Method for improving quality of catalyst product

Abstract

The invention discloses a method for improving the quality of a catalyst product. The method comprises the following steps: selecting high-purity and low-impurity-content raw materials; pretreating the raw materials; mixing the raw materials; a forming method is selected according to application requirements, and forming parameters are optimized; roasting the raw materials under a certain roasting condition; carrying out activating treatment on the roasted raw materials; an online monitoring system is introduced in the production process; carrying out comprehensive quality inspection on each batch of catalyst; and detailed production records and quality files are established for each batch of products. By optimizing the whole process from raw material selection to finished product inspection, it is ensured that the catalyst has higher activity, selectivity and stability, the application effect of the catalyst is remarkably improved, the product consistency and economical efficiency are finally improved, and by improving the purity and uniformity of the raw materials and through the synergistic effect of physical and chemical cleaning, the product quality is improved. The problem that impurities remain on the surfaces of raw materials is solved, and preconditions are provided for uniform mixing and stable forming.

Description

TECHNICAL FIELD

[0002] The present application relates to the technical field of catalysts, in particular to a method for improving the quality of catalyst products. BACKGROUND

[0004] Catalysts play a crucial role in the chemical industry and are widely used in petroleum refining, petrochemicals, coal chemical industry, fine chemical industry and other fields. The quality of catalysts directly affects the reaction efficiency, product yield and production cost. However, in actual production process, due to various factors, the quality of catalysts may fluctuate, leading to unstable reaction effect, and further affecting the economy and environmental protection of the entire production process.

[0005] In the prior art, although some methods have been used to improve the performance of catalysts, these methods often focus on the adjustment of catalyst formula or the selection of active components, while ignoring the influence of production process on the quality of final products.

[0006] In the Chinese patent document with publication number CN111359678B, a catalyst continuous production device and method are disclosed, which includes a raw material mixing mechanism and a molding mechanism. The raw material mixing mechanism includes a mixing kettle body, several layers of partitions are fixedly arranged inside the mixing kettle body, the mixing kettle body is divided into several chambers by the partitions, the partitions are uniformly distributed with several circular holes of the same size, the circular holes on each layer of the partitions gradually increase from top to bottom, and a scraper is rotatably arranged in each chamber. The molding mechanism includes a machine box connected with the mixing kettle body, an extrusion screw is rotatably arranged in the machine box, a molding die is arranged at one end of the machine box, and a motor is arranged at the other end of the machine box to drive the extrusion screw. The beneficial effects of the present application are: increasing the contact area of the additives or liquid raw materials with the solid raw materials, improving the quality of the catalyst products and ensuring the stability of the product properties through continuous and layered extrusion. However, the catalyst product activity of the catalyst continuous production device and method is poor.

[0007] Production of high purity low arsenic anhydrous hydrogen fluoride containing low levels of arsenic impurities by oxidizing the arsenic impurities in contact with hydrogen peroxide in anhydrous hydrogen fluoride product or intermediate product in the process of making HF in the presence of a catalyst comprising a catalytic amount of a component selected from the group consisting of molybdenum, molybdenum compounds, vanadium and vanadium compounds and phosphate compounds. The volatile trivalent arsenic impurities in the anhydrous hydrogen fluoride are oxidized to non-volatile pentavalent arsenic compounds, and the resulting mixture is distilled to recover high purity anhydrous hydrogen fluoride having reduced arsenic impurities. In one embodiment, an oxidizing agent such as nitric acid or nitrate is added to the reaction mixture to oxidize organic compounds, but the production of high purity low arsenic anhydrous hydrogen fluoride catalyst product has poor stability.

[0008] A method for producing high purity isobutene includes supplying a mixed C4 feed stream to a catalytic distillation column, which can contain a butene isomerization catalyst. The 1-butene is isomerized to 2-butene while the 2-butene is separated from isobutane and isobutene in the catalytic distillation column. The overhead product, including isobutane and isobutene, is then condensed in an overhead system and supplied to a fractionator, where the isobutane is separated from the isobutene. The method also includes operating the catalytic distillation column with a column overhead temperature greater than a fractionator bottom temperature and heating a portion of the fractionator bottom stream by indirect heat exchange with at least a portion of the catalytic distillation column overhead product to produce a heated bottom stream (reboil steam) for supply to the fractionator and to cool the overhead product, but the production of high purity isobutene catalyst product has poor stability.

[0009] In order to solve the above-mentioned problems existing in the prior art, a method for improving the quality of catalyst products is provided, which is a problem worthy of research. SUMMARY

[0011] The purpose of the present application is to overcome the shortcomings of the production process having little effect on the quality of the final product, and to provide a method for improving the quality of catalyst products, which achieves the technical effect of making the catalyst products have higher activity, selectivity and stability.

[0012] The purpose of the present application is achieved by the following technical solutions:

[0013] A method for improving the quality of catalyst products, comprising the following steps:

[0014] Step one: select high purity, low impurity content raw materials;

[0015] Step two: pretreat the raw materials to remove surface impurities and contaminants;

[0016] Step 3: Mix the raw materials;

[0017] Step 4: Select the molding method according to application requirements and optimize the molding parameters;

[0018] Step 5: Roast the raw materials under specific roasting conditions;

[0019] Step Six: Select an activator to activate the calcined raw materials;

[0020] Step 7: Introduce an online monitoring system during the production process to monitor changes in the physicochemical properties of the catalyst in real time;

[0021] Step 8: Conduct a comprehensive quality inspection on each batch of catalyst;

[0022] Step 9: Establish detailed production records and quality files for each batch of products to achieve full traceability management;

[0023] By optimizing the entire process from raw material selection to finished product inspection, the catalyst is ensured to have higher activity, selectivity and stability, which significantly improves its application effect and ultimately enhances product consistency and economy.

[0024] Optionally, the purity of the raw materials in step one exceeds 99.9%, especially for active ingredients such as metal oxides and precious metals. Improving the purity of the raw materials ensures the quality of the catalyst and overcomes the performance instability caused by raw material fluctuations in traditional methods.

[0025] Optionally, the pretreatment in step two includes acid washing, alkaline washing, and ultrasonic cleaning to improve the purity and uniformity of the raw materials. Through the synergistic effect of physicochemical cleaning, the problem of residual impurities on the surface of the raw materials is solved, providing the prerequisite for uniform mixing and stable molding.

[0026] Optionally, in the mixing process of step three, high-speed stirring is performed first, followed by grinding and mixing using a ball mill, and finally spray drying is used to reduce the moisture content in the raw materials, so that the raw materials are fully mixed and avoid local concentrations that are too high or too low. Through the multi-stage mixing process, the active components are evenly distributed, and the mechanical strength and reaction consistency of the catalyst are improved.

[0027] Optionally, the molding method in step four includes extrusion molding, tablet molding, or granulation. The molding parameters include pressure, temperature, and humidity. By selecting the molding method and molding parameters, an ideal physical structure and mechanical strength can be obtained. By parametrically controlling the molding process, the problems of loose structure or insufficient strength in traditional methods can be solved, and the needs of different application scenarios can be adapted.

[0028] Optionally, the calcination conditions in step five are as follows: under an air or nitrogen atmosphere, the temperature is raised to 500-600℃ at a rate of 1-2℃ / min, and the calcination is maintained for 3-4 hours, so that the active ingredients in the catalyst can form a stable crystal structure under optimal conditions, while avoiding excessive sintering or decomposition.

[0029] Optionally, the activation agent in step six includes hydrogen, oxygen, and water vapor, which activates the active sites on the surface of the catalyst, enhances the catalytic performance, and determines the optimal activation temperature, time, pressure, and other parameters through experiments to maximize the activation effect.

[0030] Optionally, the online monitoring system in step seven includes X-ray diffraction monitoring, scanning electron microscopy, and specific surface area testers, which can monitor the changes in the physical and chemical properties of the catalyst in real time, adjust the production process parameters in a timely manner, achieve dynamic optimization of the production process, avoid the hysteresis of offline detection, and improve the real-time nature and precision of quality control.

[0031] Optionally, the quality detection in step eight includes appearance inspection, chemical composition analysis, physical property testing, and catalytic performance evaluation, which can ensure that the product quality meets the standard requirements, identify defects (such as composition deviation or uneven structure) in advance, reduce the rejection rate, and through a comprehensive quality inspection system, guarantee the reliability and consistency of each batch of products, and support the effectiveness of the traceability management system.

[0032] Positive effects: 1. The method for improving the quality of catalyst products optimizes the whole process from raw material selection to finished product inspection, ensures that the catalyst has higher activity, selectivity, and stability, significantly improves its application effect, and ultimately improves product consistency and economy.

[0033] 2. The method for improving the quality of catalyst products improves the purity and uniformity of the raw materials, and solves the problem of residual impurities on the surface of the raw materials through the synergistic effect of physical and chemical cleaning, providing a prerequisite for uniform mixing and stable molding.

[0034] 3. The method for improving the quality of catalyst products obtains ideal physical structure and mechanical strength through the selection of molding methods and parameters, solves the problem of loose structure or insufficient strength in traditional methods through parameterized control of the molding process, and meets the needs of different application scenarios. BRIEF DESCRIPTION OF DRAWINGS

[0036] Figure 1 The flowchart of the present application is shown in the figure;

[0037] Figure 2 The performance comparison chart of Example 2 of the present application is shown in the figure;

[0038] Figure 3Performance comparison chart for embodiment 3 of the present application. DETAILED DESCRIPTION

[0040] Embodiments of the present application are described in detail below, examples of which are shown in the accompanying drawings, wherein the same or similar reference numerals represent the same or similar elements or elements having the same or similar functions throughout. The embodiments described below by reference to the drawings are exemplary and are intended to explain the present application, and cannot be understood as limiting the present application.

[0041] Embodiment 1

[0042] As shown in the figure, a method for improving the quality of catalyst products includes the following steps: Figure 1

[0043] Step one: select raw materials with high purity and low impurity content;

[0044] Step two: pretreat the raw materials to remove surface impurities and contaminants;

[0045] Step three: mix the raw materials;

[0046] Step four: select a molding method according to application requirements and optimize molding parameters;

[0047] Step five: calcine the raw materials under certain calcination conditions;

[0048] Step six: select an activator to activate the calcined raw materials;

[0049] Step seven: introduce an online monitoring system during production to monitor the physical and chemical property changes of the catalyst in real time;

[0050] Step eight: conduct comprehensive quality inspection on each batch of catalyst;

[0051] Step nine: establish detailed production records and quality archives for each batch of products to achieve full-process traceable management;

[0052] Through full-process optimization from raw material selection to finished product inspection, the catalyst has higher activity, selectivity and stability, significantly improving its application effect, and ultimately improving product consistency and economy.

[0053] The purity of the raw materials in step one exceeds 99.9%, especially for active ingredients such as metal oxides and noble metals, increasing the purity of the raw materials to ensure the quality of the catalyst, overcoming the performance instability problem caused by raw material fluctuations in traditional methods.

[0054] ​The pretreatment in step two includes acid washing, alkali washing and ultrasonic cleaning, which improves the purity and uniformity of the raw materials. Through the synergistic effect of physical and chemical cleaning, the problem of residual impurities on the surface of the raw materials is solved, providing a prerequisite for uniform mixing and stable molding.

[0055] In the mixing process of step three, high-speed stirring is first performed, then grinding and mixing are performed using a ball mill, and finally the water content in the raw materials is reduced through spray drying, so that the raw materials are fully mixed and local concentration is avoided. Through the multi-stage mixing process, the uniform distribution of active components is ensured, and the mechanical strength and reaction consistency of the catalyst are improved.

[0056] The molding method in step four includes extrusion molding, tablet molding or granulation. The molding parameters include pressure, temperature and humidity. Through the selection of molding method and molding parameters, the ideal physical structure and mechanical strength are obtained. Through parameterized control of the molding process, the problems of loose structure or insufficient strength in traditional methods are solved, and the needs of different application scenarios are adapted.

[0057] The calcination conditions in step five are as follows: in an air or nitrogen atmosphere, the temperature is raised to 500-600°C at a rate of 1-2°C / min, and the calcination is carried out for 3-4 hours. This allows the active components in the catalyst to form a stable crystal structure under optimal conditions, while avoiding excessive sintering or decomposition.

[0058] The activation agent in step six includes hydrogen, oxygen and water vapor, which activates the active sites on the surface of the catalyst, enhances the catalytic performance, and determines the optimal activation temperature, time, pressure and other parameters through experiments to maximize the activation effect.

[0059] The online monitoring system in step seven includes X-ray diffraction monitoring, scanning electron microscopy and specific surface area tester, which monitors the physical and chemical property changes of the catalyst in real time, adjusts the production process parameters in time, realizes the dynamic optimization of the production process, avoids the hysteresis of offline detection, and improves the real-time and accuracy of quality control.

[0060] The quality detection in step eight includes appearance inspection, chemical composition analysis, physical property test and catalytic performance evaluation, which ensures that the product quality meets the standard requirements, identifies defects (such as composition deviation or structure unevenness) in advance, reduces the rejection rate, and through the comprehensive quality inspection system, guarantees the reliability and consistency of each batch of products, and supports the effectiveness of the traceability management system.

[0061] Example 2

[0062] Raw material selection: high-purity titanium dioxide is selected as the carrier material, nickel powder is selected as the active component, and an appropriate amount of additive is added.

[0063] Pretreatment: Soak titanium dioxide in dilute nitric acid for 2 hours, then rinse repeatedly with deionized water until neutral; ultrasonically clean nickel powder with ethanol for 15 minutes, then dry for later use.

[0064] Mixing: Add the pretreated titanium dioxide, nickel powder and additives to a high-speed mixer in a certain proportion and mix for 30 minutes to ensure that the components are evenly distributed.

[0065] Molding: Cylindrical particles are prepared by extrusion molding. Parameters such as extrusion speed and template aperture are controlled to ensure uniform particle size.

[0066] Calcination: The shaped catalyst is placed in a muffle furnace and heated to 500°C at a heating rate of 1°C / min under air atmosphere, and calcined at a constant temperature for 4 hours.

[0067] Activation: The calcined catalyst is placed in a tube furnace, hydrogen is introduced, and it is activated at 300°C for 2 hours.

[0068] Quality Inspection: Various performance tests were conducted on the finished product. The results showed that the catalyst has high activity and selectivity, meeting the expected targets (e.g., Figure 2 (As shown).

[0069] The purity of the raw materials is controlled at 99.95%. The pretreatment adopts the synergistic effect of "dilute nitric acid washing + ultrasonic cleaning" to achieve a surface impurity removal rate of over 98%, laying the foundation for improved activity. The mixing process involves "30 minutes of high-speed stirring + 2 hours of ball milling + spray drying", which improves the dispersion uniformity of the active component nickel by 40% and avoids the decrease in selectivity caused by excessively high local concentration. The calcination adopts a slow heating rate of 1℃ / min, which reduces the sintering of the active components. The nickel grain size is controlled at 15nm, which is smaller than that of the traditional process (22nm), and the number of active sites is significantly increased.

[0070] Example 3

[0071] Raw material selection: Alumina micro powder is selected as the carrier material, palladium powder is selected as the active ingredient, and an appropriate amount of stabilizer is added.

[0072] Pretreatment: Soak alumina micro powder in hydrofluoric acid for 1 hour, then rinse it with deionized water; ultrasonically clean palladium powder with anhydrous ethanol for 10 minutes, then dry it for later use.

[0073] Mixing: Add the pretreated alumina micro powder, palladium powder and stabilizer to a ball mill in a certain proportion and ball mill for 24 hours to ensure that the components are fully mixed.

[0074] Forming: The catalyst is prepared into circular sheet-like catalysts with a diameter of 10 mm by a tableting method, and the tableting pressure is controlled at 10 MPa to maintain the mechanical strength of the sheet-like catalysts.

[0075] Calcination: The shaped catalyst is placed in a tube furnace and heated to 600°C at a heating rate of 2°C / min under a nitrogen atmosphere, and calcined at a constant temperature for 3 hours.

[0076] Activation: The calcined catalyst is placed in a fixed-bed reactor, steam is introduced, and the catalyst is activated at 400°C for 1 hour.

[0077] Quality Inspection: Various performance tests were conducted on the finished product. The results showed that the catalyst has good stability and a long service life, meeting the expected targets (e.g., Figure 3 (As shown).

[0078] The pretreatment process employs hydrofluoric acid pickling followed by anhydrous ethanol ultrasonic cleaning to effectively remove sodium and calcium impurities from the alumina support surface, increasing the specific surface area of ​​the support by 30% and providing ample space for palladium particle dispersion. The molding pressure is controlled at 10 MPa, and combined with calcination at 600℃ under a nitrogen atmosphere, the catalyst structure becomes dense with uniform pore distribution, significantly improving mechanical strength compared to traditional processes and meeting the long-term operational requirements of industrial plants. During steam activation, the combination of activation temperature (400℃) and time (1 hour) ensures that palladium is primarily distributed as Pd. 0 The presence of valence states (accounting for 89%) significantly enhances catalytic activity and stability.

[0079] All data in Examples 2 and 3 are the average of three parallel experiments, with a relative standard deviation (RSD) ≤ 2.3%, indicating good data repeatability and high reliability. In the performance comparison, "traditional process" refers to conventional production methods that do not adopt the full-process optimization of this invention (such as 99.5% raw material purity, only single acid washing pretreatment, and no online monitoring).

[0080] This invention achieves simultaneous improvement in catalyst activity, selectivity, and stability through synergistic optimization of multiple processes, including raw materials, pretreatment, molding, and calcination. Compared with existing technologies (such as patent CN111359678B), the catalyst activity is improved by more than 8%, and the stability is improved by more than 10%.

[0081] The working principle of this invention is as follows:

[0082] With full-process optimization as the core, combined with high-purity raw materials, multi-step processing, parameterized control and real-time monitoring, the activity, selectivity, stability and mechanical strength of the catalyst are significantly improved, while reducing production fluctuations and costs. This solves the limitation of "emphasizing formulation and neglecting process" in existing technologies. Through refined production management, the reliability and traceability of catalyst product quality are achieved, meeting the needs of high-end chemical applications.

[0083] The above is only used to illustrate the technical solution of the present invention and is not intended to limit it. Any other modifications or equivalent substitutions made by those skilled in the art to the technical solution of the present invention, as long as they do not depart from the spirit and scope of the technical solution of the present invention, should be covered within the scope of the claims of the present invention.

Claims

1. A method for improving the quality of catalyst products, characterized in that, Includes the following steps: Step 1: Select high-purity raw materials with low impurity content; Step 2: Pre-treat the raw materials to remove surface impurities and contaminants; Step 3: Mix the raw materials; Step 4: Select the molding method according to application requirements and optimize the molding parameters; Step 5: Roast the raw materials under specific roasting conditions; Step Six: Select an activator to activate the calcined raw materials; Step 7: Introduce an online monitoring system during the production process to monitor changes in the physicochemical properties of the catalyst in real time; Step 8: Conduct a comprehensive quality inspection on each batch of catalyst; Step 9: Establish detailed production records and quality files for each batch of products.

2. The method for improving the quality of catalyst products according to claim 1, characterized in that: The purity of the raw materials used in step one exceeds 99.9%.

3. The method for improving the quality of catalyst products according to claim 1, characterized in that: The pretreatment in step two includes acid washing, alkaline washing, and ultrasonic cleaning.

4. The method for improving the quality of catalyst products according to claim 1, characterized in that: In the mixing process of step three, high-speed stirring is performed first, followed by grinding and mixing using a ball mill, and finally spray drying is used to reduce the moisture content of the raw materials.

5. The method for improving the quality of catalyst products according to claim 1, characterized in that: The molding method in step four includes extrusion molding, tableting molding, or granulation, and the molding parameters include pressure, temperature, and humidity.

6. The method for improving the quality of catalyst products according to claim 1, characterized in that: The calcination conditions in step five are as follows: under an air or nitrogen atmosphere, the temperature is increased to 500-600℃ at a heating rate of 1-2℃ / min, and then calcined at a constant temperature for 3-4 hours.

7. The method for improving the quality of catalyst products according to claim 1, characterized in that: The activator in step six includes hydrogen, oxygen, and water vapor.

8. The method for improving the quality of catalyst products according to claim 1, characterized in that: The online monitoring system in step seven includes X-ray diffraction monitoring, scanning electron microscopy, and a specific surface area analyzer.

9. A method for improving the quality of catalyst products according to claim 1, characterized in that: The quality inspection in step eight includes visual inspection, chemical composition analysis, physical performance testing, and catalytic performance evaluation.

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