A method for loading a catalyst in a BDO dehydrogenation reactor

Abstract

The present application relates to the technical field of BDO dehydrogenation reaction, and specifically discloses a BDO dehydrogenation reactor catalyst loading method, which comprises the following steps: step one: raw material preparation, wherein the raw material comprises 1,4-butanediol and a catalyst for dehydrogenation reaction with 1,4-butanediol; step two: screening, weighing and sub-packaging of the catalyst in the raw material through a catalyst screening device; step three: precise loading of the catalyst in step two through a catalyst column device; step four: differential pressure test of the catalyst column device in step three, and then putting into a dehydrogenation reactor; and step five: closing the dehydrogenation reactor head, pressure test, leak detection, replacement, system feeding and start-up. The present application solves the problem of low conversion efficiency of traditional BDO (1,4-butanediol) in the dehydrogenation reaction.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of BDO dehydrogenation reaction, and particularly discloses a BDO dehydrogenation reactor catalyst loading method. BACKGROUND

[0002] N-methyl pyrrolidone, Chinese alias: NMP; 1-methyl-2 pyrrolidone; N-methyl-2-pyrrolidone. Colorless transparent oily liquid, slightly amine odor. Low volatility, thermal stability, chemical stability are good, can be volatile with water vapor. Hygroscopic. Light sensitive. Easily soluble in water, ethanol, diethyl ether, acetone, ethyl acetate, chloroform and benzene, can dissolve most of the organic and inorganic compounds, polar gas, natural and synthetic polymer compounds. N-methyl pyrrolidone is widely used in lithium battery, medicine, pesticide, pigment, cleaning agent, insulating material and other industries;

[0003] In the prior art, GBL (gamma-butyrolactone) is an important intermediate product of an NMP (N-methyl pyrrolidone) process device, and the GBL (gamma-butyrolactone) needs to be generated by reacting and dehydrogenating a raw material BDO and a copper catalyst, and the loading effect of the catalyst seriously affects the service life of the catalyst and the conversion rate of the GBL, thereby being a material consumption loss to the production raw material BDO;

[0004] In the conventional copper catalyst loading in a BDO (1,4-butanediol) dehydrogenation synthesis reactor, the following deficiencies and disadvantages exist:

[0005] 1. Before the catalyst is loaded, a large amount of carbon dust is attached to the outer surface of the catalyst, which leads to excessive impurities in the product during catalyst reduction and original feeding and starting, and affects the quality of the GBL product, and the pump filter is blocked during the whole production process;

[0006] 2. The catalyst, porcelain balls and short pipes are prone to be mixed and loaded during the loading process, different differential pressures of the pipes are caused, the GBL conversion rate is affected, and the raw material consumption is increased;

[0007] 3. The catalyst is not completely reduced, and the activity and service life of the catalyst are affected;

[0008] 4. The loading time is long, and the loading efficiency is affected;

[0009] The loading quantity of each coil of the catalyst seriously affects the BDO conversion rate, and the production energy consumption is increased by increasing or reducing the temperature of the heat conducting oil and the motor frequency of the hydrogen compressor;

[0010] To this end, the present application relates to an improved BDO dehydrogenation reactor catalyst loading scheme, which can make the BDO dehydrogenation system reactor safe, effective and fast during the catalyst loading process, prolong the service life of the catalyst, improve the conversion rate of GBL in the synthesis catalyst reaction, reduce the by-product generation of BDO in the dehydrogenation conversion process, reduce the consumption of BDO raw materials, and improve the yield and quality of GBL. SUMMARY

[0011] The present application aims to solve the problem of low conversion efficiency of traditional BDO (1,4-butanediol) in dehydrogenation reaction.

[0012] In order to achieve the above purpose, the present application provides the following basic scheme:

[0013] A BDO dehydrogenation reactor catalyst loading method, comprising the following steps:

[0014] Step one: raw material preparation, the raw material includes 1,4-butanediol and catalyst for dehydrogenation reaction with 1,4-butanediol;

[0015] Step two: screening, weighing and sub-packaging of the catalyst in the raw material by catalyst screening device;

[0016] Step three: precise loading of the catalyst in step two by catalyst column device;

[0017] Step four: differential pressure test of the catalyst column device in step three, and putting into the dehydrogenation reactor;

[0018] Step five: closing the dehydrogenation reactor head, pressure test, leak detection, replacement, system feeding and start-up

[0019] The principle and effect of the basic scheme are:

[0020] 1. Compared with the prior art, in the existing catalyst loading scheme, the catalyst surface is attached with carbon dust, and the loading steps are prone to mixed loading and missing loading, which leads to uneven catalyst loading weight of each column and non-compliance of differential pressure test of each column, affecting the service life of the reaction catalyst and the conversion rate of GBL, and the original attached surface carbon dust of the catalyst more easily affects the reduction of the original catalyst and the quality of the GBL product during the original start-up, increasing the energy consumption of the production and the by-products in the process.

[0021] The catalyst loading scheme adopted by the present application changes the catalyst loading steps and details the catalyst loading scheme. The screening, proportional weighing and precise loading process of each step before and during catalyst loading are added, which effectively improves the service life of the catalyst, improves the conversion rate of GBL in the synthesis catalyst reaction, reduces the by-product generation of BDO in the dehydrogenation conversion process, reduces the consumption of BDO raw materials, and improves the yield and quality of GBL.

[0022] 2. Compared with the prior art, the filling process is increased with the marking of the rubber plug detailing each operation step, so that the catalyst is not missed and mixed during the filling process, and the service life of the catalyst is prolonged.

[0023] 3. The catalyst screening device is provided, the screening aperture of the catalyst screening device is only adjusted, the gravity of the catalyst is converted into the shaking force of the catalyst screening device, the screening effect is better, the filling weight of each column tube catalyst in the reactor is accurately calculated by the catalyst screening device, the GBL conversion rate is increased, and the GBL yield and quality are improved.

[0024] Further, the catalyst in step one is a copper powder catalyst, and the preparation method of the copper powder catalyst is as follows:

[0025] A1: A copper nitrate solution is mixed with a sodium carbonate solution in a certain proportion, a precipitate is generated, the precipitate is filtered, and after filtration, it is washed, dried, calcined, and crushed;

[0026] A2: The crushed copper powder is sampled, and the sample is added to a reaction tube for catalyst activity determination.

[0027] Further, the drying temperature in step A1 is 100°C, the calcination temperature is 450°C, and the entire step is carried out in a normal pressure environment.

[0028] Further, the catalyst screening device comprises a support frame, a screening structure detachably connected with the support frame, and a weighing structure installed at the bottom of the screening structure, the screening structure comprises a screening assembly, bosses fixed at both ends of the screening assembly, and a plurality of installation slots opened on the screening assembly, both ends of the support frame are provided with connection slots, the bosses are used in cooperation with the connection slots, and the top of the screening assembly is provided with a plurality of inflow holes for the inflow of the catalyst.

[0029] Further, the bottom of each installation slot is fixed with a first spring, and each installation slot is detachably provided with a screen mesh, and the aperture of the screen mesh decreases from top to bottom.

[0030] Further, a button is slidably connected to the boss, the inside of one end of the screening assembly close to the button is provided with a spring rod connected with the button, and the other end of the spring rod penetrates out of the upper top of the installation slot and is provided with a second spring.

[0031] Further, the weighing structure comprises a weighing tube, a rotating plate rotatably connected in the inside of the weighing tube, and an air pump fixed to the bottom in the inside of the weighing tube, an elastic rod is arranged between the rotating plate and the air pump, the outer periphery of the elastic rod is wrapped with an air bag connected with the air pump, the left end of the rotating plate is provided with a rotating shaft, and the elastic rod is arranged at the right end of the rotating plate.

[0032] Further, the catalyst column device comprises a column threaded with the weighing tube, a first plug for marking, a first porcelain ball, a second porcelain ball and a weighing sensor arranged on the first porcelain ball arranged in sequence between the first porcelain ball and the second porcelain ball, and the weighing sensor is electrically connected with the air pump.

[0033] Further, the catalyst is arranged between the first porcelain ball and the second porcelain ball, the catalyst is columned by weighing the first porcelain ball, and the second porcelain ball is sealed.

[0034] Further, the second plug for marking that the differential pressure test is being performed is wound around the periphery of the column in step four when the differential pressure test is performed on the catalyst column device, and the first plug and the second plug are different in color. BRIEF DESCRIPTION OF DRAWINGS

[0035] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the embodiment description will be briefly introduced. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative labor.

[0036] Figure 1 A structure schematic diagram of a catalyst screening device in a BDO dehydrogenation reactor catalyst loading method according to an embodiment of the present application is shown;

[0037] Figure 2 A structure schematic diagram of a weighing structure in a BDO dehydrogenation reactor catalyst loading method according to an embodiment of the present application is shown;

[0038] Figure 3 An enlarged schematic diagram of an installation groove position in a BDO dehydrogenation reactor catalyst loading method according to an embodiment of the present application is shown;

[0039] Figure 4 An enlarged schematic diagram of a boss position in a BDO dehydrogenation reactor catalyst loading method according to an embodiment of the present application is shown;

[0040] Figure 5 A flow chart of a BDO dehydrogenation reactor catalyst loading method according to an embodiment of the present application is shown. DETAILED DESCRIPTION

[0041] In order to further illustrate the technical means and effects adopted by the present application to achieve the predetermined application purposes, the specific embodiments, structures, features and effects according to the present application are described in detail as follows in combination with the drawings and preferred embodiments.

[0042] The reference signs in the drawings of the specification include: support frame 1, support rod 2, screen 3, screening structure 4, inflow hole 5, boss 6, button 7, mounting groove 8, connecting groove 9, rotating plate 10, elastic rod 11, air pump 12, tube bank 13, rotating shaft 14, air bag 16, first rubber plug 17, first porcelain ball 18, first spring 20, spring rod 21, second spring 22.

[0043] The embodiments are as shown in Figure 1 、 Figure 2 、 Figure 3 、 Figure 4 and Figure 5

[0044] A BDO dehydrogenation reactor catalyst loading method, comprising the following steps:

[0045] Step one: raw material preparation, the raw material includes 1,4 butanediol and catalyst for dehydrogenation reaction with 1,4 butanediol;

[0046] Specifically: including 1,4 butanediol raw material and catalyst preparation for dehydrogenation reaction, the catalyst is prepared by the applicant, the catalyst adopts powder catalyst commonly used in dehydrogenation reaction, the catalyst in step one is copper powder catalyst, and the preparation method of the copper powder catalyst is as follows:

[0047] A1: the copper nitrate solution is mixed with the sodium carbonate solution in a certain proportion, a precipitate is generated, the precipitate is filtered, and after filtering, it is washed, dried, calcined and crushed;

[0048] A2: after crushing, the copper powder sample is taken, the sample is added to the reaction tube for catalyst activity determination, the drying temperature in step A1 is 100°C, the calcination temperature is 450°C, the whole step is carried out in a normal pressure environment, after obtaining the copper powder catalyst, the activity of the copper powder catalyst needs to be determined, the activity of the copper powder catalyst is determined by a measuring instrument, and the copper powder catalyst with activity is put into step two;

[0049] Step two: the catalyst in the raw material is screened, weighed and subpackaged through the catalyst screening device;

[0050] Specifically: as shown in Figures 1 to 4 , the catalyst screening device includes a support frame 1, a screening structure 4 detachably connected with the support frame 1, and a weighing structure mounted at the bottom of the screening structure 4, the screening structure 4 includes a screening assembly, bosses 6 fixed at both ends of the screening assembly, and a plurality of mounting grooves 8 opened on the screening assembly, both ends of the support frame 1 are provided with connecting grooves 9, the bosses 6 are used in cooperation with the connecting grooves 9, the top of the screening assembly is provided with a plurality of inflow holes 5 for the inflow of the catalyst, the bottom of each mounting groove 8 is fixedly connected with a first spring 20, and each mounting groove 8 is detachably provided with a screen 3, and the hole diameters of the screens 3 gradually decrease from top to bottom. ​

[0051] Firstly, the catalyst screening device is installed, the bottom of the support frame 1 is fixed with several support rods 2 for supporting the whole support, then the filling requirements are determined, the aperture of the screen 3 is determined, the appropriate screen 3 is selected, the screen 3 in the bottom installation slot 8 is a 5 mesh screen 3, as shown in Figure 1 The screen 3 is inserted into the installation slot 8, as shown in Figure 3 The screen 3 is placed on the first spring 20, and the weight of the screen 3 is borne by the first spring 20, and then the support frame 1 and the screening structure 4 are installed, as shown in Figure 4 Specifically, the boss 6 is slidably connected with the button 7, the inside of the left end of the screening assembly close to the button 7 is provided with a spring rod 21 connected with the button 7, the other end of the spring rod 21 is provided with a second spring 22, when the support frame 1 and the screening structure 4 are installed, the boss 6 moves towards the inside, the spring rod 21 is pressed, the second spring 22 at the right end is driven to extend out, for the screen 3, the upper end and the lower end of the screen 3 are respectively provided with the second spring 22 and the first spring 20;

[0052] Then, the copper powder catalyst is poured from the inflow hole 5 and stays on the screen 3 for a short time, the screen 3 is subjected to gravity, the first spring 20 is compressed, and the screen 3 moves downward, as time goes on, the gravity of the catalyst in the screen decreases, the first spring 20 will reset, the upward force makes the screen 3 move upward and touch the second spring 22, as long as the catalyst is continuously poured into the inflow hole 5, the screen 3 will vibrate when the catalyst passes through the screen, which will facilitate the screening of the catalyst, making the screening of the catalyst more smooth and improving the screening effect.

[0053] Then, the screened catalyst frame enters the weighing structure, the weighing structure includes a weighing pipe, a rotating plate 10 rotatably connected inside the weighing pipe, and a gas pump 12 fixed to the bottom inside the weighing pipe, an elastic rod 11 is arranged between the rotating plate 10 and the gas pump 12, the outer periphery of the elastic rod 11 is wrapped with a gas bag 16 connected with the gas pump 12, the left end of the rotating plate 10 is provided with a rotating shaft 14, the rotating shaft 14 is arranged on the left side inner wall of the weighing pipe, and the elastic rod 11 is arranged at the right end of the rotating plate 10.

[0054] As shown in Figure 2 The weight of the catalyst makes the rotating plate 10 rotate downward, compresses the spring rod 21, and exposes the gap, the catalyst continuously enters the catalyst column pipe 13 device from the gap, specifically: the catalyst column pipe 13 device includes a column pipe 13 threadedly connected with the weighing pipe, a first plug 17 for marking, a first porcelain ball 18, a second porcelain ball and a weighing sensor arranged on the first porcelain ball 18 are arranged in the column pipe 13 in sequence, and the weighing sensor is electrically connected with the gas pump 12.

[0055] Step three: the catalyst in step two is accurately filled through the catalyst column pipe 13 device;

[0056] Specifically: the catalyst is placed between the first porcelain ball 18 and the second porcelain ball, weighed by the first porcelain ball 18, and the second porcelain ball is sealed to realize the catalyst column loading. The first plug 17 is placed at the bottom of the column tube 13, and the value of the weighing sensor is set. Once the dropped catalyst reaches this value, the air pump 12 starts to inflate the air bag 16, forcing the elastic rod 11 to stop compressing. The elastic rod 11 no longer compresses, so that the rotating plate 10 cannot be turned downward by gravity, the gap is blocked, and the catalyst no longer flows into the column tube 13. Precise filling is completed, and then the second porcelain ball is installed on the upper surface of the catalyst. The column tube 13 step is completed.

[0057] Step four: the catalyst column tube 13 device of step three is subjected to differential pressure test and is put into a dehydrogenation reactor. When the catalyst column tube 13 device is subjected to differential pressure test in step four, a second plug for marking that differential pressure test is being performed is connected to the periphery of the column tube 13. The first plug 17 and the second plug are different in color. The plug marking increases the detail of each operation step, so that the catalyst is not missed or mixed during the filling process, and the service life of the catalyst is prolonged.

[0058] Step five: close the dehydrogenation reactor head, test pressure, detect leakage, replace, and system feed start.

[0059] Specifically: the dehydrogenation reactor adopts a common reactor, and the catalyst column tube 13 device subjected to differential pressure test is placed in the catalyst layer of the dehydrogenation reactor.

[0060] Compared with the prior art:

[0061] 1. During the filling process, the plug marking increases the detail of each operation step, so that the catalyst is not missed or mixed during the filling process, and the service life of the catalyst is prolonged.

[0062] 2. The catalyst is sieved by the screen 3 before being filled, the dust attached to the surface of the catalyst and the impurities affecting the product are removed, the impurities are prevented from entering the entire impurity, and the conversion efficiency is improved.

[0063] 3. The filling weight of the catalyst of each column tube 13 in the reactor is accurately calculated, the GBL conversion rate is increased, and the GBL yield and quality are improved.

[0064] The device solves the problem of low conversion efficiency of traditional BDO (1,4 butanediol) in the dehydrogenation reaction.

[0065] The above merely describes the preferred embodiments of the present application, and is not intended to limit the present application in any form. Although the present application has been disclosed with the preferred embodiments as above, it is not intended to limit the present application. Any person skilled in the art can make some changes or modifications to the above disclosed technical content to obtain equivalent embodiments with equivalent changes, as long as the changes or modifications do not deviate from the technical solution of the present application. Any modification, change, equivalent change and modification of the above embodiments made according to the technical essence of the present application still belong to the scope of the technical solution of the present application.

Claims

1. A BDO dehydrogenation reactor catalyst loading method characterized by: The method comprises the following steps: Step one: raw material preparation, the raw material includes 1,4 butanediol and catalyst for dehydrogenation reaction with 1,4 butanediol; Step two: screening, weighing and subpackaging the catalyst in the raw material through a catalyst screening device; Step three: precise loading of the catalyst in step two through a catalyst column device; Step four: differential pressure test of the catalyst column device in step three, and putting into a dehydrogenation reactor; Step five: closing the dehydrogenation reactor head, pressure test, leak detection, replacement, system feeding and start-up. The catalyst screening device comprises a support frame, a screening structure detachably connected with the support frame, and a weighing structure installed at the bottom of the screening structure, the screening structure comprises a screening assembly, bosses fixed at both ends of the screening assembly, and a plurality of installation grooves opened on the screening assembly, both ends of the support frame are provided with connection grooves, the bosses are used in cooperation with the connection grooves, and a plurality of inflow holes for catalyst inflow are arranged at the top of the screening assembly; The weighing structure comprises a weighing tube, a rotating plate rotatably connected in the weighing tube, and an air pump fixed at the bottom in the weighing tube, an elastic rod is arranged between the rotating plate and the air pump, the outer periphery of the elastic rod is wrapped with an air bag connected with the air pump, a rotating shaft is arranged at the left end of the rotating plate, and the elastic rod is arranged at the right end of the rotating plate; The catalyst column device comprises a column threadedly connected with the weighing tube, a first plug for marking, a first porcelain ball, a second porcelain ball arranged in sequence in the column, and a weighing sensor arranged on the first porcelain ball, and the weighing sensor is electrically connected with the air pump.

2. The BDO dehydrogenation reactor catalyst loading method of claim 1, wherein, The catalyst in step one is a copper powder catalyst, and the preparation method of the copper powder catalyst is as follows: A1: a copper nitrate solution is mixed with a sodium carbonate solution in a certain proportion, stirred to generate a precipitate, the precipitate is filtered, and after filtration, the precipitate is washed, dried, calcined and crushed; A2: after crushing, the copper powder is sampled, and the sample is added to a reaction tube for catalyst activity determination.

3. The BDO dehydrogenation reactor catalyst loading method of claim 2, wherein, The drying temperature in step A1 is 100 DEG C, the calcination temperature is 450 DEG C, and the whole step is carried out in a normal pressure environment.

4. The BDO dehydrogenation reactor catalyst loading method of claim 1, wherein, The bottom of the installation groove is fixed with a first spring, and the installation groove is detachably provided with a screen.

5. The BDO dehydrogenation reactor catalyst loading method of claim 1, wherein, A button is slidably connected to the boss, a spring rod connected with the button is arranged in the end of the screening assembly close to the button, and the other end of the spring rod is provided with a second spring which passes out of the upper top of the installation groove.

6. The BDO dehydrogenation reactor catalyst loading method of claim 1, wherein, The catalyst is placed between the first porcelain ball and the second porcelain ball, the catalyst is weighed through the first porcelain ball, and the catalyst is columned by the sealing of the second porcelain ball.

7. The BDO dehydrogenation reactor catalyst loading method of claim 1, wherein, When the catalyst column device is subjected to differential pressure test in step four, a second plug for marking that the differential pressure test is being carried out is wound around the periphery of the column, and the first plug and the second plug are different in color.

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