Preparation method of a chemical and stirring device capable of segmented discharging
By designing a stirring device that allows for segmented feeding, high-purity preparation of N-methyl-α-oxophenylacetamide was achieved, solving the problems of low material utilization and inconvenient operation in existing technologies, and improving preparation efficiency and convenience.
Patent Information
- Application Number
- CN202310442268.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-04-23
- Publication Date
- 2025-12-05
- Estimated Expiration
- 2043-04-23
AI Technical Summary
The purity of N-methyl-α-oxophenylacetamide in the existing technology is low, the materials used in the preparation method cannot be fully utilized, and the steps of adding and stirring are carried out separately, which makes the operation inconvenient.
A method for preparing a chemical is provided, comprising a stepwise preparation method and a stirring device, including the synthesis steps of methyl mandelate, N-methylmandelic acid amide and N-methyl-α-oxophenylacetamide, and a segmented feeding stirring device designed to achieve segmented feeding, mixing, static stratification and removal of chemical agents through motor-driven stirring blades and separation components.
This improved the purity and effectiveness of the materials used in the preparation of N-methyl-α-oxophenylacetamide, enhanced the utilization rate of the materials, simplified the operation process, and increased convenience for staff.
Smart Images

Figure CN116786012B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of chemical preparation, in particular to a chemical preparation method and a segmented feeding stirring device. BACKGROUND
[0002] N-methyl-a-oxophenylacetamide is a chemical that can be used for pharmaceuticals. Currently, after the preparation of N-methyl-a-oxophenylacetamide is completed, its purity is relatively low, and the preparation materials cannot be fully utilized.
[0003] In the process of preparing N-methyl-a-oxophenylacetamide, two chemical reagents need to be added to the original chemical reagent and mixed and stirred. After mixing is completed, it needs to be static, and the separated substances are separated. However, the actual adding, stirring and other steps are carried out separately, which makes the actual operation process not convenient and affects the convenience of the operator. SUMMARY
[0004] This section aims to summarize some aspects of the embodiments of the present application and briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section and the abstract and title of the specification to avoid obscuring the purpose of this section, abstract and title. Such simplifications or omissions cannot be used to limit the scope of the present application.
[0005] In view of the above or the problem that the purity is relatively low and the preparation materials cannot be fully utilized in the prior art, the present application is proposed.
[0006] Therefore, the purpose of the present application is to provide a chemical preparation method.
[0007] To solve the above technical problems, the present application provides the following technical scheme: a chemical preparation method, the method comprising the following steps,
[0008] Synthesis of methyl mandelate:
[0009] Put mandelic acid 300g, methanol 500g into the bottle, add sulfuric acid 30g at 30℃ or below, after dropping, warm up to reflux for 5 hours, recover methanol, cool to room temperature, add toluene 1000ml, water 1000ml, stir and stand, separate layers, wash with 10% sodium carbonate aqueous solution to PH8, wash the toluene layer with water twice, recover toluene under reduced pressure, and distill the residue 300g;
[0010] After adding the chemical reagent, the stirring device is used to mix and stir the chemical reagents added together to ensure that the chemical reagent can fully react when it is static.
[0011] As a preferred scheme of the preparation method of the chemical of the present application, wherein: synthesis of N-methyl-a-oxo benzene acetic amide:
[0012] In the middle of the methyl mandelate 300g, 300g of methanol, drop 30% methylamine methanol solution at 50-60℃, drop time is about 3 hours, after dropping, keep at 555-600℃ for 6 hours, recover methanol, the residue is N-methyl mandelate crude product directly used in the next step.
[0013] As a preferred scheme of the preparation method of the chemical of the present application, wherein: synthesis of N-methyl-a-oxo benzene acetic amide:
[0014] In the bottle, sodium hypochlorite solution, tetrabutylammonium bromide, N-methyl mandelate is added in batches at 0-5℃, the adding time is 5 hours, after adding, keep at 0-5℃ for 3 hours, then warm up to 15-20℃, keep for 10 hours, solid is precipitated, centrifugal, washed with water, the crude product is refined with toluene, light yellow solid is obtained, the content is more than 99%.
[0015] The preparation method of the chemical of the present application has the beneficial effects that: after the step-by-step preparation, the content of N-methyl-a-oxo benzene acetic amide after preparation is high, and the purity is good, thereby effectively improving the use effect of N-methyl-a-oxo benzene acetic amide and the utilization rate of preparation materials.
[0016] In view of the actual adding, stirring and other steps in the actual use process are separately carried out, which is not convenient in the actual operation process.
[0017] Therefore, another object of the present application is to provide a stirring device capable of segmented feeding.
[0018] To solve the above technical problems, the present application further provides the following technical scheme: a stirring device capable of segmented feeding, which is used for the mixing and stirring step required in the preparation process of methyl mandelate, and
[0019] The installation mechanism comprises a base, a support column fixedly connected to the top end of the base, and a top plate fixedly connected to the top end of the support column, the top end of the top plate is fixedly connected with a fixing frame, the inside of the fixing frame is provided with a liquid storage bottle, the top end of the top plate is fixedly connected with a mounting plate, the outside of the support column is fixedly connected with a middle layer plate, one end of the middle layer plate is fixedly connected with a mounting frame, and the inside of the mounting frame is provided with a connecting component;
[0020] The connecting component comprises a bifurcated pipe arranged in the inside of the mounting frame, a connecting pipe fixedly connected to the top end of the bifurcated pipe, and a square block fixedly connected to the outside of the connecting pipe, the inside of the square block is provided with a flow limiting component, and the outside of the flow limiting component is adaptedly installed with a pressing component.
[0021] The driving mechanism comprises a motor mounted outside the mounting plate, a rotating rod fixedly connected to the output end of the motor, and a first connecting block fixedly connected to the outside of the rotating rod, the bottom end of the rotating rod is fixedly connected with a first friction block, the outside of the rotating rod is provided with an output component, the bottom end of the rotating rod is provided with a stirring component, and the outside of the stirring component is provided with a control component.
[0022] The output component comprises a connecting plate fixedly connected to the bottom end of the top plate, a sleeve ring sleeved on the outside of the rotating rod, and a second spring sleeved on the outside of the rotating rod, the outside of the sleeve ring is fixedly connected with a second connecting block, one end of the second connecting block is hingedly connected with a hinge rod, one end of the hinge rod is hingedly connected with a connecting rod, the other end of the connecting rod is hingedly connected with the first connecting block, one end of the connecting rod is fixedly connected with a fixed rod, and one end of the fixed rod is fixedly connected with a magnetic ball block.
[0023] The storage mechanism comprises a mixing barrel arranged at the top end of the base, a liquid outlet pipe fixedly connected to the outside of the mixing barrel, and a transmission gear rotatably connected to the top end of the middle layer plate, the outside of the middle layer plate is provided with a transmission component, and the outside of the mixing barrel is provided with a separation component.
[0024] The transmission component comprises a connecting rod rotatably connected to the inside of the middle layer plate, a driven gear fixedly connected to the top end of the connecting rod, and a first bevel gear fixedly connected to the bottom end of the connecting rod.
[0025] As a preferred scheme of the segmentable feeding stirring device, the flow limiting assembly comprises an embedded block fixedly connected to the inside of the square block, a guide rod fixedly connected to the inside of the embedded block, and a sliding plate slidingly connected to the outside of the guide rod, the outside of the guide rod is sleeved with a first spring, the outside of the embedded block is fixedly connected with a sliding rail, the inside of the sliding rail is slidingly connected with a blocking plate, and one end of the blocking plate is fixedly connected with the sliding plate.
[0026] As a preferred scheme of the segmentable feeding stirring device, the pressing assembly comprises a suspension frame fixedly connected to the bottom end of the top plate, a push rod slidingly connected to the bottom end of the suspension frame, and a hemispherical block fixedly connected to one end of the push rod.
[0027] The other end of the push rod is fixedly connected with the blocking plate.
[0028] As a preferred scheme of the segmental feeding stirring device, the stirring component comprises an outer rod fixedly connected to the inner side of the collar, an inner strip fixedly connected to the inner wall of the outer rod, and an inner rod slidingly connected to the bottom end of the outer rod, the outer side of the inner rod is fixedly connected with a protruding block, the outer side of the inner rod is fixedly connected with a disc, the outer side of the inner rod is fixedly connected with a rotating blade, and the bottom end of the inner rod is fixedly connected with a stirring blade.
[0029] As a preferred scheme of the segmental feeding stirring device, the control component comprises a cylindrical block sleeved on the outer side of the disc, a toothed disc fixedly connected to the outer side of the cylindrical block, and a magnetic ring block fixedly connected to the top end of the toothed disc.
[0030] The top end of the cylindrical block is fixedly connected with a second friction block.
[0031] As a preferred scheme of the segmental feeding stirring device, the separation component comprises a separation pipe fixedly connected to the outer side of the mixing barrel, a bottom pipe fixedly connected to the bottom end of the separation pipe, and a third spring fixedly connected to the inner bottom end of the bottom pipe, the top end of the third spring is fixedly connected with a blocking plate, one end of the separation pipe is internally provided with a one-way valve, the separation pipe is fixedly connected with a blocking block internally, the bottom end of the separation pipe is threadedly connected with a sampling bottle, and the other end of the separation pipe is internally provided with a negative pressure assembly.
[0032] As a preferred scheme of the segmental feeding stirring device, the negative pressure assembly comprises a support frame fixedly connected to the inside of the separation pipe, a rotating shaft rotatably connected to the inside of the support frame, and a fan blade fixedly connected to the outer side of the rotating shaft.
[0033] The other end of the rotating shaft is fixedly connected with a second bevel gear.
[0034] The segmental feeding stirring device has the following advantages: the two groups of chemical reagents in the liquid storage bottles can be segmentedly fed into the mixing barrel by starting the motor, the mixing effect is preliminarily improved, the spiral blade on the outer side of the inner rod and the stirring blade are driven to rotate, the speed of the two chemical reagents entering the mixing barrel is improved through the spiral blade, the chemical reagents in the mixing barrel are fully stirred through the stirring blade, the inner rod stops rotating after stirring is completed, the stirring blade is separated from the chemical reagents in the mixing barrel, and the subsequent chemical reagents are statically stratified.
[0035] When the chemical medicine is static stratification, it will drive the gas inside the separation tube to be continuously discharged under the operation of the fan, and due to the special shape design of the separation tube and the cooperation of the blocking plate, the chemical medicine inside the mixing barrel can be fully stratified, when the stratification is completed, the upper liquid of the internal chemical medicine is sucked out and stored in the sampling bottle, and the outer valve is opened, the lower liquid of the internal chemical medicine is taken out. Compared with the traditional step-by-step operation mode, the device can integrally complete the adding, stirring and mixing, static stratification and taking out of the chemical medicine, so as to greatly improve the convenience of the operator during operation, and effectively improve the practicability of the device. BRIEF DESCRIPTION OF DRAWINGS
[0036] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed in the embodiment description will be briefly introduced as follows. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative labor. Among them:
[0037] Figure 1 It is the overall schematic diagram of the present application.
[0038] Figure 2 It is another state schematic diagram of the overall of the present application.
[0039] Figure 3 It is the overall front view schematic diagram of the present application.
[0040] Figure 4 It is the flow limiting component schematic diagram of the present application.
[0041] Figure 5 It is the driving mechanism schematic diagram of the present application.
[0042] Figure 6 It is the internal schematic diagram of the outer rod of the present application.
[0043] Figure 7 It is the stirring component schematic diagram of the present application.
[0044] Figure 8 It is the cross-sectional schematic diagram of the present application.
[0045] Figure 9 It is the negative pressure component schematic diagram of the present application. DETAILED DESCRIPTION
[0046] In order to make the above-mentioned purposes, features and advantages of the present application more obvious and easy to understand, the specific embodiments of the present application will be described in detail below with reference to the drawings of the specification.
[0047] In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application. However, it will be apparent to one skilled in the art that the present application can be practiced without the specific details set forth in this description. In other instances, well-known methods have not been described in detail in order to avoid unnecessarily obscuring the present application. Therefore, the present application is not intended to be limited by the specific embodiments disclosed below, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
[0048] Second, the "one embodiment" or "an embodiment" referred to herein means a specific feature, structure, or characteristic under discussion that can be included in at least one implementation of the present application. The appearances of "in one embodiment" or "in an embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are they necessarily mutually exclusive of one another.
[0049] Embodiment 1
[0050] Reference Figures 1-9 For the first embodiment of the present application, the embodiment provides a preparation method of a chemical, the method comprising the following steps,
[0051] Synthesis of methyl mandelate:
[0052] Methyl mandelate 300g, methanol 300g, 30% methylamine methanol solution was added at 50-60°C, the dropwise time was about 3 hours, after the dropwise addition, the mixture was heated at 55-60°C for 6 hours, and the residual material was the crude N-methyl mandelate which was directly used in the next step.
[0053] After the chemical reagent is added, a stirring device is used to mix and stir the chemical reagents added together, so that the chemical reagents can fully react when they are static.
[0054] Specifically, synthesis of N-methyl mandelamide:
[0055] Methyl mandelate 300g, methanol 300g, 30% methylamine methanol solution was added at 50-60°C, the dropwise time was about 3 hours, after the dropwise addition, the mixture was heated at 55-60°C for 6 hours, and the residual material was the crude N-methyl mandelate which was directly used in the next step.
[0056] Further, synthesis of N-methyl-a-oxo benzene acetylamide:
[0057] In the bottle, sodium hypochlorite solution and tetrabutylammonium bromide were added, and N-methyl mandelamide was added in batches at 0-5°C, the addition time was 5 hours, after the addition, the mixture was heated at 0-5°C for 3 hours, and then heated at 15-20°C for 10 hours, solid was precipitated, centrifuged, washed with water, and the crude product was refined with toluene to obtain a yellow solid with a content of more than 99%.
[0058] In summary, through the above steps, the content of N-methyl-a-oxo benzene acetic amide is high and the purity is good after the preparation, thereby effectively improving the use effect of N-methyl-a-oxo benzene acetic amide and the utilization rate of the preparation material.
[0059] Example 2
[0060] Reference Figures 1-6 For the second embodiment of the present application, unlike the previous embodiment, this embodiment provides a segmented feeding stirring device for the mixing and stirring steps required in the preparation process of methyl amygdalate, and
[0061] The mounting mechanism 100 comprises a base 101, a support column 102 fixedly connected to the top end of the base 101, and a top plate 103 fixedly connected to the top end of the support column 102. The top end of the top plate 103 is fixedly connected with a fixing frame 104, the inside of the fixing frame 104 is provided with a liquid storage bottle 105, the top end of the top plate 103 is fixedly connected with a mounting plate 106, the outside of the support column 102 is fixedly connected with a middle layer plate 107, one end of the middle layer plate 107 is fixedly connected with a mounting frame 108, and the inside of the mounting frame 108 is provided with a connecting component 109.
[0062] The connecting component 109 comprises a bifurcated pipe 109a arranged in the inside of the mounting frame 108, a connecting pipe 109b fixedly connected to the top end of the bifurcated pipe 109a, and a square block 109c fixedly connected to the outside of the connecting pipe 109b. The inside of the square block 109c is provided with a flow limiting assembly 109d, and the outside of the flow limiting assembly 109d is adapted to be mounted with a pressing assembly 109e.
[0063] The driving mechanism 200 comprises a motor 201 adapted to be mounted on the outside of the mounting plate 106, a rotating rod 202 fixedly connected to the output end of the motor 201, and a first connecting block 203 fixedly connected to the outside of the rotating rod 202. The bottom end of the rotating rod 202 is fixedly connected with a first friction block 204, the outside of the rotating rod 202 is provided with an output component 205, the bottom end of the rotating rod 202 is provided with a stirring component 206, and the outside of the stirring component 206 is provided with a control component 207.
[0064] The output component 205 comprises a connecting plate 205a fixedly connected to the bottom end of the top plate 103, a sleeve ring 205b sleeved outside the rotating rod 202, and a second spring 205c sleeved outside the rotating rod 202. The outer side of the sleeve ring 205b is fixedly connected with a second connecting block 205d. One end of the second connecting block 205d is hingedly connected with a hinged rod 205e. One end of the hinged rod 205e is hingedly connected with a connecting rod 205f. The other end of the connecting rod 205f is hingedly connected with the first connecting block 203. One end of the connecting rod 205f is fixedly connected with a fixed rod 205g. One end of the fixed rod 205g is fixedly connected with a magnetic ball block 205h.
[0065] The storage mechanism 300 comprises a mixing barrel 301 arranged at the top end of the base 101, a liquid outlet pipe 302 fixedly connected outside the mixing barrel 301, and a transmission gear 303 rotatably connected at the top end of the middle layer plate 107. The outer side of the middle layer plate 107 is provided with a transmission component 304. The outer side of the mixing barrel 301 is provided with a separation component 305.
[0066] The transmission component 304 comprises a connecting rod 304a rotatably connected inside the middle layer plate 107, a driven gear 304b fixedly connected at the top end of the connecting rod 304a, and a first bevel gear 304c fixedly connected at the bottom end of the connecting rod 304a.
[0067] Specifically, the flow limiting assembly 109d comprises an embedded block 109d-1 fixedly connected inside the square block 109c, a guide rod 109d-2 fixedly connected inside the embedded block 109d-1, and a sliding plate 109d-3 slidingly connected outside the guide rod 109d-2. The outer side of the guide rod 109d-2 is sleeved with a first spring 109d-4. The outer side of the embedded block 109d-1 is fixedly connected with a sliding rail 109d-5. The sliding rail 109d-5 is slidingly connected with a blocking plate 109d-6 inside. One end of the blocking plate 109d-6 is fixedly connected with the sliding plate 109d-3.
[0068] Further, the pressing assembly 109e comprises a hanging bracket 109e-1 fixedly connected to the bottom end of the top plate 103, a push rod 109e-2 slidingly connected to the bottom end of the hanging bracket 109e-1, and a hemispherical block 109e-3 fixedly connected to one end of the push rod 109e-2.
[0069] The other end of the push rod 109e-2 is fixedly connected with the blocking plate 109d-6.
[0070] In use, by adding two chemical agents that need to be added into two groups of liquid storage bottles 105, and the chemical agent that needs to be mixed into the mixing bucket 301, by starting the motor 201, the motor 201 drives the rotating rod 202 to rotate, which drives the first connecting block 203 and the connecting rod 205f hinged to the first connecting block 203 to rotate, so that the connecting rod 205f drives the magnetic ball block 205h to rotate through the fixed rod 205g, so that the magnetic ball block 205h gradually extends and rotates outward under the centrifugal force generated by rotation, and continuously extends outward under the cooperation of the hinged rod 205e and the matching sleeve ring 205b, and the sleeve ring 205b slides downward outside the rotating rod 202, the sleeve ring 205b slides downward and stretches the second spring 205c, and the magnetic ball block 205h continuously extends and rotates, which extrudes the surface of the hemispherical block 109e-3, and under the extrusion force, the hemispherical block 109e-3 is pushed by the push rod 109e-2 to push the blocking plate 109d-6 to slide in the slide rail 109d-5, the blocking plate 109d-6 pushes the sliding plate 109d-3 to slide outside the guide rod 109d-2 and extrudes the first spring 109d-4, which makes it shrink, and the blocking plate 109d-6 slides into the inner block 109d-1, so that the liquid in the liquid storage bottle 105 flows downward, and enters the mixing bucket 301 through the connecting pipe 109b and the bifurcated pipe 109a, when the magnetic ball block 205h does not extrude the hemispherical block 109e-3, the blocking plate 109d-6 slides reversely and resets under the elasticity of the first spring 109d-4, so as to prevent the chemical agent in the liquid storage bottle 105 from flowing downward.
[0071] Because three groups of magnetic ball blocks 205h continuously extend and rotate, the magnetic ball blocks 205h continuously extrude the two groups of hemispherical blocks 109e-3, so that the chemical agents in the two groups of liquid storage bottles 105 can flow downward in sections, until the magnetic ball block 205h rotates to be perpendicular to the rotating rod 202 under the action of centrifugal force, at which time the magnetic ball block 205h cannot extrude the hemispherical block 109e-3, so that the chemical agents in the two groups of liquid storage bottles 105 cannot flow downward.
[0072] In summary, by starting the motor 201, the magnetic ball block 205h can be driven to rotate, and under the action of centrifugal force, it will continuously extend outward, so that the magnetic ball block 205h can extrude the two half ball blocks 109e-3, and the chemical reagents in the two groups of liquid storage bottles 105 can continuously flow down in sections. When the magnetic ball block 205h rotates to be perpendicular to the rotating rod 202 under the action of centrifugal force, the magnetic ball block 205h cannot extrude the half ball block 109e-3 at this time, so that the chemical reagents in the two groups of liquid storage bottles 105 cannot flow down, so as to ensure that the appropriate two groups of chemical reagents are added, and the addition of chemical reagents is stopped, and the two groups of chemical reagents are added to the mixing barrel 301 in a segmented manner. Compared with adding one kind of chemical reagent at a time, the segmented addition method can make the mixing of multiple groups of chemical reagents more thorough, so as to ensure the quality of the prepared product.
[0073] Embodiment 3
[0074] With reference to Figures 1-7 For the third embodiment of the present application, unlike the previous embodiment, the embodiment provides a stirring component 206, which includes an outer rod 206a fixedly connected to the inside of the sleeve 205b, an inner strip plate 206b fixedly connected to the inner wall of the outer rod 206a, and an inner rod 206c slidingly connected to the bottom end of the outer rod 206a. The outer side of the inner rod 206c is fixedly connected with a protrusion 206d, the outer side of the inner rod 206c is fixedly connected with a disc 206e, the outer side of the inner rod 206c is fixedly connected with a rotating blade 206f, and the bottom end of the inner rod 206c is fixedly connected with a stirring blade 206g.
[0075] Specifically, the control component 207 includes a cylindrical block 207a sleeved on the outside of the disc 206e, a tooth disc 207b fixedly connected to the outside of the cylindrical block 207a, and a magnetic ring block 207c fixedly connected to the top end of the tooth disc 207b.
[0076] The top end of the cylindrical block 207a is fixedly connected with a second friction block 207d.
[0077] In use, when the collar 205b slides downward while rotating by the magnetic ball block 205h, the outer rod 206a is caused to slide downward, so that the outer rod 206a is in contact with the protrusions 206d on the outer side of the inner rod 206c through the inner side of the inner strip plate 206b, so that the outer rod 206a is caused to rotate while rotating the inner rod 206c, so that the inner rod 206c is caused to rotate while rotating the spiral blades 206f and the stirring blades 206g on the outer side of the inner rod 206c, and since the spiral blades 206f are arranged in the main pipe of the bifurcated pipe 109a, the speed of the two chemical agents entering the mixing barrel 301 in stages can be improved, and under the operation of the stirring blades 206g, the multiple chemical agents in the mixing barrel 301 are stirred to be fully mixed, and when the magnetic ball block 205h rotates to the rotating rod 202, the spiral blades 206f and the stirring blades 206g on the outer side of the inner rod 206c are still rotated, so that the last two groups of chemical agents entering the mixing barrel 301 can be fully stirred and mixed.
[0078] In summary, by starting the motor 201, the two groups of chemical agents in the two liquid storage bottles 105 are caused to flow downward in stages, while the spiral blades 206f and the stirring blades 206g on the outer side of the inner rod 206c are caused to rotate, so that the speed of the two groups of chemical agents entering the mixing barrel 301 can be improved, and the multiple chemical agents in the mixing barrel 301 can be stirred by the stirring blades 206g, so that the multiple chemical agents in the mixing barrel 301 can still be stirred after the last part of the chemical agents enters the mixing barrel 301, so that they are fully mixed.
[0079] Embodiment 4
[0080] Referring to Figures 1-9 For the fourth embodiment of the present application, unlike the previous embodiment, the embodiment provides a separation component 305, which includes a separation pipe 305a fixedly connected to the outer side of the mixing barrel 301, a bottom pipe 305b fixedly connected to the bottom end of the separation pipe 305a, and a third spring 305c fixedly connected to the inner bottom end of the bottom pipe 305b, the top end of the third spring 305c is fixedly connected with a baffle plate 305d, one end of the separation pipe 305a is internally provided with a one-way valve 305e, the separation pipe 305a is internally fixedly connected with a stop block 305f, the bottom end of the separation pipe 305a is threadedly connected with a sampling bottle 305g, and the other end of the separation pipe 305a is internally provided with a negative pressure assembly 305h.
[0081] Specifically, the negative pressure assembly 305h includes a support frame 305h-1 fixedly connected to the inside of the separation pipe 305a, a rotating shaft 305h-2 rotatably connected to the inside of the support frame 305h-1, and a fan blade 305h-3 fixedly connected to the outer side of the rotating shaft 305h-2.
[0082] The other end of the rotating shaft 305h-2 is fixedly connected with a second bevel gear 305h-4.
[0083] In use, when the magnetic ball block 205h rotates to be perpendicular to the rotating rod 202, since the magnetic ball block 205h and the magnetic ring block 207c are positive and negative respectively, an attractive force is generated, so that when the magnetic ball block 205h continuously rotates to be perpendicular to the rotating rod 202, the magnetic ring block 207c slides upward under the action of the attraction between opposite poles, so as to drive the gear disc 207b and the cylindrical block 207a to slide upward. Since the magnetic ball block 205h is always perpendicular to the rotating rod 202 under the centrifugal force, only the magnetic ring block 207c slides upward, and the disc 206e is arranged inside the cylindrical block 207a, so as to drive the inner rod 206c to slide upward, so that the protrusion 206d on the outer side of the inner rod 206c slides to the inner top end of the outer rod 206a, so that the inner strip plate 206b does not contact the protrusion 206d at this time, so that the rotation of the outer rod 206a cannot drive the inner rod 206c to rotate, so that the stirring blade 206g stops rotating. Since the inner rod 206c slides upward, the stirring blade 206g is separated from the chemical agent in the mixing barrel 301, and the cylindrical block 207a slides upward, so that the second friction block 207d contacts the first friction block 204. At this time, the rotation of the rotating rod 202 drives the cylindrical block 207a to rotate through the first friction block 204 and the second friction block 207d, so that the gear disc 207b on the outer side of the cylindrical block 207a rotates, and the gear disc 207b drives the driven gear 304b to rotate through the transmission gear 303, the driven gear 304b drives the first bevel gear 304c to rotate through the connecting rod 304a, the first bevel gear 304c drives the fan blade 305h-3 fixed on the outer side of the rotating shaft 305h-2 to rotate through the second bevel gear 305h-4, and the chemical agent in the mixing barrel 301 is in a static state at this time, and stratification is gradually generated.
[0084] The fan blade 305h-3 can discharge the gas in the separation tube 305a during rotation, and since the middle part of the separation tube 305a has a larger diameter than the two ends, the fan blade 305h-3 cannot quickly discharge the gas in the separation tube 305a, thereby ensuring that the chemicals in the mixing bucket 301 can be fully stationary and complete the layering. When the gas in the separation tube 305a is discharged, a negative pressure is generated, which causes the blocking plate 305d to gradually rise under the negative pressure and stretch the third spring 305c, thereby again increasing the time for the chemicals in the mixing bucket 301 to be stationary to ensure that the layering is completed. When the blocking plate 305d is stopped by the stopper 305f, the one-way valve is opened due to the continuous discharge of gas in the separation tube 305a, thereby allowing the upper liquid of the chemicals in the mixing bucket 301 to enter the separation tube 305a and then enter the sampling bottle 305g through the separation tube 305a. Since the outlet tube 302 is provided with a valve, when the upper layer of chemicals in the mixing bucket 301 is extracted, the valve is opened, and the chemicals at the bottom of the mixing bucket 301 can be extracted.
[0085] In summary, by starting the motor 201, the chemicals in the two groups of liquid storage bottles 105 can be segmented into the mixing bucket 301, thereby preliminarily improving the mixing effect, and driving the helical blades 206f on the inner rod 206c and the stirring blades 206g to rotate, thereby improving the speed of the two chemicals entering the mixing bucket 301 through the helical blades 206f, and fully stirring the chemicals in the mixing bucket 301 through the stirring blades 206g. When the stirring is completed, the inner rod 206c stops rotating, and the stirring blades 206g are separated from the chemicals in the mixing bucket 301, thereby ensuring the effect of subsequent chemical layering.
[0086] When the chemicals are stationary and layered, the gas in the separation tube 305a is continuously discharged under the operation of the fan blade 305h-3. Due to the special shape of the separation tube 305a and the cooperation of the blocking plate 305d, the chemicals in the mixing bucket 301 can be fully layered. When the layering is completed, the upper liquid of the chemicals is extracted and stored in the sampling bottle 305g, and the lower liquid of the chemicals can be extracted by opening the valve outside the outlet tube 302. Compared with the traditional step-by-step operation method, this device can complete the addition, stirring and mixing, stationary layering, and extraction of chemicals in one body, thereby greatly improving the convenience of the operator during operation and effectively improving the practicality of the device.
[0087] It is important to note that the construction and arrangement of the application shown in the various exemplary embodiments is illustrative only. Although only a few embodiments have been described in detail in this disclosure, those skilled in the art who review the present disclosure will readily appreciate that many modifications are possible (e.g., variations in sizes, dimensions, structures, shapes and proportions of the various elements, values of parameters, mounting arrangements, use of materials, colors, orientations, etc.) without materially departing from the novel teachings and advantages of the subject matter described herein. For example, elements shown as integrally formed can be constructed of multiple parts or elements, the position of elements can be reversed or otherwise varied, and the nature or number of elements or positions can be altered or varied. Thus, the foregoing description is by way of example only, and is not intended to be limiting. The application is limited only as defined in the following claims and equivalents thereto. The sequence of any process or method steps, or the order in which they are carried out, can be altered or re-ordered without departing from the scope of the application. Any "articles of manufacture" or "manufacturing" as described herein are intended to encompass structures constructed of a multitude of different physical elements or components. In the claims, any means-plus-function clause is intended to cover the structures described herein as performing the recited function and also cover structures yet to be invented which perform the recited function but operate in a different manner. Other substitutions, modifications, changes and omissions can be made in the design, operating conditions and arrangement of the exemplary embodiments without departing from the scope of the application as expressed in the appended claims.
[0088] Also, to provide a concise description of the exemplary embodiments, not all features of an actual implementation can be described (that is, not all implementations can include all of the features described or optional implementations can include only a subset of the features described).
[0089] It will be appreciated that in the development of any actual implementation, as in any engineering or design project, numerous implementation-specific decisions can be made. Such development efforts can inevitably lead to modifications, not all of which can be foreseen in advance. Such modifications are not to be regarded as a departure from the spirit and scope of the present application, and all such modifications are intended to be included within the scope of the present application. The disclosure is not a complete description of the actual implementation, nor is it intended to be so; thus, what is actually devised can depart from what is described in this disclosure.
[0090] It should be noted that the above examples are merely intended to illustrate the technical solutions of the present application but not to limit the present application, and although the present application is described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present application can be modified or equivalently replaced without departing from the spirit and scope of the present application, and all such modifications and equivalents are intended to be included within the scope of the claims of the present application.
Claims
1. A batchable downer mixing device characterized by: A mixing and stirring step required in the preparation process of methyl salicylate, and The mounting mechanism (100) comprises a base (101), a support column (102) fixedly connected to the top end of the base (101), and a top plate (103) fixedly connected to the top end of the support column (102), and the top end of the top plate (103) is fixedly connected with a fixing frame (104), and the inside of the fixing frame (104) is provided with a liquid storage bottle (105), and the top end of the top plate (103) is fixedly connected with a mounting plate (106), and the outer side of the support column (102) is fixedly connected with a middle layer plate (107), and one end of the middle layer plate (107) is fixedly connected with a mounting frame (108), and the inner side of the mounting frame (108) is provided with a connecting component (109); Wherein, the connecting component (109) comprises a bifurcated pipe (109a) arranged in the inner side of the mounting frame (108), a connecting pipe (109b) fixedly connected to the top end of the bifurcated pipe (109a), and a square block (109c) fixedly connected to the outer side of the connecting pipe (109b), the inside of the square block (109c) is provided with a flow limiting assembly (109d), and the outer side of the flow limiting assembly (109d) is fitted with a pressing assembly (109e); The driving mechanism (200) comprises a motor (201) fittedly installed on the outer side of the mounting plate (106), a rotating rod (202) fixedly connected to the output end of the motor (201), and a first connecting block (203) fixedly connected to the outer side of the rotating rod (202), and the bottom end of the rotating rod (202) is fixedly connected with a first friction block (204), and the outer side of the rotating rod (202) is provided with an output component (205), and the bottom end of the rotating rod (202) is provided with a stirring component (206), and the outer side of the stirring component (206) is provided with a control component (207); Wherein, the output component (205) comprises a connecting plate (205a) fixedly connected to the bottom end of the top plate (103), a sleeve ring (205b) sleeved on the outer side of the rotating rod (202), and a second spring (205c) sleeved on the outer side of the rotating rod (202), the outer side of the sleeve ring (205b) is fixedly connected with a second connecting block (205d), one end of the second connecting block (205d) is hinged with a hinge rod (205e), one end of the hinge rod (205e) is hinged with a link rod (205f), the other end of the link rod (205f) is hinged with the first connecting block (203), one end of the link rod (205f) is fixedly connected with a fixed rod (205g), one end of the fixed rod (205g) is fixedly connected with a magnetic ball block (205h); and, The storage mechanism (300) comprises a mixing barrel (301) arranged at the top end of the base (101), a liquid outlet pipe (302) fixedly connected to the outside of the mixing barrel (301), and a transmission gear (303) rotatably connected to the top end of the middle layer plate (107), and the outside of the middle layer plate (107) is provided with a transmission component (304), and the outside of the mixing barrel (301) is provided with a separation component (305); The transmission component (304) comprises a connecting rod (304a) rotatably connected to the inside of the middle layer plate (107), a driven gear (304b) fixedly connected to the top end of the connecting rod (304a), and a first bevel gear (304c) fixedly connected to the bottom end of the connecting rod (304a); The separation component (305) comprises a separation pipe (305a) fixedly connected to the outside of the mixing barrel (301), a bottom pipe (305b) fixedly connected to the bottom end of the separation pipe (305a), and a third spring (305c) fixedly connected to the inside bottom end of the bottom pipe (305b), the top end of the third spring (305c) is fixedly connected with a baffle plate (305d), one end of the inside of the separation pipe (305a) is provided with a check valve (305e), the inside of the separation pipe (305a) is fixedly connected with a stop block (305f), the bottom end of the separation pipe (305a) is threadedly connected with a sampling bottle (305g), and the other end of the inside of the separation pipe (305a) is provided with a negative pressure assembly (305h); The negative pressure assembly (305h) comprises a support frame (305h-1) fixedly connected to the inside of the separation pipe (305a), a rotating shaft (305h-2) rotatably connected to the inside of the support frame (305h-1), and a fan blade (305h-3) fixedly connected to the outside of the rotating shaft (305h-2); The other end of the rotating shaft (305h-2) is fixedly connected with a second bevel gear (305h-4).
2. The segmentable downfeed mixer of claim 1, wherein: The flow limiting assembly (109d) comprises an embedded block (109d-1) fixedly connected to the inside of the square block (109c), a guide rod (109d-2) fixedly connected to the inside of the embedded block (109d-1), and a sliding plate (109d-3) slidingly connected to the outside of the guide rod (109d-2), the outside of the guide rod (109d-2) is sleeved with a first spring (109d-4), the outside of the embedded block (109d-1) is fixedly connected with a sliding rail (109d-5), the inside of the sliding rail (109d-5) is slidingly connected with a blocking plate (109d-6), and one end of the blocking plate (109d-6) is fixedly connected with the sliding plate (109d-3).
3. The segmentable downfeed mixer of claim 2, wherein: The pressing assembly (109e) comprises a hanging frame (109e-1) fixedly connected to the bottom end of the top plate (103), a push rod (109e-2) slidingly connected to the bottom end of the hanging frame (109e-1), and a hemispherical block (109e-3) fixedly connected to one end of the push rod (109e-2); Another end of the push rod (109e-2) is fixedly connected with the barrier plate (109d-6).
4. A segmentable blanking device according to claim 2 or 3, characterized in that: The stirring component (206) comprises an outer rod (206a) fixedly connected to the inside of the collar (205b), an inner strip plate (206b) fixedly connected to the inner wall of the outer rod (206a), and an inner rod (206c) slidingly connected to the bottom end of the outer rod (206a), the outer side of the inner rod (206c) is fixedly connected with a protruding block (206d), the outer side of the inner rod (206c) is fixedly connected with a disc (206e), the outer side of the inner rod (206c) is fixedly connected with a rotating blade (206f), and the bottom end of the inner rod (206c) is fixedly connected with a stirring blade (206g).
5. The segmentable downfeed mixer of claim 4, wherein: The control component (207) comprises a cylindrical block (207a) sleeved on the outside of the disc (206e), a tooth disc (207b) fixedly connected to the outside of the cylindrical block (207a), and a magnetic ring block (207c) fixedly connected to the top end of the tooth disc (207b); The top end of the cylindrical block (207a) is fixedly connected with a second friction block (207d).
6. A method for preparing a chemical product, wherein the mixing and stirring are carried out using the sectionalized downer mixer according to any one of claims 1 to 5, characterized in that: The method Comprise the following steps, Synthesis of methyl mandelate: Put mandelic acid 300g, methanol 500g into a bottle, add sulfuric acid 30g at below 30℃, after dropping, warm up to reflux for 5 hours, recover methanol, cool to room temperature, add toluene 1000ml, water 1000ml, stir and stand, separate layers, wash with 10% sodium carbonate aqueous solution to PH8, wash toluene layer with water twice, recover toluene under reduced pressure, and evaporate the residue 300g; After adding the chemical reagent, the stirring device is used to mix and stir the chemical reagents added together, so that the chemical reagents can fully react when they are static in the later stage; Synthesis of N-methyl mandelamide: Put methyl mandelate 300g and methanol 300g into a bottle, add 30% methylamine methanol solution at 50-60℃, the dropping time is 3 hours, after dropping, warm up to 55-60℃ for 6 hours, recover methanol, and the residue is the crude product of N-methyl mandelamide, which is directly used for the next reaction; Synthesis of N-methyl-a-oxophenylacetamide: Put sodium hypochlorite solution and tetrabutylammonium bromide into a bottle, add N-methyl mandelamide in batches at 0-5℃, the adding time is 5 hours, after adding, warm up to 0-5℃ for 3 hours, then warm up to 15-20℃ for 10 hours, solid is precipitated, centrifugal, wash with water, refine the crude product with toluene, and a light yellow solid is obtained, the content is more than 99%.
Citation Information
Patent Citations
Compound as well as synthesis method and application thereof
CN114315753A
Ball mill and method for manufacturing slurry using same
KR1020140013256A