Preparation system of hydrogenation catalyst

Abstract

The utility model relates to the technical field of catalyst preparation, and discloses a preparation system of a hydrogenation catalyst, the preparation system of the hydrogenation catalyst comprises a liquid preparation unit, a dissolving and preparing unit, a dipping unit and a weighing unit, the liquid preparation unit comprises a liquid preparation kettle, the liquid preparation kettle is provided with an acid liquor inlet and an alkali liquor inlet which are respectively provided with a control valve; the dissolving and preparing unit comprises a dissolving and preparing tank and a heating device, the dissolving and preparing tank is communicated with the liquid preparing kettle, and the heating device is used for heating slurry in the dissolving and preparing tank; the dipping unit comprises a dipping kettle communicated with the dissolving and preparing tank, and the dipping kettle is provided with a carrier inlet; the weighing unit comprises a slurry dosage groove and a carrier stock bin which are respectively provided with a weighing device, the slurry dosage groove is arranged on a communicating pipeline of the liquid preparation kettle and the dissolving preparation tank, and the carrier stock bin is communicated with the carrier inlet. The continuous hydrogenation catalyst production device has the advantages of continuous hydrogenation catalyst production, cost reduction and labor intensity reduction.

Description

TECHNICAL FIELD

[0001] The utility model relates to hydrogenation catalyst preparation technical field, concretely relates to a kind of preparation system of hydrogenation catalyst. BACKGROUND

[0002] In recent years, with the continuous increase of ethylene production capacity and the trend of increasingly inferior and heavy cracking feedstock, the production of ethylene by-products cracking gasoline and heavy fraction has significantly increased. In order to make full use of these by-products, it is of great significance to develop high-value downstream products. In the traditional ethylene production process, cracking gasoline and heavy fraction not only account for a large proportion of by-products, but also bring challenges to subsequent treatment due to their complex chemical composition. These by-products contain a large amount of aromatic hydrocarbons, olefins and heterocyclic compounds, which can be used for the production of fuel and basic chemicals to some extent, but their low added value limits the improvement of overall economic benefits.

[0003] Currently, the market demand for high-performance chemicals and clean energy is increasing, and the traditional treatment method is not up to the task. Therefore, improving the conversion efficiency and product value of these by-products has become an important issue in the chemical industry. Hydrogenation technology, as an effective chemical conversion means, can promote the conversion of by-products to higher value-added products such as olefins, gasoline and diesel by removing impurities and unsaturated components in the by-products. However, existing hydrogenation catalysts still have limitations in catalytic efficiency, selectivity and long-term stability, especially when dealing with heavy feedstock, the performance and service life of the catalyst are often affected.

[0004] The existing production technology of cracking gasoline hydrogenation catalyst needs manual feeding, measuring, sub-packaging and conveying, resulting in high labor intensity, low daily output and inability to meet the needs of high-quality development. INVENTION CONTENTS

[0005] The utility model aims at overcoming the problems of existing production technology that needs manual feeding, measuring, sub-packaging and conveying, resulting in high labor intensity, low daily output and inability to meet the needs of high-quality development, and provides a preparation system of hydrogenation catalyst, which has the advantages of continuous production of hydrogenation catalyst, reduced cost and labor intensity.

[0006] To achieve the above-mentioned purpose, the utility model provides a preparation system of hydrogenation catalyst, which comprises:

[0007] The liquid preparation unit comprises a liquid preparation kettle, and the liquid preparation kettle has an acid liquid inlet and an alkali liquid inlet each provided with a control valve;

[0008] The solution preparation unit comprises a solution preparation tank and a heating device, the solution preparation tank is in communication with the liquid preparation kettle, and the heating device is used for heating the slurry in the solution preparation tank;

[0009] The impregnation unit comprises an impregnation kettle connected with the dissolving tank, and the impregnation kettle is provided with a carrier inlet;

[0010] The weighing unit comprises a slurry dosing tank and a carrier bin, each of which is provided with a weighing device, the slurry dosing tank is installed on the connecting pipeline of the dissolving tank and the dissolving tank, and the carrier bin is connected with the carrier inlet.

[0011] By the above technical scheme, the preparation system of the hydrogenation catalyst can realize continuous production of the hydrogenation catalyst, which helps to improve the production efficiency of the catalyst, reduce the cost, reduce the labor intensity, improve the daily average output, and is easy to realize automation. BRIEF DESCRIPTION OF DRAWINGS

[0012] Figure 1 is a flow schematic diagram of the preparation system of the hydrogenation catalyst of the specific embodiment;

[0013] REFERENCE SIGNS

[0014] REFERENCE SIGNS

[0015] 1 alkali tank;2 acid tank;3 dissolving tank;4 dissolving tank pH value on-line monitor;5 slurry dosing tank;9 dissolving tank;11 carrier bin;13 impregnation kettle;15 impregnation kettle pH value on-line detector;17 temperature measuring instrument;19 palladium ion on-line spectrometer;21 discharge kettle;23 light sensing device;25 drying box;26 roller kiln. DETAILED DESCRIPTION

[0016] The specific embodiments described herein are intended to be illustrative only and are not intended to limit the scope of the present application. Other embodiments within the scope of the present application are possible and will be readily apparent to those of ordinary skill in the art.

[0017] The endpoints of the ranges and any values disclosed herein are not limited to the precise values stated. The endpoints of the ranges and any values are provided as approximate descriptions of the ranges and are understood to be open-ended. Each range disclosed herein is to be understood to include individual values, and sub-ranges, falling within the stated range. In other words, any numerical value within the range is specifically contemplated. For values which are less than one, or contain an exponent, e.g., 0.1, 0.01, etc., the decimal equivalent or exact fractional value is so contemplated in this disclosure. For values which are greater than one or contain a fraction, or are not in decimal form, such as 1 / 2, 1 / 4, 2 1 / 2, etc., the equivalent decimal, exact fraction, or exact decimal value is so contemplated in this disclosure. For numerical ranges that end with "Ct", "Cm", or "Cp", it is intended to mean that each individual number falling within that range, and fractions thereof, are contemplated in this disclosure.

[0018] The utility model discloses a kind of preparation systems of hydrogenation catalyst, such as Figure 1As shown, the hydrogenation catalyst preparation system comprises a weighing unit and sequentially connected liquid preparation unit, solution preparation unit and impregnation unit; wherein, the liquid preparation unit comprises a liquid preparation kettle 3 for preparing impregnation liquid, the liquid preparation kettle 3 is provided with acid liquid inlet and alkali liquid inlet each provided with a control valve; the solution preparation unit comprises a solution preparation tank 9 and a heating device, the solution preparation tank 9 is communicated with the liquid preparation kettle 3, and the heating device is used for heating the slurry in the solution preparation tank 9; the impregnation unit comprises an impregnation kettle 13 communicated with the solution preparation tank 9, and the impregnation kettle 13 is provided with a carrier inlet; the weighing unit comprises a slurry dosing tank 5 and a carrier bin 11 each provided with a weighing device, the slurry dosing tank 5 is installed on the communication pipeline of the liquid preparation kettle 3 and the solution preparation tank 9, and the carrier bin 11 is communicated with the carrier inlet, specifically, the impregnation liquid prepared in the liquid preparation kettle 3 enters the slurry dosing tank 5 for weighing, then enters the solution preparation tank 9 for heating, and then enters the impregnation kettle 13 to be contacted and impregnated with the carrier weighed by the carrier bin 11.

[0019] The hydrogenation catalyst preparation system can realize continuous production of hydrogenation catalyst, improve the production efficiency of the catalyst, reduce the cost, reduce the labor intensity, improve the daily output, and meet the demand of high-quality development.

[0020] In the utility model, the material and specification of the liquid preparation kettle, the solution preparation tank, the impregnation kettle, the slurry dosing tank 5 and the carrier bin 11 are not specially required, for example, the material of the slurry dosing tank 5 can be plastic, the volume range can be 100-500L, the inner wall material of the carrier bin 11 can be enamel glass, the volume can be 300-800L, the liquid preparation kettle can adopt plastic, the volume range can be 300-800L, the inner wall material of the solution preparation tank can be enamel glass, the volume can be 150-500L, and the inner wall material of the impregnation kettle can be enamel glass, and the volume can be 150-500L; the utility model does not have special requirements for the weighing device and the heating device, and they can be conventional weighing devices and heating devices in the prior art, for example, the weighing device can be an electronic scale in the field.

[0021] The liquid preparation unit comprises an acid liquid tank 2 communicated with the acid liquid inlet and an alkali liquid tank 1 communicated with the alkali liquid inlet.

[0022] The impregnation kettle 13 and the liquid preparation kettle 3 are each provided with a stirring device in the prior art to improve the mixing efficiency of the materials.

[0023] The impregnation kettle 13 is provided with a conventional heater and a temperature measuring instrument 17, and the temperature measuring instrument 17 can be an online temperature measuring instrument to detect the temperature of the materials in the impregnation kettle.

[0024] As shown in the figure, Figure 1As shown, the impregnation vessel 13 is equipped with an outlet pipeline, on which a delivery pump is installed and connected to an online palladium ion spectrometer 19 for detecting the palladium ion content of the impregnation solution.

[0025] To facilitate pH value detection, the hydrogenation catalyst preparation system includes a pH measuring device. This device comprises an online pH monitor 4 for monitoring the pH of the slurry in the mixing tank 3 and an online pH detector 15 for monitoring the pH of the slurry in the impregnation tank 13. In this invention, there are no special requirements for the online pH monitor 4 for the mixing tank and the online pH detector 15 for the impregnation tank; commercially available online pH detectors can be used.

[0026] The control valves for the acid and alkali inlets can be solenoid valves. The online pH monitor for the mixing tank is electrically connected to the solenoid valves installed at the acid and alkali inlets, respectively. It can automatically control the addition of alkali and acid according to the set pH value to automatically regulate the slurry in the mixing tank.

[0027] The hydrogenation catalyst preparation system includes a solid-liquid separation unit, which includes a discharge vessel 21 and a photosensitive device 23. The discharge vessel 21 is connected to the impregnation vessel 13 and is equipped with a rinsing water inlet. The discharge vessel 21 is equipped with a rinsing water outlet pipeline. After the catalyst in the impregnation vessel is impregnated, it is fed into the discharge vessel 21 for rinsing. The rinsing water outlet pipeline is equipped with a photosensitive device 23. When the rinsing water in the rinsing water outlet pipeline becomes transparent again, the catalyst rinsing is considered to be completed.

[0028] The hydrogenation catalyst preparation system includes a drying unit for drying and calcining the catalyst after rinsing. The drying unit comprises a connected roller kiln 26 and a drying chamber 25 equipped with a hot air blower. The drying chamber 25 is connected to the discharge vessel 21. This invention does not have special requirements for the roller kiln 26 and the drying chamber 25; commercially available roller kilns 26 and drying chambers 25 equipped with hot air blowers can be used. Further details regarding these requirements will not be elaborated upon here.

[0029] To increase the throughput of the hydrogenation catalyst preparation system of this invention or to add utility production lines, such as Figure 1 As shown, the hydrogenation catalyst preparation system has at least two parallel preparation processes. Specifically, the solvent preparation unit includes at least two solvent preparation tanks 9 connected in parallel, the impregnation unit includes at least two impregnation kettles 13 connected in parallel, the weighing unit includes at least two slurry dosing tanks 5 connected in parallel and at least two carrier silos 11 connected in parallel, and the solid-liquid separation unit includes at least two discharge kettles 21 connected in parallel, with a photosensitive device 23 installed on the rinsing water outlet pipeline of each discharge kettle 21.

[0030] It is understandable that, such as Figure 1As shown, the hydrogenation catalyst preparation system of this invention, as needed, is equipped with control valves at the inlet of each container or on the flow pipeline between containers. To facilitate automatic control, commercially available solenoid valves can be used. To further achieve automation, the aforementioned solenoid valves, the heating device of the dissolution unit in the preparation system, the stirring device of the impregnation vessel 13 and the liquid preparation vessel 3, the heater of the impregnation vessel 13, the thermometer 17, the palladium ion online spectrometer 19, the impregnation vessel pH online detector 15, the liquid preparation vessel pH online monitor 4, the photosensitive device 23, the transfer pump, and other electric equipment can be centrally controlled using the Siemens SIMATIC S7400 system. The field equipment of the device is connected to the upper-level S7400 system through the SIMATIC S7200 or S7300 system. The aforementioned hydrogenation catalyst preparation system of this invention is designed to easily improve the automation level of the hydrogenation catalyst preparation process.

[0031] Based on the foregoing disclosure, this utility model discloses a method for preparing a hydrogenation catalyst. The preparation method employs the hydrogenation catalyst preparation system described in this utility model, and includes:

[0032] 1) Prepare the impregnation solution in the mixing tank 3, and adjust the pH value of the impregnation solution by feeding acid solution through the acid inlet or alkali solution through the alkali inlet.

[0033] 2) The preset weight of impregnation liquid is fed into the dissolving tank 9 through the slurry dosing tank 5 and heated to the preset temperature by the heating device;

[0034] 3) The impregnation solution in the dissolution tank 9 in step 2) is fed into the impregnation vessel 13, and the carrier of a predetermined weight is fed into the impregnation vessel 13 through the carrier hopper 11 for impregnation to obtain the hydrogenation catalyst.

[0035] The method for preparing the hydrogenation catalyst of this invention enables continuous production of hydrogenation catalyst, which helps to improve the production efficiency of the catalyst, reduce costs, reduce labor intensity, increase daily output, and meet the needs of high-quality development.

[0036] In some embodiments of this utility model, in step 1), palladium solution, additives and water are mixed in a mixing tank to obtain an impregnation solution. Preferably, the palladium solution is selected from a 10wt%-30wt% aqueous solution of chloropalladium acid, and the additives are 40wt%-70wt% aqueous solution of ammonium chloroacetate. More preferably, the mass ratio of the 10wt%-30wt% aqueous solution of chloropalladium acid, the 40wt%-70wt% aqueous solution of ammonium chloroacetate and water is 3-5:1:10-200.

[0037] In some embodiments of this utility model, the time for mixing palladium solution, additives and water in the mixing tank in step 1) is 20-55 minutes.

[0038] In some embodiments of this utility model, in step 1), the acid solution is selected from citric acid aqueous solution and / or glacial acetic acid aqueous solution, preferably citric acid aqueous solution; the alkaline solution is selected from one or more of potassium carbonate aqueous solution, potassium nitrate aqueous solution, and potassium hydroxide aqueous solution, preferably potassium carbonate aqueous solution.

[0039] In some embodiments of this utility model, the pH range of the impregnation solution in the preparation vessel in step 1) can be controlled to be 2-5.

[0040] In some embodiments of this utility model, the preset temperature in step 2) is 20-100℃.

[0041] In some embodiments of this invention, the weight ratio of the impregnation liquid to the carrier in step 3) is 16:9-27:10. This invention has no special requirements for the carrier and can be a conventional carrier in hydrogenation catalysts, such as an alumina carrier.

[0042] In some embodiments of this utility model, the amount of carrier added to a single impregnation vessel in step 3) is 200-600 kg.

[0043] In some embodiments of this utility model, the soaking time in step 3) is 5-60 minutes.

[0044] In some embodiments of this utility model, the temperature range of the impregnation kettle is controlled to be 20-100°C during step 3) of the impregnation process.

[0045] In some embodiments of this utility model, step 3) the impregnation process is divided into at least two stages, preferably at least three stages, and more preferably the stirring frequency and / or impregnation temperature of each stage are the same or different.

[0046] In some embodiments of this invention, the stirring frequency in step 3) decreases as the impregnation stage increases.

[0047] In some embodiments of this utility model, the stirring frequency of each stage in step 3) is as follows: the stirring frequency is 5-40Hz when the soaking time is within 10 minutes, the stirring frequency is 5-30Hz when the soaking time is 10-30 minutes, and the stirring frequency is 5-20Hz when the soaking time exceeds 30 minutes.

[0048] In some embodiments of this invention, the immersion temperature in step 3) increases as the immersion stage increases.

[0049] In some embodiments of this utility model, the impregnation temperatures at each stage of step 3) are as follows: the initial temperature after the impregnation liquid and the carrier are mixed is 60±10℃, the impregnation temperature after 10 minutes of impregnation is 35~100℃, and the impregnation temperature after 25 minutes of impregnation is 80~110℃.

[0050] In some embodiments of this utility model, in step 3), the palladium ion content of the impregnation solution in the impregnation vessel is detected by an online palladium ion spectrometer, wherein the measurement cycle is 5-15 min / time.

[0051] In this invention, when the readings of the palladium ion online spectrometer 19, the temperature measuring instrument 17 of the impregnation vessel, and the pH value monitoring instrument of the impregnation vessel are all within the specified range and stable, it indicates that the carrier has been completely impregnated. In some embodiments of this invention, the preparation method further includes:

[0052] 4) Feed the fully impregnated material from step 3) into the discharge vessel for rinsing until the photosensitive device installed on the rinsing water outlet pipeline detects that the rinsing water has returned to transparency, then the catalyst rinsing is considered complete;

[0053] 5) The flushed catalyst is fed sequentially into the drying box and roller kiln for drying and calcination.

[0054] In some embodiments of this utility model, in step 5), the air volume of the hot air blower of the drying oven is preferably 1500-3000 m³ / h. 3 / h, hot air temperature 80-200℃.

[0055] In some embodiments of this utility model, in step 5), the preferred calcination temperature is 300-800℃.

[0056] The advantages of this utility model will be illustrated by the following embodiments, but this utility model is not limited thereto. Unless otherwise specified, the experimental methods in the following embodiments are conventional methods in the art. Unless otherwise specified, the experimental materials used in the following embodiments are commercially available. Unless otherwise specified, the reagent dosages are those used in conventional experimental operations. Unless otherwise defined, the technical terms used in the following detailed embodiments have the same meaning as commonly understood by those skilled in the art to which this utility model pertains.

[0057] In the following embodiments:

[0058] The test method for bulk density adopts GB / T 6286-2021;

[0059] The test method for crushing strength adopts HG / T 2782-2011;

[0060] The test method for wear rate adopts HG / T 2976-2011;

[0061] The specific surface area test method adopts GB / T 5816-2008.

[0062] Example 1

[0063] Adopting such Figure 1The hydrogenation catalyst preparation system shown prepares a cracked gasoline hydrogenation catalyst, comprising the following:

[0064] 1) Add 10wt% chloropalladium acid aqueous solution, 70wt% ammonium chloroacetate aqueous solution, and water to the mixing tank 3 at a mass ratio of 15:4:100, and mix for 30 minutes with stirring at 15Hz. During this process, add citric acid aqueous solution from acid tank 2 or potassium carbonate aqueous solution from alkali tank 1 according to the reading of the pH value online monitoring instrument 4 in the mixing tank to make the pH of the mixture 3.5. The mixing tank is made of plastic and has a volume of 500L. The alkali tank and acid tank are made of glass and preferably have a volume of 350L.

[0065] 2) Divide the mixture obtained in 1) equally into two parallel slurry dosing tanks 5. Each slurry dosing tank 5 is connected to an electronic scale and can dispense a specified weight of slurry. The slurry dosing tank is made of plastic and has a volume of 300L. The weight of the slurry in each slurry dosing tank is 300kg.

[0066] 3) Transfer the slurry from each slurry dosage tank 5 in 2) into its respective dissolving tank 9 and heat it to 75°C. The dissolving tank is equipped with an online temperature monitor and a heater. The inner wall of the dissolving tank is made of enamel and has a volume of 450L. During the slurry heating process, the online temperature monitor can be used to check whether the set value has been reached.

[0067] 4) Transfer the slurry from the two dissolving tanks 9 in 3) into their respective impregnation tanks 13. Add the alumina carrier from the two carrier silos 11 into their respective impregnation tanks 13, stir and mix, and begin impregnation. Each carrier silo 11 is connected to an electronic scale. Each carrier silo 11 can hold a set weight of carrier. The inner walls of the impregnation tank and the carrier silos are made of enamel. The impregnation tank has a volume of 450L, and the carrier silos have a volume of 750L.

[0068] The carrier added to a single impregnation tank is 450 kg, and the impregnation time is 30 minutes. The stirring frequency of the stirrer in the impregnation tank is 20 Hz within the first 10 minutes of impregnation, 15 Hz from 10 to 30 minutes, and 10 Hz after impregnation for more than 30 minutes.

[0069] The initial temperature of the impregnation solution and the carrier after mixing in the impregnation vessel is 60℃, the temperature is 75℃ after 10 minutes of impregnation, and the temperature is 95℃ after 25 minutes of impregnation; each impregnation vessel is connected to an online palladium ion spectrometer 19, with a measurement cycle of 10 minutes / time;

[0070] When the readings of the palladium ion online spectrometer, the temperature online monitor, and the pH value online monitor of the impregnation vessel are within the specified range and stable, it indicates that the alumina carrier has been completely impregnated.

[0071] 5) After all the materials that have been fully impregnated in 4) are transferred to their respective discharge vessels for solid-liquid separation, they are sent to the drying box 25 for drying. The discharge vessel is equipped with rinsing water and a photosensitive device 23 is installed at the bottom outlet. The rinsing water is connected to the photosensitive device 23 and is used to rinse the catalyst. When the photosensitive device 23 detects that the rinsing water has returned to transparency, the catalyst rinsing is considered to be completed.

[0072] The discharge vessel is made of glass enamel and has a volume of 450L; the hot air blower in the drying oven has an air volume of 2200 m³ / m³. 3 / h; Temperature 150℃;

[0073] 6) The catalyst obtained in 5) is transferred to roller kiln 26 for calcination. The roller kiln is under normal pressure, the inner wall material is refractory brick, and the temperature is 750℃.

[0074] Results: The average daily catalyst yield was 1.4t, the bulk density was 0.3±0.05g / ml, the crushing strength was ≥60N / cm, the wear rate was ≤0.8%, the specific surface area was 180±20㎡ / g, and the production of hydrogenation catalyst required 9 people / day.

[0075] Example 2

[0076] Unlike Example 1, 1) 15 wt% aqueous solution of chloropalladium acid, 50 wt% aqueous solution of ammonium chloroacetate, and water were added to the mixing tank 3 at a mass ratio of 9:3:50 and mixed at a stirring speed of 20 Hz for 25 min. Citric acid aqueous solution in acid tank 2 or potassium nitrate aqueous solution in alkali tank 1 was added according to the reading of the pH value online monitoring instrument 4 of the mixing tank to make the pH of the mixture 5. The mixing tank was made of plastic with a volume of 500 L, and the alkali tank and acid tank were made of glass with a volume of 350 L each.

[0077] 2) Divide the mixture obtained in 1) equally into two parallel slurry dosing tanks 5. Each slurry dosing tank 5 is connected to an electronic scale and can dispense a specified weight of slurry. The slurry dosing tank is made of plastic and has a volume of 300L. The weight of the slurry in each slurry dosing tank is 300kg.

[0078] 3) Transfer the slurry from each slurry dosage tank 5 in 2) into its respective dissolving tank 9 and heat it to 35°C. The dissolving tank is equipped with an online temperature monitor and a heater. The inner wall of the dissolving tank is made of enamel and has a volume of 450L. During the slurry heating process, the online temperature monitor can be used to check whether the set value has been reached.

[0079] 4) Transfer the slurry from the two dissolving tanks 9 in 3) into their respective impregnation tanks 13. Add the alumina carrier from the two carrier silos 11 into their respective impregnation tanks 13, stir and mix, and begin impregnation. Each carrier silo 11 is connected to an electronic scale. Each carrier silo 11 can hold a set weight of carrier. The inner walls of the impregnation tank and the carrier silos are made of enamel. The impregnation tank has a volume of 450L, and the carrier silos have a volume of 750L.

[0080] The carrier added to a single impregnation vessel is 480 kg, and the impregnation time is 55 minutes. The stirring frequency of the stirrer in the impregnation vessel is 35 Hz within the first 10 minutes of impregnation; the stirring frequency is 20 Hz within 10-30 minutes; and the stirring frequency is 5 Hz after impregnation for more than 30 minutes.

[0081] The initial temperature of the impregnation solution and the carrier after mixing in the impregnation vessel is 65℃. After 10 minutes of impregnation, the temperature is 100℃, and after 25 minutes of impregnation, the temperature is 110℃. Each impregnation vessel is connected to an online palladium ion spectrometer 19, with a measurement cycle of 6 minutes / time.

[0082] When the readings of the palladium ion online spectrometer, the temperature online monitor, and the pH value online monitor of the impregnation vessel are within the specified range and stable, it indicates that the alumina carrier has been completely impregnated.

[0083] 5) After all the materials that have been fully impregnated in 4) are transferred to their respective discharge vessels for solid-liquid separation, they are sent to the drying box 25 for drying. The discharge vessel is equipped with rinsing water and a photosensitive device 23 is installed at the bottom outlet. The rinsing water is connected to the photosensitive device 23 and is used to rinse the catalyst. When the photosensitive device 23 detects that the rinsing water has returned to transparency, the catalyst rinsing is considered to be completed.

[0084] The discharge vessel is made of glass enamel and has a volume of 450L; the hot air blower in the drying oven has an air volume of 1500 m³ / m³. 3 / h; Temperature 80℃;

[0085] 6) The catalyst obtained in 5) is transferred to roller kiln 26 for calcination. The roller kiln is under normal pressure, the inner wall material is refractory brick, and the temperature is 300℃.

[0086] Results: The average daily catalyst yield was 1.5t, the bulk density was 0.5±0.03g / ml, the crushing strength was ≥65N / cm, the wear rate was ≤0.5%, the specific surface area was 170±10㎡ / g, and the production of hydrogenation catalyst required 9 people / day.

[0087] Example 3

[0088] 1) Add 25wt% chloropalladium acid aqueous solution, 65wt% ammonium chloroacetate aqueous solution and water to the mixing tank 3 at a mass ratio of 5:1:45, and mix at a stirring speed of 25Hz for 50min. During this process, add glacial acetic acid aqueous solution from acid tank 2 or potassium hydroxide aqueous solution from alkali tank 1 according to the reading of the pH value online monitoring instrument 4 in the mixing tank to make the pH of the mixture 2. The mixing tank is made of plastic and has a volume of 500L. The alkali tank and acid tank are made of glass and preferably have a volume of 350L.

[0089] 2) Divide the mixture obtained in 1) equally into two parallel slurry dosing tanks 5. Each slurry dosing tank 5 is connected to an electronic scale and can dispense a specified weight of slurry. The slurry dosing tank is made of plastic and has a volume of 300L. The weight of the slurry in each slurry dosing tank is 300kg.

[0090] 3) Transfer the slurry from each slurry dosage tank 5 in 2) into its respective dissolving tank 9 and heat it to 95°C. The dissolving tank is equipped with an online temperature monitor and a heater. The inner wall of the dissolving tank is made of enamel and has a volume of 450L. During the slurry heating process, the online temperature monitor can be used to check whether the set value has been reached.

[0091] 4) Transfer the slurry from the two dissolving tanks 9 in 3) into their respective impregnation tanks 13. Add the alumina carrier from the two carrier silos 11 into their respective impregnation tanks 13, stir and mix, and begin impregnation. Each carrier silo 11 is connected to an electronic scale. Each carrier silo 11 can hold a set weight of carrier. The inner walls of the impregnation tank and the carrier silos are made of enamel. The impregnation tank has a volume of 450L, and the carrier silos have a volume of 750L.

[0092] The carrier was added to each impregnation vessel in a 300 kg volume, and the impregnation time was 20 minutes. The stirring frequency of the stirrer in the impregnation vessel was 20 Hz during the first 10 minutes of impregnation, and 12 Hz after 10 minutes. The initial temperature of the impregnation solution and carrier after mixing in the impregnation vessel was changed to 70 ℃, and the temperature was 85 ℃ after 10 minutes of impregnation. Each impregnation vessel was connected to a palladium ion online spectrometer 19, with a measurement cycle of 15 min / time.

[0093] When the readings of the palladium ion online spectrometer, the temperature online monitor, and the pH value online monitor of the impregnation vessel are within the specified range and stable, it indicates that the alumina carrier has been completely impregnated.

[0094] 5) After all the materials that have been fully impregnated in 4) are transferred to their respective discharge vessels for solid-liquid separation, they are sent to the drying box 25 for drying. The discharge vessel is equipped with rinsing water and a photosensitive device 23 is installed at the bottom outlet. The rinsing water is connected to the photosensitive device 23 and is used to rinse the catalyst. When the photosensitive device 23 detects that the rinsing water has returned to transparency, the catalyst rinsing is considered to be completed.

[0095] The discharge vessel is made of glass enamel and has a volume of 450L; the hot air blower in the drying oven has an air volume of 2800 m³ / m³. 3 / h; Temperature 190℃;

[0096] 6) The catalyst obtained in 5) is transferred to roller kiln 26 for calcination. The roller kiln is under normal pressure, the inner wall material is refractory brick, and the temperature is 550℃.

[0097] Results: The average daily catalyst yield was 1.2t, the bulk density was 0.8±0.02g / ml, the crushing strength was ≥55N / cm, the wear rate was ≤1%, the specific surface area was 150±20㎡ / g, and the production of hydrogenation catalyst required 9 people / day.

[0098] Example 4

[0099] Unlike Example 1, the stirring frequency of the stirrer in the impregnation tank was maintained at 20Hz during the impregnation process, and the air volume of the hot air blower in the drying oven 25 was 1800 m³ / m³. 3 / h; temperature 180℃. The catalyst obtained after drying is transferred to roller kiln 26 for calcination. The roller kiln is under normal pressure, and the inner wall material is refractory brick. The temperature is 700℃.

[0100] Results: The average daily catalyst yield was 1.4t, the catalyst bulk density was 0.1±0.05g / ml, the crushing strength was ≥50N / cm, the wear rate was ≤3%, the specific surface area was 150±5㎡ / g, and the production of hydrogenation catalyst required 9 people / day.

[0101] Example 5

[0102] Unlike Example 1, the stirring frequency of the stirrer in the impregnation tank was maintained at 20 Hz during the impregnation process.

[0103] Results: The average daily catalyst yield was 1.3t, the catalyst bulk density was 0.1±0.05g / ml, the crushing strength was ≥65N / cm, the wear rate was ≤5%, the specific surface area was 155±5㎡ / g, and the production of hydrogenation catalyst required 9 people / day.

[0104] Example 6

[0105] Unlike Example 1, the temperature during the impregnation process was 75°C, and the airflow of the hot air blower in the drying oven 25 was set to 1100 m³ / m³. 3 / h; temperature 145℃. The dried catalyst is transferred to roller kiln 26 for calcination. The roller kiln is under normal pressure, with the inner wall material being refractory bricks, and the temperature is 650℃.

[0106] Results: The average daily catalyst yield was 1.4 t, the catalyst bulk density was 0.25 ± 0.02 g / ml, and the crushing strength was...

[0107] ≥65N / cm, wear rate ≤1.3%, specific surface area 145±3㎡ / g, production of hydrogenation catalyst requires 9 people / day.

[0108] Example 7

[0109] Unlike Example 1, the temperature was maintained at 75°C during the impregnation process.

[0110] Results: The average daily catalyst yield was 1.3t, the catalyst bulk density was 0.3±0.07g / ml, the crushing strength was ≥45N / cm, the wear rate was ≤2%, the specific surface area was 155±5㎡ / g, and the production of hydrogenation catalyst required 9 people / day.

[0111] Comparative Example 1

[0112] Unlike Example 1, manual feeding, measurement, packaging and conveying are used, but otherwise the process is the same as in Example 1.

[0113] Results: The average daily catalyst yield was 720 kg, the catalyst bulk density was 0.5 ± 0.05 g / ml, the crushing strength was ≥ 60 N / cm, the wear rate was ≤ 10%, the specific surface area was 155 ± 5 m² / g, and the production of hydrogenation catalyst required 13 people / day.

[0114] The preferred embodiments of the present invention have been described in detail above with reference to the accompanying drawings; however, the present invention is not limited thereto. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, including the combination of various specific technical features in any suitable manner. To avoid unnecessary repetition, the present invention will not describe the various possible combinations separately. However, these simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention.

Claims

1. A system for preparing a hydrogenation catalyst, characterized in that, The preparation system for the hydrogenation catalyst includes: The liquid preparation unit includes a liquid preparation vessel (3), which has an acid inlet and an alkali inlet, each equipped with a control valve; The dissolution unit includes a dissolution tank (9) and a heating device. The dissolution tank (9) is connected to the liquid preparation vessel (3). The heating device is used to heat the slurry in the dissolution tank (9). The impregnation unit includes an impregnation vessel (13) connected to the dissolution tank (9), and the impregnation vessel (13) has a carrier inlet; The weighing unit includes a slurry dosing tank (5) and a carrier silo (11), each equipped with a weighing device. The slurry dosing tank (5) is installed on the connecting pipeline between the dispensing vessel (3) and the dissolving tank (9). The carrier silo (11) is connected to the carrier inlet.

2. The preparation system for the hydrogenation catalyst according to claim 1, characterized in that, The solution preparation unit includes an acid tank (2) connected to the acid inlet and an alkali tank (1) connected to the alkali inlet.

3. The preparation system for the hydrogenation catalyst according to claim 1, characterized in that, The impregnation tank (13) and the liquid preparation tank (3) are each equipped with a stirring device; and / or The impregnation vessel (13) is equipped with a thermometer (17); and / or The impregnation vessel (13) is equipped with an outlet pipeline, on which a delivery pump is installed and connected to an online palladium ion spectrometer (19).

4. The preparation system for the hydrogenation catalyst according to claim 1, characterized in that, The hydrogenation catalyst preparation system includes a pH measuring device, which includes an online pH monitor (4) for monitoring the pH of the slurry in the mixing tank (3).

5. The preparation system for the hydrogenation catalyst according to claim 4, characterized in that, The pH measuring device includes an online pH meter (15) for detecting the pH of the slurry in the impregnation tank (13).

6. The preparation system for the hydrogenation catalyst according to claim 1, characterized in that, The hydrogenation catalyst preparation system includes a solid-liquid separation unit, which includes a discharge vessel (21). The discharge vessel (21) is connected to the impregnation vessel (13) and is provided with a rinsing water inlet. The discharge vessel (21) is provided with a rinsing water outlet pipeline.

7. The preparation system for the hydrogenation catalyst according to claim 6, characterized in that, The solid-liquid separation unit includes a photosensitive device (23) installed on the flushing water outlet pipeline.

8. The preparation system for the hydrogenation catalyst according to claim 1, characterized in that, The hydrogenation catalyst preparation system includes a drying unit, which includes a roller kiln (26) connected to each other and a drying box (25) equipped with a hot air blower. The drying box (25) is connected to the discharge vessel (21).

9. The preparation system for the hydrogenation catalyst according to any one of claims 1-8, characterized in that, The dissolution unit includes at least two dissolution tanks (9) connected in parallel, the impregnation unit includes at least two impregnation kettles (13) connected in parallel, and the weighing unit includes at least two slurry dosing tanks (5) connected in parallel and at least two carrier silos (11) connected in parallel.

10. The preparation system for the hydrogenation catalyst according to claim 9, characterized in that, The solid-liquid separation unit includes at least two discharge vessels (21) connected in parallel, and each discharge vessel (21) has a photosensitive device (23) installed on its flushing water outlet line.

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