CN1207299C

CN1207299C - Cyclodipentene preparation process

Info

Publication number: CN1207299C
Application number: CN 03138766
Authority: CN
Inventors: 吴世华; 司志华; 黄唯平; 于刚; 王道强; 赵维君
Original assignee: NANKAI FINE CHEMICAL SCIENCE AND TECHNOLOGY Co LTD DONGYING
Current assignee: Shandong Dongchang Fine Chemical Technology Co ltd
Priority date: 2003-07-09
Filing date: 2003-07-09
Publication date: 2005-06-22
Anticipated expiration: 2023-07-09
Also published as: CN1513855A

Abstract

The present invention discloses a technological flow path for industrially preparing cyclopentadiene sodium, which comprises the following steps: (1), dicyclopentadiene is depolymerized into single ring pentadiene; (2), the single ring pentadiene is metered and cooled, and the cooling temperature is between subzero 10 DEG C and 10 DEG C; (3), tetrahydrofuran solvents and sodium sand are successively added in a reaction kettle; (4) the feed inlet of the reaction kettle is closed, and air and water contents in the reaction kettle are eliminated; (5) the single ring pentadiene is dropped for preparing cyclopentadiene sodium, and reaction speed is controlled by controlling the addition speed of the single ring pentadiene; (6), a cooling measure is carried out for keeping the temperature of the reaction kettle to be at 0 to 10 DEG C; (7), hydrogen gas produced in the reaction process escapes from exhaust holes arranged at the upper part of the reaction kettle, when hydrogen gas enters a glass liquid sealed bottle through a guide pipe, hydrogen gas is released at a high point, and liquid paraffin wax is contained in the liquid sealed bottle. The technique has the characteristics of simple technology, convenient operation and temperature control and enhances reaction conversion rate and economic benefit.

Description

Produce cyclopentadiene sodium technology

Technical field: the invention discloses a kind of industry and produce the technical process of cyclopentadiene sodium.

Background technology: cyclopentadiene sodium is the compound that cyclopentadiene and sodium Metal 99.5 reaction form, and its purposes is the raw material as high effective gasoline antiknock (cyclopentadienyl manganese), the present domestic correlation technique report that still do not have.

Summary of the invention: purpose of the present invention is exactly the above-mentioned defective that exists at prior art, and a kind of cyclopentadiene sodium technology of producing is provided

Technical process of the present invention comprises: after (1) dicyclopentadiene depolymerizes to the monocycle pentadiene; (2) monocycle pentadiene metering, cooling, 10 ℃ of cooling temperatures--between 10 ℃; (3) in reactor, successively add tetrahydrofuran solvent and sodium sand; (4) capping still charging opening is got rid of reactor hollow G﹠W branch; (5) drip the monocycle pentadiene and produce cyclopentadiene sodium, add monocycle pentadiene speed by control and come controls reaction speed; (6) take cooling provision, with the temperature that keeps reactor at 0 ℃-10 ℃; (7) hydrogen that produces in the reaction process is provided with the venting hole from the top of reactor and overflows, enter glass fluid-tight bottle through conduit after, the emptying of high point fills whiteruss in the fluid-tight bottle.

Present technique innovation part is: 1, the monocycle pentadiene is added in the reactor with the method that drips and react with sodium Metal 99.5, can come control reaction temperature by the control rate of addition, make temperature of reaction be unlikely to too high; 2, because cyclopentadiene normally exists with the dicyclopentadiene form, could participate in reaction after must depolymerizing to the monocycle pentadiene, and the monocycle pentadiene preserves at low temperatures, slow down its autohemagglutination speed, thus the transformation efficiency that raising is reacted; 3, because the rapid oxidation of meeting in air of cyclopentadiene sodium, so necessary strict secluding air in reaction and preservation process, the hydrogen that produces during while allows again and reacts can be overflowed smoothly, adopt glass envelope bottle in the present technique, hydrogen is overflowed by the fluid-tight bottle, can secluding air, can observe reaction end intuitively again; 4, destroyed because cyclopentadiene sodium can react with water, so (particularly tetrahydrofuran (THF)) can not have too many moisture in the reactant, the present technique characteristics are earlier tetrahydrofuran (THF) and sodium Metal 99.5 to be added in the reactor before dripping cyclopentadiene, make that water reacts dehydration in sodium Metal 99.5 and the tetrahydrofuran (THF), just begin to drip the monocycle pentadiene after dehydration is finished.The characteristics of present technique are that technology is simple, and handled easily and temperature control have improved the transformation efficiency and the economic benefit of reaction.

Description of drawings: accompanying drawing is a process flow sheet of the present invention.

Embodiment:

Referring to accompanying drawing, dicyclopentadiene A enters monocycle pentadiene scale tank 2 after depolymerization still 1 depolymerizes to the monocycle pentadiene, be provided with spiral coil cooling tube in the scale tank 2, and scale tank is provided with the cold insulation chuck outward.-10 ℃ refrigerant B enters spiral coil cooling tube and chuck respectively, makes the monocycle pentadiene be in low-temperature condition all the time.Tetrahydrofuran (THF) adds earlier in the reactor 3 as solvent, sodium sand is added in the reactor 3 capping still charging opening again.With nitrogen air displacement in the reactor 3 is fallen, started agitator 4 then and stir.Deng moisture in the tetrahydrofuran (THF) taken off clean after, then begin to drip monocycle pentadiene C and produce cyclopentadiene sodium.Can discharge a large amount of heats in the reaction process, the one, add monocycle pentadiene speed by the control system and come controls reaction speed, speed of response can not be too fast, otherwise the still temperature is raise rapidly, causes the accident; The 2nd, the heat that the reaction back produces is pulled away by the refrigerant B in the reaction chuck, to keep lower still temperature (0 ℃-10 ℃).The hydrogen F that produces row in the reaction is overflowed by reactor top, and behind glass fluid-tight bottle 5, the emptying of high point fills whiteruss, with secluding air in the fluid-tight bottle 5.When no longer including the hydrogen effusion in the fluid-tight bottle, think that reaction finishes, the cyclopentadiene sodium that reaction generates is dissolved in the interior tetrahydrofuran solvent of still, and the tetrahydrofuran solution of cyclopentadiene sodium is the product that will make.

Claims

1, a kind of technology of producing cyclopentadiene sodium is characterized in that technical process comprises: after (1) dicyclopentadiene depolymerizes to the monocycle pentadiene; (2) monocycle pentadiene metering, cooling, 10 ℃ of cooling temperatures--between 10 ℃; (3) in reactor, successively add solvent and sodium sand; (4) capping still charging opening is got rid of reactor hollow G﹠W branch; (5) drip the monocycle pentadiene and produce cyclopentadiene sodium, add monocycle pentadiene speed by control and come controls reaction speed; (6) take cooling provision, with the temperature that keeps reactor at 0 ℃-10 ℃; (7) get rid of the hydrogen that produces in the reaction process.

2, the cyclopentadiene sodium technology of producing according to claim 1, it is characterized in that: described solvent is a tetrahydrofuran (THF).

3, the cyclopentadiene sodium technology of producing according to claim 1 is characterized in that: the hydrogen that produces in the reaction process is provided with the venting hole from the top of reactor and overflows, enter glass fluid-tight bottle through conduit after, the emptying of high point fills whiteruss in the fluid-tight bottle.