CN105195063B - A kind of decarboxylation device that cyclopentanone is prepared for adipic acid - Google Patents
A kind of decarboxylation device that cyclopentanone is prepared for adipic acid Download PDFInfo
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- CN105195063B CN105195063B CN201510630531.3A CN201510630531A CN105195063B CN 105195063 B CN105195063 B CN 105195063B CN 201510630531 A CN201510630531 A CN 201510630531A CN 105195063 B CN105195063 B CN 105195063B
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- adipic acid
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- cyclopentanone
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Abstract
The invention discloses a kind of decarboxylation device that cyclopentanone is prepared for adipic acid, belong to field of chemical equipment.The present invention includes dissolution kettle；Dissolution kettle is provided with the first valve by the first pipeline communication reactor, the first pipeline；Reactor connects the entrance of circulating pump by second pipe, and second pipe is provided with the second valve；The bottom for the fixed bed reactors that the outlet of circulating pump is vertically arranged by the 3rd pipeline communication, the side of fixed bed reactors passes through the 4th pipeline communication reactor；The top of fixed bed reactors is provided with condenser by the 5th pipeline communication receiver, the 5th pipeline；Heat-insulation layer is coated with outside first pipeline, second pipe, the 3rd pipeline, the 4th pipeline and fixed bed reactors.Simple in construction, easy to operate, adipic acid high conversion rate of the invention and cyclopentanone separative efficiency height.
Description
Technical field
The present invention relates to field of chemical equipment, more particularly to a kind of decarboxylation device that cyclopentanone is prepared for adipic acid.
Background technology
At present, domestic cyclopentanone manufacturing enterprise, is all to use heat transfer oil electric heating method, adipic acid to add reaction after melting
Kettle, adds catalyst, and reacting kettle jacketing conduction oil directly heats up, and reactor temperature reaches 250 DEG C -260 DEG C, heat conduction oil temperature
Degree reaches 280 DEG C -290 DEG C.
It is colourless liquid under cyclopentanone, normal temperature, fusing point is -58 DEG C, and boiling point is 130.6 DEG C.It is white under adipic acid, normal temperature
Crystallization, fusing point is 152 DEG C.
This method has the disadvantage：
First, the adipic acid decarboxylation cycle is long, is unfavorable for the performance of equipment capacity；Adipic acid is chronically under hot environment, portion
Divide carbonization, reduce the conversion ratio of adipic acid, add production cost；
2nd, reaction terminates catalyst with the releasing of bottom tar, it is impossible to reclaims, adds production cost.
In view of adipic acid decarboxylation prepares the shortcoming of cyclopentanone presence in the prior art, research and design is a set of de- for adipic acid
The equipment that carboxylic prepares cyclopentanone is significant.
The content of the invention
Not enough in order to make up the above, the invention provides a kind of simple in construction, easy to operate, adipic acid high conversion rate and ring
The high decarboxylation device that cyclopentanone is prepared for adipic acid of pentanone separative efficiency.
The technical scheme is that：
A kind of decarboxylation device that cyclopentanone is prepared for adipic acid, including for containing and melting the dissolution kettle 1 of adipic acid；
The dissolution kettle 1 connects reactor 3 by the first pipeline A, and the first pipeline A is provided with the first valve 2；The reactor 3
The entrance of circulating pump 5 is connected by second pipe B, the second pipe B is provided with the second valve 4；The outlet of the circulating pump 5
The bottom of fixed bed reactors 6 being vertically arranged is connected by the 3rd pipeline C, the sides of the fixed bed reactors 6 passes through the
Four pipeline D connect reactor 3；The top of the fixed bed reactors 6 connects receiver 8, the 5th pipe by the 5th pipeline E
Road E is provided with condenser 7；Outside the first pipeline A, second pipe B, the 3rd pipeline C, the 4th pipeline D and fixed bed reactors 6
Bread is covered with heat-insulation layer.
Preferably, the valve 4 of the first valve 2 and second is check valve.Check valve can prevent adverse current, it is ensured that
That reacts is normally carried out.
Preferably, the dissolution kettle 1 and reactor 3 include agitating device and heater.Heater mesh
For heating and thermal insulation, make adipic acid be in molten state, agitating device ensure homogeneous heating.
Preferably, the 5th pipeline E includes two vertical pipeline sections and an inclination pipeline section, the inclination pipeline section
Between two vertical pipeline sections, the high-end side for being located at close fixed bed reactors 6 for tilting pipeline section；The condenser 7
It is arranged on inclination pipeline section.Cyclopentanone is gaseous state at high temperature, and adipic acid liquid passes through the fixed bed reactors equipped with catalyst and given birth to
Into gaseous cyclopentanone, gaseous state cyclopentanone enters the 5th pipeline by the top of fixed bed reactors.Condenser, which is located at, tilts pipeline section
Condensation effect can be increased, and can prevent condensed cyclopentanone from flowing backward to fixed bed reactors.
Preferably, the 4th pipeline D and the interface of fixed bed reactors 6 top edge and catalyst top surface are neat
It is flat.Unreacted liquid adipic acid flows into reactor 3 by catalyst top layer, and all catalyst can be made to be utilized effectively.Certainly,
As long as the 4th pipeline D can be with as long as ensure unreacted more than catalyst top surface with the interface upper limb of fixed bed reactors 6
Liquid adipic acid circulation flow into reactor 3.
Preferably, the 4th pipeline D is obliquely installed, and the 4th pipeline D is with the interface of fixed bed reactors 6
4th pipeline D's is high-end.4th pipeline D is obliquely installed, and unreacted adipic acid can smoothly flow back to reactor 3.
Using the decarboxylation device of the present invention, when preparing cyclopentanone using adipic acid, adipic acid is first placed in dissolution kettle 1, plus
Heat to adipic acid is completely melt（170-190℃）, it is not necessary to temperature is too high；The adipic acid of liquid is entered by dissolution kettle 1 to react
Kettle 3, liquid adipic acid is further heated to reaction temperature in reactor 3（230-240℃）, then start circulating pump 5, follow
Liquid adipic acid in reactor 3 is pumped to fixed bed reactors 6 by ring pump 5, and adipic acid flows through fixed bed reaction from the bottom to top
Catalyst in device 6, completes decarboxylic reaction in adipic acid from the bottom to top flow process, generates gaseous state cyclopentanone and is steamed with water
Gas and carbon dioxide.The condensed device 7 of gaseous state cyclopentanone gas of generation is received after condensing by receiver 8.And it is unreacted oneself two
Acid flow to reactor 3 by the 4th pipeline D.
The process of cyclopentanone, including step are prepared using the decarboxylation device：
1）Adipic acid is added into dissolution kettle 1, and is heated to 190-200 DEG C, while the heat conduction oil temperature of reactor 3 is added
Heat is to 230-245 DEG C；
2）When adipic acid is completely melt as liquid, the first valve 2 is opened, liquid adipic acid is entered by dissolution kettle 1 to react
When adipic acid temperature in kettle 3, question response kettle 3 is upgraded to 210-220 DEG C, opens the second valve 4 and simultaneously open circulating pump 5, by oneself two
Acid is pumped to fixed bed reactors 6, and adipic acid is from the bottom to top by the catalyst in fixed bed reactors 6；
3）The gaseous state cyclopentanone for reacting generation flows into receiver 8 by the 5th pipeline E, and cyclopentanone flows through the 5th pipeline E mistake
Liquid is cooled in journey；When adipic acid is pumped to the 4th pipeline D and fixed bed reactors 6 interface, unreacted liquid
Intimate diacid flows back to reactor 3 by the 4th pipeline D.
Beneficial effects of the present invention are：
1st, the present invention prepares the decarboxylation device of cyclopentanone for adipic acid, and high temperature adipic acid need not be actionless in reaction
In kettle, but circulated in apparatus of the present invention, solve the problem of adipic acid is carbonized at reactor bottom in the prior art.
2nd, using apparatus of the present invention, catalyst can be repeatedly used, and be economized on resources, and reduce cost.
3rd, it is short reaction time using apparatus of the present invention, and high income；Yield is substantially increased, economic benefit is improved.
4th, apparatus of the present invention are simple in construction, easy to operate, and cyclopentanone separative efficiency is high.
Brief description of the drawings
Fig. 1 prepares the structural representation of the decarboxylation device of cyclopentanone for the present invention for adipic acid.
Embodiment
Embodiment 1
As shown in figure 1, the present invention prepares the decarboxylation device of cyclopentanone for adipic acid, including for containing and melting oneself two
The dissolution kettle 1 of acid.Dissolution kettle 1 connects reactor 3 by the first pipeline A, and the first pipeline A is provided with the first valve 2, in order to prevent
Flow backwards, the first valve 2 is check valve.Dissolution kettle 1 and reactor 3 include agitating device and heater.Heater purpose
For heating and thermal insulation, adipic acid is set to be in molten state, agitating device ensures homogeneous heating.
Reactor 3 connects the entrance of circulating pump 5 by second pipe B, and second pipe B is provided with the second valve 4, in order to anti-
Only flow backwards, the second valve 4 is check valve；The outlet of circulating pump 5 connects the fixed bed reactors being vertically arranged by the 3rd pipeline C
6 bottom.Why fixed bed reactors 6 will be vertically arranged, and be in order that liquid adipic acid passes through catalyst, increasing from the bottom to top
Plus the time of contact of adipic acid and catalyst.
The side of fixed bed reactors 6 connects reactor 3 by the 4th pipeline D；4th pipeline D and fixed bed reactors 6
The top edge of interface is flushed with catalyst top surface.Unreacted liquid adipic acid flows into reactor 3 by catalyst top layer, can make institute
There is catalyst to be utilized effectively.Certainly, if the 4th pipeline D and the interface upper limb of fixed bed reactors 6 catalyst top surface with
On can be with, as long as ensureing that unreacted liquid adipic acid circulation flows into reactor 3.Preferably, the 4th pipeline D
It is obliquely installed, the 4th pipeline D is the high-end of the 4th pipeline D with the interface of fixed bed reactors 6.4th pipeline D is obliquely installed, not instead
The adipic acid answered can smoothly flow back to reactor 3.
The top of fixed bed reactors 6 connects receiver 8 by the 5th pipeline E, and the 5th pipeline E is provided with condenser 7；The
Five pipeline E include two vertical pipeline sections and an inclination pipeline section, and tipping tube section is located between two vertical pipeline sections, tilts the height of pipeline section
End is located at close to the side of fixed bed reactors 6；Vertical pipeline section is as short as possible, the damage flow backwards after the cooling for reducing cyclopentanone
Lose.Condenser 7 is arranged on inclination pipeline section.Cyclopentanone is gaseous state at high temperature, and adipic acid liquid passes through the fixation equipped with catalyst
Bed reactor generates gaseous cyclopentanone, and gaseous state cyclopentanone enters the 5th pipeline by the top of fixed bed reactors.Condenser position
It can increase condensation effect in tilting pipeline section, and can prevent condensed cyclopentanone from flowing backward to fixed bed reactors.
First pipeline A, second pipe B, the 3rd pipeline C, the 4th pipeline D and the outside of fixed bed reactors 6 are coated with insulation
Layer.
Using the decarboxylation device of the present invention, when preparing cyclopentanone using adipic acid, adipic acid is first placed in dissolution kettle 1, plus
Heat to adipic acid is completely melt（190-200℃）, it is not necessary to temperature is too high；The adipic acid of liquid is entered by dissolution kettle 1 to react
Kettle 3, liquid adipic acid is further heated to reaction temperature in reactor 3（210-220℃）, then start circulating pump 5, follow
Liquid adipic acid in reactor 3 is pumped to fixed bed reactors 6 by ring pump 5, and adipic acid flows through fixed bed reaction from the bottom to top
Catalyst in device 6, completes decarboxylic reaction in adipic acid from the bottom to top flow process, generates gaseous state cyclopentanone and is steamed with water
Gas and carbon dioxide.The condensed device 7 of gaseous state cyclopentanone gas of generation is received after condensing by receiver 8.And it is unreacted oneself two
Acid flow to reactor 3 by the 4th pipeline D.
Embodiment 2
The process of cyclopentanone is prepared using the device disclosed in embodiment 1：
1）Adipic acid is added into dissolution kettle 1, and is heated to 190-200 DEG C, while the heat conduction oil temperature of reactor 3 is added
Heat is to 230-245 DEG C；
2）When adipic acid is completely melt as liquid, the first valve 2 is opened, liquid adipic acid is entered by dissolution kettle 1 to react
When adipic acid temperature in kettle 3, question response kettle 3 is upgraded to 210-220 DEG C, opens the second valve 4 and simultaneously open circulating pump 5, by oneself two
Acid is pumped to fixed bed reactors 6, and fixed bed reactors 6 are built with barium hydroxide catalyst, and adipic acid is from the bottom to top by solid
Catalyst in fixed bed reactor 6；
3）The gaseous state cyclopentanone for reacting generation flows into receiver 8 by the 5th pipeline E, and cyclopentanone flows through the 5th pipeline E mistake
Liquid is cooled in journey；When adipic acid is pumped to the 4th pipeline D and fixed bed reactors 6 interface, unreacted liquid
Intimate diacid flows back to dissolution kettle by the 4th pipeline D.
Using apparatus of the present invention, the conversion ratio of adipic acid is 95%, and the separative efficiency of cyclopentanone is more than 95%.
Catalyst in fixed bed reactors 6 of the present invention still has extraordinary catalytic performance after recycling 30 times.
It is computed, 100 kilograms of barium hydroxide catalyst can be catalyzed 15000 kilograms of adipic acid decomposition altogether.
Comparative example 1
The method for preparing cyclopentanone by adipic acid in the prior art：
Adipic acid is added into reactor, heating fusing adds barium hydroxide catalyst, reacting kettle jacketing conduction oil directly rises
Adipic acid temperature reaches 250 DEG C -260 DEG C in temperature, reactor, and heat conduction oil temperature reaches 280 DEG C -290 DEG C.
In existing process, after catalyst is reused 5 times, because carbonization is serious, it is remarkably decreased its catalytic efficiency；Through meter
Calculate, using existing process, 100 kilograms of barium hydroxide catalyst can be catalyzed 7500 kilograms of adipic acid decomposition altogether.
Claims (5)
1. a kind of decarboxylation device that cyclopentanone is prepared for adipic acid, it is characterised in that：Including for containing and melting adipic acid
Dissolution kettle（1）；The dissolution kettle（1）Pass through the first pipeline（A）Connect reactor（3）, first pipeline（A）Provided with the
One valve（2）；The reactor（3）Pass through second pipe（B）Connect circulating pump（5）Entrance, the second pipe（B）On set
There is the second valve（4）；The circulating pump（5）Outlet pass through the 3rd pipeline（C）Connect the fixed bed reactors being vertically arranged（6）
Bottom, the fixed bed reactors（6）Side pass through the 4th pipeline（D）Connect reactor（3）；The fixed bed reactors
（6）Top pass through the 5th pipeline（E）Connect receiver（8）, the 5th pipeline（E）It is provided with condenser（7）；Described first
Pipeline（A）, second pipe（B）, the 3rd pipeline（C）, the 4th pipeline（D）And fixed bed reactors（6）Outside is coated with heat-insulation layer；
First valve（2）With the second valve（4）It is check valve；5th pipeline（E）Including two vertical pipeline sections and one
Pipeline section is tilted, the tipping tube section is located between two vertical pipeline sections, described to tilt the high-end positioned at close to fixed bed reaction of pipeline section
Device（6）Side；The condenser（7）It is arranged on inclination pipeline section.
2. the decarboxylation device of cyclopentanone is prepared for adipic acid as claimed in claim 1, it is characterised in that：The dissolution kettle（1）
And reactor（3）Include agitating device and heater.
3. it is used for the decarboxylation device that adipic acid prepares cyclopentanone as described in claim any one of 1-2, it is characterised in that：Described
Four pipelines（D）With fixed bed reactors（6）The top edge of interface is flushed with catalyst top surface.
4. the decarboxylation device of cyclopentanone is prepared for adipic acid as claimed in claim 3, it is characterised in that：4th pipeline
（D）It is obliquely installed, the 4th pipeline（D）With fixed bed reactors（6）Interface is the 4th pipeline（D）It is high-end.
5. the process of cyclopentanone is prepared using decarboxylation device described in claim 1, it is characterised in that including step：
1）To dissolution kettle（1）Middle addition adipic acid, and be heated to 190-200 DEG C, while by reactor（3）Heat conduction oil temperature add
Heat is to 230-245 DEG C；
2）When adipic acid is completely melt as liquid, the first valve is opened（2）, liquid adipic acid is by dissolution kettle（1）Into reaction
Kettle（3）, question response kettle（3）In adipic acid temperature when being upgraded to 210-220 DEG C, open the second valve（4）And open circulating pump
（5）, adipic acid is pumped to fixed bed reactors（6）, adipic acid is from the bottom to top by fixed bed reactors（6）Interior catalysis
Agent；
3）The gaseous state cyclopentanone of generation is reacted by the 5th pipeline（E）Flow into receiver（8）, cyclopentanone flows through the 5th pipeline（E）'s
During be cooled to liquid；When adipic acid is pumped to the 4th pipeline（D）With fixed bed reactors（6）Interface when, not instead
The liquid adipic acid answered is by the 4th pipeline（D）Flow back to reactor（3）.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510630531.3A CN105195063B (en) | 2015-09-29 | 2015-09-29 | A kind of decarboxylation device that cyclopentanone is prepared for adipic acid |
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| CN201510630531.3A CN105195063B (en) | 2015-09-29 | 2015-09-29 | A kind of decarboxylation device that cyclopentanone is prepared for adipic acid |
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| CN105195063B true CN105195063B (en) | 2017-10-27 |
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| CN105585825A (en) | 2016-03-07 | 2016-05-18 | 杨红梅 | Biodegradable polyester composition |
| CN105713356B (en) | 2016-03-07 | 2017-05-31 | 杨红梅 | A kind of Biodegradable polyester composition |
| CN105585824A (en) | 2016-03-07 | 2016-05-18 | 金发科技股份有限公司 | Biodegradable polyester composition |
| CN109939574A (en) * | 2019-04-17 | 2019-06-28 | 山东国润生物医药有限公司 | A kind of continuous decarboxylic reaction tower of cyclopentanone |
| CN114471403A (en) * | 2022-01-19 | 2022-05-13 | 南京延长反应技术研究院有限公司 | Device and method for polycondensing polyol by using cyclic compound |
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|---|---|---|---|---|
| US2811559A (en) * | 1954-10-22 | 1957-10-29 | Armour & Co | Method of decarboxylating higher fatty acids over magnesium catalysts |
| US5600013A (en) * | 1993-05-28 | 1997-02-04 | Rhone-Poulenc Chimie | Preparation of cyclic ketones |
| CN103044226A (en) * | 2012-12-26 | 2013-04-17 | 淮安万邦香料工业有限公司 | Method for preparing cyclopentanone from adipic acid |
| CN203803486U (en) * | 2013-12-20 | 2014-09-03 | 上海三爱富新材料股份有限公司 | Continuous decarboxylic reaction device |
-
2015
- 2015-09-29 CN CN201510630531.3A patent/CN105195063B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2811559A (en) * | 1954-10-22 | 1957-10-29 | Armour & Co | Method of decarboxylating higher fatty acids over magnesium catalysts |
| US5600013A (en) * | 1993-05-28 | 1997-02-04 | Rhone-Poulenc Chimie | Preparation of cyclic ketones |
| CN103044226A (en) * | 2012-12-26 | 2013-04-17 | 淮安万邦香料工业有限公司 | Method for preparing cyclopentanone from adipic acid |
| CN203803486U (en) * | 2013-12-20 | 2014-09-03 | 上海三爱富新材料股份有限公司 | Continuous decarboxylic reaction device |
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Effective date of registration: 20230413 Address after: 251600 High end raw material drug base north of Keyuan Street and west of Hehe Road in Shanghe County Economic Development Zone, Jinan City, Shandong Province Patentee after: Jinan Dinghao Pharmaceutical Technology Co.,Ltd. Address before: 274000 High tech Development Zone, Mudan District, Heze City, Shandong Province (at the intersection of Changcheng Road and Lanzhou Road) Patentee before: SHANDONG GREEN BIO-PHARMACEUTICAL Co.,Ltd. |