CN217887996U - Preparation facilities of copper p-toluenesulfonate - Google Patents
Preparation facilities of copper p-toluenesulfonate Download PDFInfo
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- CN217887996U CN217887996U CN202221627540.9U CN202221627540U CN217887996U CN 217887996 U CN217887996 U CN 217887996U CN 202221627540 U CN202221627540 U CN 202221627540U CN 217887996 U CN217887996 U CN 217887996U
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Abstract
The utility model relates to a preparation facilities of copper p-toluene sulfonate, including the mounting bracket, from last to installing fixed reactor, concentrator and crystallizer down in proper order on the mounting bracket, the reactor is four mouthfuls of flasks, and four bottlenecks are provided with electric agitator, thermometer, H type fractionator and the charging means of putting and taking the condenser respectively, the bottle bottom of four mouthfuls of flasks is equipped with the discharging pipe, and the chuck is installed to the discharging pipe lower extreme; the concentrator is a three-mouth flask, three bottle mouths are respectively provided with an emptying throttle, a reduced pressure distillation device and a feeding pipe, the upper end of the feeding pipe is coaxially provided with a lower chuck, the bottom of the flask is provided with a discharging pipe, and the discharging pipe is connected with the crystallizer; the filter assembly is installed between the upper chuck plate and the lower chuck plate, one side of the filter assembly is rotatably installed on the installation frame through the connecting rod, and the upper chuck plate, the filter assembly and the lower chuck plate are sealed and locked through the pins to form the suction filter. The utility model discloses simple structure, modern design, preparation are high-efficient and safe.
Description
Technical Field
The utility model belongs to the technical field of fine chemical industry preparation, a preparation, especially a preparation facilities to copper toluene sulfonate is related to the preparation of copper toluene sulfonate.
Background
Sulfuric acid is an excellent catalyst for esterification and acetalization, but has strong acidity and strong corrosivity, and is particularly easy to prepare toxic limiting products, so that the sulfuric acid used for p-toluenesulfonic acid as a catalyst at present has a plurality of advantages. The p-toluenesulfonic acid is organic strong acid without oxidability, the acidity of the p-toluenesulfonic acid is equivalent to that of sulfuric acid, so the p-toluenesulfonic acid can replace sulfuric acid to be widely used for various chemical reactions, has better effect than sulfuric acid, is mild in property, is not easy to generate side reactions such as oxidation and carbonization, and has high product purity and light color; but still have very strong corrosivity to the apparatus, and react and product mix, separate difficult, dangerous article, use and prepare and pay great attention to, therefore adopted and regarded as the catalyst to replace p-toluenesulfonic acid as copper p-toluenesulfonate, said copper p-toluenesulfonate not merely can overcome the deficiency as catalyst of p-toluenesulfonic acid, and have better catalyst performance, and copper p-toluenesulfonate has advantages such as not absorbing moisture, high activity can be reused; therefore, the research on the preparation device of the copper toluene sulfonate is very important.
No patent literature relevant to the present application is found by search.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to overcome prior art's weak point, provide a simple structure, novel in design, prepare high-efficient and safe preparation facilities to toluene sulfonic acid copper.
The utility model provides a its technical problem take following technical scheme to realize:
a preparation device of copper p-toluenesulfonate comprises a mounting frame, wherein a reactor, a concentrator and a crystallizer are sequentially and fixedly arranged on the mounting frame from top to bottom, the reactor and the concentrator are both arranged in a split type switchable heating cooling jacket, the reactor is a four-mouth flask, an electric stirrer is arranged at a middle bottle opening, a thermometer is arranged at a left bottle opening, an H-shaped fractionator with a condenser is arranged at a right bottle opening, a feeder is arranged at a rear bottle opening, a discharge pipe with a throttle is arranged at the central part of the bottle bottom of the four-mouth flask, and an upper chuck is coaxially arranged at the lower end of the discharge pipe; the concentrator is a three-mouth flask, a left-side bottle mouth is provided with an emptying throttle, a right-side bottle mouth is connected with a reduced pressure distillation device, a middle bottle mouth is a feeding pipe, the upper end of the middle bottle mouth is coaxially provided with a lower chuck, the center part of the bottle bottom is provided with a discharging pipe with a throttle, and the discharging pipe is connected with a crystallizer; the coaxial mounting has filtering component between the last (holding) chuck of reactor and the lower (holding) chuck of concentrator, filtering component rotates through the connecting rod to be installed on the mounting bracket on one side, just go up (holding) chuck, filtering component and lower (holding) chuck and still seal the locking through the pin and form the suction filter.
And the upper chuck comprises a cover-shaped body, the top of the cover-shaped body is provided with a feed pipe, the port of the cover-shaped body is a ground port and is tightly connected with a ground port tip at the lower end of a reactor discharge pipe, and the bottom of the cover-shaped body is a carefully ground hollow round table.
The lower chuck comprises a cylinder body, a funnel is coaxially arranged in the cylinder body, a carefully ground hollow circular truncated cone is arranged at the top of the cylinder body, the inner wall of the hollow circular truncated cone is connected with the upper end of the funnel, and a vacuum branch pipe with a throttle is arranged on one side of the cylinder body and is connected with a vacuum system; the bottom of the cylinder body is a ground tip which is tightly connected with a ground port at the upper end of a feed pipe of the concentrator.
Moreover, the filtering component comprises a sieve plate, the sieve plate is in a circular truncated cone structure, and filter paper is arranged on the sieve plate; the upper surfaces of two sides of the sieve plate are symmetrically provided with jacks, the upper surfaces of two sides of the hollow round platform of the upper chuck plate and the upper surface of two sides of the hollow round platform of the lower chuck plate are provided with pin holes, the jacks and the pin holes are coaxially arranged when being installed, and are sealed and locked through pins to form a suction filter, so that the suction filtration effect is realized; and a lifting handle is further arranged on one side of the sieve plate.
The vacuum distillation device comprises a Kjeldahl fractionation head, the lower port of the Kjeldahl fractionation head is communicated and connected with a three-neck flask, the upper pipe orifice on the left side of the Kjeldahl fractionation head is provided with an air inlet capillary with a spiral clamp, and the air inlet capillary is directly communicated with the bottom of the concentrator to adjust the size of inlet air; the thermometer is arranged on the upper pipe orifice of the right side, the liquid outlet of the thermometer is connected with a straight condenser in a communicating way, and the other end of the straight condenser is connected with a solvent receiving bottle in a communicating way through a decompression receiving pipe and is used for collecting the solvent evaporated by decompression concentration.
The feeder comprises a funnel body, a discharge pipe is coaxially arranged at the bottom end of the funnel body, a ground pin is arranged at the bottom of the discharge pipe, and the ground pin can be tightly connected with a ground opening of a bottle mouth of the four-mouth flask; the top end of the funnel body is provided with a top plate, a rotating cylinder is rotatably mounted on the top plate through a rotating shaft, a plurality of channels are uniformly distributed on the upper surface of the rotating cylinder at intervals along the circumference of the rotating cylinder, one channel is an extension channel, and the top port of the extension channel is sealed by a sealing plug; the other channels are storage channels for storing materials; the top port of the material storage channel is arranged by a sealing turnover cover, and a feed opening is arranged on the upper surface of the top plate corresponding to the position of the extension channel; a rotary handle is arranged on the side wall of the rotary cylinder corresponding to the position of the extension channel; the rotary drum is driven to rotate, so that the feeding in multiple times is realized.
In addition, a limiting groove is formed on the circumferential side wall of the rotary cylinder corresponding to the central position of each channel; and still be provided with stop gear on the lateral wall of funnel body upper end internal surface, stop gear includes limit stop, spring and spacing ball, the one end of spring sets up spacing ball, limit stop sets up in the spring both sides, spacing ball is located limit stop one end, and clamps with the spacing recess of rotatory section of thick bamboo.
The utility model has the advantages that:
the device is made of borosilicate glass, so that the device has good thermal stability, chemical stability and visibility; the whole process is clear at a glance, and the observation and control operation are convenient; and the parts are connected by grinding openings, so that the disassembly, assembly and cleaning of equipment are facilitated; the preparation process is completed by feeding reaction, hot filtering, concentration and crystallization at one time, so that the operation is simplified;
the filter assembly of the device is rotatably installed on the installation frame through the connecting rod, is clamped between the upper chuck plate and the lower chuck plate and is sealed and locked through the pin to form a filter, when filter paper needs to be replaced, the pin is only required to be detached, then the sieve plate is rotated out to replace the filter paper, then the sieve plate is rotated to be between the upper chuck plate and the lower chuck plate and is locked through the pin, and the disassembling steps are greatly reduced, so that the filter paper is replaced more conveniently, and meanwhile, the safety of experimenters is protected;
the utility model discloses the charging means that sets up is a device that can feed in raw material many times through the rotation, need not the staff and opens the bottle plug at every turn when carrying out the reaction and weigh reinforced, has improved experimental efficiency greatly, simultaneously because paratoluenesulfonic acid is the noxious material, because the rotatory reinforced mode of this device, can avoid contacting with paratoluenesulfonic acid to provide the experiment guarantee for the experimenter.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic view of the structure of the feeder of the present invention;
FIG. 3 is a perspective view of the feeder of the present invention;
fig. 4 is a schematic structural diagram of the filtering assembly of the present invention.
Detailed Description
The present invention will be described in more detail with reference to the following embodiments, which are provided by way of illustration and not limitation, and the scope of the present invention should not be limited thereby.
A preparation device of copper p-toluenesulfonate comprises a mounting frame 1, wherein a reactor 13, a concentrator 4 and a crystallizer 2 are sequentially and fixedly arranged on the mounting frame from top to bottom, the reactor is a four-mouth flask, an electric stirrer 12 is arranged at a middle bottle mouth, a thermometer 8 is arranged at a left bottle mouth, an H-shaped fractionator 11 with a condenser 10 is arranged at a right bottle mouth, a feeder 9 is arranged at a rear bottle mouth, a discharge pipe 14 with a throttle is arranged at the central part of the bottom of the four-mouth flask, and an upper chuck 15 is coaxially arranged at the lower end of the discharge pipe; the concentrator is a three-neck flask, the left side bottle mouth is provided with a emptying throttle 5, the right side bottle mouth is connected with a reduced pressure distillation device, the middle bottle mouth is a feeding pipe, the upper end of the feeding pipe is coaxially provided with a lower chuck plate 17, the central part of the bottle bottom is provided with a discharging pipe with a throttle, and the discharging pipe is connected with the crystallizer; a filter assembly 16 is coaxially arranged between an upper chuck plate of the reactor and a lower chuck plate of the concentrator, one side of the filter assembly is rotatably arranged on the mounting frame through a connecting rod 6, and the upper chuck plate, the filter assembly and the lower chuck plate are sealed and locked through pins;
the upper chuck comprises a cover-shaped body, the top of the cover-shaped body is provided with a feed pipe, the port of the cover-shaped body is a grinding opening which can be tightly connected with a grinding opening tip at the lower end of a reactor discharge pipe, and the bottom of the cover-shaped body is a carefully ground hollow round table; the lower chuck comprises a cylinder body, a funnel is coaxially arranged in the cylinder body, a carefully ground hollow circular truncated cone is arranged at the top of the cylinder body, the inner wall of the hollow circular truncated cone is connected with the upper end of the funnel, and a vacuum branch pipe 7 with a throttle is arranged at one side of the cylinder body and is connected with a vacuum system; the bottom of the cylinder body is provided with a grinding tip which is tightly connected with a grinding opening at the upper end of a feed pipe of the concentrator;
the filter assembly comprises a sieve plate 16, the sieve plate is in a circular truncated cone structure, and filter paper is arranged on the sieve plate; the upper surfaces of two sides of the sieve plate are symmetrically provided with jacks 16-1, the upper surfaces of two sides of the hollow round platform of the upper chuck plate and the hollow round platform of the lower chuck plate are provided with pin holes, the jacks and the pin holes are coaxially arranged when being installed, and are sealed and locked through pins to form a suction filter, so that the suction filtration effect is realized; when the filter paper needs to be replaced, only the pin needs to be detached, then the handle of the sieve plate is pulled, the sieve plate is rotated out to replace the filter paper, then the sieve plate is rotated to a position between the upper chuck plate and the lower chuck plate and locked through the pin, the disassembling steps are greatly reduced, the filter paper is more convenient to replace, and meanwhile, the safety of experimenters is protected;
the reduced pressure distillation device comprises a Kjeldahl fractionation head 19, the lower port of the Kjeldahl fractionation head is communicated and connected with a three-neck flask, the upper pipe orifice on the left side of the Kjeldahl fractionation head is provided with an air inlet capillary with a spiral clamp, the air inlet capillary is directly communicated with the bottom of a concentrator and adjusts the size of air inlet through the air inlet capillary, so that bumping during reduced pressure concentration is prevented, the upper pipe orifice on the right side is provided with a thermometer 8, the liquid outlet of the thermometer is communicated and connected with a straight condenser 20, and the other end of the straight condenser is communicated and connected with a solvent receiving bottle 21 through a reduced pressure receiving pipe and used for collecting a solvent evaporated by reduced pressure concentration;
the feeder comprises a funnel body 9-4, a discharge pipe 9-1 is coaxially arranged at the bottom end of the funnel body, a ground pin is arranged at the bottom of the discharge pipe, and the ground pin can be tightly connected with a ground opening of a bottle mouth of a four-mouth flask; the top end of the funnel body is provided with a top plate, a rotating cylinder 9-9 is rotatably mounted on the top plate through a rotating shaft 9-7, a plurality of channels are uniformly distributed on the upper surface of the rotating cylinder at intervals along the circumference of the rotating cylinder, one channel is an extension channel 9-6, and the top port of the extension channel is sealed by a sealing plug; the other channels are storage channels 9-8 for storing reactants needing to be fed in a plurality of times; the top port of the material storage channel is arranged by a sealing turnover cover, and the upper surface of the top plate corresponding to the position of the extension channel is provided with a feed opening 9-3; and a rotary handle 9-5 is arranged on the side wall of the rotary cylinder corresponding to the position of the extension channel; the rotary drum is driven to rotate, so that the feeding in multiple times is realized;
in the specific implementation of the utility model, in order to rotate the rotary cylinder at fixed points, limit grooves 9-10 are respectively formed on the circumferential side wall of the rotary cylinder corresponding to the central position of each channel; a limiting mechanism 9-2 is further arranged on the side wall of the inner surface of the upper end of the funnel body, the limiting mechanism comprises a limiting stop, a spring and a limiting ball, the limiting stop is arranged at one end of the spring and is arranged on two sides of the spring, and the limiting ball is located at one end of the limiting stop and is clamped with the limiting groove of the rotary cylinder;
in the specific implementation of the utility model, the reactor and the concentrator are both arranged in a split type switchable heating and cooling jacket 3;
the bottle mouths of the four-mouth flask and the three-mouth flask are standard ground mouths;
the utility model discloses specifically operate:
closing a discharging throttle of the reactor, adjusting a three-way throttle of the H-type fractionator to a position where reflux liquid completely returns to the reactor, introducing water to a condenser, and adjusting a feeder to a position where a feed opening and an extension channel are coaxially arranged; respectively putting the amount of copper oxide required to be added each time in a storage channel, opening a sealing plug on an extension channel, adding water into a reactor, stirring, adding paratoluenesulfonic acid powder to dissolve the paratoluenesulfonic acid powder, and covering the sealing plug; rotating the rotary cylinder, adding a certain amount of CuO powder under stirring for several times, heating and refluxing, and stirring to rotate all the time without stopping at will; refluxing for 3h, and finishing the reaction; stopping heating, cooling, stirring and keeping running; closing a discharge throttle and an emptying throttle of the concentrator and a vacuum branch pipe throttle of the reduced pressure distillation device, opening the vacuum branch pipe throttle on the lower chuck, and connecting the vacuum branch pipe throttle to a vacuum system; opening a discharging valve of the reactor, performing suction filtration, and slowly flowing filtrate into a concentrator; after the suction filtration is finished, opening a vent throttle of the concentrator, closing a vacuum branch pipe throttle on the lower chuck plate, separating a vacuum decompression system, and cooling the filtrate; closing an emptying throttle of the concentrator, opening a vacuum branch pipe throttle of the reduced pressure distillation device, connecting the vacuum branch pipe throttle to a vacuum pressure reduction system, adjusting a screw clamp to control the size of inlet air, performing reduced pressure concentration and preventing bumping; and (4) after the concentration is finished, emptying, closing a vacuum branch pipe joint of the reduced pressure distillation device, and separating from a vacuum reduced pressure system. Opening a discharging throttle of the concentrator to discharge a concentrated solution, and allowing the concentrated solution to enter a crystallizer for crystallization and draining; and (5) using ethanol as a solvent for secondary recrystallization to obtain a finished product.
The device is made of borosilicate glass, so that the device has good thermal stability, chemical stability and visibility; the whole process is clear at a glance, and the observation and control operation are convenient; and the parts are connected by grinding openings, so that the disassembly, assembly and cleaning of equipment are facilitated; the preparation process is completed by feeding reaction, hot filtering, concentration and crystallization at one time, so that the operation is simplified;
the filter assembly of the device is rotatably installed on the installation frame through the connecting rod, is clamped between the upper chuck plate and the lower chuck plate and is sealed and locked through the pin to form a filter, when filter paper needs to be replaced, the pin is only required to be detached, then the sieve plate is rotated out to replace the filter paper, then the sieve plate is rotated to be between the upper chuck plate and the lower chuck plate and is locked through the pin, and the disassembling steps are greatly reduced, so that the filter paper is replaced more conveniently, and meanwhile, the safety of experimenters is protected;
the utility model discloses the charging means that sets up is a device that can feed in raw material many times through the rotation, need not the staff and opens the bottle plug at every turn when carrying out the reaction and weigh reinforced, has improved experimental efficiency greatly, simultaneously because paratoluenesulfonic acid is the noxious material, because the rotatory reinforced mode of this device, can avoid contacting with paratoluenesulfonic acid to provide the experiment guarantee for the experimenter.
Although the embodiments of the present invention and the accompanying drawings are disclosed for illustrative purposes, those skilled in the art will appreciate that: various substitutions, changes and modifications are possible without departing from the spirit and scope of the present invention and the appended claims, and therefore, the scope of the present invention is not limited to the disclosure of the embodiments and the accompanying drawings.
Claims (7)
1. The utility model provides a preparation facilities of copper p-toluenesulfonate which characterized in that: the reactor and the concentrator are both arranged in a split type switchable heating cooling jacket, the reactor is a four-mouth flask, an electric stirrer is arranged at the middle bottle opening, a thermometer is arranged at the left bottle opening, an H-shaped fractionator with a condenser is arranged at the right bottle opening, a feeder is arranged at the rear bottle opening, a discharge pipe with a throttle is arranged at the central part of the bottle bottom of the four-mouth flask, and an upper chuck is coaxially arranged at the lower end of the discharge pipe; the concentrator is a three-mouth flask, a left-side bottle mouth is provided with an emptying throttle, a right-side bottle mouth is connected with a reduced pressure distillation device, a middle bottle mouth is a feeding pipe, the upper end of the middle bottle mouth is coaxially provided with a lower chuck, the center part of the bottle bottom is provided with a discharging pipe with a throttle, and the discharging pipe is connected with a crystallizer; the coaxial mounting has filtering component between the last (holding) chuck of reactor and the lower (holding) chuck of concentrator, filtering component rotates through the connecting rod to be installed on the mounting bracket on one side, just go up (holding) chuck, filtering component and lower (holding) chuck and still seal the locking through the pin and form the suction filter.
2. The apparatus for preparing copper p-toluenesulfonate according to claim 1, wherein: the upper chuck comprises a cover-shaped body, the top of the cover-shaped body is provided with a feeding pipe, the port of the cover-shaped body is a ground port and is tightly connected with a ground port tip at the lower end of a discharging pipe of the reactor, and the bottom of the cover-shaped body is a carefully ground hollow round table.
3. The apparatus for preparing copper p-toluenesulfonate according to claim 1, wherein: the lower chuck comprises a cylinder body, a funnel is coaxially arranged in the cylinder body, a carefully ground hollow circular truncated cone is arranged at the top of the cylinder body, the inner wall of the hollow circular truncated cone is connected with the upper end of the funnel, and a vacuum branch pipe with a throttle is arranged on one side of the cylinder body and is connected with a vacuum system; the bottom of the cylinder body is provided with a grinding tip which is tightly connected with a grinding opening at the upper end of a feeding pipe of the concentrator.
4. The apparatus for preparing copper p-toluenesulfonate according to claim 1, wherein: the filter assembly comprises a sieve plate, the sieve plate is in a round platform structure, and filter paper is arranged on the sieve plate; the upper surfaces of two sides of the sieve plate are also symmetrically provided with inserting holes, the upper surfaces of two sides of the hollow round platform of the upper chuck plate and the upper surface of two sides of the hollow round platform of the lower chuck plate are both provided with pin holes, the inserting holes and the pin holes are coaxially arranged when being installed, and the pin holes are sealed and locked to form a suction filter, so that the suction filtration effect is realized; and a lifting handle is further arranged on one side of the sieve plate.
5. The apparatus for preparing copper p-toluenesulfonate according to claim 1, wherein: the vacuum distillation device comprises a Kjeldahl fractionation head, the lower port of the Kjeldahl fractionation head is communicated and connected with a three-neck flask, the upper pipe orifice on the left side of the Kjeldahl fractionation head is provided with an air inlet capillary with a spiral clamp, and the air inlet capillary is directly communicated with the bottom of the concentrator to adjust the size of inlet air; the thermometer is arranged on the upper pipe orifice of the right side, the liquid outlet of the thermometer is connected with a straight condenser in a communicating way, and the other end of the straight condenser is connected with a solvent receiving bottle in a communicating way through a decompression receiving pipe and is used for collecting the solvent evaporated by decompression concentration.
6. The apparatus for preparing copper p-toluenesulfonate according to claim 1, wherein: the feeder comprises a funnel body, a discharge pipe is coaxially arranged at the bottom end of the funnel body, a ground pin is arranged at the bottom of the discharge pipe, and the ground pin can be tightly connected with a grinding port of a bottle mouth of the four-mouth flask; the top end of the funnel body is provided with a top plate, a rotating cylinder is rotatably mounted on the top plate through a rotating shaft, a plurality of channels are uniformly distributed on the upper surface of the rotating cylinder at intervals along the circumference of the rotating cylinder, one channel is an extension channel, and the top port of the extension channel is sealed by a sealing plug; the other channels are storage channels for storing materials; the top port of the material storage channel is arranged by a sealing turnover cover, and a feed opening is arranged on the upper surface of the top plate corresponding to the position of the extension channel; a rotary handle is arranged on the side wall of the rotary cylinder corresponding to the position of the extension channel; the rotary drum is driven to rotate, so that the feeding in multiple times is realized.
7. The apparatus for preparing copper p-toluenesulfonate according to claim 1, wherein: limiting grooves are formed in the circumferential side wall of the rotary cylinder corresponding to the center of each channel; and a limiting mechanism is further arranged on the side wall of the inner surface of the upper end of the funnel body and comprises a limiting stop block, a spring and a limiting ball, the limiting ball is arranged at one end of the spring and is arranged on two sides of the spring, and the limiting ball is located at one end of the limiting stop block and clamped with a limiting groove of the rotary cylinder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202221627540.9U CN217887996U (en) | 2022-06-28 | 2022-06-28 | Preparation facilities of copper p-toluenesulfonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202221627540.9U CN217887996U (en) | 2022-06-28 | 2022-06-28 | Preparation facilities of copper p-toluenesulfonate |
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| Publication Number | Publication Date |
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| CN217887996U true CN217887996U (en) | 2022-11-25 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202221627540.9U Active CN217887996U (en) | 2022-06-28 | 2022-06-28 | Preparation facilities of copper p-toluenesulfonate |
Country Status (1)
| Country | Link |
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| CN (1) | CN217887996U (en) |
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- 2022-06-28 CN CN202221627540.9U patent/CN217887996U/en active Active
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