutes, the degree of release of gaseous hydrogen chloride is 75%, after 50 minutes, 100%. The remaining solvent contains all the original amount of amine. Example 16. Example 1 is repeated with the difference that a solution of 4.9 g of trioctylamine hydrochloride in 19.2 g of octadecane is treated at 250 ° C in a nitrogen atmosphere supplied in the amount of 47 l / h. At the same time, the degree of excretion of zoobium hydrochloride 70% after 70 minutes, and after 10 minutes 100%. The remaining solvent contains all the original amount of amine. The invention method for the simultaneous production of tri-or dialkylamines of hydrogen chloride from the hydrochlorides of the corresponding amines by treating them in an inert hydrocarbon solvent, is different from 990636
    u and with the fact that, for the purpose of higher-Sources of information,
    The efficiency of the process, taken into account during the examination, is carried out at 100-250С in anhydrous. one . Soc.Chein. 3nd. 67 ,, environment in an inert gas atmosphere. .with. it8-51.
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    同族专利:
    公开号 | 公开日
    EP0003472B1|1981-09-16|
    EP0003472A2|1979-08-22|
    BE874111A|1979-08-13|
    IT7947958D0|1979-02-09|
    FR2416864A1|1979-09-07|
    NL7901090A|1979-08-15|
    DE2805933B1|1979-08-23|
    DE2805933C2|1980-04-30|
    US4230681A|1980-10-28|
    EP0003472A3|1979-09-05|
    JPS54117410A|1979-09-12|
    DE2861101D1|1981-12-03|
    GB2017680A|1979-10-10|
    GB2017680B|1982-07-07|
    引用文献:
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    DE2836580C3|1978-08-21|1981-11-05|Chemische Werke Hüls AG, 4370 Marl|Process for the separation of hydrogen chloride and hydrogen bromide|
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    DE3130810A1|1981-08-04|1983-02-24|Chemische Werke Hüls AG, 4370 Marl|METHOD FOR PRODUCING COPPER-CHLORIDE FROM COPPER-OXICHLORIDE WITH TERTIAL AMINE HYDROCHLORIDES|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE2805933A|DE2805933C2|1978-02-13|1978-02-13|Process for splitting off hydrogen chloride from solutions of amine hydrochlorides|
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