Preparation method and preparation device of titanium mordenite molecular sieve

By using liquid-solid phase method and ultrasonic assisted method in the preparation of titanium mercury zeolite molecular sieve, the problems of high-temperature energy consumption and long reaction time in the existing methods are solved, and high-efficiency and low-energy Ti-MOR preparation is achieved.

CN119683643AActive Publication Date: 2025-03-25SHANDONG UNIV OF TECH
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Patent Information

Application Number
CN202510198843.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-02-24
Publication Date
2025-03-25
Estimated Expiration
2045-02-24

AI Technical Summary

Technical Problem

In the existing preparation methods of titanium mercury zeolite molecular sieve, high temperature conditions of the gas-solid phase method lead to high energy consumption, and TiCl4 reacts with ambient water vapor to form HCl acid mist corrosion equipment, the liquid-solid phase method has a long reaction time and limited selection of titanium source solution.

Method used

Ti-MOR was prepared by reacting dealuminized mordenite with ammonium fluorotitanate solution directly in contact with the liquid-solid phase method, and an ultrasonic field was introduced into the ultrasonic field through an ultrasonic oscillator to assist in strengthening the mass transfer efficiency of liquid-solid phase, improving the reaction rate and shortening the reaction time.

Benefits of technology

It realizes efficient preparation of Ti-MOR under mild reaction conditions, reduces energy consumption, shortens reaction time, and avoids equipment corrosion.

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Abstract

The invention discloses a preparation method and a preparation device of a titanium mordenite molecular sieve, and the preparation method comprises the following steps: firstly, carrying out roasting activation treatment by taking industrial hydrogen-type mordenite as a parent body, and then realizing framework dealumination through acid pickling so as to form dealuminated mordenite with hydroxyl nest defect sites; then, an optimized liquid-solid phase titanizing reaction system is adopted, and an ultrasonic wave external field auxiliary oscillation technology is combined, so that the dealuminated mordenite and a titanium source solution are subjected to a high-efficiency liquid-solid phase titanizing reaction at room temperature and normal pressure, and the titanium mordenite molecular sieve is prepared. Compared with a high-temperature gas-solid phase method, the liquid-solid phase method has the advantages that the process is easy to control, and the energy consumption is obviously reduced; compared with a traditional liquid-solid phase method, the method has the advantages that the mass transfer efficiency of a solid-liquid interface is effectively enhanced through a proper titanium source and introduction of an ultrasonic-assisted liquid-solid phase reaction mechanism, and the titanizing process can be completed in a short time under the conditions of room temperature and normal pressure.
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Description

Technical Field

[0001] The invention relates to a method and a device for preparing a titanium mordenite molecular sieve. Background Art

[0002] Oximes, as important downstream products of ketones, are key intermediates in the field of bulk chemicals. For example, butanone oxime can replace toxic hydrazine compounds as boiler deoxidizers or anti-skinning agents; cyclohexanone oxime, for example, can be used to synthesize caprolactam through Beckmann rearrangement, which is a precursor for the production of nylon 6. Nylon 6 can be processed into nylon fibers, plastics, etc., which are closely related to people's daily lives. The traditional process for synthesizing oximes is a non-catalytic reaction between hydroxylamine derivatives and ketones. According to the different synthesis pathways of hydroxylamine, it can be divided into three types: hydroxylamine phosphate method, Raschig method and nitric oxide reduction method. However, the process is cumbersome, the equipment is severely corroded, and the by-products seriously pollute the environment. In order to replace the traditional process of preparing oximes from hydroxylamine, the modern process for preparing oximes is to use titanium silicalite / H 2 O 2 The system catalyzes the ammoximation reaction of ketones with high selectivity, namely H 2 O 2 and NH 3 The generation of NH under the catalysis of Ti in the active center of titanium silicate molecular sieve 2 OH, NH 2 OH further reacts with ketones to form corresponding oximes. The reaction conditions of the ammoximation process are mild, and the by-product is H 2 O. Less discharge of three wastes, which is of great significance to the green development of industrial preparation of oxime.

[0003] Titanium mordenite molecular sieve (Ti-MOR) is a titanium silicon molecular sieve widely used in the industrial field, and it shows good catalytic performance in the ammoximation reaction. Its preparation methods are mainly divided into traditional hydrothermal method and post-synthesis method. The traditional hydrothermal method is difficult to synthesize Ti-MOR. The alkali metal in the raw material easily leads to the deactivation of the framework active center Ti, and the element Ti is difficult to be highly dispersed in the system, which leads to the easy formation of TiO on the surface of the molecular sieve. 2 , the catalytic performance decreases. The post-synthesis method includes the gas-solid phase method and the liquid-solid phase method, both of which use the existing mordenite molecular sieve as the matrix and introduce active Ti sites by replacing part of the framework aluminum. The typical process flow of the gas-solid phase method includes: using a strong acid to remove most of the aluminum in the matrix molecular sieve to form a hydroxyl nest defect site to obtain dealuminated mordenite, and then using N 2 As carrier gas, TiCl 4 The gas-solid phase reaction with the defect site realizes the embedding of the element Ti into the skeleton. At present, although the gas-solid phase method is the main way to prepare Ti-MOR, the high temperature conditions of the process lead to high energy consumption and TiCl 4It is easy to react with water vapor in the environment to generate a large amount of HCl acid mist to corrode equipment. In comparison, the liquid-solid phase method directly contacts the dealuminated mordenite molecular sieve with the titanium source solution at room temperature to complete the titaniumization reaction. The process has mild reaction conditions, low energy consumption, and easy control of the process, but the liquid-solid phase titaniumization reaction time is too long and there are fewer suitable titanium source solutions. Summary of the invention

[0004] In order to overcome the shortcomings of the prior art, the present invention provides a method and a preparation device for titanium mordenite molecular sieve. The liquid-solid phase method has the advantages of mild reaction conditions, easy process control and low energy consumption. After the mordenite molecular sieve is dealuminated, the dealuminated mordenite is used to react with a suitable ammonium fluorotitanate solution to directly prepare Ti-MOR by liquid-solid phase titanation. An ultrasonic oscillator is used to introduce an ultrasonic field to assist in enhancing the liquid-solid phase mass transfer efficiency, thereby improving the liquid-solid phase titanation reaction rate and greatly shortening the reaction time.

[0005] In order to solve the above technical problems, the present invention provides the following technical solutions: a method for preparing titanium mordenite molecular sieve, comprising the following steps: S1, using industrial hydrogen-type mordenite as the matrix, placing it in a muffle furnace for calcination activation treatment, the calcination temperature is 700 degrees Celsius, and the calcination time is 6 hours; S2, acid washing and dealuminization of the mordenite molecular sieve treated in S1 with a strong acid, filtering, washing, drying and calcining to obtain the dealuminized mordenite molecular sieve; S3, dispersing the dealuminated mordenite molecular sieve prepared in S2 into a certain concentration of ammonium fluorotitanate solution, then placing the dealuminated mordenite molecular sieve dispersion into a polytetrafluoroethylene container, and placing the polytetrafluoroethylene container in an ultrasonic oscillator, stirring and ultrasonicating, to carry out a liquid-solid phase titanation reaction; S4. Filter the liquid-solid phase, wash the sample with hot deionized water, and place the washed sample in an oven for drying and muffle furnace for calcination in turn to finally obtain titanium mordenite molecular sieve Ti-MOR.

[0006] As a preferred technical solution of the present invention, the mass of the industrial hydrogen-type mordenite raw powder in S1 is 10-30 grams.

[0007] As a preferred technical solution of the present invention, the solid-liquid ratio of the mordenite molecular sieve to the strong acid solution in S2 is 1g: (10-20) mL, the strong acid can be nitric acid, sulfuric acid or hydrochloric acid, the concentration of the strong acid solution is 6 mol / L, normal pressure, the pickling temperature is 120-150 degrees Celsius, and the pickling time is 8-12 hours.

[0008] As a preferred technical solution of the present invention, the oven temperature used in the drying process in S2 is 80 degrees Celsius, the drying time is 12 hours, the muffle furnace roasting temperature is 550 degrees Celsius, and the roasting time is 6 hours.

[0009] As a preferred technical solution of the present invention, the solid-liquid ratio of dealuminated mordenite molecular sieve to ammonium fluorotitanate solution in S3 is 1g: (10-20) mL, the concentration of ammonium fluorotitanate solution is 0.1-0.5 mol / L, normal pressure, titanation temperature is 20-60 degrees Celsius, and the titanation time is 1-6 hours.

[0010] As a preferred technical solution of the present invention, in S4, the temperature of hot deionized water is 40-80 degrees Celsius, the oven temperature is 80 degrees Celsius, the drying time is 12 hours, the muffle furnace roasting temperature is 550 degrees Celsius, and the roasting time is 6 hours.

[0011] The invention discloses a titanium mordenite molecular sieve preparation device, which is applied to the titanium mordenite molecular sieve preparation method, and comprises a base, a lifting mechanism, a placement plate and a positioning mechanism. An ultrasonic oscillator is arranged on the base, the placement plate is arranged in the ultrasonic oscillator, and a polytetrafluoroethylene container is arranged on the placement plate through a positioning mechanism. The lifting mechanism is used to drive the placement plate to lift and lower, so as to take the polytetrafluoroethylene container out of or put it into the ultrasonic oscillator.

[0012] As a preferred technical solution of the present invention, the lifting mechanism includes a support column arranged on a base, a support base is arranged on the support column, a motor is installed on the support base, a first threaded rod is connected to the power output end of the motor, a moving block is installed on the first threaded rod, the outer side of the moving block is connected to a lifting frame through a connecting plate, and the placement plate is installed in the lifting frame.

[0013] As a preferred technical solution of the present invention, a slide rail is provided outwardly on one side of the support column toward the support base, a slider is provided inside the slide rail, and the slider is connected to the moving block.

[0014] As a preferred technical solution of the present invention, the positioning mechanism includes a fixed plate arranged on the surface of the placing plate, a second threaded rod is horizontally inserted in the fixed plate, a limiting clamp is provided at one end of the second threaded rod facing the polytetrafluoroethylene container, and a handle is provided at the end of the second threaded rod away from the limiting clamp.

[0015] Compared with the prior art, the present invention can achieve the following beneficial effects: the liquid-solid phase method has the advantages of mild reaction conditions, better process control, and low energy consumption. After the mordenite molecular sieve is dealuminated, the dealuminated mordenite is directly contacted with an ammonium fluorotitanate solution to prepare Ti-MOR. The ultrasonic oscillator is used to introduce an ultrasonic field to assist in enhancing the mass transfer efficiency, thereby increasing the liquid-solid phase titanation reaction rate at room temperature and pressure and shortening the reaction time. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 XRD spectra of titanium mordenite molecular sieves of Examples 1 and 2 of the present invention; Figure 2 It is a schematic diagram of the overall structure of the present invention from a first viewing angle; Figure 3 It is a structural schematic diagram of the lifting frame of the present invention; Figure 4 It is a schematic structural diagram of the limit clamp of the present invention; Figure 5 It is a schematic structural diagram of the fixing plate of the present invention.

[0017] Among them: 1. base; 2. placement plate; 3. ultrasonic oscillator; 4. polytetrafluoroethylene container; 5. support column; 6. support base; 7. motor; 8. first threaded rod; 9. moving block; 10. connecting plate; 11. lifting frame; 12. slide rail; 13. slider; 14. fixed plate; 15. second threaded rod; 16. limit clamp; 17. handle. DETAILED DESCRIPTION

[0018] In order to make the technical means, creative features, objectives and effects achieved by the present invention easy to understand, the present invention is further described below in conjunction with specific embodiments, but the following embodiments are only preferred embodiments of the present invention, not all. Based on the embodiments in the implementation mode, other embodiments obtained by those skilled in the art without creative work all belong to the protection scope of the present invention. The experimental methods in the following embodiments, unless otherwise specified, are conventional methods, and the materials, reagents, etc. used in the following embodiments, unless otherwise specified, can all be obtained from commercial channels. Embodiment 1:

[0019] This embodiment proposes a method for preparing titanium mordenite molecular sieve, comprising the steps of: S1. Using industrial hydrogen-type mordenite as the matrix, placing it in a muffle furnace for calcination and activation treatment. The mass of mordenite is 10 grams, the calcination temperature is 700 degrees Celsius, and the calcination time is 6 hours.

[0020] S2, the mordenite molecular sieve treated with S1 was mixed with 6 mol / L nitric acid solution at a solid-liquid ratio of 1g:10mL, refluxed and acid-washed for 10 hours, filtered, washed, dried, and calcined to obtain the dealuminated mordenite molecular sieve. The acid-washing temperature was 140 degrees Celsius, normal pressure; the drying temperature was 80 degrees Celsius, the time was 12 hours; the calcination temperature was 550 degrees Celsius, the time was 6 hours.

[0021] S3, the dealuminated mordenite molecular sieve prepared in S2 is dispersed into a certain concentration of ammonium fluorotitanate solution, and then the mixed solution is placed in a polytetrafluoroethylene container 4, and the polytetrafluoroethylene container 4 is placed in an ultrasonic oscillator 3, the polytetrafluoroethylene container 4 is stirred, and the ultrasonic oscillator 3 is turned on to make the ultrasonic oscillator 3 ultrasonically oscillate the polytetrafluoroethylene container 4 to perform a liquid-solid phase titaniumization reaction. The titaniumization time is 6 hours, the titaniumization temperature is 30 degrees Celsius, and the pressure is normal.

[0022] S4, filter the liquid and solid phases, wash the sample with hot deionized water, and place the washed sample in an oven for drying and muffle furnace for roasting, and finally obtain titanium mordenite molecular sieve Ti-MOR. The deionized water temperature is 60 degrees Celsius; the drying temperature is 80 degrees Celsius, the time is 12 hours; the roasting temperature is 550 degrees Celsius, and the time is 6 hours.

[0023] Ultrasonic oscillator belongs to the prior art and will not be described in detail here. The ultrasonic oscillator is used to increase the diffusion contact reaction between the dealuminated mordenite molecular sieve and the titanium source solution, accelerate the titanium replenishment process, and shorten the time for preparing Ti-MOR by liquid-solid phase method.

[0024] As attached Figure 1 As shown in the XRD spectrum, the titanium mordenite molecular sieve prepared by liquid-solid phase titanation reaction has a θ =9.78, 13.59°, 19.70°, 22.45°, 25.78°, 26.47° and 27.74° show typical MOR topological structure characteristic diffraction peaks, indicating that the Ti-MOR prepared by the above steps does not destroy its MOR topological structure. Embodiment 2:

[0025] S1. Using industrial hydrogen-type mordenite as the matrix, placing it in a muffle furnace for calcination and activation treatment. The mass of mordenite is 10 grams, the calcination temperature is 700 degrees Celsius, and the calcination time is 6 hours.

[0026] S2, the mordenite molecular sieve treated with S1 was mixed with 6 mol / L nitric acid solution at a solid-liquid ratio of 1g:10mL, refluxed and acid-washed for 10 hours, filtered, washed, dried, and calcined to obtain the dealuminated mordenite molecular sieve. The acid-washing temperature was 140 degrees Celsius, normal pressure; the drying temperature was 80 degrees Celsius, the time was 12 hours; the calcination temperature was 550 degrees Celsius, the time was 6 hours.

[0027] S3, dispersing the dealuminated mordenite molecular sieve prepared in S2 into a certain concentration of ammonium fluorotitanate solution, and then placing the mixed solution into a polytetrafluoroethylene container 4, stirring the polytetrafluoroethylene container 4 to perform a liquid-solid phase titanation reaction. The titanation time is 6 hours, the titanation temperature is 30 degrees Celsius, and the pressure is normal.

[0028] S4, filter the liquid and solid phases, wash the sample with hot deionized water, and place the washed sample in an oven for drying and muffle furnace for roasting, and finally obtain titanium mercerized molecular sieve Ti-MOR. The deionized water temperature is 60 degrees Celsius; the drying temperature is 80 degrees Celsius, the time is 12 hours; the roasting temperature is 550 degrees Celsius, and the time is 6 hours.

[0029] As attached Figure 1 As shown in the XRD spectrum, the titanium mordenite molecular sieve prepared by liquid-solid phase titanation reaction has a θ =9.78, 13.59°, 19.70°, 22.45°, 25.78°, 26.47° and 27.74° show typical MOR topological structure characteristic diffraction peaks, indicating that the Ti-MOR prepared by the above steps does not destroy its MOR topological structure.

[0030] Comparative Example 1: The difference from step S1 of Example 1 is that the mordenite molecular sieve is not calcined, and the rest is the same as Example 1.

[0031] Comparative Example 2: The difference from step S1 of Example 2 is that the mordenite molecular sieve is not calcined, and the rest is the same as Example 2.

[0032] Comparative Example 3: The difference from step S2 of Example 1 is that 6 mol / L sulfuric acid is used to dealuminate the molecular sieve, and the rest is the same as Example 1.

[0033] Comparative Example 4: The difference from step S2 of Example 1 is that 6 mol / L hydrochloric acid is used to dealuminate the molecular sieve, and the rest is the same as in Example 1.

[0034] Comparative Example 5: The difference from step S3 of Example 1 is that the titaniumization temperature is 60 degrees Celsius, and the rest is the same as Example 1.

[0035] Comparative Example 6: The difference from step S3 of Example 2 is that the titaniumization temperature is 60 degrees Celsius, and the rest is the same as Example 2.

[0036] Comparative Example 7: The difference from step S3 of Example 1 is that the concentration of the titanium source solution is 0.1 mol / L, and the rest is the same as Example 1.

[0037] Comparative Example 8: The difference from step S3 of Example 2 is that the concentration of the titanium source solution is 0.1 mol / L, and the rest is the same as Example 2.

[0038] Comparative Example 9: The difference from step S4 of Example 1 is that the washing temperature of hot deionized water is 40 degrees Celsius, and the rest is the same as Example 1.

[0039] The application of titanium mercerized molecular sieve with MOR structure in ammoximation reaction. The specific implementation steps are as follows: (1) The titanium mordenite molecular sieve prepared in Example 1 and Example 2 was used as a catalyst in an amount of 0.2 g.

[0040] (2) Design a reaction process for the ammoximation of butanone, in which the raw material ratio is: the molar ratio of butanone to hydrogen peroxide is 1:1.1, and the molar ratio of butanone to ammonia is 1:1.6. The reaction conditions are: temperature 65 degrees Celsius, normal pressure, solvent 85% tert-butyl alcohol, and the contact time between the reaction raw material liquid and the titanium mordenite molecular sieve catalyst is 120 minutes. After the reaction is completed, the slurry is centrifuged, and the filtrate is analyzed by gas chromatography to calculate the butanone conversion rate and butanone oxime selectivity.

[0041] (3) Self-designed cyclohexanone ammoximation reaction process, in which the raw material ratio is: cyclohexanone to hydrogen peroxide molar ratio is 1:1.2, cyclohexanone to ammonia molar ratio is 1:1.7. The reaction conditions are: temperature 70 degrees Celsius, normal pressure, solvent 85% tert-butyl alcohol, and the contact time between the reaction raw material liquid and the titanium mordenite molecular sieve catalyst is 120 minutes. After the reaction is completed, the slurry is centrifuged, and the filtrate is analyzed by gas chromatography to calculate the cyclohexanone conversion rate and cyclohexanone oxime selectivity. The catalytic reaction results are as follows: The catalysts prepared in Comparative Examples 1 to 9 were subjected to butanone ammoximation and cyclohexanone ammoximation reactions according to the above steps, respectively, to obtain the following results: A titanium mordenite molecular sieve preparation device is applied to a titanium mordenite molecular sieve preparation method, comprising a base 1, a lifting mechanism, a placement plate 2 and a positioning mechanism, an ultrasonic oscillator 3 is arranged on the base 1, the placement plate 2 is arranged in the ultrasonic oscillator 3, a polytetrafluoroethylene container 4 is arranged on the placement plate 2 through the positioning mechanism, and the lifting mechanism is used to drive the placement plate 2 to lift and lower, so as to take the polytetrafluoroethylene container 4 out of or put it into the ultrasonic oscillator 3. The lifting mechanism includes a support column 5 arranged on a base 1, a support base 6 is arranged on the support column 5, a motor 7 is installed on the support base 6, a first threaded rod 8 is connected to the power output end of the motor 7, a moving block 9 is installed on the first threaded rod 8, a lifting frame 11 is connected to the outer side of the moving block 9 through a connecting plate 10, and the placement plate 2 is installed in the lifting frame 11. As the motor 7 drives the first threaded rod 8 to rotate, the slider 13 slides in the slide rail 12 along the length direction of the slide groove, converting the rotary motion into linear motion, driving the moving block 9 to move on the support column 5, so that the moving frame is lifted and lowered, and the placement plate 2 drives the polytetrafluoroethylene container 4 to be taken out of the ultrasonic oscillator 3. The support column 5 is provided with a slide rail 12 outwardly toward the side of the support base 6, and a slider 13 is arranged in the slide rail 12. The slider 13 is connected to the moving block 9 to facilitate the movement of the lifting frame 11. The positioning mechanism includes a fixed plate 14 arranged on the surface of the placement plate 2, a second threaded rod 15 is inserted transversely in the fixed plate 14, a limiting clamp 16 is arranged at one end of the second threaded rod 15 facing the polytetrafluoroethylene container 4, and a handle 17 is arranged at one end of the second threaded rod 15 away from the limiting clamp 16. A circular groove for placing the polytetrafluoroethylene container 4 is provided in the center of the surface of the placement plate 2. With the rotation of the handle 17, the second threaded rod 15 is driven to axially feed in the fixed plate 14, so that the limiting clamp 16 moves toward the polytetrafluoroethylene container 4, and the positioning mechanism is provided with two, and a limiting area for fixing the polytetrafluoroethylene container 4 is formed between the two limiting clamps 16. A threaded hole matching the second threaded rod 15 is provided on the surface of the fixed plate 14, so that the second threaded rod 15 can be axially fed toward the polytetrafluoroethylene container 4 after rotation.

[0042] In the present invention, unless otherwise clearly specified and limited, a first feature being "above" or "below" a second feature may include that the first and second features are in direct contact, or may include that the first and second features are not in direct contact but are in contact through another feature between them. Moreover, a first feature being "above", "above" and "above" a second feature includes that the first feature is directly above and obliquely above the second feature, or simply indicates that the first feature is higher in level than the second feature. A first feature being "below", "below" and "below" a second feature includes that the first feature is directly below and obliquely below the second feature, or simply indicates that the first feature is lower in level than the second feature.

[0043] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above implementation regulations. The above implementation regulations and descriptions are only preferred examples of the present invention and are not used to limit the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, which fall within the scope of the present invention. The scope of protection of the present invention is defined by the attached claims and their equivalents.

Claims

1. A method for preparing titanium mordenite molecular sieve, characterized in that: The following steps are involved: S1, using industrial hydrogen-type mordenite as the matrix, placing it in a muffle furnace for calcination activation treatment, the calcination temperature is 700 degrees Celsius, and the calcination time is 6 hours; S2, acid washing and dealuminization of the mordenite molecular sieve treated in S1 with a strong acid, filtering, washing, drying and calcining to obtain the dealuminized mordenite molecular sieve; S3, dispersing the dealuminated mordenite molecular sieve prepared in S2 into a certain concentration of ammonium fluorotitanate solution, then placing the dealuminated mordenite molecular sieve dispersion into a polytetrafluoroethylene container, and placing the polytetrafluoroethylene container in an ultrasonic oscillator, stirring and ultrasonicating, to carry out a liquid-solid phase titanation reaction; S4. Filter the liquid-solid phase, wash the sample with hot deionized water, and place the washed sample in an oven for drying and muffle furnace for calcination in turn to finally obtain titanium mordenite molecular sieve Ti-MOR.

2. The method for preparing titanium mordenite molecular sieve according to claim 1, characterized in that: The mass of the industrial hydrogen-type mordenite raw powder in S1 is 10-30 grams.

3. The method for preparing titanium mordenite molecular sieve according to claim 1, characterized in that: The solid-liquid ratio of mordenite molecular sieve to strong acid solution in S2 is 1g: (10-20) mL. The strong acid can be nitric acid, sulfuric acid or hydrochloric acid. The concentration of the strong acid solution is 6 mol / L, normal pressure, pickling temperature is 120-150 degrees Celsius, and the pickling time is 8-12 hours.

4. The method for preparing titanium mordenite molecular sieve according to claim 1, characterized in that: The drying process in S2 is carried out at an oven temperature of 80 degrees Celsius for 12 hours, and at a muffle furnace temperature of 550 degrees Celsius for 6 hours.

5. The method for preparing titanium mordenite molecular sieve according to claim 1, characterized in that: The solid-liquid ratio of dealuminated mordenite molecular sieve to ammonium fluorotitanate solution in S3 is 1g: (10-20) mL, the concentration of ammonium fluorotitanate solution is 0.1-0.5 mol / L, normal pressure, titanation temperature is 20-60 degrees Celsius, and the titanation time is 1-6 hours.

6. The method for preparing titanium mordenite molecular sieve according to claim 1, characterized in that: In S4, the temperature of hot deionized water is 40-80 degrees Celsius, the oven temperature is 80 degrees Celsius, the drying time is 12 hours, the muffle furnace roasting temperature is 550 degrees Celsius, and the roasting time is 6 hours.

7. Titanium mordenite molecular sieve preparation device, characterized in that: The method for preparing titanium mordenite molecular sieve according to claim 1 comprises a base (1), a lifting mechanism, a placement plate (2) and a positioning mechanism, wherein an ultrasonic oscillator (3) is arranged on the base (1), the placement plate (2) is arranged in the ultrasonic oscillator (3), a polytetrafluoroethylene container (4) is arranged on the placement plate (2) via the positioning mechanism, and the lifting mechanism is used to drive the placement plate (2) to lift and lower, so as to take the polytetrafluoroethylene container (4) out of or put it into the ultrasonic oscillator (3).

8. The titanium mordenite molecular sieve preparation device according to claim 7, characterized in that: The lifting mechanism comprises a support column (5) arranged on a base (1), a support base (6) being arranged on the support column (5), a motor (7) being mounted on the support base (6), a first threaded rod (8) being connected to a power output end of the motor (7), a moving block (9) being mounted on the first threaded rod (8), a lifting frame (11) being connected to the outer side of the moving block (9) via a connecting plate (10), and the placement plate (2) being mounted in the lifting frame (11).

9. The titanium mordenite molecular sieve preparation device according to claim 8, characterized in that: A slide rail (12) is provided outwardly on one side of the support column (5) facing the support base (6), a slide block (13) is provided inside the slide rail (12), and the slide block (13) is connected to the moving block (9).

10. The titanium mordenite molecular sieve preparation device according to claim 9, characterized in that: The positioning mechanism comprises a fixing plate (14) arranged on the surface of the placement plate (2), a second threaded rod (15) being inserted transversely into the fixing plate (14), a limiting clamp (16) being arranged at one end of the second threaded rod (15) facing the polytetrafluoroethylene container (4), and a handle (17) being arranged at one end of the second threaded rod (15) away from the limiting clamp (16).

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