CN109277056B - Azeotropic catalytic reaction tower - Google Patents
Azeotropic catalytic reaction tower Download PDFInfo
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- CN109277056B CN109277056B CN201811358822.1A CN201811358822A CN109277056B CN 109277056 B CN109277056 B CN 109277056B CN 201811358822 A CN201811358822 A CN 201811358822A CN 109277056 B CN109277056 B CN 109277056B
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- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 25
- 239000003054 catalyst Substances 0.000 claims abstract description 67
- 238000006243 chemical reaction Methods 0.000 claims abstract description 58
- 239000007788 liquid Substances 0.000 claims abstract description 46
- 238000010438 heat treatment Methods 0.000 claims abstract description 37
- 230000003197 catalytic effect Effects 0.000 claims abstract description 35
- 230000018044 dehydration Effects 0.000 claims abstract description 25
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 25
- 238000012856 packing Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000011347 resin Substances 0.000 claims description 19
- 229920005989 resin Polymers 0.000 claims description 19
- 239000002253 acid Substances 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 5
- 239000003930 superacid Substances 0.000 claims description 5
- 239000006260 foam Substances 0.000 claims description 4
- 230000000737 periodic effect Effects 0.000 claims description 4
- 229910052573 porcelain Inorganic materials 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 3
- 238000003491 array Methods 0.000 claims 4
- 229910021472 group 8 element Inorganic materials 0.000 claims 1
- 239000004576 sand Substances 0.000 claims 1
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- 238000010992 reflux Methods 0.000 description 16
- BGJSXRVXTHVRSN-UHFFFAOYSA-N 1,3,5-trioxane Chemical group C1OCOCO1 BGJSXRVXTHVRSN-UHFFFAOYSA-N 0.000 description 15
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 15
- 239000012071 phase Substances 0.000 description 15
- 239000012024 dehydrating agents Substances 0.000 description 11
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
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- 238000006116 polymerization reaction Methods 0.000 description 5
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 4
- 230000002194 synthesizing effect Effects 0.000 description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 3
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D323/00—Heterocyclic compounds containing more than two oxygen atoms as the only ring hetero atoms
- C07D323/04—Six-membered rings
- C07D323/06—Trioxane
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The azeotropic catalytic reaction tower comprises a reaction tower, wherein a demister is arranged at the inner top end of the reaction tower, and the lower part of the demister comprises an azeotropic dehydration section positioned at the upper part and a catalytic section positioned at the lower part; the azeotropic dehydration section is provided with tower internals, and the tower internals comprise any one of structured packing or tower plates; the tube nest comprises a plurality of vertically arranged tube nest, a module catalyst is filled in the tube nest, a heating liquid flow channel is arranged between the outer wall of the tube nest and the inner wall of the reaction tower, the top and the bottom of the tube nest are respectively provided with a closed baffle plate for closing the upper end and the lower end of the heating liquid channel, and a plurality of openings are arranged on the baffle plates and communicated with the two openings of the corresponding tube nest; the reaction raw materials flowing down from the azeotropic dehydration section sequentially pass through a plurality of sections of catalytic sections to be discharged; the top of the reaction tower is provided with a gas phase outlet, the bottom of the reaction tower is provided with a discharge hole, the side wall of the reaction tower is provided with a heating liquid inlet and a heating liquid outlet respectively at the bottom of the tubular bed and the top of the opposite side, and the middle part of the reaction tower is communicated with a feed inlet on the side wall of the reaction tower. The invention can solve the technical problems of complex process, long time, dispersion and low efficiency of the traditional equipment.
Description
Technical Field
The invention relates to a device for synthesizing trioxymethylene, in particular to an azeotropic catalytic reaction tower.
Background
Trioxymethylene is an important chemical raw material and has very wide application. The prior art has a mature synthetic technology route: the trioxymethylene is synthesized by using 35-45% formaldehyde aqueous solution as raw material and liquid sulfuric acid as catalyst, thus bringing about the congenital deficiency to the process of synthesizing trioxymethylene: the three wastes are discharged more, the production environment is poor, the flow is long, the investment is large, the corrosion of production equipment is serious, and the like, so the development of a new technology with high efficiency, energy conservation, cleanness and environmental protection is imperative.
The existing synthesis methods are as follows: the preparation method comprises the steps of (1) concentrating formaldehyde aqueous solution with the content of 35-45% under reduced pressure, heating to 100 ℃, entering an enamel reaction kettle, catalyzing with 2-10% sulfuric acid, evaporating and concentrating trioxymethylene aqueous solution, extracting and refining again, and drying to obtain a final finished product. The traditional equipment has complex process, long time and low efficiency in the application process, so that the reaction equipment which can integrate azeotropic dehydration and catalysis and can efficiently prepare trioxymethylene is urgently needed.
Disclosure of Invention
In order to overcome the defects and shortcomings of the technology, the invention provides an azeotropic catalytic reaction tower, which solves the technical problems that the process is complex, the time is long, the equipment is dispersed, and the trioxymethylene cannot be produced in an integrated manner in a high-efficiency manner in the application process of traditional equipment.
The invention adopts the following technical scheme:
the azeotropic catalytic reaction tower comprises a reaction tower, wherein a demister is arranged at the inner top end of the reaction tower, the lower part of the demister comprises an azeotropic dehydration section positioned at the upper part and a catalytic section positioned at the lower part, and a distributor and a grating plate are sequentially arranged at the top of the azeotropic dehydration section from top to bottom; the top of the catalytic section is provided with a distributor and a grating plate in sequence from top to bottom, and the bottom of the catalytic section is provided with the distributor, a cushion layer and the grating plate in sequence from top to bottom; the azeotropic dehydration section is provided with tower internals, and the tower internals comprise any one of structured packing or tower plates; the tower internals are selected to comprise structured packing, the number of the structured packing filling sections is N, and N is less than or equal to 1 and less than or equal to 100, the height of each section is 1-3 m, a distributor and a grating plate are arranged between each section, and the distributor is arranged on the grating plate; or the tower internals comprise tower plates, wherein the number of the tower plates is M, and M is less than or equal to 1 and less than or equal to 100; the catalytic section comprises a tubular bed, the number of the catalytic section is N, N is more than or equal to 1 and less than or equal to 10, and a distributor, a cushion layer and a grating plate are sequentially arranged between the sections from top to bottom;
the tube nest comprises a plurality of vertically arranged tube nest, a module catalyst is filled in the tube nest, a heating liquid flow channel is arranged between the outer wall of the tube nest and the inner wall of the reaction tower, the top and the bottom of the tube nest are respectively provided with a closed baffle plate for closing the upper end and the lower end of the heating liquid flow channel, and a plurality of openings are arranged on the baffle plates and communicated with the two openings of the corresponding tube nest; the reaction raw materials flowing down from the azeotropic dehydration section sequentially pass through each distributor, the cushion layer, the grating plate and the tube array in the multi-section catalytic section to be discharged;
the top of the reaction tower is provided with a gas phase outlet, the bottom of the reaction tower is provided with a discharge hole, the side wall of the reaction tower is provided with a heating liquid inlet at the bottom of the tubular bed, the opposite side of the heating liquid inlet is provided with a heating liquid outlet at the top of the tubular bed on the side wall of the reaction tower, the distributor at the uppermost part of the reaction tower is communicated with a first backflow liquid inlet arranged on the side wall of the reaction tower, the distributor at the lowermost part of the reaction tower is communicated with a second backflow liquid inlet arranged on the side wall of the reaction tower, and the distributor above the tower internals is communicated with a feed inlet arranged on the side wall of the reaction tower.
The cushion layer is a five-layer laminated structure formed by combining quartz sand or porcelain balls with different granularity, and the five-layer laminated structure is five-level grading: the granularity of the uppermost layer is close to or slightly larger than that of the catalyst, the granularity of the lowermost layer is slightly larger than the gap dimension of the grating plate, three layers are arranged in a mode of gradually increasing from top to bottom and the upper and lower granularity is connected, and the thickness of each layer is 5-15 cm.
The demister, the distributor and the grating plate are all made of stainless steel.
And each catalytic section is provided with a heating liquid inlet and a heating liquid outlet.
The module catalyst comprises a catalyst, a wire mesh and a wire mesh corrugated plate, wherein the module catalyst is formed by arranging the wire mesh and the wire mesh corrugated plate in parallel at intervals, catalyst particles are held between two wire mesh plates to form a catalyst layer, and the catalyst particles in the catalyst layer are separated by the wire mesh corrugated plate; the catalyst layers in the module catalyst are arranged at intervals.
The catalyst particles are spherical or beaded strong acid resin catalysts, high temperature resistant strong acid resin catalysts or metal-loaded super acid resin catalysts.
The type of the load metal is main group II and VIII elements of the periodic table, and the load amount is 1-20% of the exchange amount of the resin catalyst.
The invention has the following positive and beneficial effects:
the method replaces the connection of a plurality of distributed components in the existing equipment, integrates a plurality of functions into one reaction tower, greatly simplifies the production process, shortens the reaction time, and has obvious effect in efficiently preparing the trioxymethylene.
After the formaldehyde aqueous solution is mixed with the entrainer, under the synergistic effect of azeotropic dehydration and concentration catalysis, the high-purity trioxymethylene product is produced, the defects and drawbacks of the existing water absorption technology, concentration technology, sulfuric acid catalysis technology and extraction drying technology are overcome, and a new technological process route with advantages of mild technological conditions, short technological process, small investment, quick response, high efficiency, low consumption, cleanness and environmental protection is created.
Drawings
FIG. 1 is a flow chart of an azeotropic catalytic reaction tower for use in a process for synthesizing trioxymethylene;
FIG. 2 is a schematic diagram of the structure of a modular catalyst at a single tube array cross section.
Figure number: 1-reaction column, 101-gas phase outlet, 102-first reflux inlet, 103-inlet, 104-heating liquid inlet, 105-outlet, 106-heating liquid outlet, 107-second reflux inlet, 2-condenser one, 3-condenser one, 4-coalescer, 5-reflux pump one, 6-heater, 7-raw material feed pump, 8-finished rectifying column, 9-reboiler, 10-condenser two, 11-condenser two, 12-reflux pump two, 13-foam remover, 14-distributor, 15-column internals, 16-column bed, 17-column, 18-cushion layer, 19-grid plate, 40-module catalyst, 401-catalyst layer, 402-wire mesh, 403-corrugated metal plate.
Detailed Description
The following describes the embodiments of the present invention further with reference to the drawings.
The following examples are given for the purpose of illustration only and are not intended to limit the embodiments of the invention. Various other changes and modifications may be made by one of ordinary skill in the art in light of the following description, and such obvious changes and modifications are contemplated as falling within the spirit of the present invention.
Referring to fig. 1, an azeotropic catalytic reaction tower comprises a reaction tower 1, wherein a demister 13 is arranged at the inner top end of the reaction tower 1, the lower part of the demister 13 comprises an azeotropic dehydration section positioned at the upper part and a catalytic section positioned at the lower part, and a distributor 14 and a grating plate 19 are sequentially arranged at the top of the azeotropic dehydration section from top to bottom; the top of the catalytic section is provided with a distributor 14 and a grating plate 19 in sequence from top to bottom, and the bottom of the catalytic section is provided with the distributor 14, a cushion layer 18 and the grating plate 19 in sequence from top to bottom; the azeotropic dehydration section is provided with a tower internal part 15, and the tower internal part 15 comprises any one of structured packing or tower plates; the tower internal part 15 is selected to comprise structured packing, the number of the structured packing filling sections is N, and N is less than or equal to 1 and less than or equal to 100, the height of each section is 1-3 meters, a distributor 14 and a grating plate 19 are arranged between each section, and the distributor 14 is arranged above the grating plate 19; or the tower inner part 15 is selected from a tower plate, wherein the number of the tower plates is M, and M is more than or equal to 1 and less than or equal to 100; the catalytic section comprises a tubular bed 16, the number of the catalytic section is N, N is more than or equal to 1 and less than or equal to 10, and a distributor 14, a cushion layer 18 and a grid plate 19 are sequentially arranged between the sections from top to bottom;
the tube nest 16 comprises a plurality of vertically arranged tube nest 17, a module catalyst 40 is filled in the tube nest 17, a heating liquid flow channel is arranged between the outer wall of the tube nest 17 and the inner wall of the reaction tower 1, the top and the bottom of the tube nest 16 are respectively provided with a closed baffle plate for closing the upper end and the lower end of the heating liquid channel, and a plurality of openings are arranged on the baffle plates and communicated with the two openings of the corresponding tube nest 17; the reaction raw materials flowing down from the azeotropic dehydration section pass through each distributor 14, the cushion layer 18, the grating plate 19 and the tube array 17 in the multi-section catalytic section in sequence to be discharged;
the top of the reaction tower 1 is provided with a gas phase outlet 101, the bottom of the reaction tower 1 is provided with a discharge hole 105, the side wall of the reaction tower 1 is provided with a heating liquid inlet 104 at the bottom of the tubular bed 16, the opposite side of the heating liquid inlet 104 is provided with a heating liquid outlet 106 at the top of the tubular bed 16 on the side wall of the reaction tower 1, a distributor 14 at the uppermost part of the reaction tower 1 is communicated with a first backflow liquid inlet 102 arranged on the side wall of the reaction tower, a distributor 14 at the lowermost part of the reaction tower 1 is communicated with a second backflow liquid inlet 107 arranged on the side wall of the reaction tower, and a distributor 14 above a tower internal 15 is communicated with a feed inlet 103 arranged on the side wall of the reaction tower 1.
The cushion layer 18 is a five-layer laminated structure formed by combining quartz sand or porcelain balls with different granularity, and the five-layer laminated structure is five-level grading: i.e. the granularity of the uppermost layer is close to or slightly larger than that of the catalyst, the granularity of the lowermost layer is slightly larger than the gap dimension of the grating plate 19, three layers are arranged in a mode of gradually increasing from top to bottom and the upper and lower granularity are connected, and the thickness of each layer is 5-15 cm.
The demister 13, the distributor 14 and the grating plate 19 are all made of stainless steel.
Each of the catalytic sections is provided with a heating liquid inlet 104 and a heating liquid outlet 106.
Referring to fig. 2, the module catalyst 40 comprises a catalyst, a wire mesh 402 and a wire mesh corrugated plate 403, the module catalyst 40 is arranged in parallel by the wire mesh 402 and the wire mesh corrugated plate 403 at intervals, the catalyst particles are held between two pieces of the wire mesh 402 to form a catalyst layer 401, and the catalyst particles in the catalyst layer 401 are separated by the wire mesh corrugated plate 403; the catalyst layers 401 in the module catalyst 40 are disposed at intervals.
The catalyst particles are spherical or beaded strong acid resin catalysts, high temperature resistant strong acid resin catalysts or metal-loaded super acid resin catalysts.
The type of the load metal is main group II and VIII elements of the periodic table, and the load amount is 1-20% of the exchange amount of the resin catalyst.
The general process of the reaction of the invention is that the heated mixed phase raw material with dehydrating agent is introduced from the feed port 103 of the azeotropic dehydration section, the mixed phase is divided into two phases after entering the reaction tower 1, the gas phase is discharged from the gas phase outlet 101, the liquid phase falls into the tubular bed 16 through the tower internal 15 to participate in the catalytic reaction, the dehydrating agent liquid phase entering from the first reflux liquid inlet 102 falls into the tubular bed 16 while dehydrating, the dehydrating agent liquid phase entering from the second reflux liquid inlet 107 participates in the catalytic reaction in the tubular bed 16, the heating liquid (such as hot water) entering from the heating liquid inlet 104 circulates in the heating liquid flow channel at the periphery of the tubular 17 to provide necessary temperature for the reaction, the liquid phase product is discharged from the discharge port 105 after the catalytic reaction is finished, and the gas phase product is discharged again through the gas phase outlet 101.
The following is the working procedure of the azeotropic catalytic reaction tower of the invention applied to the synthesis of trioxymethylene:
firstly, a raw material feed pump 7 and a heater 6 are used for mixing and heating a formaldehyde aqueous solution and a dehydrating agent, and then the mixture is led into an azeotropic dehydration section of a reaction tower 1 from a feed port 103 for dehydration, and the dehydration result is divided into two phases: the vapor phase (water vapor and dehydrating agent gas) rises to enter the evaporation section and flows out of the tower through the vapor phase outlet 101, the vapor in the vapor phase and the dehydrating agent vapor are condensed through the condenser I2 and the condensing tank I3, water is separated after the layer separation of the coalescer 4, dehydrating agent liquid is divided into three paths after passing through the reflux pump I5, one path enters the tubular bed 16 from the second reflux liquid inlet 107 for recycling, and the other path returns to the first reflux liquid inlet 102 of the azeotropic dehydration section of the azeotropic catalytic reaction tower for recycling, and the other path enters the finished product rectifying tower 8; the liquid phase falls into the catalytic section under the action of gravity, enters the tubular bed 16 for catalytic polymerization reaction, and particularly, the residual unvaporized dehydrating agent (dichloroethane) can continuously descend along with the material aqueous solution (formaldehyde aqueous solution) with increased concentration, and enters the tubular bed 16 for catalytic polymerization reaction under the action of the catalyst. In this process, a heating liquid (hot water) is introduced from a heating liquid inlet 104 to provide a necessary temperature for the polymerization reaction, and is discharged from a heating liquid outlet 106, and the resultant aqueous trioxymethylene solution is discharged from a discharge port 105 at the bottom of the reaction column 1.
The following is an integral unit for synthesizing trioxymethylene by using an azeotropic catalytic reaction tower:
the dehydration device comprises a raw material feeding pump 7, a heater 6, a reaction tower 1, a first condenser 2, a first condensing tank 3, a first reflux pump 5, a finished product rectifying tower 8 and the like which are sequentially connected, wherein raw materials and a dehydrating agent firstly enter a tube side in the heater 6 to be heated, then enter an azeotropic dehydration section of an azeotropic catalytic reaction tower to be dehydrated, and the dehydration result is divided into two phases: the gas phase rises into the evaporation section and flows out of the tower; the liquid phase falls under the influence of gravity into the catalytic section and enters the tubular bed 16 for polymerization. The polymerization product is led into the existing commercial finished product rectifying tower 8, and the finished product of the trioxymethylene is obtained after fine fractionation.
The feed inlet 103 of the reaction tower 1 of the azeotropic catalytic reaction tower is connected with the heater 6, and the gas phase outlet 101 is connected with the condenser I2; the heating liquid inlet 104 and the heating liquid outlet 106 are respectively connected with a hot water pump and a hot water collecting system, the first reflux liquid inlet 102 is connected with the reflux pump I5, and the discharge outlet 105 is connected with the finished product rectifying tower 8.
The feeding port of the finished product rectifying tower 8 is connected with the discharging port 105 of the azeotropic catalytic reaction tower; the gas phase outlet is sequentially connected with a second condenser 10, a second condensation tank 11 and a second reflux pump 12; the outlet of the second reflux pump 12 is divided into two paths, one path is connected with the reflux outlet of the finished product rectifying tower 8, and the other path is connected with the first reflux inlet 102 of the azeotropic catalytic reaction tower; the discharge port is connected with a device for collecting or receiving finished trioxymethylene.
In the above technical scheme, the azeotropic dehydrating agent added into the azeotropic catalytic reaction tower from the raw material feed pump 7 is any one of dichloroethane, benzene, aromatic hydrocarbon and cyclohexane, or a mixture of two or more of them in any proportion.
In the technical scheme, if the tower internal part 15 in the azeotropic catalytic reaction tower is structured packing, the number of filling sections is N, N is less than or equal to 1 and less than or equal to 100, and the height of each section is 1-3 m; a distributor 14 and a grating plate 19 are arranged between each two sections; if the column plates are column plates, the number of theoretical plates is M, and M is less than or equal to 1 and less than or equal to 100, and the foam remover 13 is arranged at the top end of the column.
In the technical scheme, the catalytic section of the azeotropic catalytic reaction tower is a tubular bed section, and the number of the designed sections of the catalytic section is N, and N is more than or equal to 1 and less than or equal to 10; between each section are a distributor 14, a mat 18, a grid plate 19, see fig. 1.
In the above technical solution, the demister 13, the distributor 14, and the grating plate 19 are all made of stainless steel;
in the above technical solution, the cushion layer 18 is quartz sand or porcelain ball. The function of which is to allow the passage of the liquid phase fluid while the catalyst in the retention tube 17 is exposed ≡!
The grid plates 19 function as support mats 18.
In the above technical scheme, the catalyst in the tube array 17 is a strong acid resin catalyst, a high temperature resistant strong acid resin catalyst, and a metal-loaded super acid resin catalyst; preferably, the high-temperature resistant strong acid resin catalyst in the form of sphere or bead or the modular catalyst with the active catalyst component of strong acid resin catalyst, high-temperature resistant super acid resin catalyst loaded with metal is adopted, and the structure of the modular catalyst 40 is the same as that of the modular catalyst in the patent 201620189729.2.
The type of the load metal is main group II and VIII elements of the periodic table, and the load amount is 1-20% of the exchange amount of the resin catalyst;
in the above technical scheme, the finished product rectifying tower 8 is a conventional tower and can be sold in the market.
The catalytic reaction temperature in the shell-and-tube bed 16 is 70-110 ℃, the hot water temperature is 80-120 ℃, and the hot water path is the shell pass.
In the technical scheme, the number of the 17 tubes of each section of the tube array is F, and F is less than or equal to 1 and less than or equal to 10x10 4 The method comprises the steps of carrying out a first treatment on the surface of the Each pipe diameter is E, and E is more than or equal to 2 and less than or equal to 30cm.
In the technical scheme, the dehydrating agent is any one of pure benzene, aromatic hydrocarbon, dichloroethane and cyclohexane, or a mixture of two or more of pure benzene, aromatic hydrocarbon, dichloroethane and cyclohexane mixed according to any proportion.
Example 1
The tower internals 15 are structured packing, 2 sections are filled, and the height of each section is 2 meters; between each section there is a distributor 14 and a grating plate 19 from top to bottom.
The column bed 16 is arranged in one section, each section is 1m high, 3 columns 17 are arranged in each section, and the diameter of each column 17 is 5cm.
Example two
The column internals 15 are trays with a height of 4 m.
The column bed 16 is arranged into two sections, each section is 1m high, 3 columns 17 are arranged in each section, the diameter of each column 17 is 5cm, and a distributor 14, a cushion layer 18 and a grid plate 19 are arranged between each section from top to bottom.
All of the structures not described in detail in this application are existing structures that are mature in the industry.
The foregoing examples are merely illustrative of the technical concept and technical features of the present invention, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made according to the essence of the present invention should be included in the scope of the present invention.
Claims (7)
1. The azeotropic catalytic reaction tower comprises a reaction tower (1) and is characterized in that a foam remover (13) is arranged at the inner top end of the reaction tower (1), the lower part of the foam remover (13) comprises an azeotropic dehydration section positioned at the upper part and a catalytic section positioned at the lower part, and a distributor (14) and a grating plate (19) are sequentially arranged at the top of the azeotropic dehydration section from top to bottom; the top of the catalytic section is sequentially provided with a distributor (14) and a grating plate (19) from top to bottom, and the bottom of the catalytic section is sequentially provided with the distributor (14), a cushion layer (18) and the grating plate (19) from top to bottom; the azeotropic dehydration section is provided with a tower internal part (15), and the tower internal part (15) comprises any one of structured packing or tower plates; the tower internal part (15) is selected from a structured packing, the number of the structured packing filling sections is N, the number of the structured packing filling sections is less than or equal to 1 and less than or equal to 100, the height of each section is 1-3 meters, a distributor (14) and a grating plate (19) are arranged between each section, and the distributor (14) is arranged on the grating plate (19); or the tower internal part (15) is selected from a tower plate, wherein the number of the tower plates is M, and M is more than or equal to 1 and less than or equal to 100; the catalytic section comprises a tubular bed (16), the number of the catalytic section is N, N is more than or equal to 1 and less than or equal to 10, and a distributor (14), a cushion layer (18) and a grating plate (19) are sequentially arranged between the sections from top to bottom;
the tube array bed (16) comprises a plurality of vertically arranged tube arrays (17), a module catalyst (40) is filled in the tube arrays (17), a heating liquid flow channel is arranged between the outer wall of the tube arrays (17) and the inner wall of the reaction tower (1), the top and the bottom of the tube array bed (16) are respectively provided with a closed baffle plate for closing the upper end and the lower end of the heating liquid channel, and a plurality of openings are arranged on the baffle plates and are communicated with two openings of the corresponding tube arrays (17); the reaction raw materials flowing down from the azeotropic dehydration section sequentially pass through each distributor (14), a cushion layer (18), a grating plate (19) and a tube array (17) in the multi-section catalytic section to be discharged;
the top of the reaction tower (1) is provided with a gas phase outlet (101), the bottom of the reaction tower is provided with a discharge hole (105), the side wall of the reaction tower (1) is provided with a heating liquid inlet (104) at the bottom of the tubular bed (16), the opposite side of the heating liquid inlet (104) is provided with a heating liquid outlet (106) at the top of the tubular bed (16) on the side wall of the reaction tower (1), a distributor (14) at the uppermost part of the reaction tower (1) is communicated with a first backflow liquid inlet (102) arranged on the side wall of the reaction tower, a distributor (14) at the lowermost part is communicated with a second backflow liquid inlet (107) arranged on the side wall of the reaction tower, and a distributor (14) above a tower internal (15) at the middle part is communicated with a feed inlet (103) arranged on the side wall of the reaction tower (1).
2. The azeotropic catalytic reactor according to claim 1, wherein the mat (18) is a five-layer layered structure comprising silica sand or porcelain spheres combined in different particle sizes, the five-layer layered structure being a five-stage grading: the granularity of the uppermost layer is close to or slightly larger than that of the catalyst, the granularity of the lowermost layer is slightly larger than the gap dimension of the grating plate (19), three layers are arranged in a mode of gradually increasing from top to bottom and the upper and lower granularity is connected, and the thickness of each layer is 5-15 cm.
3. The azeotropic catalytic reactor according to claim 1, wherein the demister (13), distributor (14), and grating plate (19) are all made of stainless steel.
4. The azeotropic catalytic reactor according to claim 1, wherein each of said catalytic segments is provided with a heating fluid inlet (104) and a heating fluid outlet (106).
5. The azeotropic catalytic reactor according to claim 1, wherein said modular catalyst (40) comprises a catalyst, a wire mesh (402), and a wire mesh corrugated plate (403), said modular catalyst (40) being disposed in parallel with said wire mesh (402) and said wire mesh corrugated plate (403) being spaced apart, said catalyst particles being held between two of said wire mesh (402) to form a catalyst layer (401), and said catalyst particles within said catalyst layer (401) being disposed in spaced apart relation by said wire mesh corrugated plate (403); the catalyst layers (401) in the module catalyst (40) are arranged at intervals.
6. The azeotropic catalytic reactor according to claim 5, wherein the catalyst particles are spherical or beaded strong acid resin catalysts, high temperature resistant strong acid resin catalysts or metal supported super acid resin catalysts.
7. The azeotropic catalytic reactor according to claim 6, wherein the loading metal is selected from the group consisting of group II and group VIII elements of the periodic table of elements, and the loading is from 1 to 20% of the resin catalyst exchange capacity.
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