专利摘要:

公开号:SU955854A3
申请号:SU762419860
申请日:1976-11-11
公开日:1982-08-30
发明作者:Жан Жийе Филипп;Анриш Гастон
申请人:Сосьете Шимик Де Шарбоннаж (Фирма);
IPC主号:
专利说明:

'' The invention relates to the processing of reaction mass in the catalytic alkylation of aromatic hydrocarbons and can be used in the chemical and petrochemical industries.
After alkylation, alkylates containing a certain amount of dissolved catalytic complex and a catalytic complex consisting of minerals and hydrocarbons are separated by decantation. Alkylates must be purified in order to isolate them.
Closest to the proposed is a method of purification of hydrocarbons generated during the alkylation of aromatic compounds in the presence of aluminum chloride, including neutral. lysing the reaction mixture with anhydrous ammonia and separating the formed 'mineral salts by decantation [1L · The disadvantage of this method is not a high enough degree. purification of alkylates and the duration of the separation process by decantation 36-80 hours
The purpose of the invention is to increase the degree of purification and speed up the process.
This goal is achieved by the fact that in the known method, including the neutralization of the reaction mixture with anhydrous ammonia and the separation of the formed mineral salts by decantation, after neutralization, an additional treatment is carried out with water.
Water is used in the form of steam.
Water is introduced in an amount of 1020 wt.% From the separated salts.
A neutral gas stream is used to introduce water vapor.
Cleaning is carried out at a temperature that ensures the presence of water in the gas phase.
The treatment is subjected to a catalytic complex containing aluminum chloride, hydrochloric acid, aromatic and alkyl aromatic hydrocarbons. ·
Nitrogen is used as a neutral gas stream. The proportion of water vapor and nitrogen is calculated so that free water does not appear in the reactor, which depends on the temperature in it. After decantation at the bottom of the column receive
955854 4 on the boiling point at boiling point. Ammonia is returned to the converter.
Thus, the proposed method allows you to completely and in a short time to clear alkylates from mineral salts in the processes of catalytic alkylation of aromatic compounds.
a phase enriched with a salt, which can be processed, for example, by centrifugation, then filtration, in the head of the column receive a fraction containing no salts.
-Example. The reaction mixture obtained by leaving the ash alkylation reactor with ethylene in the presence of chloride (aluminum as a catalyst and ethyl chloride as a promoter) is subjected to purification. The reaction mass consisting of 50 l / h of acid alkylate containing 60 ml of dissolved complex and 100 ml / h of acidic alkylate containing 60 ml of the dissolved complex and 100 ml / h of the oily phase of the complex is treated in a tubular catalyst with a diameter of 5 cm and a height of 100 cm. It is stirred using a circulation pump with a capacity of 300 l / h.
200 nl / h of ammonia are introduced into the bottom of the catalyst, excess ammonia is collected at the head of the catalyst, and the alkylate is distilled to extract ethylbenzene.
Under these conditions, the catalyst decomposes completely. ammonium chloride and the salt resulting from the interaction of A1C1 3 and NH j.
kg / h of neutralized alkylate is fed to the flocculator reactor with a diameter of 5 cm and a height of .60 cm
Alkylate contains 0.5 wt.% Salts. 200 nl / h of heated nitrogen and 35 ml / h of water vapor are fed into the lower flocculator zone. The temperature in the flocculator is 50-60 ° C. From the flocculator, the reaction mixture is introduced into the decanter. A mixture containing 5 times more salts is collected in the lower part of the decanter than in the starting alkylate, which is then centered to give a clarified salt free alkylate and sludge. The decanted alkali coming out of the Upper part of the decanter and not containing salts is mixed with clarified alkylate, filtered and degassed in a column25
Editor A. Frolova
权利要求:
Claims (6)
[1]
t,. . The invention relates to the processing of the reaction mass in the catalytic alkylation of aromatic hydrocarbons and can be used in chemical and petrochemical oxidation. After the alkylation, decantation separates the methyls containing some dissolved catalytic complex and the catalytic complex consisting of minerals and hydrocarbons. It is necessary to clean the alkylates in order to distinguish them. Closest to the proposed method is the purification of hydrocarbons, which are decomposed by the alkylation of aromatic compounds in the presence of aluminum chloride, including neutralizing the reaction mixture with anhydrous ammonia and separating the formed mineral salts by decantation1,13. The disadvantage of this method is the insufficiently high degree of purification of alkylates and the duration of the separation process by decantation of 36-80 hours. The purpose of the invention is to increase the degree of purification and accelerate the process. This goal is achieved by the fact that in a known method, including the neutralization of the reaction mixture with anhydrous ammonia and the separation of the formed mineral salts by decantation, after neutralization, additional treatment with water is carried out. Water is used in the form of steam. Water is introduced in an amount of 1020 wt.% Of the separated salts. For the introduction of water vapor, a neutral gas flow is used. The purification is carried out at a temperature that ensures the presence of water in the gas phase. The treatment is subjected to a catalytic complex containing aluminum chloride, hydrochloric acid, aromatic and alkyl aromatic hydrocarbons. Nitrogen is used as a neutral gas stream. The proportion of water vapor and nitrogen is calculated so that free water does not appear in the reactor, which depends on the temperature in it. After decantation, a phase enriched in salt is obtained in the lower part of the column, which can be treated, for example, by centrifugation, then filtration, in the head of the column I get a fraction that does not contain salts. -Example. The reaction mixture obtained at the outlet of the alkylation of the bisole with ethylene in the presence of chloride: aluminum as a catalyst and ethyl chloride as a promoter is purified. The reaction mass consisting of 50 l / h acid alkylate, containing 60 ml of the dissolved complex and 100 ml / h of acid alkylate, containing 60 MP of the dissolved complex and 100 ml / h of the oily phase of the complex, is treated in a tubular neutralizer with a diameter of 5 cm and 100 cm high. Stir with a circulating pump with a capacity of 300 l / h. 200 nl / h of ammonia are injected into the lower part of the neutralizer, an excess of ka is collected at the head of the neutralizer, and the alkylate is distilled to extract ethylbenzene. Under these conditions, the catalyst is completely decomposed. ammonium chloride and the salt resulting from the interaction of A1Cl3 and NHj. 40 kg / h of neutralized alkyl is fed to the reactor-flocculator with a diameter of 5 cm and a height of .60 cm. The alkylate contains 0.5 wt.% Salts. 200 nl / h of heated nitrogen and 35 ml / h of water vapor are supplied to the lower zone of the flocculator. Flocculator temperature 50-60С. From the flocculator, the reaction mixture is introduced into the decanter. in the lower part of the decanter, a mixture containing 5 times more salts is collected than in Kilate, which is then centered, and a clarified alkylate, containing no salts, and sludge are obtained. The decanted alkyl, leaving the upper part of the decanter and not containing salts, is mixed with the clarified alkyme, filtered and degassed to a column not at boiling point. Ammonia is returned to the neutralizer. Thus, the proposed method makes it possible to completely and quickly remove alkylates from mineral salts during the catalytic alkylation of aromatic compounds. Claim 1. A method for purifying hydrocarbons formed by alkylation of aromatic compounds in the presence of aluminum chloride from mineral salts, including neutralizing the reaction mixture with anhydrous ammonia i decanting the resulting mineral salts and with In order to increase the degree of purification and acceleration of the process, after neutralization, additional treatment with water is carried out.
[2]
2. Method 1, characterized in that water is used in the form of steam.
[3]
3. Method according to claims, 1 and 2. About t that is injected into the water in an amount of 10-20 wt.% From separable salts. ,
[4]
4. Method no, niil-3, o tl and h and yu and the fact that for the introduction of water vapor using a neutral gas stream.
[5]
5. The method according to claims 1-4, that is, and that the cleaning is carried out at a temperature that ensures that the water flows in the gas phase.
[6]
6. The method according to claims 1-5, characterized in that the processing is under-. catalytic complex containing aluminum chloride, hydrochloric acid, aromatic and alkylaromatic hydrocarbons. Sources of information taken into account during the examination 1. French patent 2256131, l. C 07 S 7/00, 1975.
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同族专利:
公开号 | 公开日
PT65786B|1978-05-10|
DK155593B|1989-04-24|
SE7612113L|1977-05-14|
FI61681C|1982-09-10|
MX4893E|1982-12-09|
NO763847L|1977-05-16|
DE2651698C2|1983-10-13|
US4117023A|1978-09-26|
NO150078C|1984-08-22|
DE2651698A1|1977-06-02|
NO150078B|1984-05-07|
SE428013B|1983-05-30|
DK511776A|1977-05-14|
FI61681B|1982-05-31|
DK155593C|1989-09-18|
FI763222A|1977-05-14|
PT65786A|1976-12-01|
引用文献:
公开号 | 申请日 | 公开日 | 申请人 | 专利标题

US2376088A|1939-10-04|1945-05-15|Dow Chemcial Company|Method of treating friedel-crafts reaction liquors|
US3499054A|1968-08-19|1970-03-03|Continental Oil Co|Purification of detergent alkylates|
US3679770A|1970-08-10|1972-07-25|Standard Oil Co|Process for removal of catalyst complex|
US3703559A|1970-11-25|1972-11-21|Continental Oil Co|Purification of detergent alkylates|JPH0333692B2|1983-02-28|1991-05-20|Kyowa Kagaku Kogyo Kk|
FR2566770B1|1984-06-27|1986-11-14|Inst Francais Du Petrole|IMPROVED PROCESS FOR REMOVING NICKEL, ALUMINUM AND CHLORINE FROM OLEFIN OLIGOMERS|
US4940833A|1988-11-29|1990-07-10|Phillips Petroleum Company|Olefin monomer separation process|
US5743298A|1996-04-22|1998-04-28|Techniflo Corporation|Spring pulsation dampener|
US5996632A|1998-12-14|1999-12-07|Aeroquip Corporation|Pressure relief adapter|
US20080033227A1|2006-08-03|2008-02-07|David Campbell Graves|Recovery of sulfur value in an alkylation process|
法律状态:
优先权:
申请号 | 申请日 | 专利标题
FR7534704A|FR2331379B1|1975-11-13|1975-11-13|
FR7534703A|FR2331537B1|1975-11-13|1975-11-13|
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