CN114507128A - Refining process of p-toluic acid - Google Patents
Refining process of p-toluic acid Download PDFInfo
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- CN114507128A CN114507128A CN202210145586.5A CN202210145586A CN114507128A CN 114507128 A CN114507128 A CN 114507128A CN 202210145586 A CN202210145586 A CN 202210145586A CN 114507128 A CN114507128 A CN 114507128A
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Abstract
The invention relates to the technical field of material refining, in particular to a p-toluic acid refining process, which can conveniently refine a p-toluic acid product generated by catalytic oxidation, improve the purity of the p-toluic acid product and is simple to operate; the method comprises the following steps: s1, centrifugal treatment: adding the acid product into a centrifuge for high-speed centrifugation; s2, filtering: filtering the material after centrifugal treatment; s3, adding a solvent: adding methanol with three times volume of the p-toluic acid product into a centrifuge; s4, refluxing: adding the mixed materials into a reflux device for reflux treatment; s5, cooling and throwing: rapidly cooling the material subjected to the reflux treatment to 20 ℃, and throwing the material; s6, mother liquor recovery: after the material throwing is finished, the temperature is raised to recover the mother liquor in the material, and the recovered mother liquor can be reused; s7, product recovery: and finally, drying the product, grinding the product into powder and collecting the powder.
Description
Technical Field
The invention relates to the technical field of material refining, in particular to a refining process of p-toluic acid.
Background
The p-toluic acid is white or light yellow crystalline powder, the melting point is 179-182 ℃, the boiling point is 274-275 ℃, the p-toluic acid is easily soluble in methanol and ether and is insoluble in hot water and can be volatilized along with water vapor; phthalic acid obtained by oxidation can be used as an intermediate of medicines, photosensitive materials, pesticides and organic pigments, and is mainly used for preparing hemostatic aromatic acid, p-formonitrile, p-toluyl chloride, photosensitive materials and the like.
Disclosure of Invention
In order to solve the technical problems, the invention provides the p-toluic acid refining process which can conveniently refine the p-toluic acid product generated by catalytic oxidation, improve the purity of the p-toluic acid product and is simple to operate.
The invention relates to a refining process of p-toluic acid, which comprises the following steps:
s1, centrifugal treatment: adding the prepared p-toluic acid product into a centrifuge for high-speed centrifugation;
s2, filtering: filtering the material after the centrifugal treatment, filtering out supernatant, and collecting and centralizing precipitates;
s3, adding a solvent: adding methanol with volume being three times that of a p-toluic acid product into a centrifuge, uniformly mixing the methanol and the p-toluic acid product by the centrifuge, and then leading out the mixture;
s4, refluxing: adding the mixed materials into a reflux device for reflux treatment;
s5, cooling and throwing: rapidly cooling the material subjected to the reflux treatment to 20 ℃, and throwing the material;
s6, mother liquor recovery: after the material throwing is finished, the temperature is raised to recover the mother liquor in the material, and the recovered mother liquor can be reused;
s7, product recovery: and finally, drying the product, grinding the product into powder and collecting the powder.
Specifically, the temperature of the reflux treatment is 70-80 ℃, and the time of the reflux treatment is 48-112 min.
Specifically, when the mother liquor is recycled, the temperature of the solution is raised to 95-100 ℃, methanol in the solution is evaporated, and the evaporated methanol can be recycled after being condensed and recycled.
The invention relates to a p-toluic acid refining process, which is based on a backflow device when in recovery treatment, and comprises a heating tank, a heating seat, two groups of fixed shafts, a driving mechanism, a feeding pipe, a discharging pipe and the backflow device, wherein the top of the heating tank is communicated with a discharging port, the backflow device is arranged at the discharging port, the feeding pipe and the discharging pipe are both communicated with the heating tank, two groups of control valves are respectively arranged on the feeding pipe and the discharging pipe, the heating seat is arranged inside the heating tank, the two groups of fixed shafts penetrate through the side wall of the heating tank and are fixedly connected with the heating seat, the contact parts of the two groups of fixed shafts and the heating tank are mechanically sealed, the driving mechanism is arranged in the lower half area of the heating tank, and the driving mechanism is positioned below the heating seat.
Specifically, actuating mechanism includes motor, speed reducer, transmission shaft, roating seat and multiunit rotating fan blade, the motor sets up in speed reducer input end department, the speed reducer sets up on the heating jar outer wall, the transmission shaft is located inside the heating jar to transmission shaft one end is passed the heating jar and is connected with the speed reducer output, transmission shaft and heating jar contact department mechanical seal to the transmission shaft other end and heating jar inner wall rotatable coupling, the roating seat cover is established to the transmission shaft on, multiunit rotating fan blade all installs on the roating seat to roating seat and multiunit rotating fan blade all are located the heating seat below.
Specifically, the return mechanism includes back flow, spiral condenser pipe, inlet tube and outlet pipe, the back flow is installed in discharge gate department, the spiral condenser pipe sets up in the back flow intraduct to spiral condenser pipe both ends communicate with back flow both ends respectively, inlet tube and outlet pipe all communicate with the back flow.
Specifically, still include two sets of communicating pipes, two sets of communicating pipes communicate with charge tube and row material pipe respectively.
Compared with the prior art, the invention has the beneficial effects that: according to the method, the methyl-p-toluic acid product generated by catalytic oxidation is subjected to sufficient reflux refining treatment by using methanol, the reflux temperature and the reflux time are controlled, so that a byproduct in the methyl-p-toluic acid product is separated from the methyl-p-toluic acid, the material is thrown after cooling, the methyl-p-toluic acid is sufficiently dissolved in the methanol, the methanol is evaporated out in a distillation mode, the methyl-p-toluic acid is gradually separated out to obtain a product with higher purity, the purity of the methyl-p-toluic acid product can be effectively improved by using the method, and the product purity reaches 99.5-99.8%, and the method is simple and convenient to operate.
Drawings
FIG. 1 is a schematic view of a reflow apparatus used in the present invention;
FIG. 2 is a partial schematic view of the return mechanism;
FIG. 3 is a partial schematic view of the drive mechanism;
FIG. 4 is a schematic view of the heating base and the stationary shaft in cooperation;
in the drawings, the reference numbers: 1. a heating tank; 2. a heating base; 3. a fixed shaft; 4. a feed tube; 5. a discharge pipe; 6. a control valve; 7. a motor; 8. a speed reducer; 9. a drive shaft; 10. a rotating base; 11. rotating the fan blades; 12. a return pipe; 13. a spiral condenser tube; 14. a water inlet pipe; 15. a water outlet pipe; 16. a communication pipe is provided.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The equipment adopted by the invention comprises a centrifuge, the reflux equipment, a material throwing machine, evaporation recovery equipment and grinding equipment,
the reflux equipment of the invention is shown in figures 1-4, and comprises a heating tank 1, a heating seat 2, two groups of fixed shafts 3, a driving mechanism, a feeding pipe 4, a discharging pipe 5 and a reflux mechanism, wherein the top of the heating tank 1 is communicated with a discharging port, the reflux mechanism is arranged at the discharging port, the reflux mechanism comprises a reflux pipe 12, a spiral condenser pipe 13, a water inlet pipe 14 and a water outlet pipe 15, the reflux pipe 12 is arranged at the discharging port, the spiral condenser pipe 13 is arranged inside the reflux pipe 12, two ends of the spiral condenser pipe 13 are respectively communicated with two ends of the reflux pipe 12, the water inlet pipe 14 and the water outlet pipe 15 are both communicated with the reflux pipe 12, the feeding pipe 4 and the discharging pipe 5 are both communicated with the heating tank 1, two groups of control valves 6 are respectively arranged on the feeding pipe 4 and the discharging pipe 5, and two groups of communicating pipes 16 are respectively communicated with the feeding pipe 4 and the discharging pipe 5, the heating seat 2 is arranged inside the heating tank 1, two groups of fixed shafts 3 penetrate through the side wall of the heating tank 1 and are fixedly connected with the heating seat 2, the contact parts of the two groups of fixed shafts 3 and the heating tank 1 are mechanically sealed, a driving mechanism is arranged in the lower half area of the heating tank 1 and comprises a motor 7, a speed reducer 8, a transmission shaft 9, a rotating seat 10 and a plurality of groups of rotating fan blades 11, the motor 7 is arranged at the input end of the speed reducer 8, the speed reducer 8 is arranged on the outer wall of the heating tank 1, the transmission shaft 9 is positioned inside the heating tank 1, one end of a transmission shaft 9 penetrates through the heating tank 1 and is connected with the output end of the speed reducer 8, the contact part of the transmission shaft 9 and the heating tank 1 is mechanically sealed, and the other end of transmission shaft 9 and 1 inner wall rotatable coupling of heating jar, swivel mount 10 cover are established to transmission shaft 9 on, and multiunit rotating fan blade 11 all installs on swivel mount 10 to swivel mount 10 and multiunit rotating fan blade 11 all are located heating seat 2 below.
Example 1
A refining process of p-toluic acid comprises the following steps:
s1, centrifugal treatment: adding the prepared p-toluic acid product into a centrifuge for high-speed centrifugation;
s2, filtering: filtering the material after centrifugal treatment, filtering out supernatant, and collecting and centralizing the precipitate;
s3, adding a solvent: adding methanol with volume being three times that of a p-toluic acid product into a centrifuge, uniformly mixing the methanol and the p-toluic acid product by the centrifuge, and then leading out the mixture;
s4, refluxing: opening a control valve on a feeding pipe, adding the mixed materials into a backflow device through a communicating pipe and the feeding pipe, closing the control valve, continuously introducing cooling water into the backflow pipe through a water adding pipe, discharging the cooling water through a water outlet pipe after the backflow pipe is filled with the cooling water, leading out a power supply used by a heating seat through a group of fixed shafts, electrifying and starting the heating seat, controlling the heating temperature of the heating seat to be 70-74 ℃, heating the materials in a heating tank through the heating seat, electrifying and starting a motor, reducing the speed of power output by the motor through a speed reducer, driving a transmission shaft to drive a rotary seat and a plurality of groups of rotary fan blades to rotate, driving the materials in the heating tank to circularly flow along the outer surface of the heating seat, improving the heating uniformity, simultaneously playing a role of fully mixing the materials, evaporating the materials in the heating process, entering a spiral condensation pipe, condensing the materials in the spiral condensation pipe through the circulation of the cooling water and returning the materials to the heating tank, carrying out sufficient reflux treatment, wherein the time of the reflux treatment is 48-60 min;
s5, cooling and throwing: rapidly cooling the material subjected to the reflux treatment to 20 ℃, opening a control valve on a discharge pipe, detaching a reflux pipe, leading the material out of reflux equipment, and adding the material into a material throwing machine for throwing;
s6, mother liquor recovery: after the material throwing is finished, adding the solution into evaporation recovery equipment, raising the temperature to 95-100 ℃, evaporating methanol in the solution, condensing and recovering the evaporated methanol, and recycling the methanol for reuse;
s7, product recovery: and finally, drying the product, adding the dried product into grinding equipment, grinding the dried product into powder and collecting the powder.
The method has the advantages that the methyl-p-toluic acid product generated by catalytic oxidation is subjected to sufficient reflux refining treatment by adopting methanol, the reflux temperature and reflux time are controlled, so that a byproduct in the methyl-p-toluic acid product is separated from the methyl-p-toluic acid, the material is thrown after cooling, the methyl-p-toluic acid is sufficiently dissolved in the methanol, the methanol is evaporated out in a distillation mode, the methyl-p-toluic acid is gradually separated out to obtain a product with higher purity, the purity of the methyl-p-toluic acid product can be effectively improved by adopting the method, and the product purity reaches 99.5%, and the method is simple and convenient to operate.
Example 2
A refining process of p-toluic acid comprises the following steps:
s1, centrifugal treatment: adding the prepared p-toluic acid product into a centrifuge for high-speed centrifugation;
s2, filtering: filtering the material after centrifugal treatment, filtering out supernatant, and collecting and centralizing the precipitate;
s3, adding a solvent: adding methanol with volume being three times that of a p-toluic acid product into a centrifuge, uniformly mixing the methanol and the p-toluic acid product by the centrifuge, and then leading out the mixture;
s4, refluxing: opening a control valve on a feeding pipe, adding the mixed materials into a backflow device through a communicating pipe and the feeding pipe, closing the control valve, continuously introducing cooling water into the backflow pipe through a water adding pipe, discharging the cooling water through a water outlet pipe after the backflow pipe is filled with the cooling water, leading out a power supply used by a heating seat through a group of fixed shafts, electrifying and starting the heating seat, controlling the heating temperature of the heating seat to be 70-74 ℃, heating the materials in a heating tank through the heating seat, electrifying and starting a motor, reducing the speed of power output by the motor through a speed reducer, driving a transmission shaft to drive a rotary seat and a plurality of groups of rotary fan blades to rotate, driving the materials in the heating tank to circularly flow along the outer surface of the heating seat, improving the heating uniformity, simultaneously playing a role of fully mixing the materials, evaporating the materials in the heating process, entering a spiral condensation pipe, condensing the materials in the spiral condensation pipe through the circulation of the cooling water and returning the materials to the heating tank, carrying out sufficient reflux treatment, wherein the time of the reflux treatment is 60-80 min;
s5, cooling and throwing: rapidly cooling the material subjected to the reflux treatment to 20 ℃, opening a control valve on a discharge pipe, detaching a reflux pipe, leading the material out of reflux equipment, and adding the material into a material throwing machine for throwing;
s6, mother liquor recovery: after the material throwing is finished, adding the solution into evaporation recovery equipment, raising the temperature to 95-100 ℃, evaporating methanol in the solution, condensing and recovering the evaporated methanol, and recycling the methanol for reuse;
s7, product recovery: and finally, drying the product, adding the dried product into grinding equipment, grinding the dried product into powder and collecting the powder.
The method has the advantages that the methyl-p-toluic acid product generated by catalytic oxidation is subjected to sufficient reflux refining treatment by adopting methanol, the reflux temperature and reflux time are controlled, so that a byproduct in the methyl-p-toluic acid product is separated from the methyl-p-toluic acid, the material is thrown after cooling, the methyl-p-toluic acid is sufficiently dissolved in the methanol, the methanol is evaporated out in a distillation mode, the methyl-p-toluic acid is gradually separated out to obtain a product with higher purity, the purity of the methyl-p-toluic acid product can be effectively improved by adopting the method, and the product purity reaches 99.5%, and the method is simple and convenient to operate.
Example 3
A refining process of p-toluic acid comprises the following steps:
s1, centrifugal treatment: adding the prepared p-toluic acid product into a centrifuge for high-speed centrifugation;
s2, filtering: filtering the material after centrifugal treatment, filtering out supernatant, and collecting and centralizing the precipitate;
s3, adding a solvent: adding methanol with volume being three times that of a p-toluic acid product into a centrifuge, uniformly mixing the methanol and the p-toluic acid product by the centrifuge, and then leading out the mixture;
s4, refluxing: opening a control valve on a feeding pipe, adding the mixed materials into a backflow device through a communicating pipe and the feeding pipe, closing the control valve, continuously introducing cooling water into the backflow pipe through a water adding pipe, discharging the cooling water through a water outlet pipe after the backflow pipe is filled with the cooling water, leading out a power supply used by a heating seat through a group of fixed shafts, electrifying and starting the heating seat, controlling the heating temperature of the heating seat to be 70-74 ℃, heating the materials in a heating tank through the heating seat, electrifying and starting a motor, reducing the speed of power output by the motor through a speed reducer, driving a transmission shaft to drive a rotary seat and a plurality of groups of rotary fan blades to rotate, driving the materials in the heating tank to circularly flow along the outer surface of the heating seat, improving the heating uniformity, simultaneously playing a role of fully mixing the materials, evaporating the materials in the heating process, entering a spiral condensation pipe, condensing the materials in the spiral condensation pipe through the circulation of the cooling water and returning the materials to the heating tank, carrying out sufficient reflux treatment, wherein the time of the reflux treatment is 80-100 min;
s5, cooling and throwing: rapidly cooling the material subjected to the reflux treatment to 20 ℃, opening a control valve on a discharge pipe, detaching a reflux pipe, leading the material out of reflux equipment, and adding the material into a material throwing machine for throwing;
s6, mother liquor recovery: after the material throwing is finished, adding the solution into evaporation recovery equipment, raising the temperature to 95-100 ℃, evaporating methanol in the solution, condensing and recovering the evaporated methanol, and recycling the methanol for reuse;
s7, product recovery: and finally, drying the product, adding the dried product into grinding equipment, grinding the dried product into powder and collecting the powder.
The method has the advantages that the methyl-p-toluic acid product generated by catalytic oxidation is subjected to sufficient reflux refining treatment by adopting methanol, the reflux temperature and reflux time are controlled, so that a byproduct in the methyl-p-toluic acid product is separated from the methyl-p-toluic acid, the material is thrown after cooling, the methyl-p-toluic acid is sufficiently dissolved in the methanol, the methanol is evaporated out in a distillation mode, the methyl-p-toluic acid is gradually separated out to obtain a product with higher purity, the purity of the methyl-p-toluic acid product can be effectively improved by adopting the method, and the product purity reaches 99.8%, and the method is simple and convenient to operate.
Example 4
A refining process of p-toluic acid comprises the following steps:
s1, centrifugal treatment: adding the prepared p-toluic acid product into a centrifuge for high-speed centrifugation;
s2, filtering: filtering the material after centrifugal treatment, filtering out supernatant, and collecting and centralizing the precipitate;
s3, adding a solvent: adding methanol with volume being three times that of a p-toluic acid product into a centrifuge, uniformly mixing the methanol and the p-toluic acid product by the centrifuge, and then leading out the mixture;
s4, refluxing: opening a control valve on a feeding pipe, adding the mixed materials into a backflow device through a communicating pipe and the feeding pipe, closing the control valve, continuously introducing cooling water into the backflow pipe through a water adding pipe, discharging the cooling water through a water outlet pipe after the backflow pipe is filled with the cooling water, leading out a power supply used by a heating seat through a group of fixed shafts, electrifying and starting the heating seat, controlling the heating temperature of the heating seat to be 70-74 ℃, heating the materials in a heating tank through the heating seat, electrifying and starting a motor, reducing the speed of power output by the motor through a speed reducer, driving a transmission shaft to drive a rotary seat and a plurality of groups of rotary fan blades to rotate, driving the materials in the heating tank to circularly flow along the outer surface of the heating seat, improving the heating uniformity, simultaneously playing a role of fully mixing the materials, evaporating the materials in the heating process, entering a spiral condensation pipe, condensing the materials in the spiral condensation pipe through the circulation of the cooling water and returning the materials to the heating tank, carrying out sufficient reflux treatment, wherein the time of the reflux treatment is 100-112 min;
s5, cooling and throwing: rapidly cooling the material subjected to the reflux treatment to 20 ℃, opening a control valve on a discharge pipe, detaching a reflux pipe, leading the material out of reflux equipment, and adding the material into a material throwing machine for throwing;
s6, mother liquor recovery: after the material throwing is finished, adding the solution into evaporation recovery equipment, raising the temperature to 95-100 ℃, evaporating methanol in the solution, condensing and recovering the evaporated methanol, and recycling the methanol for reuse;
s7, product recovery: and finally, drying the product, adding the dried product into grinding equipment, grinding the dried product into powder and collecting the powder.
The method has the advantages that the methyl-p-toluic acid product generated by catalytic oxidation is subjected to sufficient reflux refining treatment by adopting methanol, the reflux temperature and reflux time are controlled, so that a byproduct in the methyl-p-toluic acid product is separated from the methyl-p-toluic acid, the material is thrown after cooling, the methyl-p-toluic acid is sufficiently dissolved in the methanol, the methanol is evaporated out in a distillation mode, the methyl-p-toluic acid is gradually separated out to obtain a product with higher purity, the purity of the methyl-p-toluic acid product can be effectively improved by adopting the method, and the product purity reaches 99.8%, and the method is simple and convenient to operate.
Example 5
A refining process of p-toluic acid comprises the following steps:
s1, centrifugal treatment: adding the prepared p-toluic acid product into a centrifuge for high-speed centrifugation;
s2, filtering: filtering the material after centrifugal treatment, filtering out supernatant, and collecting and centralizing the precipitate;
s3, adding a solvent: adding methanol with three times volume of the p-toluic acid product into a centrifuge, uniformly mixing the methanol and the p-toluic acid product by the centrifuge, and then leading out the mixture;
s4, refluxing: opening a control valve on a feeding pipe, adding the mixed materials into a backflow device through a communicating pipe and the feeding pipe, closing the control valve, continuously introducing cooling water into the backflow pipe through a water feeding pipe, discharging the cooling water through a water outlet pipe after the backflow pipe is filled with the cooling water, leading out a power supply used by a heating seat through a group of fixed shafts, electrifying and starting the heating seat, controlling the heating temperature of the heating seat to be 74-77 ℃, heating the materials in a heating tank through the heating seat, electrifying and starting a motor, reducing the speed of power output by the motor through a speed reducer, driving a transmission shaft to drive a rotary seat and a plurality of groups of rotary fan blades to rotate, driving the materials in the heating tank to circularly flow along the outer surface of the heating seat, improving the heating uniformity, simultaneously playing a role of fully mixing the materials, evaporating the materials in the heating process, entering a spiral condensation pipe, condensing the materials in the spiral condensation pipe through the circulation of the cooling water and returning the materials to the heating tank, carrying out sufficient reflux treatment, wherein the time of the reflux treatment is 80-100 min;
s5, cooling and throwing: rapidly cooling the material subjected to the reflux treatment to 20 ℃, opening a control valve on a discharge pipe, detaching a reflux pipe, leading the material out of reflux equipment, and adding the material into a material throwing machine for throwing;
s6, mother liquor recovery: after the material throwing is finished, adding the solution into evaporation recovery equipment, raising the temperature to 95-100 ℃, evaporating methanol out, condensing and recovering the evaporated methanol, and recycling the methanol for reuse;
s7, product recovery: and finally, drying the product, adding the dried product into grinding equipment, grinding the dried product into powder and collecting the powder.
The method has the advantages that the methyl-p-toluic acid product generated by catalytic oxidation is subjected to sufficient reflux refining treatment by adopting methanol, the reflux temperature and reflux time are controlled, so that a byproduct in the methyl-p-toluic acid product is separated from the methyl-p-toluic acid, the material is thrown after cooling, the methyl-p-toluic acid is sufficiently dissolved in the methanol, the methanol is evaporated out in a distillation mode, the methyl-p-toluic acid is gradually separated out to obtain a product with higher purity, the purity of the methyl-p-toluic acid product can be effectively improved by adopting the method, and the product purity reaches 99.6%, and the method is simple and convenient to operate.
Example 6
A refining process of p-toluic acid comprises the following steps:
s1, centrifugal treatment: adding the prepared p-toluic acid product into a centrifuge for high-speed centrifugation;
s2, filtering: filtering the material after centrifugal treatment, filtering out supernatant, and collecting and centralizing the precipitate;
s3, adding a solvent: adding methanol with volume being three times that of a p-toluic acid product into a centrifuge, uniformly mixing the methanol and the p-toluic acid product by the centrifuge, and then leading out the mixture;
s4, refluxing: opening a control valve on a feeding pipe, adding the mixed materials into a backflow device through a communicating pipe and the feeding pipe, closing the control valve, continuously introducing cooling water into the backflow pipe through a water adding pipe, discharging the cooling water through a water outlet pipe after the backflow pipe is filled with the cooling water, leading out a power supply used by a heating seat through a group of fixed shafts, electrifying and starting the heating seat, controlling the heating temperature of the heating seat to be 77-80 ℃, heating the materials in a heating tank through the heating seat, electrifying and starting a motor, reducing the speed of power output by the motor through a speed reducer, driving a transmission shaft to drive a rotary seat and a plurality of groups of rotary fan blades to rotate, driving the materials in the heating tank to circularly flow along the outer surface of the heating seat, improving the heating uniformity, simultaneously playing a role of fully mixing the materials, evaporating the materials in the heating process, entering a spiral condensation pipe, condensing the materials in the spiral condensation pipe through the circulation of the cooling water and returning the materials to the heating tank, carrying out sufficient reflux treatment, wherein the time of the reflux treatment is 80-100 min;
s5, cooling and throwing: rapidly cooling the material subjected to the reflux treatment to 20 ℃, opening a control valve on a discharge pipe, detaching a reflux pipe, leading the material out of reflux equipment, and adding the material into a material throwing machine for throwing;
s6, mother liquor recovery: after the material throwing is finished, adding the solution into evaporation recovery equipment, raising the temperature to 95-100 ℃, evaporating methanol in the solution, condensing and recovering the evaporated methanol, and recycling the methanol for reuse;
s7, product recovery: and finally, drying the product, adding the dried product into grinding equipment, grinding the dried product into powder and collecting the powder.
The method has the advantages that the methyl-p-toluic acid product generated by catalytic oxidation is subjected to sufficient reflux refining treatment by adopting methanol, the reflux temperature and reflux time are controlled, so that a byproduct in the methyl-p-toluic acid product is separated from the methyl-p-toluic acid, the material is thrown after cooling, the methyl-p-toluic acid is sufficiently dissolved in the methanol, the methanol is evaporated out in a distillation mode, the methyl-p-toluic acid is gradually separated out to obtain a product with higher purity, the purity of the methyl-p-toluic acid product can be effectively improved by adopting the method, and the product purity reaches 99.7%, and the method is simple and convenient to operate.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A p-toluic acid refining process is characterized by comprising the following steps:
s1, centrifugal treatment: adding the prepared p-toluic acid product into a centrifuge for high-speed centrifugation;
s2, filtering: filtering the material after centrifugal treatment, filtering out supernatant, and collecting and centralizing the precipitate;
s3, adding a solvent: adding methanol with volume being three times that of a p-toluic acid product into a centrifuge, uniformly mixing the methanol and the p-toluic acid product by the centrifuge, and then leading out the mixture;
s4, refluxing: adding the mixed materials into a reflux device for reflux treatment;
s5, cooling and throwing: rapidly cooling the material subjected to the reflux treatment to 20 ℃, and throwing the material;
s6, mother liquor recovery: after the material throwing is finished, the temperature is raised to recover the mother liquor in the material, and the recovered mother liquor can be reused;
s7, product recovery: and finally, drying the product, grinding the product into powder and collecting the powder.
2. The refining process of p-toluic acid according to claim 1, wherein the temperature of the reflux treatment is 70 to 80 ℃, and the time of the reflux treatment is 48 to 112 min.
3. The process for refining p-toluic acid according to claim 1, wherein the mother liquor is recovered by raising the temperature of the mother liquor to 95 to 100 ℃ and evaporating methanol therefrom, and the evaporated methanol is condensed and recovered for reuse.
4. The refining process of p-toluic acid according to claim 1, wherein, in the recycling treatment, the recycling treatment is carried out based on a recycling apparatus comprising a heating tank (1), a heating base (2), two sets of fixed shafts (3), a driving mechanism, a feeding pipe (4), a discharging pipe (5) and a recycling mechanism, wherein a discharge port is arranged at the top of the heating tank (1) in a communicating manner, the recycling mechanism is arranged at the discharge port, the feeding pipe (4) and the discharging pipe (5) are both communicated with the heating tank (1), two sets of control valves (6) are respectively arranged on the feeding pipe (4) and the discharging pipe (5), the heating base (2) is arranged inside the heating tank (1), the two sets of fixed shafts (3) both penetrate through the side wall of the heating tank (1) and are fixedly connected with the heating base (2), and the contact part of the two sets of fixed shafts (3) and the heating tank (1) is mechanically sealed, the driving mechanism is arranged in the lower half area of the heating tank (1) and is positioned below the heating seat (2).
5. The refining process of p-toluic acid according to claim 4, wherein the driving mechanism comprises a motor (7), a speed reducer (8), a transmission shaft (9), a rotating base (10) and a plurality of sets of rotating fan blades (11), the motor (7) is arranged at the input end of the speed reducer (8), the speed reducer (8) is arranged on the outer wall of the heating tank (1), the transmission shaft (9) is positioned inside the heating tank (1), one end of a transmission shaft (9) penetrates through the heating tank (1) and is connected with the output end of the speed reducer (8), the contact part of the transmission shaft (9) and the heating tank (1) is mechanically sealed, and the other end of the transmission shaft (9) is rotatably connected with the inner wall of the heating tank (1), the rotating base (10) is sleeved on the transmission shaft (9), the plurality of groups of rotating fan blades (11) are all arranged on the rotating base (10), and the rotating base (10) and the multiple groups of rotating fan blades (11) are both positioned below the heating base (2).
6. The refining process of p-toluic acid according to claim 4, wherein the reflux mechanism comprises a reflux pipe (12), a spiral condenser pipe (13), a water inlet pipe (14) and a water outlet pipe (15), the reflux pipe (12) is installed at the water outlet, the spiral condenser pipe (13) is arranged inside the reflux pipe (12), two ends of the spiral condenser pipe (13) are respectively communicated with two ends of the reflux pipe (12), and the water inlet pipe (14) and the water outlet pipe (15) are both communicated with the reflux pipe (12).
7. The refining process of p-toluic acid according to claim 4, further comprising two sets of communicating tubes (16), said two sets of communicating tubes (16) being communicated with the feed pipe (4) and the discharge pipe (5), respectively.
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