Reactor for preparing organic peroxides via the intermediate of a solid hydroperoxide
A reactor which comprises a vessel ( 1 ) with a vessel bottom ( 2 ), a stirrer ( 3 ) arranged in the vessel, an emergency discharge valve ( 4 ) arranged in the vessel bottom for emptying the reactor in less than 600 seconds and at least one filtration device ( 5 ) arranged in the vessel bottom is suitable for the safe preparation of organic peroxides. The process for preparing an organic peroxide comprises the steps of preparing a solid hydroperoxide in the form of a suspension in the reactor, filtering the suspension through the filtration device ( 5 ) arranged in the vessel bottom ( 2 ) while retaining the solid hydroperoxide in the reactor and reacting the hydroperoxide with an alkylating agent, an acylating agent or a carbonyl compound.
1. A reactor for preparing organic peroxides, comprising:
a) a vessel ( 1 ) with a vessel bottom ( 2 ) and comprising a stirrer ( 3 );
b) at least one filtration device ( 5 ) located in said vessel bottom;
c) an emergency discharge valve ( 4 ) located in said vessel bottom and a separate shutoff valve ( 6 ); wherein:
i) said shutoff valve ( 6 ) is positioned so that fluid passing from said vessel ( 1 ) through said shutoff valve ( 6 ) also passes through said filtration device ( 5 );
ii) said emergency discharge valve ( 4 ) is positioned so that fluid passing from said vessel ( 1 ) through said emergency discharge valve ( 4 ) does not pass through said filtration device ( 5 ).
2. The reactor of claim 1 , wherein said filtration device ( 5 ) is a frit which is flush in said vessel bottom ( 2 ).
3. The reactor of claim 1 , wherein said emergency discharge valve is a valve for emptying the reactor in less than 600 seconds.
4. The reactor of claim 1 , further comprising at least one cooling device ( 9 ) located in said vessel bottom ( 2 ) and projecting into the interior of said vessel ( 1 ).
5. A process for preparing an organic peroxide, comprising the steps of:
a) preparing a solid hydroperoxide in the form of a suspension in the reactor of claim 1 ;
b) filtering the suspension through the filtration device ( 5 ) located in the vessel bottom ( 2 ) while retaining the solid hydroperoxide in the reactor; and
c) reacting the hydroperoxide with an alkylating agent, an acylating agent or a carbonyl compound.
6. The process of claim 5 , wherein said solid hydroperoxide is 2,5-dimethylhexane-2,5-dihydroperoxide.
7. The process of claim 5 , wherein said solid hydroperoxide is suspended in a wash liquid between step b) and step c) and the resulting suspension is filtered through said filtration device ( 5 ) located in the vessel bottom ( 2 ) while retaining the solid hydroperoxide in the reactor.
8. The process of claim 5 , wherein, in step c), said hydroperoxide is reacted with a tertiary alcohol in the presence of a strong acid.
9. The process of claim 5 , wherein, in step c), said hydroperoxide is reacted with an acylating agent selected from the group consisting of: a carboxylic acid chloride; a carboxylic anhydride; and a chloroformate.
10. The process of claim 9 , wherein said acylating agent is a carboxylic acid chloride selected from the group consisting of: acetyl chloride; isobutyryl chloride; pivaloyl chloride; 2-ethylhexanoylchloride; 3,5,5-trimethylhexanoyl chloride; neodecanoyl chloride; and benzoyl chloride.
11. The process of claim 9 , wherein said acylating agent is a chloroformate selected from the group consisting of: isopropyl chloroformate; n-butyl chloroformate; sec-butyl chloroformate; 2-ethylhexyl chloroformate; myristyl chloroformate; cetyl chloroformate; cyclohexyl chloroformate; and 4-tert-butylcyclohexyl chloroformate.
12. The process of claim 5 , wherein, in step c), said hydroperoxide is reacted with acetone.
13. A reactor for preparing organic peroxides, comprising:
a) a vessel ( 1 ) with a vessel bottom ( 2 ) and comprising a stirrer ( 3 );
b) an emergency discharge valve ( 4 ) located in said vessel bottom ( 2 );
c) at least one filtration device ( 5 ) located in said vessel bottom ( 2 ); and
d) at least one cooling device ( 9 ) located in said vessel bottom ( 2 ) and projecting into the interior of said vessel ( 1 ).
14. The reactor of claim 13 , wherein said filtration device ( 5 ) is a frit which is flush in said vessel bottom ( 2 ).
15. The reactor of claim 13 , wherein said emergency discharge valve is a valve for emptying the reactor in less than 600 seconds.
16. A process for preparing an organic peroxide, comprising the steps of:
a) preparing a solid hydroperoxide in the form of a suspension in the reactor of claim 13 ;
b) filtering the suspension through the filtration device ( 5 ) located in the vessel bottom ( 2 ) while retaining the solid hydroperoxide in the reactor; and
c) reacting the hydroperoxide with an alkylating agent, an acylating agent or a carbonyl compound.
17. The process of claim 16 , wherein said solid hydroperoxide is 2,5-dimethylhexane-2,5-dihydroperoxide.
18. The process of claim 16 , wherein said solid hydroperoxide is suspended in a wash liquid between step b) and step c) and the resulting suspension is filtered through said filtration device ( 5 ) located in the vessel bottom ( 2 ) while retaining the solid hydroperoxide in the reactor.
19. The process of claim 16 , wherein, in step c), said hydroperoxide is reacted with a tertiary alcohol in the presence of a strong acid.
20. The process of claim 16 , wherein, in step c), said hydroperoxide is reacted with an acylating agent selected from the group consisting of: a carboxylic acid chloride, a carboxylic anhydride; and a chloroformate.
21. The process of claim 20 , wherein said acylating agent is a carboxylic acid chloride selected from the group consisting of: acetyl chloride; isobutyryl chloride; pivaloyl chloride; 2-ethylhexanoylchloride; 3,5,5-trimethylhexanoyl chloride;
neodecanoyl chloride; and benzoyl chloride.
22. The process of claim 20 , wherein said acylating agent is a chloroformate selected from the group consisting of: isopropyl chloroformate; n-butyl chloroformate; sec-butyl chloroformate; 2-ethylhexyl chloroformate; myristyl chloroformate; cetyl chloroformate; cyclohexyl chloroformate; and 4-tert-butylcyclohexyl chloroformate.
23. The process of claim 20 , wherein, in step c), said hydroperoxide is reacted with acetone.