CN1762568A - Novel catalytic reaction and separation device - Google Patents
Novel catalytic reaction and separation device Download PDFInfo
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- CN1762568A CN1762568A CN 200510029723 CN200510029723A CN1762568A CN 1762568 A CN1762568 A CN 1762568A CN 200510029723 CN200510029723 CN 200510029723 CN 200510029723 A CN200510029723 A CN 200510029723A CN 1762568 A CN1762568 A CN 1762568A
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Abstract
The invention discloses a new catalysis reaction with separation device. Wherein, one opening of heating container connects with separator; arranging a reactor on upper port of a feeding pole linked with separator; putting catalyst layer in reactor with upper port connected to middle opening of cluster connecting pipe linked with pressure-sustaining drop device and cooling pipe respective on left and right joint openings; connecting decompressor and two receivers by one connection pipe on upper port of cooling pipe; connecting the water separator with valve on cluster connecting pipe of cooling pipe lower with middle opening of receiver; connecting separator to receiver by side branch pipe; inserting a thermometer in middle interface of cluster connecting pipe to solid-catalyst layer of rector 4 to measure its temperature. This invention needs not to consider fill method of catalyst to execute reaction and separation.
Description
Technical field
The present invention relates to a kind of catalytic reaction and be integrated, reach reaction and separate the device that carries out simultaneously with separating.More particularly, in the presence of solid catalyst, acid and alcohol carry out esterification, its boiling point of ester of obtaining of reaction be higher than acid and pure boiling point and realization response with separate the device that carries out simultaneously.
Background technology
The catalytic distillation process is a kind of new Chemical Engineering method that grows up the eighties in last century, and it is that catalytic reaction and rectifying separation process are integrated, and reaches reaction and carries out with separating simultaneously.At present, catalytic rectification process is solid catalyst to be made the filler (being called catalytic filler) with certain geometrical shape insert in the reaction fractionating tower, this just requires catalyst that bigger granularity is arranged, sometimes catalyst to be processed into form of bio-carrier with Web materials, the solid catalyst of a lot of better performances is thinner because of granularity, be difficult for being processed into the required form of bio-carrier of catalytic distillation and can't use, have because of catalyst granules too thin, so that resistance is big in the catalytic distillation process, be difficult to realize catalytic distillation, and cause general liquid phenomenon, thereby, limited the practical application of catalytic distillation.Therefore, need a kind of filling mode that need not to consider catalyst, do not worry vapour lock, general liquid phenomenon, and, can under normal pressure or decompression, can both implement to react and a kind of device of separation process.
Summary of the invention
The present invention will provide a kind of filling mode that need not to consider catalyst, and, can under normal pressure or decompression, can both implement to react and a kind of novel catalytic reaction and the separator of separation process.
In order to realize the technical scheme of the object of the invention employing: a kind of novel catalytic reaction and separator comprise Heated container, separator, reactor.Wherein, a mouth of Heated container connects separator, be connected with filled column on the separator, be connected with reactor on the filled column upper port, be equipped with catalyst layer in the reactor, the reactor upper port links to each other with mouth in the bull tube connector, be connected with the constant voltage liquid-drop machine on the connector of bull tube connector left side, be connected with condenser pipe on the connector of right side, the condenser pipe upper port connects decompressor and two receivers by a communicating pipe, wherein, be connected by valve between communicating pipe and two receivers; Condenser pipe has valve on the bull tube connector of below water knockout drum links to each other with mouth in the receiver; Separator links to each other with receiver with valve by the side arm; Be inserted with thermometer in the interface in the bull tube connector, and thermometer is inserted in the catalyst layer of reactor 4, is used to measure the temperature of catalyst reactor layer.Catalyst in the catalyst layer is a solid catalyst.
Separator is by outer tube, recipient is formed with the L shaped pipe of band vacuum valve, and wherein connector links to each other with Heated container with filled column about the outer tube, can adopt insertion connection or flange to connect, the diameter of connector is 1/2 of an outer tube diameter, and the height of outer tube is 2 times of its diameter; Recipient is infundibulate, bore and highly be respectively 6/5 times and 1/2 times of its connector diameter; The vertical end of L shaped pipe is fixed on the bottom of recipient, it highly is 1/2 of a recipient height, diameter is 1/3 of a recipient bore, place in the middle of the vertical component effect, the spout hole that to have a diameter be vertical component effect diameter 1/2, the horizontal position of L shaped pipe is fixed on the outer tube, it highly is positioned at from 10mm place, outer tube lower end, the funneled ports of recipient is 1/2 of a recipient bore apart from the last connector of separator, the diameter of the horizontal position diameter of L shaped pipe and the vertical component effect of L shaped pipe is identical, has vacuum valve on the horizontal external part of L shaped pipe.
Reactor is made up of outer tube and inner sleeve, wherein connector links to each other with the bull tube connector with filled column about the outer tube, can adopt to insert and connect or the flange connection, the diameter of connector is 1/2 of an outer tube diameter, the height of outer tube is 4-10 a times of its diameter, the upper end bore of inner sleeve is 6/5 times of connector diameter, the stack shell diameter of inner sleeve is identical with the connector diameter, the bottom is airtight, the side of being close to the bottom has 4 apertures of dividing equally, hole diameter is about 1/3 of an inner sleeve diameter, be 2 times away from bottom to the hole diameter place, card is installed, and inner sleeve is fixed on the inboard of outer tube, and the diameter of connector up and down of its top and distance from bottom outer tube is identical with the stack shell diameter of inner sleeve.
The present invention is owing to adopted by Heated container, separator, reactor, constant voltage liquid-drop machine, condenser pipe, catalytic reaction and separator that receiver etc. are formed, therefore, need not to consider the filling mode of catalyst, do not worry vapour lock, general liquid phenomenon, and, can under normal pressure or decompression, can both implement catalytic reaction and separation process.
Description of drawings
Fig. 1 is a structural representation of the present invention.
The specific embodiment
The present invention is further illustrated below in conjunction with drawings and Examples.
As shown in Figure 1, a kind of novel catalytic reaction and separator, an interface of Heated container 1 connects separator 2, separator 2 upper port bonding pad posts 3, filled column 3 upper port coupled reaction devices 4, reactor 4 upper port connect bull tube connector 5, insert thermometer among the middle interface 5a of bull tube connector 5, and thermometer is inserted among the catalyst layer 4a of reactor 4.Be equipped with catalyst layer 4a in the reactor, catalyst is a solid catalyst.Be equipped with constant voltage liquid-drop machine b on the connector 5b of left side in the bull tube connector 5
1, being equipped with condenser pipe 6 on the connector 5c of right side, condenser pipe 6 connects decompressor and receiver a by a communicating pipe
1With receiver a
2, communicating pipe and receiver a
1And receiver a
2Between valve is housed; Arm is a water knockout drum 7 under the connector 5c of right side, and water knockout drum 7 has valve 7a, by the connector connection receiver a of valve 7a bottom
1, the side arm of separator 2 connects receiver a by valve 2a
2
Separator 2 is made up of the L shaped pipe of outer tube 2c and recipient 2b and band vacuum valve.Outer tube 2c is connecting portion up and down, according to the material difference, adopts to insert to connect to be connected with flange, and the diameter of connector is about 1/2 of an outer tube diameter, and the height of outer tube 2c is about 2 times of its diameter.Recipient 2b is a funnel-shaped structure, bore and highly be respectively about 6/5 times and 1/2 times of connector diameter.The vertical end of L shaped pipe is fixed on recipient 2b bottom, and it highly is about 1/2 of a recipient 2b height, and diameter is about 1/3 of a recipient 2b bore, and locates in the middle of the vertical component effect of L shaped pipe, opens the spout hole that a diameter is a vertical component effect diameter about 1/2.The horizontal position of L shaped pipe is fixed on the outer tube, and it highly is positioned at from 10mm place, outer tube 2c lower end, and the diameter of diameter and vertical component effect is identical, band vacuum valve 2a on the horizontal external part of L shaped pipe.
Reactor 4 is made up of outer tube 4b and inner sleeve 4c.Outer tube 4b is connecting portion up and down, according to used material, adopt to insert to connect and be connected with flange, the diameter of connector is about 1/2 of an outer tube diameter, the height of outer tube 4b is 4-10 a times of its diameter, the upper end bore of inner sleeve 4c is about 6/5 times of connector diameter, the stack shell diameter of inner sleeve 4c is identical with the connector diameter, shut the bottom, be close to the side of bottom and open 4 apertures of dividing equally, hole diameter is about 1/3 of an inner sleeve diameter, be 2 times away from bottom to the hole diameter place, card is installed, inner sleeve 4c is fixed on the inboard of outer tube 4b, after inner sleeve 4c was fixing, the diameter of connector up and down of its top and distance from bottom outer tube 4b was identical with the stack shell diameter of inner sleeve.
Each assembly of the present invention can adopt following two kinds of materials commonly used:
One. glass material
Heating container 1 all adopts the insertion of standard 24 grounds to be connected with separator 2, separator 2 and filled column 3, filled column 3 and reactor 4, reactor 4 and bull tube connector 5, bull tube connector 5 and condenser pipe 6.Water knockout drum 7 and receiver a
1The employing pressure hose connects.Communicating pipe is adopted pressure hose.
Two. metal material
Heating container 1 all adopts flange to be connected with separator 2, separator 2 and filled column 3, filled column 3 and reactor 4, reactor 4 and bull tube connector 5, bull tube connector 5 and condenser pipe 6.Water knockout drum 7 and receiver a
1The employing metallic conduit connects.Communicating pipe is adopted metallic conduit.
The invention process method one:
Heat Heated container 1 earlier, make the ester gasification that adds in advance in the Heated container 1, then, drip the mixed liquor of acid and alcohol, make acid, alcohol is reaction in reactor 4, reactant liquor flow to packed tower 3 through the below of reactor 4 spout hole, in packed tower 3, and unreacted acid, water and ester steam generation heat exchange that alcohol and reaction generate, make unreacted acid, the water volatilization that alcohol and reaction generate, its rising steam is in reactor 4, outer tube 4b is between 4c, enter spherical condensation tube 6, after the cooling, water-oil separating in water knockout drum 7, acid, alcohol reenters reaction in the reactor 4.Product ester from reactor 4 below spout holes flow out after packed tower separates, from being arranged in the recipient 2b of packed tower 3 lower ends, flows out with certain reflux ratio, by receiver a
2Collect.
In the Heated container 1, the purpose that adds ester in advance is to guarantee in course of reaction, can obtain the ester of higher degree.
In the course of reaction, when using resin catalyst, because resin catalyst has certain heat endurance, temperature is crossed high resin and is just lost catalytic effect, so gasification temperature of reactant liquor, just need decompression if be higher than the catalytic temperature of resin catalyst, make the rising vapor (steam) temperature of reactant liquor, be controlled at the catalytic temperature scope of resin by decompression.
Implementation method two:
After will counting the even mixing of gram resin and a certain amount of quartz sand, join among the inner sleeve 4c of reactor 4, in the there-necked flask of 250ml, add the n-butyl acetate of tens of milliliters 98%, in constant pressure funnel, add the mixed liquor of acetate, n-butanol.The heating there-necked flask, make the n-butyl acetate gasification in the flask, after treating that n-butyl acetate steam rises to condenser pipe 6, when condensation reflux liquid is arranged, begin to drip the mixed liquor of acetate and n-butanol, simultaneously, open the valve on the recipient a1, collect the n-butyl acetate that reaction obtains, and regularly divide and remove the water that reaction generates in the water knockout drum 7.
Implementation method three:
After will counting the even mixing of gram resin and a certain amount of quartz sand, join among the inner sleeve 4c of reactor 4; In the there-necked flask of 250ml, add the isoamyl acetate of tens of milliliters more than 98%, in constant pressure funnel b1, add the mixed liquor of acetate, isoamyl alcohol.Decompression down, the heating there-necked flask, make the isoamyl acetate gasification, after treating that isoamyl acetate steam rises to condenser pipe 6, when condensation reflux liquid is arranged, begin to drip acetate and isoamyl alcohol mixed liquor, simultaneously, open the valve on the recipient a1, collect the isoamyl acetate that reaction obtains, and regularly divide and remove the water that reaction generates in the water knockout drum 7.
Claims (4)
1. novel catalytic reaction and separator, comprise Heated container (1), separator (2), reactor (4), it is characterized in that, a mouth of described Heated container (1) connects separator (2), be connected with filled column (3) on the separator (2), be connected with reactor (4) on filled column (3) upper port, be equipped with catalyst layer (4a) in the reactor (4), reactor (4) upper port links to each other with mouth in the bull tube connector (5), is connected with constant voltage liquid-drop machine (b1) on the bull tube connector left side connector (5b), be connected with condenser pipe (6) on the right side connector (5c), condenser pipe (6) upper port by connect a communicating pipe decompressor and receiver (a1, a2), wherein, (a1 connects by valve between a2) for communicating pipe and receiver; Condenser pipe (6) has valve (7a) on below bull tube connector (5) water knockout drum (7) links to each other with mouth in the receiver (a1); Separator (2) links to each other with receiver (a2) with valve (2a) by the side arm; Be inserted with thermometer in the middle interface of bull tube connector (5), and thermometer is inserted in the catalyst layer of reactor (4), is used for measuring the temperature of reactor (4) catalyst layer (4a).
2. described novel catalytic reaction of root a tree name claim 1 and separator, it is characterized in that, described separator (2) is by outer tube (2c), the L shaped pipe of recipient (2b) and band vacuum valve is formed, wherein outer tube (2c) up and down connector link to each other with Heated container (1) with filled column (3), can adopt to insert to connect or the flange connection, the diameter of connector is 1/2 of outer tube (2c) diameter, and the height of outer tube (2c) is 2 times of its diameter; Recipient (2b) is infundibulate, bore and highly be respectively 6/5 times and 1/2 times of its connector diameter; The vertical end of L shaped pipe is fixed on the bottom of recipient (2b), it highly is 1/2 of recipient (2b) height, diameter is 1/3 of recipient (2b) bore, place in the middle of the vertical component effect, the spout hole that to have a diameter be vertical component effect diameter 1/2, the horizontal position of L shaped pipe is fixed on the outer tube (2c), it highly is positioned at from 10mm place, outer tube (2c) lower end, the funneled ports of recipient is 1/2 of a recipient bore apart from the last connector of separator, the horizontal position diameter of L shaped pipe is identical with the diameter of the vertical component effect of L shaped pipe, has vacuum valve (2a) on the horizontal external part of L shaped pipe.
3. described novel catalytic reaction of root a tree name claim 1 and separator, it is characterized in that, described reactor (4) is made up of outer tube (4b) and inner sleeve (4c), wherein outer tube (4b) up and down connector link to each other with bull tube connector (5) with filled column (3), can adopt to insert and connect or the flange connection, the diameter of connector is 1/2 of outer tube (4b) diameter, the height of outer tube (4b) is 4-10 a times of its diameter, the upper end bore of inner sleeve (4c) is 6/5 times of connector diameter, the stack shell diameter of inner sleeve (4c) is identical with the connector diameter, the bottom is airtight, the side of being close to the bottom has 4 apertures of dividing equally, hole diameter is about 1/3 of inner sleeve (4c) diameter, be 2 times away from bottom to the hole diameter place, card is installed, and inner sleeve (4c) is fixed on the inboard of outer tube (4b), and the diameter of connector up and down of its top and distance from bottom outer tube (4b) is identical with the stack shell diameter of inner sleeve.
4. described novel catalytic reaction of root a tree name claim 1 and separator is characterized in that, employed catalyst is a solid catalyst in the described catalyst layer (4a).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100297235A CN100371062C (en) | 2005-09-16 | 2005-09-16 | Novel catalytic reaction and separation device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100297235A CN100371062C (en) | 2005-09-16 | 2005-09-16 | Novel catalytic reaction and separation device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1762568A true CN1762568A (en) | 2006-04-26 |
| CN100371062C CN100371062C (en) | 2008-02-27 |
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ID=36747017
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100297235A Expired - Fee Related CN100371062C (en) | 2005-09-16 | 2005-09-16 | Novel catalytic reaction and separation device |
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| Country | Link |
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| CN (1) | CN100371062C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102814205A (en) * | 2011-06-09 | 2012-12-12 | 上海恩氟佳科技有限公司 | Self-stirring distillation reactor |
| CN103822937A (en) * | 2012-11-16 | 2014-05-28 | 哈尔滨飞机工业集团有限责任公司 | Boiling point testing method for trichloroethylene bath solution |
| CN105381622A (en) * | 2015-10-16 | 2016-03-09 | 哈尔滨理工大学 | Continuous reduced pressure distillation apparatus and method for refining branched fatty acyl chloride by using apparatus thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1036648C (en) * | 1994-07-16 | 1997-12-10 | 广西大学 | Method and equipment for continuous catalyzing rectifying production of n-butyester acetate |
| US6833483B2 (en) * | 2001-01-16 | 2004-12-21 | The Governors Of The University Of Alberta | Process for production of alcohols |
| CN2513666Y (en) * | 2001-11-22 | 2002-10-02 | 上海应用技术学院 | Depressing continuous catalytic reacting and separating device with condensation double sleeves |
-
2005
- 2005-09-16 CN CNB2005100297235A patent/CN100371062C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102814205A (en) * | 2011-06-09 | 2012-12-12 | 上海恩氟佳科技有限公司 | Self-stirring distillation reactor |
| CN103822937A (en) * | 2012-11-16 | 2014-05-28 | 哈尔滨飞机工业集团有限责任公司 | Boiling point testing method for trichloroethylene bath solution |
| CN105381622A (en) * | 2015-10-16 | 2016-03-09 | 哈尔滨理工大学 | Continuous reduced pressure distillation apparatus and method for refining branched fatty acyl chloride by using apparatus thereof |
| CN105381622B (en) * | 2015-10-16 | 2017-08-18 | 哈尔滨理工大学 | The method that Branched fatty acyl chlorides is refined using continuous vacuum distillation apparatus |
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| Publication number | Publication date |
|---|---|
| CN100371062C (en) | 2008-02-27 |
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Granted publication date: 20080227 Termination date: 20100916 |