CN219232295U - Fixed bed reactor for preparing methyl hexahydrophthalic anhydride by catalytic hydrogenation - Google Patents
Fixed bed reactor for preparing methyl hexahydrophthalic anhydride by catalytic hydrogenation Download PDFInfo
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- CN219232295U CN219232295U CN202223219043.8U CN202223219043U CN219232295U CN 219232295 U CN219232295 U CN 219232295U CN 202223219043 U CN202223219043 U CN 202223219043U CN 219232295 U CN219232295 U CN 219232295U
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Abstract
The utility model discloses a fixed bed reactor for preparing methyl hexahydrophthalic anhydride by catalytic hydrogenation, which comprises a shell, an oil distribution device and a catalyst bed layer. The shell is provided with a raw material inlet and a product outlet; the oil distribution device is arranged in the shell and connected with the raw material inlet, and a plurality of vibration sheets are arranged on the oil distribution deviceThe meta-type is used for scattering methyl tetrahydrophthalic anhydride; the catalyst bed layer is arranged in the shell and comprises a columnar surface layer, and Pd-Ni/Al is arranged in the surface layer 2 O 3 A catalyst. According to the technical scheme, the oil distribution device is arranged in the shell of the fixed bed reactor, and the plurality of vibration units are arranged on the oil distribution device, so that scattered methyltetrahydrophthalic anhydride can fully contact Pd-Ni/Al in the surface layer 2 O 3 The catalyst can fully react with hydrogen, so that the yield is improved, and the consumption of raw materials is reduced.
Description
Technical Field
The utility model belongs to the technical field of chemical reactors, and particularly relates to a fixed bed reactor for preparing methyl hexahydrophthalic anhydride by catalytic hydrogenation.
Background
The existing industrial catalyst for producing the methyl hexahydrophthalic anhydride by catalytic hydrogenation mainly uses Raney nickel, and the Raney nickel catalyst has a plurality of defects (low mechanical strength and easy powdering loss). In addition, the production process of the domestic methyl hexahydrophthalic anhydride mainly uses an intermittent reaction kettle, the production process generally mixes methyl tetrahydrophthalic anhydride with a certain amount of Raney nickel catalyst, hydrogenation reaction is completed at 80-120 ℃ and 2.00-6.00 MPa for 12-16 hours, static separation is carried out, the catalyst is recycled, the catalyst lost in the process of supplementing and separating by adding fresh catalyst is added, and crude products are obtained after separation and are further distilled to obtain the industrial application methyl hexahydrophthalic anhydride; or noble metal catalysts are used in hydrogenation reaction, generally, noble metals such as Pt, pd and the like are loaded on carriers such as active carbon, aluminum oxide, molecular sieve and the like, the catalyst amount and the reaction raw materials are mixed according to a certain proportion, the hydrogenation reaction is completed after 6-16 hours at 80-120 ℃ and 2.00-6.00 MPa, and the catalyst is subjected to static separation and recycled. The method can also adopt a two-step hydrogenation method, wherein the first step takes Ni-based catalyst as hydrogenation catalyst, the Ni-based catalyst is mixed with raw materials in a certain proportion, the hydrogenation reaction is stopped when the saturation is 60-80% after 4-8 hours at the temperature of 80-120 ℃ and the pressure of 2.00-2.50 MPa, the hydrogenation reaction is stopped, the stationary separation is carried out, the catalyst is recycled, the feed liquid which is not hydrogenated is subjected to the second hydrogenation reaction, the second step takes Pt or Pd as hydrogenation catalyst, the Pt or Pd is usually carried on an inert carrier such as active carbon in a certain proportion, the hydrogenation reaction is completed after 2-6 hours at the temperature of 80-120 ℃ and the pressure of 2.00-3.00 MPa, the stationary separation is carried out, and the catalyst is recycled.
In summary, the current domestic processes for producing methyl hexahydrophthalic anhydride by catalytic hydrogenation are all intermittent production processes, and a great deal of research is conducted on how to improve the product quality by intermittent operation. However, the batch production process itself has disadvantages in terms of reduced consumption of raw materials.
Disclosure of Invention
The utility model mainly aims to provide a process for preparing methyl hexahydrophthalic anhydride by catalytic hydrogenation, and aims to solve the technical problem that raw material consumption cannot be reduced in the existing production process for preparing methyl hexahydrophthalic anhydride by catalytic hydrogenation.
In order to achieve the above object, the present utility model provides a fixed bed reactor for preparing methyl hexahydrophthalic anhydride by catalytic hydrogenation, comprising:
a shell provided with a raw material inlet and a product outlet;
the oil distribution device is arranged in the shell and connected with the raw material inlet, and a plurality of vibration units are arranged on the oil distribution device and are used for scattering methyl tetrahydrophthalic anhydride; the method comprises the steps of,
the catalyst bed layer comprises a columnar surface layer, wherein Pd-Ni/Al is arranged in the surface layer 2 O 3 A catalyst.
Optionally, the raw material inlet comprises a plurality of hydrogen inlets and methyl tetrahydrophthalic anhydride inlets, and each hydrogen inlet is respectively arranged on the upper side, the middle side and the lower side of the shell.
Optionally, the catalyst bed layer includes an upper surface layer, a lower surface layer, and a plurality of vertically arranged central column layers, each of which is arranged between and communicates with the upper surface layer and the lower surface layer.
Optionally, a circulation channel is arranged between the central column layers, and a heat dissipation medium inlet and a heat dissipation medium outlet are formed at the positions of the shell corresponding to the circulation channel.
Optionally, each vibration unit is distributed corresponding to each central column layer.
Optionally, the oil distribution device comprises a plurality of pipe frames which are communicated with the raw material inlet and are parallel to each other, each pipe frame is provided with a plurality of openings, and the vibration unit is arranged at the opening.
According to the technical scheme, the oil distribution device is arranged in the shell of the fixed bed reactor, and the plurality of vibration units are arranged on the oil distribution device, so that scattered methyltetrahydrophthalic anhydride can fully contact Pd-Ni/Al in the surface layer 2 O 3 The catalyst can fully react with hydrogen, so that the yield is improved, and meanwhile, the consumption of raw materials and the catalyst is reduced.
Drawings
In order to more clearly illustrate the embodiments of the present utility model or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present utility model, and other related drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a perspective view of one embodiment of a fixed bed reactor for preparing methyl hexahydrophthalic anhydride by catalytic hydrogenation provided by the utility model;
FIG. 2 is a side view of FIG. 1;
FIG. 3 is a cross-sectional view of FIG. 1;
FIG. 4 is a bottom view of the oil distribution device of FIG. 1;
FIG. 5 is a cross-sectional view of the tube rack of FIG. 4;
FIG. 6 is a cross-sectional view of a lamina within the circulation channel of FIG. 3;
fig. 7 is a cross-sectional view of a lamina in the circulation channel of fig. 3.
Description of the reference numerals: the reactor comprises a fixed bed reactor-100, a shell-1, a hydrogen inlet-11, a methyltetrahydrophthalic anhydride inlet-12, an oil distribution device-2, a pipe rack-21, an opening-211, a vibration unit-22 and a catalyst bed layer-3Upper surface layer-31, lower surface layer-32, central column layer-33, circulation channel-34, heat-dissipating medium inlet-35, heat-dissipating medium outlet-36, pd-Ni/Al 2 O 3 Catalyst-37.
The achievement of the objects, functional features and advantages of the present utility model will be further described with reference to the accompanying drawings, in conjunction with the embodiments.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present utility model more clear, the technical solutions of the embodiments of the present utility model will be clearly and completely described below. It will be apparent that the described embodiments are only some, but not all, embodiments of the utility model.
The specific conditions were not specified in the examples, and the examples were conducted under the conventional conditions or the conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention. In addition, the meaning of "and/or" as it appears throughout includes three parallel schemes, for example "A and/or B", including the A scheme, or the B scheme, or the scheme where A and B are satisfied simultaneously. In addition, the technical solutions of the embodiments may be combined with each other, but it is necessary to base that the technical solutions can be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be regarded as not exist and not within the protection scope of the present utility model. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
The production process of the domestic methyl hexahydrophthalic anhydride mainly uses an intermittent reaction kettle, and a one-step method or a two-step method is adopted, the catalyst amount and the reaction raw materials are mixed according to a certain proportion, and crude products are separated after the reaction; when the reaction is completed, a large amount of nitrogen and hydrogen are required to be replaced, and the defects of high replacement times, high hydrogen loss and high energy consumption of feeding and discharging operations exist; and the catalyst is easy to poison, difficult to separate and easy to entrain into a distillation system.
In view of the above, the present utility model provides a fixed bed reactor for preparing methyl hexahydrophthalic anhydride by catalytic hydrogenation, fig. 1-6 are an embodiment of the fixed bed reactor provided by the present utility model, please refer to fig. 1-6, and the fixed bed reactor 100 includes a housing 1, an oil distribution device 2 and a catalyst bed 3.
Specifically, the shell 1 is a cylindrical reaction kettle, and a raw material inlet and a product outlet are formed in the shell 1; the oil distribution device 2 is arranged in the shell 1 and is connected with the raw material inlet, a plurality of vibration units 22 are arranged on the oil distribution device 2, and when the methyl tetrahydrophthalic anhydride passes through the oil distribution device 2, the vibration units 22 on the oil distribution device 2 can break up the methyl tetrahydrophthalic anhydride; the catalyst bed layer 3 comprises a columnar surface layer which is arranged in the middle of the shell 1, and Pd-Ni/Al is arranged in the surface layer 2 O 3 A catalyst 37. It should be noted that the vibration unit 22 is a piezoelectric ceramic, and the methyl tetrahydrophthalic anhydride passing through the vibration unit 22 is changed into a liquid mist form of Pd-Ni/Al falling on the catalyst bed 3 through rapid shaking by converting electric energy into mechanical energy 2 O 3 A catalyst 37.
In the technical scheme of the utility model, the oil distribution device 2 is arranged in the shell 1 of the fixed bed reactor 100, and a plurality of vibration units 22 are arranged on the oil distribution device 2, so that the scattered methyltetrahydrophthalic anhydride can fully contact Pd-Ni/Al in the surface layer of the catalyst bed 3 2 O 3 The catalyst can fully react with hydrogen, so that the yield is improved, and compared with a batch reactor, the scheme does not need stirring and hydrogen replacement, and the consumption of raw materials and the catalyst is reduced.
Please refer to fig. 2 and 3, in order to make the Pd-Ni/Al 2 O 3 The catalyst 37 can be fully utilized, the reaction layout is more fully, the raw material inlet comprises a plurality of hydrogen inlets 11 and a methyl tetrahydrophthalic anhydride inlet 12, and each hydrogen inlet 11 is respectively arranged on the upper side, the middle part and the lower side of the shell 1, so that hydrogen can respectively pass through the upper side and the lower side of the surface layer, and the hydrogenation reaction is more fully performed. It should be noted that the number of the substrates,the oil distribution device 2 is communicated with the methyl tetrahydrophthalic anhydride inlet 12, the product outlet comprises an outlet for hydrogen internal circulation, the outlet is arranged at the top of the reactor, the product outlet also comprises an outlet of crude methyl hexahydrophthalic anhydride, and the outlet is arranged at the bottom of the reactor (not shown in the figure).
Referring to fig. 2 and 3, since the hydrogenation process for preparing methyl hexahydrophthalic anhydride is an exothermic reaction, when the reaction proceeds in the catalyst bed 3, the local temperature is rapidly increased, the reaction rate is affected, and side reactions are easily generated. In order to improve the internal heat dissipation effect, the catalyst bed 3 comprises an upper surface layer 31, a lower surface layer 32 and a plurality of vertically arranged central column layers 33, wherein Pd-Ni/Al are respectively arranged in the catalyst bed 2 O 3 A catalyst 37, each of the center pillar layers 33 is provided between the upper surface layer 31 and the lower surface layer 32, and communicates the upper surface layer 31 and the lower surface layer 32. The lower surface layer 32 is provided with a bottom plate (not shown) for Pd-Ni/Al 2 O 3 The catalyst 37, the said bottom plate has leak holes used for spilling crude product of methyl hexahydrophthalic anhydride; in order to prevent the catalyst from falling off, an organic ultrafiltration membrane, such as polyvinylidene fluoride (PVDF), is further laid on the bottom plate, and correspondingly, a top plate having the same function may be provided on the upper surface layer 31. Wherein the hydrogen inlet 11 located in the middle is above the upper surface layer 31, and the hydrogen inlet 11 located at the lower side is below the lower surface layer 32, so that hydrogen can react on the upper and lower surface layers of the catalyst bed 3.
Further, referring to fig. 3, 6 and 7, a circulation channel 34 is provided between each central column layer 33, the circulation channel 34 is provided between the upper surface layer 31 and the lower surface layer 32, and a plurality of layers are separated, so that a heat dissipation medium can form a multi-layer circulation, and heat dissipation efficiency is improved, a heat dissipation medium inlet 35 and a heat dissipation medium outlet 36 are provided at the positions of the casing 1 corresponding to the circulation channels 34, and the heat dissipation medium can use hydrogen as a heat carrier to timely transfer reaction heat, thereby effectively avoiding local overheating phenomenon and reducing side reactions; of course, this hydrogen is circulated and introduced into the fixed bed reactor 100 together with the hydrogen inlet 11.
In addition, each of the vibration units 22 is distributed corresponding to the position of each of the center pillar layers 33, so that the unreacted methyl tetrahydrophthalic anhydride of the upper surface layer 31 and the methyl hexahydrophthalic anhydride produced by the reaction can be rapidly concentrated and enter the center pillar layers 33 and the lower surface layer 32 to react.
Referring to fig. 4 and 5, the oil distribution device 2 includes a plurality of parallel tube frames 21 connected to the raw material inlet, a plurality of openings 211 are formed in each tube frame 21 at equal intervals, and the vibration unit 22 is disposed at the opening 211. When raw material liquid methyl tetrahydrophthalic anhydride enters the pipe frame 21 from the methyl tetrahydrophthalic anhydride inlet 12, the methyl tetrahydrophthalic anhydride respectively flows into each branched pipe, and the gaps on each branched pipe drip irrigation downwards, and pass through the vibration unit 22 during drip irrigation, the vibration unit 22 breaks up rapidly to form small-particle liquid mist, so that the methyl tetrahydrophthalic anhydride can fall on the catalyst bed 3 more uniformly, and further can react with hydrogen fully. Wherein the vibration unit 22 is made of piezoelectric ceramics, is cylindrical in shape, and is arranged in the branch pipe of the pipe frame 21 through a fixed rod; the piezoelectric ceramic is a ceramic material capable of converting mechanical energy and electrical energy into each other—a piezoelectric effect, and each vibration unit 22 is connected in series by an electric wire and electrically connected to a power source and a controller (not shown) outside the housing 1.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples merely represent a few embodiments of the present application, which are described in more detail and are not to be construed as limiting the scope of the utility model. It should be noted that it would be apparent to those skilled in the art that various modifications and improvements could be made without departing from the spirit of the present application, which would be within the scope of the present application. Accordingly, the scope of protection of the present application is to be determined by the claims appended hereto.
Claims (6)
1. A fixed bed reactor for preparing methyl hexahydrophthalic anhydride by catalytic hydrogenation, comprising:
a shell (1) provided with a raw material inlet and a product outlet;
the oil distribution device (2) is arranged in the shell (1) and is connected with the raw material inlet, and a plurality of vibration units (22) are arranged on the oil distribution device (2) and are used for scattering methyl tetrahydrophthalic anhydride; the method comprises the steps of,
the catalyst bed layer (3) is arranged on the shell (1), the catalyst bed layer (3) comprises a columnar surface layer, and Pd-Ni/Al is arranged in the surface layer 2 O 3 A catalyst (37).
2. The fixed bed reactor for preparing methyl hexahydrophthalic anhydride by catalytic hydrogenation according to claim 1, wherein the raw material inlet comprises a plurality of hydrogen inlets (11) and methyl tetrahydrophthalic anhydride inlets (12), and each hydrogen inlet (11) is respectively arranged on the upper side, the middle side and the lower side of the shell (1).
3. The fixed bed reactor for preparing methyl hexahydrophthalic anhydride by catalytic hydrogenation according to claim 1, wherein the catalyst bed (3) comprises an upper surface layer (31), a lower surface layer (32) and a plurality of vertically arranged central column layers (33), wherein each central column layer (33) is arranged between the upper surface layer (31) and the lower surface layer (32) and is communicated with the upper surface layer (31) and the lower surface layer (32).
4. A fixed bed reactor for preparing methyl hexahydrophthalic anhydride by catalytic hydrogenation according to claim 3, wherein a circulation channel (34) is arranged between the central column layers (33), and a heat dissipation medium inlet (35) and a heat dissipation medium outlet (36) are arranged at the position of the shell (1) corresponding to the circulation channel (34).
5. The fixed bed reactor for preparing methyl hexahydrophthalic anhydride by catalytic hydrogenation according to claim 3, wherein each vibration unit is distributed corresponding to each center column layer.
6. The fixed bed reactor for preparing methyl hexahydrophthalic anhydride by catalytic hydrogenation according to claim 1, wherein the oil distribution device (2) comprises a plurality of mutually parallel pipe frames (21) which are communicated with the raw material inlet, each pipe frame (21) is provided with a plurality of openings (211), and the vibration unit (22) is arranged at the openings (211).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117384122A (en) * | 2023-12-13 | 2024-01-12 | 淄博鲁华泓锦新材料集团股份有限公司 | Method for continuously producing methyl hexahydrophthalic anhydride by using membrane tube reactor |
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- 2022-12-02 CN CN202223219043.8U patent/CN219232295U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117384122A (en) * | 2023-12-13 | 2024-01-12 | 淄博鲁华泓锦新材料集团股份有限公司 | Method for continuously producing methyl hexahydrophthalic anhydride by using membrane tube reactor |
| CN117384122B (en) * | 2023-12-13 | 2024-03-29 | 淄博鲁华泓锦新材料集团股份有限公司 | Method for continuously producing methyl hexahydrophthalic anhydride by using membrane tube reactor |
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