CN101244996A - Vertical type bubbling oxidation reaction device for synthesizing naphthalic acid - Google Patents
Vertical type bubbling oxidation reaction device for synthesizing naphthalic acid Download PDFInfo
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- CN101244996A CN101244996A CNA200710079322XA CN200710079322A CN101244996A CN 101244996 A CN101244996 A CN 101244996A CN A200710079322X A CNA200710079322X A CN A200710079322XA CN 200710079322 A CN200710079322 A CN 200710079322A CN 101244996 A CN101244996 A CN 101244996A
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Abstract
The invention relates to a vertical bubbling oxidation device used for synthesizing naphthalene formic acid, which mainly comprises a cylinder (1), a head cover (2), a bottom cover (3), a liquid distributor (4), a structured packing (5), a reaction liquid (6), a gas distributor (7), a material-inlet (8) and a material-outlet (9); the reaction equipment of which is mainly vertical tubular structure; the top of the vertical tubular structure is provided with the liquid distributor (4), the structure packing (5) and the interior reaction solution(6), and the bottom is provided with the gas distributor (7) composed by ( 4 to 8 ) nozzles (71) evenly distributed from the center of the bottom. The device is provided with a rectifying section (11), a free section (12) and a reaction section (13), and the side of the device is provided with the material-inlet (8) and the material-outlet (9) according to need of the oxidation. The vertical bubbling oxidation device used for synthesizing naphthalene formic acid is simple in structure, convenient in operation, reliable in working, low in cost and simple in application, maintenance and repairing, and does not adopt a mixing device.
Description
Technical field
The present invention relates to a kind of chemical reaction synthetic equipment, relate in particular to oxygen-containing gas oxidation dialkyl group naphthalene preparation 2 in liquid phase, the vertical type bubbling oxidation reaction device of 6-naphthalic acid oxidation products.
Background technology
At present, use 2 abroad, 6-dialkyl group naphthalene oxidation preparation 2, the production technique of 6-naphthalic acid is similar to the production technique that p xylene oxidation prepares terephthalic acid, all adopt the continuously stirring bubbling reactor to realize 2,6-dialkyl group naphthalene liquid phase oxidation reaction, the domestic report of not seeing suitability for industrialized production as yet.The autoclave that band stirs because help conduct heat and the speed up gas and liquid two-phase between mass transfer, and be easy to control, therefore be chosen as 2,6-dialkyl group naphthalene liquid phase oxidation technique reactor.But the shortcoming of this reactor also is conspicuous, mainly is 2 points: the one, and the equipment complexity, maintenance cost is higher, especially there is sealing problem in high-temperature and high-pressure conditions; The 2nd, the energy consumption that stirring needs is also than higher.At the deficiency of stirred reactor, it is very necessary developing the bubbling oxidation reaction device that a kind of new synthesizing naphthalic acid uses.
Summary of the invention
According to background technology, the object of the present invention is to provide a kind of high-efficiency and energy-saving type reaction unit of using at synthesizing naphthalic acid, this device is mainly vertical tubular structure, the top is provided with liquid distributor, structured packing, interior Sheng reaction solution, the bottom is provided with the crucial gas distributor of oxidizing reaction, make oxygen-containing gas pass through reaction zone with reflux type, equipment one side is provided with the vertical type bubbling oxidation reaction device of opening for feed and discharge port.
To achieve these goals, the present invention is achieved through the following technical solutions:
The vertical type bubbling oxidation reaction device that a kind of synthesizing naphthalic acid is used, mainly by straight barrel (1), top cover (2), bottom (3), liquid distributor (4), structured packing (5), reaction solution (6), gas distributor (7), opening for feed (8) and discharge port (9) are formed, and wherein: straight barrel (1) is straight tubular construction, and its length is L, inner diameter is D, the length L of straight barrel (1) should comprise the length of the rectifying section (11) of oxidizing reaction needs, the length of free section (12) and the length H of conversion zone (13), and the length H of its conversion zone (13) should be (60～90) % of straight barrel (1) length L, be preferably (70～80) %, and H/D=2～8; The length of the free section (12) between rectifying section (11) and the conversion zone (13) should be (10～20) % of straight barrel (1) length L; Be provided with in rectifying section (11) present position and have specific surface area α=400～1500, voidage ε=0.90～0.98, the structured packing internals of preferred specific surface area α=600～1200 and voidage ε=0.92～0.96; The volume of the reaction solution (6) of filling should be (40～50) % of straight barrel (1) volume in the straight barrel (1); The top of straight barrel (1) is provided with liquid distributor (4), device has top cover (2) thereon, at bottom device bottom (3) is arranged, and be provided with the gas distributor of forming by distance bottom center uniform distribution (4～8) root jet pipe (71) (7) at its bottom bulkhead place, its total cross-sectional area is (0.5～5) % of straight barrel (1) cross-sectional area, be preferably (1～3) %, every jet pipe (71) is worked off one's feeling vent one's spleen speed for (3～15) m/s, preferred (6～10) m/s; (1/2～2/3) L place at straight barrel (1) is provided with opening for feed (8), is provided with discharge port (9) in straight barrel (1) bottom; The one-piece construction of straight barrel (1) should be able to be born the temperature of (170～240) ℃ and the pressure of (0.8～4) Mpa.
Owing to adopted technique scheme, the present invention to have following advantage and effect:
1, the present invention has controlled oxidizing reaction effectively and has carried out towards the direction of target product, and fully reduces content of by-products, improves the yield and the purity of target product, has reduced production cost simultaneously.
2, the present invention does not adopt whipping appts, and is simple in structure, and reliable operation is cheap, and working service is repaired simple and easy.
Description of drawings
Fig. 1 is a structure collectivity cross-sectional schematic of the present invention
Fig. 2 arranges the first embodiment synoptic diagram for gas distributor jet pipe of the present invention
Fig. 3 arranges the second embodiment synoptic diagram for gas distributor jet pipe of the present invention
Fig. 4 realizes 2 for the present invention, 6-dialkyl group naphthalene oxidation schema
Embodiment
Illustrate by Fig. 1, the vertical type bubbling oxidation reaction device that a kind of synthesizing naphthalic acid is used, mainly by straight barrel 1, top cover 2, bottom 3, liquid distributor 4, structured packing 5, reaction solution 6, gas distributor 7, opening for feed 8 and discharge port 9 are formed, wherein: straight barrel 1 is straight tubular construction, its length is L, and inner diameter is D, and the length L of straight barrel 1 should comprise the length of the rectifying section 11 of oxidizing reaction needs, the length of free section 12 and the length H of conversion zone 13, the length H of its conversion zone 13 should be (60～90) % of straight barrel 1 length L, is preferably (70～80) %, and H/D=2～8; The length of the free section 12 between rectifying section 11 and the conversion zone 13 should be (10～20) % of straight barrel 1 length L; Be provided with in rectifying section 11 present positions and have specific surface area α=400～1500, voidage ε=0.90～0.98, the structured packing internals of preferred specific surface area α=600～1200 and voidage ε=0.92～0.96; The volume of the reaction solution 6 of filling should be (40～50) % of straight barrel 1 volume in the straight barrel 1; The top of straight barrel 1 is provided with liquid distributor 4, device has top cover 2 thereon, at bottom device bottom 3 is arranged, and be provided with the gas distributor of forming by 4～8 jet pipes 71 of distance bottom center uniform distribution 7 at its bottom bulkhead place, its total cross-sectional area is (0.5～5) % of straight barrel 1 cross-sectional area, be preferably (1～3) %, every jet pipe 71 speed of working off one's feeling vent one's spleen is (3～15) m/s, preferred (6～10) m/s; (1/2～2/3) L place at straight barrel 1 is provided with opening for feed 8, is provided with discharge port 9 in straight barrel 1 bottom; The one-piece construction of straight barrel 1 should be able to be born the high temperature of (170～240) ℃ and the pressure of (0.8～4) Mpa.
Other knows, 2 in the liquid phase reaction of the present invention district, and 6-dialkyl group naphthalene and oxidation products thereof pass through reaction unit continuously with the form of complete mixing flow, and oxygen-containing gas passes through reaction zone with reflux type.Oxygen-containing gas is introduced from conversion zone 13 bottoms, and joins in the reactor by gas distributor 7.Gas distributor 7 is the end socket place of bottom, can be formed on the required oxygen in liquid phase reaction district.This pattern helps improving the selectivity of target product, because 2, the oxidation mechanism of 6-diisopropylnaphthalene is comparatively complicated, need the single sec.-propyl of experience to be oxidized to ketone or keto-alcohol, then be oxidized to acid, then second sec.-propyl correspondingly becomes acid by this stage oxidation, also have snperoxiaized side reaction to cause naphthalene nucleus fracture and generation trimellitic acid simultaneously, so adopt the direct air inlet of reaction zone, fully reach raw material, catalyzer mixes with oxygen-containing gas, the controlled oxidation reaction is carried out towards the direction of target product well, can fully reduce content of by-products, improves the yield and the purity of target product.
The gas distribution that charges into reactor has a very important role to oxidizing reaction, is illustrated by Fig. 2 and Fig. 3, and important structure of the present invention is formed the jet pipe of gas distributor 7 and arranged the synoptic diagram of two kinds of scheme implementation examples.
First embodiment be four jet pipes 71 apart from the center 1/2 radius R place uniform distribution, or jet pipe 71 in center, three jet pipes 71 of decentering 1/1 radius R place uniform distribution.
Second embodiment be eight jet pipes 71 apart from the center 1/2 radius R place uniform distribution, or four jet pipes 71 of decentering 1/3 radius R place uniform distribution, at decentering 2/3 radius R place uniform distribution four jet pipes 71 in addition, and both stagger mutually.
Claims (3)
1. vertical type bubbling oxidation reaction device that synthesizing naphthalic acid is used, mainly by straight barrel (1), top cover (2), bottom (3), liquid distributor (4), structured packing (5), reaction solution (6), gas distributor (7), opening for feed (8) and discharge port (9) are formed, and it is characterized in that: straight barrel (1) is straight tubular construction, and its length is L, inner diameter is D, the length L of straight barrel (1) should comprise the length of the rectifying section (11) of oxidizing reaction needs, the length of free section (12) and the length H of conversion zone (13), and the length H of its conversion zone (13) should be (60～90) % of straight barrel (1) length L, be preferably (70～80) %, and H/D=2～8; The length of the free section (12) between rectifying section (11) and the conversion zone (13) should be (10～20) % of straight barrel (1) length L; Be provided with in rectifying section (11) present position and have specific surface area α=400～1500, voidage ε=0.90～0.98, the structured packing internals of preferred specific surface area α=600～1200 and voidage ε=0.92～0.96; The volume of the reaction solution (6) of filling should be (40～50) % of straight barrel (1) volume in the straight barrel (1); The top of straight barrel (1) is provided with liquid distributor (4), device has top cover (2) thereon, at bottom device bottom (3) is arranged, and be provided with the gas distributor of forming by distance bottom center uniform distribution (4～8) root jet pipe (71) (7) at its bottom bulkhead place, its total cross-sectional area is (0.5～5) % of straight barrel (1) cross-sectional area, be preferably (1～3) %, every jet pipe (71) is worked off one's feeling vent one's spleen speed for (3～15) m/s, preferred (6～10) m/s; (1/2～2/3) L place at straight barrel (1) is provided with opening for feed (8), is provided with discharge port (9) in straight barrel (1) bottom; The one-piece construction of straight barrel (1) should be able to be born the temperature of (170～240) ℃ and the pressure of (0.8～4) Mpa.
2. the vertical type bubbling oxidation reaction device that synthesizing naphthalic acid according to claim 1 is used, it is characterized in that: gas distributor (7) be four jet pipes (71) apart from the center 1/2 radius R place uniform distribution, or the jet pipe in center (71), decentering 1/2 three jet pipes of radius R place uniform distribution (71).
3. the vertical type bubbling oxidation reaction device that synthesizing naphthalic acid according to claim 1 is used, it is characterized in that: gas distributor (7) be eight jet pipes (71) apart from the center 1/2 radius R place uniform distribution, or decentering 1/3 four jet pipes of radius R place uniform distribution (71), at decentering 2/3 radius R place uniform distribution four jet pipes (71) in addition, and both stagger mutually.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710079322XA CN101244996B (en) | 2007-02-16 | 2007-02-16 | Vertical type bubbling oxidation reaction device for synthesizing naphthalic acid |
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| Application Number | Priority Date | Filing Date | Title |
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| CN200710079322XA CN101244996B (en) | 2007-02-16 | 2007-02-16 | Vertical type bubbling oxidation reaction device for synthesizing naphthalic acid |
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| CN101244996A true CN101244996A (en) | 2008-08-20 |
| CN101244996B CN101244996B (en) | 2012-11-21 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010321A (en) * | 2010-12-04 | 2011-04-13 | 宜兴市恒兴精细化工有限公司 | Process for continuously producing isobutyric acid |
| CN114832738A (en) * | 2021-08-30 | 2022-08-02 | 煤炭科学技术研究院有限公司 | Reactor with a reactor shell |
| CN116063260A (en) * | 2021-10-29 | 2023-05-05 | 中化学科学技术研究有限公司 | Continuous oxidation process of chloro-o-xylene |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH078821B2 (en) * | 1986-09-26 | 1995-02-01 | 三井石油化学工業株式会社 | Method for producing aromatic carboxylic acid |
| CN1328236C (en) * | 2005-01-21 | 2007-07-25 | 浙江大学 | Oxidizing device for producing aromatic carboxylic acid |
| CN201006863Y (en) * | 2007-02-16 | 2008-01-16 | 北京石油化工学院 | Vertical type bubbling oxidation reaction device for synthesizing naphthalic acid |
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- 2007-02-16 CN CN200710079322XA patent/CN101244996B/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010321A (en) * | 2010-12-04 | 2011-04-13 | 宜兴市恒兴精细化工有限公司 | Process for continuously producing isobutyric acid |
| CN114832738A (en) * | 2021-08-30 | 2022-08-02 | 煤炭科学技术研究院有限公司 | Reactor with a reactor shell |
| CN116063260A (en) * | 2021-10-29 | 2023-05-05 | 中化学科学技术研究有限公司 | Continuous oxidation process of chloro-o-xylene |
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