CN201006863Y - Vertical type bubbling oxidation reaction device for synthesizing naphthalic acid - Google Patents

Vertical type bubbling oxidation reaction device for synthesizing naphthalic acid Download PDF

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Publication number
CN201006863Y
CN201006863Y CNU2007200051884U CN200720005188U CN201006863Y CN 201006863 Y CN201006863 Y CN 201006863Y CN U2007200051884 U CNU2007200051884 U CN U2007200051884U CN 200720005188 U CN200720005188 U CN 200720005188U CN 201006863 Y CN201006863 Y CN 201006863Y
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China
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straight barrel
length
reaction device
reaction
uniform distribution
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Expired - Fee Related
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CNU2007200051884U
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Chinese (zh)
Inventor
靳海波
佟泽民
郭志武
杨索和
何广湘
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Beijing Institute of Petrochemical Technology
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Beijing Institute of Petrochemical Technology
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Abstract

An upright bubble oxidation reaction device used to synthesize naphthalic acid comprises a straight barrel body (1), a roof board (2), a bottom board (3), a liquid distributing machine (4), regular filler (5), reaction liquid (6), an air distributing machine (7), a feed inlet (8) and a feed outlet (9), the reaction device is mainly an upright barrel-type structure, the reaction device contains the reaction liquid (6) inside, the top of the reaction device is provided with the liquid distributing machine (4) and the regular filler (5), the bottom of the reaction device is provided with the air distributing machine (7) which comprises four to eight jet tubes (71) homogeneously arranged at the center of the bottom of the reaction device. According to the needs of oxidation reaction, the reaction device is provided with a rectifying section (11), a free section (12) and a reaction section (13), and one side of the reaction device is provided with the feed inlet (8) and the feed outlet (9). The utility model without an agitating device is simple in structure, convenient to operation, reliable in working, low in production costs and easy to use and maintain.

Description

The vertical type bubbling oxidation reaction device that a kind of synthesizing naphthalic acid is used
Technical field
The utility model relates to a kind of chemical reaction synthetic equipment, relates 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 purpose of this utility model 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 utility model 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 utlity model has following advantage and effect:
1, the utility model has been controlled oxidizing reaction effectively and has been 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 utility model 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 the utility model structure collectivity cross-sectional schematic
Fig. 2 arranges the first embodiment synoptic diagram for gas distributor jet pipe of the present utility model
Fig. 3 arranges the second embodiment synoptic diagram for gas distributor jet pipe of the present utility model
Fig. 4 realizes 2,6-dialkyl group naphthalene oxidation schema for the utility model
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 utility model liquid phase reaction 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 utility model 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 1/2 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.
Illustrate 2 by Fig. 4,6-dialkyl group naphthalene oxidation schema illustrates the utility model residing status and effect in the oxidation flow process.

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.
CNU2007200051884U 2007-02-16 2007-02-16 Vertical type bubbling oxidation reaction device for synthesizing naphthalic acid Expired - Fee Related CN201006863Y (en)

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Application Number Priority Date Filing Date Title
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101244996B (en) * 2007-02-16 2012-11-21 北京石油化工学院 Vertical type bubbling oxidation reaction device for synthesizing naphthalic acid

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101244996B (en) * 2007-02-16 2012-11-21 北京石油化工学院 Vertical type bubbling oxidation reaction device for synthesizing naphthalic acid

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Granted publication date: 20080116

Termination date: 20110216