A synthesis process of a high-performance catalyst for isooctyl acrylate

Abstract

The application discloses a synthesis process of a high-performance catalyst for isooctyl acrylate, and specifically comprises the following steps: step one, selection and design of the catalyst; according to the characteristics and requirements of the reaction, the components and structure of the catalyst are selected, and an aluminum phosphotungstate-SO42 / ZrO composite and a sulfate modified y-Al2O catalyst material are selected; step two, synthesis of a precursor of the catalyst; according to the component and structure design of the catalyst, the corresponding precursor is synthesized; step three, activation treatment of the catalyst; step four, loading of the catalyst; and step five, characterization and evaluation of the catalyst. The synthesis process of the high-performance catalyst for isooctyl acrylate can effectively control the occurrence of a side reaction by adding a composite catalyst with high catalytic performance and completing all esterification reactions in a low-temperature environment, and can improve the conversion rate of esterification by heating for deep esterification.

Description

Technical Field

[0001] This invention relates to the field of acrylate synthesis technology, and more particularly to a synthesis process for a high-performance catalyst for isooctyl acrylate. Background Technology

[0002] Acrylic esters possess excellent gloss and color retention properties in coatings, as well as heat resistance, weather resistance, aging resistance, and strong adhesion. Their water resistance, acid and alkali resistance, stain resistance, and environmental friendliness make them widely used in the coatings and adhesives industry, pressure-sensitive adhesives industry, and construction industry. In the construction field, they are used as cement modifiers and building sealants. Furthermore, they have found extensive applications in automotive interior trim, electronic components, color printing, electrical insulation, and re-peelable tapes.

[0003] Isooctyl acrylate is produced by the esterification reaction of acrylic acid and isooctyl alcohol under the action of a catalyst. The reaction process produces corresponding exhaust gas, the main components of which include volatile acrylic acid and isooctyl alcohol. Inhalation of gaseous acrylic acid and isooctyl alcohol can cause respiratory diseases. Therefore, the exhaust gas produced by industrial production of isooctyl acrylate is a prohibited emission substance and needs to be purified to meet the emission standards before it can be released into the atmosphere. In addition, the reaction of acrylic acid and isooctyl alcohol produces water, which contains dissolved acrylic acid and isooctyl alcohol that is slightly soluble in water. Therefore, the produced water cannot be directly discharged into the environment and must be treated before it can be discharged into sewage pipes.

[0004] Existing technologies use catalytic oxidation to decompose acrylic acid and isooctanol in the exhaust gas into carbon dioxide and water. Although the wastewater generated by wastewater treatment equipment solves the exhaust gas and wastewater problems to some extent, acrylic acid in the exhaust gas and wastewater has recycling value as a synthetic raw material in industrial production. The pollutants in the wastewater are singular, and the wastewater after removing acrylic acid can be used as a cleaning water source for synthetic equipment. The above-mentioned existing technologies have the problems of low utilization rate of synthetic raw materials and large material loss. Summary of the Invention

[0005] This invention discloses a synthesis process for a high-performance catalyst for isooctyl acrylate, aiming to solve the technical problems of low utilization rate of synthetic raw materials and large material loss mentioned in the background art.

[0006] To achieve the above objectives, the present invention adopts the following technical solution:

[0007] A synthesis process for a high-performance catalyst of isooctyl acrylate specifically includes the following steps:

[0008] Step 1: Catalyst selection and design; Based on the characteristics and requirements of the reaction, select a suitable catalyst composition and structure; such as metals, metal oxides, acids and bases, etc. At the same time, the stability, activity and tolerance of the catalyst under reaction conditions must also be considered.

[0009] Step 2: Catalyst precursor synthesis; based on the catalyst's composition and structure design, synthesize the corresponding precursor; common synthesis methods include sol-gel method, co-precipitation method, impregnation method, precipitation method, etc. These methods can yield precursors with the desired structure and morphology.

[0010] Step 3: Catalyst Activation Treatment; Catalyst activation treatment aims to improve its activity and stability. Common activation methods include calcination, reduction, and oxidation. Calcination can remove impurities adsorbed on the catalyst surface, improving the catalyst's purity; reduction can reduce the oxide form of metal catalysts, improving their reducing properties; oxidation can cause metal catalysts to form corresponding oxide forms.

[0011] Step 4: Catalyst loading;

[0012] Catalyst loading involves transferring the active component onto a support to improve its stability and dispersibility. Common supports include alumina, silica gel, and carbon nanotubes. Loading methods include impregnation, dip coating, and co-precipitation. During loading, it is crucial to control the loading amount and dispersibility to enhance catalyst activity.

[0013] Step 5: Characterization and Evaluation of Catalysts; Characterization and evaluation of catalysts are crucial steps in the preparation process. The structure and properties of the catalysts are characterized using physicochemical methods, including X-ray diffraction, scanning electron microscopy, and Fourier transform infrared spectroscopy. Simultaneously, the catalysts are evaluated based on their catalytic reaction effects, such as reactivity, selectivity, and stability, to assess their performance.

[0014] In a preferred embodiment, the synthesis of isooctyl acrylate involves adding isooctanol and acrylic acid in a specific ratio to a reaction vessel, adding an appropriate amount of catalyst, and heating to the reaction temperature. The reaction temperature is typically between 120 and 150 degrees Celsius.

[0015] In a preferred embodiment, in step one, aluminum phosphotungstenate is obtained by dehydrating phosphoric acid, dissolving and reacting tungstic acid, and crystallizing and drying phosphotungstenate to obtain a pure phosphotungstenate product. This product is then reacted with aluminum metal to obtain an aluminum phosphotungstenate complex. The sulfate-modified γ-Al₂O catalyst involves filling the device with activated alumina, rinsing the filter media with water, circulating the filter with polyferric sulfate or ferric sulfate aqueous solution, and then discharging the iron salt solution. The filter media is then rinsed with water to obtain the iron salt-modified adsorbent.

[0016] An apparatus for synthesizing isooctyl acrylate catalyst includes a reactor body. A base is fixedly connected to the inner wall of the bottom end of the reactor body, and a hollow support rod is movably connected to the inner wall of the top end of the base. Multiple inner grid plates are fixedly connected to the outer wall of the hollow support rod at equal densities. An outer sleeve is movably fitted onto the outside of each inner grid plate, and multiple grid bars are provided on the outer sleeve. A slider is fixedly connected to the outer wall of the top end of each outer sleeve, and a double-headed gas rod is simultaneously connected between two sliders. A support plate is movably connected to the inner wall of the reactor body, and the support plate is equipped with… A limiting groove is provided, and the slider is movably engaged in the limiting groove. Scrapers are fixedly connected to the outer walls of the two outer jacket plates on opposite sides. A spiral conveying blade is provided inside the hollow support rod, and a motor is fixedly connected to the bottom outer wall of the spiral conveying blade. A second feed pipe is fixedly connected to the top inner wall of the hollow support rod, and a material leakage port is provided through the inner walls of the two opposite sides of the hollow support rod. A plug is movably engaged on the inner walls of the two sides of the material leakage port, and a connecting plate is fixedly connected to one outer wall of the plug. The connecting plate is fixedly connected to one outer wall of the outer jacket plate.

[0017] In a preferred embodiment, the bottom end of the inner grid plate is provided with a groove, and the connecting plate and the discharge port pass through the groove. A movable sealing ring is fixedly connected to the top outer wall of the support plate. A groove is provided on one side inner wall of the reactor body, and the movable sealing ring is movably connected to the groove. A sealing cover is fixedly connected to the top outer wall of the support plate, and the outer wall of the sealing cover is chamfered. A driving mechanism is provided at the top of the reactor body, and a gear is movably connected to one side of the driving mechanism. The gear is fixed to the outer wall of the second feed pipe. A first feed pipe is fixedly connected to the top inner wall of the reactor body, and a discharge port is fixedly connected to the bottom inner wall of the reactor body. The discharge port is located directly below the base, and a support foot is fixedly connected to the bottom outer wall of the reactor body. Multiple protrusions and multiple rubber sheets are fixedly connected at equal density on one side outer wall of the scraper, and the multiple rubber sheets are inserted into the multiple protrusions.

[0018] As shown above, the synthesis process of a high-performance catalyst for isooctyl acrylate specifically includes the following steps: Step 1, catalyst selection and design; based on the characteristics and requirements of the reaction, select suitable catalyst composition and structure, choosing aluminum phosphotungstic acid-SO42 / ZrO composite and sulfate-modified γ-Al2O catalyst materials; Step 2, catalyst precursor synthesis; based on the catalyst composition and structure design, synthesize the corresponding precursor; Step 3, catalyst activation treatment; Step 4, catalyst loading; Step 5, catalyst characterization and evaluation; catalyst characterization and evaluation are important steps in the preparation process. The catalyst's structure and performance are characterized using physicochemical methods, X-ray diffraction, scanning electron microscopy, and Fourier transform infrared spectroscopy. Simultaneously, the catalyst is evaluated based on its catalytic reaction effect. The synthesis process of the high-performance catalyst for isooctyl acrylate provided by this invention completes all esterification reactions by adding a composite catalyst with high catalytic performance and at low temperature. This ensures that the entire reaction occurs in an alcohol-excess environment, reduces side reactions, and guarantees the stability of the esterification reaction. The catalyst prepared by this invention achieves the technical advantages of high esterification conversion rate, fewer side reactions, and high purity of the finished product when preparing isooctyl acrylate. Attached Figure Description

[0019] Figure 1 This is a schematic diagram of the overall synthesis process of a high-performance catalyst for isooctyl acrylate proposed in this invention.

[0020] Figure 2 This is a schematic diagram of the external structure of a high-performance catalyst for isooctyl acrylate proposed in this invention.

[0021] Figure 3 This is a schematic diagram of the internal structure of a high-performance catalyst for isooctyl acrylate proposed in this invention.

[0022] Figure 4 This is a schematic diagram of the inner grid plate structure of a high-performance catalyst for isooctyl acrylate proposed in this invention.

[0023] Figure 5 This is a schematic diagram of the structure of a rubber sheet for a high-performance catalyst of isooctyl acrylate proposed in this invention.

[0024] Figure 6 This is a schematic diagram of the spiral conveying blade of a high-performance catalyst for isooctyl acrylate proposed in this invention.

[0025] In the attached diagram: 1. First feed pipe; 2. Drive mechanism; 3. Kettle body; 4. Support leg; 5. Discharge port; 6. Groove; 7. Movable sealing ring; 8. Scraper; 9. Outer plate; 10. Base; 11. Hollow support rod; 12. Chamfer; 13. Sealing cover; 14. Support plate; 15. Limiting groove; 16. Double-headed air rod; 17. Sliding block; 18. Grid bar; 19. Inner grid plate; 20. Protrusion; 21. Rubber sheet; 22. Second feed pipe; 23. Gear; 24. Connecting plate; 25. Motor; 26. Groove; 27. Plug; 28. Discharge port; 29. ​​Spiral conveyor blade. Detailed Implementation

[0026] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments.

[0027] The synthesis process of a high-performance catalyst for isooctyl acrylate disclosed in this invention is mainly applied to scenarios where the utilization rate of synthetic raw materials is low and the material consumption is high.

[0028] Reference Figure 1 A synthesis process for a high-performance catalyst for isooctyl acrylate specifically includes the following steps:

[0029] Step 1: Catalyst selection and design; Based on the characteristics and requirements of the reaction, select a suitable catalyst composition and structure; such as metals, metal oxides, acids and bases, etc. At the same time, the stability, activity and tolerance of the catalyst under reaction conditions must also be considered.

[0030] Step 2: Catalyst precursor synthesis; based on the catalyst's composition and structure design, synthesize the corresponding precursor; common synthesis methods include sol-gel method, co-precipitation method, impregnation method, precipitation method, etc. These methods can yield precursors with the desired structure and morphology.

[0031] Step 3: Catalyst Activation Treatment; Catalyst activation treatment aims to improve its activity and stability. Common activation methods include calcination, reduction, and oxidation. Calcination can remove impurities adsorbed on the catalyst surface, improving the catalyst's purity; reduction can reduce the oxide form of metal catalysts, improving their reducing properties; oxidation can cause metal catalysts to form corresponding oxide forms.

[0032] Step 4: Catalyst loading;

[0033] Catalyst loading involves transferring the active component onto a support to improve its stability and dispersibility. Common supports include alumina, silica gel, and carbon nanotubes. Loading methods include impregnation, dip coating, and co-precipitation. During loading, it is crucial to control the loading amount and dispersibility to enhance catalyst activity.

[0034] Step 5: Characterization and Evaluation of Catalysts; Characterization and evaluation of catalysts are crucial steps in the preparation process. The structure and properties of the catalysts are characterized using physicochemical methods, including X-ray diffraction, scanning electron microscopy, and Fourier transform infrared spectroscopy. Simultaneously, the catalysts are evaluated based on their catalytic reaction effects, such as reactivity, selectivity, and stability, to assess their performance.

[0035] In a preferred embodiment, the synthesis of isooctyl acrylate involves adding isooctanol and acrylic acid in a specific ratio to a reaction vessel, adding an appropriate amount of catalyst, and heating to the reaction temperature. Typically, the reaction temperature is between 120 and 150 degrees Celsius.

[0036] In a preferred embodiment, in step one, aluminum phosphotungstenate is obtained by dehydration of phosphoric acid, dissolution and reaction of tungstic acid, and crystallization and drying of phosphotungsten acid to obtain a pure phosphotungsten acid product, which is then reacted with aluminum metal to obtain an aluminum phosphotungstenate complex.

[0037] In a preferred embodiment, the sulfate-modified γ-Al2O catalyst is prepared by filling the device with activated alumina, rinsing the filter media with water, circulating the filter with polyferric sulfate or an aqueous solution of ferric sulfate, and then draining the iron salt solution. The filter media is then rinsed with water to obtain the iron salt-modified adsorbent.

[0038] In a preferred embodiment, the pressure for deweighting in step 5 is -95.0 kPa to -99.5 kPa, the temperature is 130°C to 150°C, and the deweighting time is 2 to 4 hours.

[0039] In a preferred embodiment, in step 1, a vacuum needs to be continuously drawn during the reaction process, from -38.0 kPa to -80 kPa, and the reaction temperature also rises slowly and uniformly.

[0040] In a preferred embodiment, the heat released by the esterification reaction can be controlled to avoid the system temperature from rising too quickly due to the exothermic reaction. This helps to control the reaction temperature, ensure the esterification rate of acrylic acid and isooctyl ester, improve reaction safety, and increase the utilization rate of materials. Good temperature control also prevents the isooctyl acrylate reactant from forming polyester, thereby increasing the yield of the target product.

[0041] In a preferred embodiment, an apparatus for synthesizing isooctyl acrylate catalyst includes a reactor body 3. A base 10 is fixedly connected to the inner wall of the bottom end of the reactor body 3, and a hollow support rod 11 is movably connected to the inner wall of the top end of the base 10. Multiple inner grid plates 19 are fixedly connected to the outer wall of the hollow support rod 11 at equal density. An outer sleeve 9 is movably fitted onto the outside of each inner grid plate 19, and multiple grid bars 18 are provided on the outer sleeve 9. A slider 17 is fixedly connected to the outer wall of the top end of each outer sleeve 9, and a double-headed gas spring 16 is simultaneously connected between two sliders 17. A support plate 14 is movably connected to the inner wall of the reactor body 3. 4 is provided with a limiting groove 15, the slider 17 is movably engaged in the limiting groove 15, and scrapers 8 are fixedly connected to the outer walls of the two outer sleeve plates 9 on opposite sides respectively. The hollow support rod 11 is provided with a spiral conveying blade 29, and a motor 25 is fixedly connected to the bottom outer wall of the spiral conveying blade 29. The top inner wall of the hollow support rod 11 is fixedly connected with a second feed pipe 22, and a material leakage port 28 is provided through the inner walls of the two opposite sides of the hollow support rod 11. A plug 27 is movably engaged on the inner walls of the two sides of the material leakage port 28, and a connecting plate 24 is fixedly connected to one side outer wall of the plug 27. The connecting plate 24 is fixedly connected to one side outer wall of the outer sleeve plate 9.

[0042] With an inner grid plate 19 and an outer jacket plate 9, during the synthesis process, the powdered catalyst raw material used for isooctyl acrylate enters the hollow support rod 11 through the second feed pipe 22, and is then transported to the bottom of the hollow support rod 11 for later use by the spiral conveying blades 29. The two output ends of the double-headed gas rod 16 extend and drive the two sliders 17 to move in opposite directions, thereby extending the outer jacket plate 9. The scraper 8 adheres to the inner wall of the reactor body 3. Thus, during retraction, the grid bars 18 on the inner grid plate 19 and the outer jacket plate 9 can be staggered to achieve high shear force stirring. When extended, the scraper 8 adheres to the inner wall of the reactor body 3 to clean the inner wall of the reactor body 3. At the same time, during the movement of the outer jacket plate 9, the plug block 27 can be moved, so that the discharge port 28 is in an open state. This allows the liquid in the reactor body 3 to be directly mixed with the powdered raw material at the bottom of the hollow support rod 11, avoiding the powdered raw material from floating on the liquid surface when added, and further optimizing the mixing efficiency.

[0043] In a preferred embodiment, the bottom end of the inner grid plate 19 is provided with a slot 26, and the connecting plate 24 and the discharge port 28 pass through the slot 26.

[0044] In a preferred embodiment, a movable sealing ring 7 is fixedly connected to the outer wall of the top end of the support plate 14, and a groove 6 is provided on one side inner wall of the reactor body 3, with the movable sealing ring 7 movably connected in the groove 6.

[0045] In a preferred embodiment, a sealing cover 13 is fixedly connected to the top outer wall of the support plate 14, and the outer wall of the sealing cover 13 is provided with a chamfer 12.

[0046] In a preferred embodiment, a drive mechanism 2 is provided at the top of the reactor body 3, and a gear 23 is movably connected to one side of the drive mechanism 2. The gear 23 is fixed to the outer wall of the second feed pipe 22.

[0047] In a preferred embodiment, a first feed pipe 1 is fixedly connected to the inner wall of the top end of the reactor body 3, and a discharge port 5 is fixedly connected to the inner wall of the bottom end of the reactor body 3. The discharge port 5 is located directly below the base 10, and a support leg 4 is fixedly connected to the outer wall of the bottom end of the reactor body 3.

[0048] By setting a sealing cover 13 and a movable sealing ring 7, the movable sealing ring 7 is movably engaged in the groove 6 to form a movable sealing space. At the same time, since the movable sealing ring 7 is connected to the sealing cover 13, it can protect the drive mechanism. In addition, with the design of the chamfer 12, the material can enter the reactor body 3 along the chamfer 12 during feeding, avoiding blockage caused by the falling material.

[0049] In a preferred embodiment, a plurality of protrusions 20 and a plurality of rubber sheets 21 are fixedly connected at equal density on one side of the outer wall of the scraper 8, and the plurality of rubber sheets 21 are inserted into the plurality of protrusions 20.

[0050] With the rubber sheet 21 and the protrusion 20, the protrusion 20 can scrape away stubborn residues on the inner wall without causing damage. When the rubber sheet 21 comes into contact with the scraped area, it can carry away the scraped waste, thereby completing a thorough cleaning.

[0051] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A high performance catalyst synthesis unit for isooctyl acrylate comprising a reactor vessel body (3) characterized in that, The bottom end inner wall of the reaction kettle body (3) is fixedly connected with a base (10), and the top end inner wall of the base (10) is movably connected with a hollow support rod (11), a plurality of inner grating plates (19) are fixedly connected to the outer wall of the hollow support rod (11) at equal density, an outer sleeve plate (9) is movably sleeved to the outer part of each inner grating plate (19), a plurality of grating strips (18) are arranged on the outer sleeve plate (9), a sliding block (17) is fixedly connected to the top end outer wall of each outer sleeve plate (9), and a double-head air rod (16) is connected between the two sliding blocks (17), the inner wall of the reaction kettle body (3) is movably connected with a support plate (14), and the support plate (14) is provided with a limiting sliding groove (15), the sliding block (17) is movably clamped in the limiting sliding groove (15), and the opposite side outer walls of the two outer sleeve plates (9) are fixedly connected with scraper plates (8) respectively, the hollow support rod (11) is provided with a spiral conveying blade (29), the bottom end outer wall of the spiral conveying blade (29) is fixedly connected with a motor (25), the top end inner wall of the hollow support rod (11) is fixedly connected with a second feeding pipe (22), and the opposite side inner walls of the hollow support rod (11) are provided with a material leakage hole (28) penetratingly, the opposite side inner walls of the material leakage hole (28) are movably clamped with plug blocks (27), one side outer wall of the plug block (27) is fixedly connected with a connecting plate (24), the connecting plate (24) is fixedly connected to one side outer wall of the outer sleeve plate (9), one side outer wall of the scraper plate (8) is fixedly connected with a plurality of protruding blocks (20) and a plurality of rubber sheets (21) at equal density, and the plurality of rubber sheets (21) are inserted in the plurality of protruding blocks (20).

2. A device for synthesizing a high-performance catalyst for isooctyl acrylate according to claim 1, characterized in that, The bottom end of the inner grating plate (19) is provided with a notch (26), and the connecting plate (24) and the material leakage hole (28) pass through the notch (26), the top end inner wall of the reaction kettle body (3) is fixedly connected with a first feeding pipe (1), and the bottom end inner wall of the reaction kettle body (3) is fixedly connected with a discharging port (5), the discharging port (5) is located directly below the base (10), and the bottom end outer wall of the reaction kettle body (3) is fixedly connected with a supporting leg (4).

3. A high performance catalyst for synthesis of iso-octyl acrylate as claimed in claim 2, wherein, The top end outer wall of the support plate (14) is fixedly connected with a movable sealing ring (7), and the side inner wall of the reaction kettle body (3) is provided with a groove (6), and the movable sealing ring (7) is movably connected in the groove (6).

4. A high performance catalyst for synthesis of iso-octyl acrylate as claimed in claim 3, wherein, The top end of the reaction kettle body (3) is provided with a driving mechanism (2), and one side of the driving mechanism (2) is movably connected with a gear (23), and the gear (23) is fixed to the outer wall of the second feeding pipe (22).

5. A high performance catalyst for synthesis of iso-octyl acrylate as claimed in claim 1, wherein, The top end outer wall of the support plate (14) is fixedly connected with a sealing cover, and the outer wall of the sealing cover is provided with a chamfer. The top end outer wall of the support plate (14) is fixedly connected with a sealing cover, and the outer wall of the sealing cover is provided with a chamfer.

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