CN202078886U - Circulating reactor for preparing hydroquinone through phenol hydroxylation - Google Patents

Circulating reactor for preparing hydroquinone through phenol hydroxylation Download PDF

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Publication number
CN202078886U
CN202078886U CN2011201630081U CN201120163008U CN202078886U CN 202078886 U CN202078886 U CN 202078886U CN 2011201630081 U CN2011201630081 U CN 2011201630081U CN 201120163008 U CN201120163008 U CN 201120163008U CN 202078886 U CN202078886 U CN 202078886U
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China
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main reactor
storage tank
hydrogen peroxide
reactor
cooling water
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Expired - Fee Related
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CN2011201630081U
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Chinese (zh)
Inventor
孔岩
张宝龙
孔庆虎
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JIANGSU HONGYUAN CHEMICAL CO Ltd
Nanjing Tech University
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JIANGSU HONGYUAN CHEMICAL CO Ltd
Nanjing Tech University
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Abstract

The utility model relates to a circulating reactor for preparing hydroquinone through phenol hydroxylation, which consists of a main reactor, a material condensation storage tank and a hydrogen peroxide storage tank; a plurality of double-layer reaction tubes are arranged in the main reactor, the outer layer is a reaction material channel, and the inner layer is a porous straight pipe for circulating hydrogen peroxide, a material, hydrogen peroxide, a cooling water inlet and a temperature measuring instrument are arranged at the lower end of the main reactor, a material, hydrogen peroxide, a cooling water outlet and a temperature measuring instrument are arranged at the upper end of the main reactor, a cooling water jacket is arranged outside the material condensation storage tank and a condensate pipe is arranged inside the material condensation storage tank for secondary condensation of the material; the material inlet at the upper end is connected with the material outlet of the main reactor, the outlet at the lower end is provided with a tee port which is respectively connected with the main reactor and a separating device. The hydrogen peroxide storage tank and the main reactor also form a circulating system. The main reactor and the upper end of the material condensation storage tank are respectively provided with an emptying port which is connected with a recycling device so as to ensure the reaction to be carried out under normal pressure.

Description

The loop reactor that is used for the phenol hydroxylation preparing benzenediol
Technical field
The utility model relates to a kind of reactor that is used for the phenol hydroxylation preparing benzenediol, particularly is applied to the loop reactor that the continuous hydroxylating of phenol and hydrogen peroxide prepares benzenediol.
Background technology
Benzenediol comprises catechol and hydroquinones, and its application is very extensive.Catechol is important agricultural chemicals and medicine intermediate, can be used for producing spices (as piperonal), dyestuff, photosensitive material, plated material, extraordinary ink, antioxidant, bactericide, light stabilizer, anticorrisive agent and promoter etc.Hydroquinones is mainly as the stabilizing agent of the developer of photographic film, anthraquinone dye, azo dyes, synthetic ammonia sulfur removal technology secondary solvent, rubber antioxidant, polymerization inhibitor, coating varnish and gasoline antioxidant etc.
Traditional benzenediol production technology, be that o-chlorphenol alkaline hydrolysis legal system catechol and aniline oxidation method for preparing hydroquinones are eliminated, and be the technology of oxidant oxidation phenol preparing benzenediol with the hydrogen peroxide, simple because of flow process, reaction condition is gentle, hydrogen peroxide is inexpensive, product is that water is pollution-free, becomes the research focus of chemical field.At present, in the world the process route of Kai Fa hydrogen peroxide oxidation phenol production benzenediol to have with the inorganic acid be the Rh ó ne-Poulenc method of catalyst and Ube method, be the Brichima method of catalyst with inorganic salts, these methods need be raw material with the high-strength hydrogen peroxide, and flow process is complicated and exist homogeneous reaction itself to be difficult to overcome shortcoming, raw material consumption height and the low problem of benzenediol selectivity, thereby limited it in industrial promotion and application.Its Ube method stops production, and the Brichima method is replaced by the Enichem method.The Enichem method with the TS-1 molecular sieve as phenyl hydroxylating catalyst, built up the process units of 5000t/a in 1986, and industry moves successfully, causes the extensive concern and the great attention of global petrochemical industry, is considered to a milestone on 20 end of the century molecular sieve catalyst development histories.Though the Enichem method has the advantage that the yield index is better, use heterogeneous catalyst and technology thereof,, use titanium-silicon molecular sieve catalyst cost height, need acetone to do solvent and frequent regeneration.
The patent No. is that the Chinese patent of ZL02261515.6 discloses a kind of reactor that phenol hydroxylation is produced benzenediol that is applied to, although this reactor can carry out successive reaction, but exist the material back-mixing serious, structure of reactor is complicated, shortcomings such as reaction selectivity is lower, thus technical-economic index influenced.
The patent No. is that the Chinese patent of ZL200920036553.7 also discloses a kind of tubular reactor that phenol hydroxylation is produced benzenediol that is used for, although this tubular reactor is having certain improvement aspect material back-mixing and the selectivity, but its device manufacturing process is higher than complexity and cost, occupation of land is many, energy consumption is bigger, is unfavorable for increasing economic efficiency.
Summary of the invention
Technical problem to be solved in the utility model is the shortcoming at existing apparatus and technology, as install the manufacturing process complexity and cost is higher, it is many to take up an area of, quiet run stability is bad etc. continuously, proposed a kind of circulating, synthesis under normal pressure, simple in structure, take up an area of less, loop reactor that continuous quiet run stability is used for the phenol hydroxylation preparing benzenediol preferably.
The technical solution of the utility model is: a kind of loop reactor that is used for the phenol hydroxylation preparing benzenediol, its construction features are made up of main reactor, material condensation storage tank and hydrogen peroxide stock chest three parts.Be provided with many double-deck reaction tubes in the main reactor, skin is the reaction mass passage, and internal layer is the straight tube with holes that is circulated throughout hydrogen oxide; The main reactor lower end is provided with material, hydrogen peroxide and cooling water inlet, temperature instrumentation, and the upper end is provided with material, hydrogen peroxide and coolant outlet, temperature instrumentation.Material condensation fluid reservoir has cooling water jecket outward, in condensate pipe is arranged, be used for the time condensation of material; The upper end charging aperture links to each other with the main reactor discharging opening; The lower end outlet is provided with three ports, links to each other with separator with main reactor respectively.Hydrogen peroxide reservoir and main reactor are also formed the circulatory system.Main reactor and material condensation storage tank upper end are provided with drain, link to each other with retracting device, guarantee to be reflected under the normal pressure to carry out.
Concrete technical scheme of the present utility model is: a kind of loop reactor that is used for the phenol hydroxylation preparing benzenediol, form by main reactor, material condensation storage tank and hydrogen peroxide stock chest; Wherein be provided with many double-deck reaction tubes in the main reactor, the main reactor bottom is provided with material inlet, hydrogen peroxide import, downside is provided with cooling water inlet, the top is provided with material outlet, hydrogen peroxide outlet and temperature instrumentation, upside is provided with coolant outlet, wherein double-deck reaction tube internal layer is the straight tube with holes that is circulated throughout hydrogen oxide that has aperture, and the outer interlayer of straight tube with holes and double-deck reaction tube is the reaction mass passage; The material condensation storage tank outside is provided with cooling water jecket, cooling water jecket upside correspondence is provided with the cooling water inlet of cooling water jecket and the coolant outlet of cooling water jecket, in the material condensation storage tank condenser pipe is arranged, wherein the condenser pipe lower end is provided with the condenser pipe cooling water inlet, and the upper end is provided with the condenser pipe coolant outlet; Material condensation storage tank top is provided with material condensation storage tank material inlet, and this material inlet links to each other with the main reactor material outlet; Material condensation storage tank lower end is provided with material condensation storage tank material outlet, connects three ports under the material outlet, links to each other with main reactor by leading to the main reactor mouth of pipe respectively, links to each other with separator by leading to the separator mouth of pipe; The hydrogen peroxide reservoir is by forming the circulatory system with the hydrogen peroxide import and the outlet of main reactor top hydrogen peroxide of main reactor bottom with main reactor; The main reactor upper end is provided with the main reactor drain, and material condensation storage tank upper end is provided with drain, and the main reactor drain links to each other and links to each other with retracting device by the connector that links to each other with retracting device with material condensation storage tank drain.
The height of preferred above-mentioned main reactor is a 1-10 rice, and internal diameter is a 0.5-5 rice.Preferred above-mentioned double-deck tube length of reaction tube is a 0.5-9.5 rice, and internal diameter is the 20-150 millimeter; The quantity of many double-deck reaction tubes is the 10-50 root in the main reactor.Preferred above-mentioned length of straight pipe with holes equates that with double-deck tube length of reaction tube double-deck reaction tube is 1.5-5 with the diameter ratio of straight tube with holes: 1; Hole diameter on the wherein preferred described straight tube with holes is the 1-10 millimeter; Little hole number is 20-200, is uniformly distributed on the straight tube with holes.
Preferred described material condensation storage tank height is a 0.5-3 rice, and internal diameter is a 0.5-3 rice; The condensation section length of spiral in material condensation storage tank is 3-150 rice, internal diameter 10-30 millimeter.Preferred described hydrogen peroxide reservoir height 0.1-2 rice, width is a 0.1-2 rice.
In the utility model, the double-deck reaction tube internal layer in main reactor inside is a straight tube with holes of carrying hydrogen peroxide, is beneficial to hydrogen peroxide and fully contacts with reaction mass.
In the reactor content exit temperature instrumentation is set, monitoring reaction device interior reaction temperature.
Outer chuck and built-in condenser pipe are set on storage tank, are used for the time condensation of material, when guaranteeing that material is circulated in the reactor, it is reacted under preference temperature.
Discharging opening is provided with three-way pipe in the storage tank bottom, and an end leads to reactor, and an end leads to separator.When product design reaches desired concn in the reaction feed liquid, close the valve on the pipe that leads to reactor, make the reaction feed liquid lead to knockout tower and be used for production, otherwise close, make it be circulated to reactor and continue reaction, to reach desired concn.
The employed catalyst of this recirculation reactor can be powdery, solid particle or liquid state, but the catalyst of the most suitable use powdery.
Double-deck reaction tube outer tube can select for use stainless steel pipes to make, and internal layer straight tube with holes can select for use carbon steel pipe to make.
Beneficial effect:
Because the utility model recirculation reactor is a circulating system and synthesis under normal pressure, compared with prior art, this better guarantee system under a steady temperature and normal pressure, carry out, kept the steady and safety operation of producing, improved reaction effect, and provide assurance for obtaining required product concentration.
Description of drawings
Fig. 1 is a structural representation of the present utility model; Wherein: I is a main reactor, II is a material condensation storage tank, and III is the hydrogen peroxide stock chest, and 1 is double-deck reaction tube, 2 is cooling water inlet, 3 is the hydrogen peroxide import, and 4 is material inlet, and 5 is cooling-water duct, 6 is coolant outlet, 7 is material outlet, and 8 is the main reactor drain, and 9 are the hydrogen peroxide outlet, 10 is the storage tank material inlet, 11 is the chuck cooling water inlet, and 12 is cooling water jecket, and 13 is the condenser pipe cooling water inlet, 14 is the storage tank material outlet, 15 is condenser pipe, and 16 is the chuck coolant outlet, and 17 is the condenser pipe coolant outlet, 18 is the storage tank drain, 19 for leading to the main reactor mouth of pipe, and 20 for leading to the separator mouth of pipe, and 21 is the mouth of pipe that links to each other with retracting device.
Fig. 2 is double-deck reaction tube; Wherein: 1 is double-deck reaction tube, and 22 is double-deck reaction tube outer tube, and 23 is the aperture on the straight tube with holes, and 24 is straight tube with holes.
The specific embodiment
Following with reference to accompanying drawing, further set forth concrete technical scheme of the present utility model, so that make those skilled in the art understand the present invention further, and do not constitute restriction to its right.
[embodiment 1] as shown in Figure 1.A kind of loop reactor that is used for the phenol hydroxylation preparing benzenediol, its structure is made up of main reactor, material condensation storage tank and hydrogen peroxide stock chest three parts.Be provided with many double-deck reaction tubes 1 among the main reactor I, the bottom is provided with material inlet 4, hydrogen peroxide import 3, and downside has cooling water inlet 2, and the top is provided with material outlet 7, hydrogen peroxide outlet 9 and temperature instrumentation, and upside has coolant outlet 6; Double-deck reaction tube 1 skin is a reaction mass passage 22, and internal layer is straight tube with holes 24 and the aperture 23 (as shown in Figure 2) thereof that is circulated throughout hydrogen oxide.There are cooling water jecket 12 and chuck cooling water inlet 11, chuck coolant outlet 16 in the material condensation storage tank II outside, in condensate pipe 15 and condensate pipe cooling water inlet 13, condensate pipe coolant outlet 17 are arranged; Upper end storage tank material inlet 10 links to each other with main reactor discharging outlet 7; Lower end storage tank material outlet 14 is provided with three ports 19,20, links to each other with separator with main reactor respectively.Hydrogen peroxide reservoir III and main reactor are also formed the circulatory system.Main reactor I and material condensation storage tank II upper end are respectively equipped with drain 8,18, link to each other with retracting device by connecting the mouth of pipe 21 that links to each other with retracting device.
[embodiment 2] embodiment 1 described loop reactor that is used for the phenol hydroxylation preparing benzenediol, main reactor I highly is 1 meter, internal diameter is 0.5 meter, evenly places 10 double-deck reaction tubes, wherein double-deck tube length of reaction tube 1m, internal diameter 30mm; The length of internal layer straight tube with holes is 1 meter, and internal diameter is 10 millimeters, and hole diameter is 2 millimeters, and number is 100 and is evenly distributed on the straight tube; The height of material condensation fluid reservoir II is 0.5 meter, and internal diameter is 0.5 meter, and spiral is 15 millimeters in the internal diameter of jar interior condenser tube, and length is 50 meters; Hydrogen peroxide reservoir III highly is 0.2 meter, and width is 0.5 meter.70 ℃ were reacted phenol conversion 18.8%, benzenediol selectivity 91.5% 30 minutes.
[embodiment 3] embodiment 1 described loop reactor that is used for the phenol hydroxylation preparing benzenediol, the main reactor height is 9.5 meters, internal diameter is 3 meters, evenly place 40 double-deck reaction tubes, wherein double-deck tube length of reaction tube is 9 meters, 50 millimeters of internal diameters, the length of internal layer straight tube with holes is 9 meters, internal diameter is 30 millimeters, and hole diameter is 8 millimeters, and number is 120; The height of material condensation fluid reservoir is 3 meters, and internal diameter is 3 meters, and spiral is 25 millimeters in the internal diameter of jar interior condenser tube, and length is 120 meters; Hydrogen peroxide reservoir height is 2 meters, and width is 1.5 meters.60 ℃ were reacted phenol conversion 17.6%, benzenediol selectivity 92.8% 60 minutes.

Claims (7)

1. a loop reactor that is used for the phenol hydroxylation preparing benzenediol is made up of main reactor (I), material condensation storage tank (II) and hydrogen peroxide stock chest (III); Wherein be provided with many double-deck reaction tubes (1) in the main reactor (I), main reactor (I) bottom is provided with material inlet (4), hydrogen peroxide import (3), downside is provided with cooling water inlet (2), the top is provided with material outlet (7), hydrogen peroxide outlet (9) and temperature instrumentation, upside is provided with coolant outlet (6), wherein double-deck reaction tube (1) internal layer is the straight tube with holes (24) that has aperture (23), and straight tube with holes (24) is reaction mass passage (22) with the outer interlayer of double-deck reaction tube (1); Material condensation storage tank (II) outside is provided with cooling water jecket (12), cooling water jecket (12) upside correspondence is provided with the cooling water inlet (11) of cooling water jecket and the coolant outlet (16) of cooling water jecket, condenser pipe (15) is arranged in the material condensation storage tank (II), wherein condenser pipe (15) lower end is provided with condenser pipe cooling water inlet (13), and the upper end is provided with condenser pipe coolant outlet (17); Material condensation storage tank (II) top is provided with material condensation storage tank material inlet (10), and material inlet (10) links to each other with main reactor material outlet (7); Material condensation storage tank (II) lower end is provided with material condensation storage tank material outlet (14), material outlet connects three ports under (14), link to each other with main reactor by leading to the main reactor mouth of pipe (19) respectively, link to each other with separator by leading to the separator mouth of pipe (20); Hydrogen peroxide reservoir (III) is by forming the circulatory system with the hydrogen peroxide import (3) and main reactor (I) the top hydrogen peroxide outlet (9) of main reactor (I) bottom with main reactor; Main reactor (I) upper end is provided with main reactor drain (8), material condensation storage tank (II) upper end is provided with drain (18), and main reactor drain (8) links to each other with material condensation storage tank drain (18) and links to each other with retracting device by the connector (21) that links to each other with retracting device.
2. according to the described loop reactor of claim 1, the height that it is characterized in that described main reactor (I) is a 1-10 rice, and internal diameter is a 0.5-5 rice.
3. according to the described loop reactor of claim 1, it is characterized in that described double-deck reaction tube (1) length is 0.5-9.5 rice, internal diameter is the 20-150 millimeter; The quantity of many double-deck reaction tubes (1) is the 10-50 root in the main reactor (I).
4. according to the described loop reactor of claim 1, it is characterized in that described straight tube with holes (24) length and double-deck reaction tube (1) equal in length, the internal diameter of double-deck reaction tube and straight tube with holes (24) is than being 1.5-5: 1.
5. according to the described loop reactor of claim 1, it is characterized in that aperture (23) diameter on the described straight tube with holes (24) is the 1-10 millimeter; Little hole number is 20-200, is uniformly distributed on the straight tube with holes (24).
6. according to the described loop reactor of claim 1, it is characterized in that described material condensation storage tank (II) highly is 0.5-3 rice, internal diameter is a 0.5-3 rice; Condenser pipe (15) length in the material condensation storage tank (II) is 3-150 rice, internal diameter 10-30 millimeter.
7. according to the described loop reactor of claim 1, it is characterized in that described hydrogen peroxide reservoir (III) height 0.1-2 rice, width is a 0.1-2 rice.
CN2011201630081U 2011-05-20 2011-05-20 Circulating reactor for preparing hydroquinone through phenol hydroxylation Expired - Fee Related CN202078886U (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
CN110217948A (en) * 2019-07-10 2019-09-10 大连民族大学 A kind of guide shell circulation flow reactor

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110217948A (en) * 2019-07-10 2019-09-10 大连民族大学 A kind of guide shell circulation flow reactor

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Granted publication date: 20111221

Termination date: 20180520