CN112029805A - Preparation method of phloroglucinol - Google Patents
Preparation method of phloroglucinol Download PDFInfo
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- CN112029805A CN112029805A CN202010757279.3A CN202010757279A CN112029805A CN 112029805 A CN112029805 A CN 112029805A CN 202010757279 A CN202010757279 A CN 202010757279A CN 112029805 A CN112029805 A CN 112029805A
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Abstract
The invention discloses a preparation method of phloroglucinol, which relates to the technical field of phloroglucinol processing and aims at solving the problem of higher preparation cost of the existing phloroglucinol. The invention can simply and conveniently prepare the phloroglucinol, has simple raw material acquisition, lower production cost and more convenient operation, can improve the purity of the phloroglucinol and the production speed of the phloroglucinol, and has simple and reasonable structure and convenient use.
Description
Technical Field
The invention relates to the technical field of phloroglucinol processing, in particular to a preparation method of phloroglucinol.
Background
Phloroglucinol is white or light yellow crystal or crystalline powder, is anhydrous at 110 ℃, is dissolved in 100 parts of water, 10 parts of ethanol and 0.5 part of pyridine, is dissolved in ether, is partially decomposed during sublimation, and is discolored by light.
The existing phloroglucinol is generally prepared by taking TNT or benzene halide as a raw material through amination and hydrolysis, such as a halophenyl amination method, and taking halophenyl or aminobenzene as a raw material, so that the price is high, the raw material source is difficult, production equipment is required to be used, the use is inconvenient, and the preparation cost is high.
Disclosure of Invention
The preparation method of phloroglucinol provided by the invention solves the problem of higher preparation cost of phloroglucinol.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of phloroglucinol comprises a preparation assembly line, wherein the preparation assembly line comprises crushing equipment, microwave processing equipment, distillation equipment, extraction equipment and fermentation equipment, a feeding hopper is installed at the top of the crushing equipment, a crushing part is installed inside the crushing equipment, a liquid outlet pipe is installed at the bottom of the crushing equipment, a receiving container is arranged on one side of the crushing equipment, the receiving container and the liquid outlet pipe work in a matched mode, a filter screen is fixed inside the crushing equipment, the filter screen is located between the crushing part and the liquid outlet pipe, and a stirring part is arranged inside the fermentation equipment;
the preparation method of the phloroglucinol also comprises the following purification steps:
s1, pouring the cleaned brown algae into a feeding hopper, conveying the brown algae to the inside of crushing equipment through the feeding hopper, crushing the brown algae by a crushing component in the crushing equipment, filtering the brown algae residues by a filter screen through a brown algae extracting solution subjected to crushing treatment, and collecting the brown algae extracting solution through a receiving container through a liquid outlet pipe;
s2, placing the brown algae extracting solution extracted in the crushing device 1 in the S1 step into a microwave processing device 2, adding a sodium bicarbonate solution, performing microwave extraction for one hour at 50 ℃, centrifuging the liquid after extraction treatment, and collecting the supernatant after treatment;
s3, placing the filtrate obtained in the step S2 into a distillation device 3, wherein the filtrate can be evaporated by the distillation device 3, and when the filtrate in the distillation device 3 is one ninth of the original volume, the obtained filtrate can be collected;
s4, placing the filtrate obtained in the step S3 into extraction equipment 4, adding a chloroform solution with the volume 12 times that of the filtrate, extracting the mixed solution by the extraction equipment 4, and collecting the extract extracted by the extraction equipment 4;
s5, placing the extract obtained in the step S4 into an extraction device 4, and evaporating the extract by a distillation device 3 to obtain the brown algae polyphenol extract;
s6, placing the brown algae polyphenol extract obtained in the step S5 into a fermentation device 5, injecting water with 8 times of the amount of the brown algae polyphenol extract into the fermentation device 5, adding aspergillus into the fermentation device 5, fermenting the materials in the fermentation device 5 through the aspergillus, and stirring the materials in the fermentation device 5 through a stirring part arranged in the fermentation device 5 to improve the fermentation rate of the materials in the fermentation device 5;
s7, when the fermentation of the materials in the fermentation equipment 5 is finished, collecting the fermentation extract, adjusting the pH of the collected fermentation extract, and when the pH of the fermentation extract is 5-5.5, obtaining the extract containing the phloroglucinol monomer;
s8, placing the extracting solution containing the phloroglucinol monomer obtained in the step S7 into a distillation device 3, evaporating the extracting solution by the distillation device 3, heating the extracting solution in the distillation device 3 to 331 ℃, collecting the evaporated liquid, and obtaining phloroglucinol liquid.
Preferably, the crushing component comprises a rotating block, a driving motor, a rotating shaft, a pushing block, a hydraulic cylinder and a grinding block, the rotating block is rotatably connected inside the crushing equipment, the driving motor is fixed on one side outside the crushing equipment, the rotating shaft is in transmission connection with the output end of the driving motor, one end, far away from the driving motor, of the rotating shaft is rotatably connected to one side, close to the driving motor, of the rotating block through a bearing, the pushing block is located on one side, far away from the driving motor, of the rotating block, the pushing block is in sliding connection with the inner wall of the crushing equipment, the hydraulic cylinder is fixed on the inner walls of two ends of the right side of the crushing equipment, the piston end of the hydraulic cylinder is fixed on one side, far away from the rotating block, of the grinding block is fixed on the opposite side of the rotating block and the pushing block, and the plurality, the output end of the feeding hopper is positioned between the rotating block and the pushing block.
Preferably, the stirring part includes step motor, axis of rotation and puddler, step motor fix with screw is in the outside one side of fermentation equipment, the axis of rotation transmission is connected on step motor's output, step motor's one end is kept away from to the axis of rotation is passed through the bearing and is rotated the connection on the left inner wall of fermentation equipment, the puddler is fixed in the axis of rotation both sides that are located fermentation equipment inside to be equipped with a plurality ofly, the puddler rotates the cover and establishes the inside at fermentation equipment.
Preferably, the bottom on fermentation equipment right side is installed the discharge pipe, install the butterfly valve on the discharge pipe.
Preferably, a rotary groove is formed in the left side of the crushing device, and the rotary shaft is rotatably connected to the inside of the rotary groove.
Preferably, a rotating groove is formed in the right side of the fermentation equipment, and the rotating shaft is rotatably connected to the inside of the rotating groove.
In the invention:
1. through the cooperation work of crushing equipment, microwave processing equipment, distillation plant, extraction equipment, fermentation equipment, magazine, filter screen, drain pipe and receptacle, simple and convenient prepares phloroglucinol, and raw and other materials acquire simply, and manufacturing cost is less, and the operation is comparatively convenient.
2. The turning block, driving motor, the apparatus further comprises a rotating shaft, promote the piece, the pneumatic cylinder, the abrasive brick, step motor, the axis of rotation, the puddler, the cooperation work of discharge pipe and butterfly valve, but high efficiency carries out crushing treatment to phloroglucinol's raw materials, and can filter crushing treatment's raw materials extract, thereby improve phloroglucinol's purity, and can carry out effectual stirring treatment to phloroglucinol's raw materials, thereby improve the fermentation rate of phloroglucinol raw materials, then improve phloroglucinol's production speed, high working property.
Drawings
Fig. 1 is a schematic structural diagram of a phloroglucinol preparation method provided by the invention.
Reference numbers in the figures: 1. a crushing device; 2. microwave processing equipment; 3. a distillation apparatus; 4. extraction equipment; 5. a fermentation device; 6. a feeding hopper; 7. rotating the block; 8. a drive motor; 9. a rotating shaft; 10. a pushing block; 11. a hydraulic cylinder; 12. grinding blocks; 13. a filter screen; 14. a liquid outlet pipe; 15. a container; 16. a stepping motor; 17. a rotating shaft; 18. a stirring rod; 19. a discharge pipe; 20. butterfly valves.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1, a phloroglucinol preparation method comprises a preparation assembly line, wherein the preparation assembly line comprises a crushing device 1, a microwave processing device 2, a distillation device 3, an extraction device 4 and a fermentation device 5, a feeding hopper 6 is installed at the top of the crushing device 1, a crushing part is installed inside the crushing device 1, a liquid outlet pipe 14 is installed at the bottom of the crushing device 1, a receiving container 15 is arranged on one side of the crushing device 1, the receiving container 15 and the liquid outlet pipe 14 work in a matched mode, a filter screen 13 is fixed inside the crushing device 1, the filter screen 13 is located between the crushing part and the liquid outlet pipe 14, and a stirring part is arranged inside the fermentation device 5.
The crushing part comprises a rotating block 7, a driving motor 8, a rotating shaft 9, a pushing block 10, a hydraulic cylinder 11 and a grinding block 12, wherein the rotating block 7 is rotatably connected inside the crushing device 1, the driving motor 8 is fixed on one side outside the crushing device 1, the rotating shaft 9 is in transmission connection with the output end of the driving motor 8, one end of the rotating shaft 9 far away from the driving motor 8 is rotatably connected on one side of the rotating block 7 close to the driving motor 8 through a bearing, the pushing block 10 is positioned on one side of the rotating block 7 far away from the driving motor 8, the pushing block 10 is in sliding connection with the inner wall of the crushing device 1, the hydraulic cylinder 11 is fixed on the inner walls of two ends of the right side of the crushing device 1, the piston end of the hydraulic cylinder 11 is fixed on one side of the pushing block 10 far away from the rotating block 7, the grinding block 12 is fixed on the opposite sides of the rotating block 7 and the pushing block 10 and, the output end of the feeding hopper 6 is positioned between the rotating block 7 and the pushing block 10.
Stirring part includes step motor 16, axis of rotation 17 and puddler 18, step motor 16 fix with screw is in the outside one side of fermentation equipment 5, the transmission of axis of rotation 17 is connected on step motor 16's output, the one end that step motor 16 was kept away from to axis of rotation 17 is passed through the bearing and is rotated the connection on the left inner wall of fermentation equipment 5, puddler 18 is fixed and is located the inside axis of rotation 17 both sides of fermentation equipment 5, and be equipped with a plurality ofly, puddler 18 rotates the cover and establishes the inside at fermentation equipment 5, discharge pipe 19 is installed to the bottom on fermentation equipment 5 right side, install butterfly valve 20 on the discharge pipe 19, through discharge pipe 19, can discharge fermentation equipment's extract.
The rotary groove has been seted up on crushing equipment 1's left side, and pivot 9 rotates to be connected in the inside of rotary groove, and through the rotary groove, pivot 9 can carry out nimble rotation.
The right side of fermentation equipment 5 has been seted up and has been rotated the groove, and axis of rotation 17 rotates to be connected in the inside that rotates the groove, and through rotating the groove, axis of rotation 17 can carry out nimble rotation.
The preparation method of the phloroglucinol also comprises the following purification steps:
s1, pouring the cleaned brown algae into the feeding hopper 6, conveying the brown algae to the inside of the crushing equipment 1 through the feeding hopper 6, crushing the brown algae through a crushing component in the crushing equipment 1, filtering the brown algae residues through the filter screen 13, and collecting the brown algae extract through the receiving container 15, wherein the brown algae extract is filtered through the liquid outlet pipe 14 and enters the receiving container 15;
s2, placing the brown algae extracting solution extracted in the crushing device 1 in the S1 step into a microwave processing device 2, adding a sodium bicarbonate solution, performing microwave extraction for one hour at 50 ℃, centrifuging the liquid after extraction treatment, and collecting the supernatant after treatment;
s3, placing the filtrate obtained in the step S2 into a distillation device 3, wherein the filtrate can be evaporated by the distillation device 3, and when the filtrate in the distillation device 3 is one ninth of the original volume, the obtained filtrate can be collected;
s4, placing the filtrate obtained in the step S3 into extraction equipment 4, adding a chloroform solution with the volume 12 times that of the filtrate, extracting the mixed solution by the extraction equipment 4, and collecting the extract extracted by the extraction equipment 4;
s5, placing the extract obtained in the step S4 into an extraction device 4, and evaporating the extract by a distillation device 3 to obtain the brown algae polyphenol extract;
s6, placing the brown algae polyphenol extract obtained in the step S5 into a fermentation device 5, injecting water with 8 times of the amount of the brown algae polyphenol extract into the fermentation device 5, adding aspergillus into the fermentation device 5, fermenting the materials in the fermentation device 5 through the aspergillus, and stirring the materials in the fermentation device 5 through a stirring part arranged in the fermentation device 5 to improve the fermentation rate of the materials in the fermentation device 5;
s7, when the fermentation of the materials in the fermentation equipment 5 is finished, collecting the fermentation extract, adjusting the pH of the collected fermentation extract, and when the pH of the fermentation extract is 5-5.5, obtaining the extract containing the phloroglucinol monomer;
s8, placing the extracting solution containing the phloroglucinol monomer obtained in the step S7 into a distillation device 3, evaporating the extracting solution by the distillation device 3, heating the extracting solution in the distillation device 3 to 331 ℃, collecting the evaporated liquid, and obtaining phloroglucinol liquid.
The working principle is as follows: when phloroglucinol needs to be prepared, clean brown algae can be poured into the feeding hopper 6 at the moment, the brown algae is conveyed to the inside of the crushing equipment 1 through the feeding hopper 6, when the brown algae is positioned between the rotating block 7 and the pushing block 10, the rotating shaft 9 is driven to rotate through the operation of the driving motor 8 at the moment, the rotating block 7 is driven to rotate, the grinding block 12 on the rotating block 7 is driven to rotate, meanwhile, the pushing block 10 can be driven to horizontally displace through the operation of the hydraulic cylinder 11, the brown algae can be pushed to horizontally displace through the pushing block 10 which horizontally displaces at the moment, when the brown algae is contacted with the rotating block 7, the effective crushing treatment can be carried out on the brown algae through the grinding block 12 at the moment, the crushed brown algae can fall on the filter screen 13 at the moment, the brown algae extracting solution which is crushed can pass through the filter screen 13, and the brown algae residues are filtered through the filter screen 13, the filtered brown algae extract enters the receiving container 15 through the liquid outlet pipe 14, the brown algae extract is collected through the receiving container 15, the brown algae extract can be placed in the microwave processing equipment 2, a sodium bicarbonate solution can be added, microwave extraction is carried out for one hour at 50 ℃, the liquid after extraction treatment is centrifuged, the treated supernatant is collected, the filtrate can be placed in the distillation equipment 3, the filtrate can be evaporated through the distillation equipment 3, the obtained filtrate can be collected when the filtrate in the distillation equipment 3 is one ninth of the original volume, the obtained filtrate can be placed in the extraction equipment 4, a chloroform solution with the volume being 12 times of the filtrate can be added, the mixed solution can be extracted through the extraction equipment 4, and then the extracted liquid of the extraction equipment 4 is collected, at this time, the obtained extract can be placed into the extraction equipment 4, at this time, the extract can be subjected to evaporation treatment by the distillation equipment 3, at this time, a brown algae polyphenol extract can be obtained, at this time, the obtained brown algae polyphenol extract can be placed into the fermentation equipment 5, at this time, water with the amount 8 times that of the brown algae polyphenol extract can be injected into the fermentation equipment 5, at this time, aspergillus is added into the fermentation equipment 5, at this time, the material in the fermentation equipment 5 can be subjected to fermentation treatment by the aspergillus, at the same time, the rotating shaft 17 can be driven to rotate by the operation of the stepping motor 16, at this time, the stirring rod 18 can be driven to rotate by the rotating shaft 17, at this time, the material in the fermentation equipment 5 can be subjected to stirring treatment by the rotating stirring rod 18, so that the fermentation rate of the material in the fermentation equipment 5 can be effectively improved, after the, at this time, the user can open the butterfly valve 20, the fermentation liquid in the fermentation equipment 5 can be discharged through the discharge pipe 19 at this time, the fermentation extracting solution can be collected at this time, the PH of the collected fermentation extracting solution can be adjusted at this time, when the PH of the fermentation extracting solution is 5-5.5, the extracting solution containing the phloroglucinol monomer can be obtained at this time, the obtained extracting solution containing the phloroglucinol monomer can be placed in the distillation equipment 3, the extracting solution can be evaporated through the distillation equipment 3 at this time, the extracting solution in the distillation equipment 3 is heated to 331 ℃, the evaporated liquid can be collected at this time, and the phloroglucinol liquid can be obtained at this time.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations and positional relationships based on those shown in the drawings, and are used only for convenience of description and simplicity of description, and do not indicate or imply that the equipment or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be considered as limiting the present invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (6)
1. The preparation method of phloroglucinol comprises a preparation production line and is characterized in that the preparation production line comprises a crushing device (1), a microwave processing device (2), a distillation device (3), an extraction device (4) and a fermentation device (5), a feeding hopper (6) is installed at the top of the crushing device (1), a crushing part is installed inside the crushing device (1), a liquid outlet pipe (14) is installed at the bottom of the crushing device (1), a receiving container (15) is arranged on one side of the crushing device (1), the receiving container (15) and the liquid outlet pipe (14) work in a matched mode, a filter screen (13) is fixed inside the crushing device (1), the filter screen (13) is located between the crushing part and the liquid outlet pipe (14), and a stirring part is arranged inside the fermentation device (5);
the preparation method of the phloroglucinol also comprises the following purification steps:
s1, pour the inside of hopper (6) into the brown algae of sanitization, carry the inside to crushing equipment (1) through hopper (6) with the brown algae, the crushing unit of accessible crushing equipment (1) inside carries out crushing treatment to the brown algae this moment, the brown algae extract by crushing treatment will pass through filter screen (13) this moment, filter the brown algae residue through filter screen (13), the inside that the filtered brown algae extract will enter into receiving container (15) through drain pipe (14) this moment, collect the brown algae extract through receiving container (15);
s2, placing the brown algae extracting solution extracted in the crushing device (1) in the S1 step into a microwave processing device (2), adding a sodium bicarbonate solution, performing microwave extraction for one hour at 50 ℃, centrifuging the liquid after extraction treatment, and collecting the supernatant after treatment;
s3, placing the filtrate obtained in the step S2 into distillation equipment (3), evaporating the filtrate by the distillation equipment (3), and collecting the obtained filtrate when the filtrate in the distillation equipment (3) is one ninth of the original volume;
s4, placing the filtrate obtained in the step S3 into extraction equipment (4), adding a chloroform solution with the volume 12 times that of the filtrate, extracting the mixed solution through the extraction equipment (4), and collecting the extract extracted by the extraction equipment (4);
s5, placing the extract obtained in the step S4 into extraction equipment (4), and evaporating the extract by distillation equipment (3) to obtain a brown algae polyphenol extract;
s6, placing the brown algae polyphenol extract obtained in the step S5 into a fermentation device (5), injecting water with 8 times of the amount of the brown algae polyphenol extract into the fermentation device (5), adding aspergillus into the fermentation device (5), fermenting the material in the fermentation device (5) through the aspergillus, and stirring the material in the fermentation device (5) through a stirring part arranged in the fermentation device (5) to improve the fermentation rate of the material in the fermentation device (5);
s7, when the fermentation of the materials in the fermentation equipment (5) is finished, collecting the fermentation extract, adjusting the pH of the collected fermentation extract, and when the pH of the fermentation extract is 5-5.5, obtaining the extract containing the phloroglucinol monomer;
s8, placing the extracting solution containing the phloroglucinol monomer obtained in the step S7 into a distillation device (3), evaporating the extracting solution through the distillation device (3), heating the extracting solution in the distillation device (3) to 331 ℃, collecting the evaporated liquid, and obtaining phloroglucinol liquid.
2. The phloroglucinol preparation method according to claim 1, characterized in that the crushing component comprises a rotating block (7), a driving motor (8), a rotating shaft (9), a pushing block (10), a hydraulic cylinder (11) and a grinding block (12), the rotating block (7) is rotatably connected inside the crushing device (1), the driving motor (8) is fixed on one side of the outside of the crushing device (1), the rotating shaft (9) is in transmission connection with the output end of the driving motor (8), one end of the rotating shaft (9) far away from the driving motor (8) is rotatably connected on one side of the rotating block (7) close to the driving motor (8) through a bearing, the pushing block (10) is positioned on one side of the rotating block (7) far away from the driving motor (8), the pushing block (10) is in sliding connection with the inner wall of the crushing device (1), and the hydraulic cylinder (11) is fixed on the inner walls of the two ends of the right side of the crushing device (1), the piston end of the hydraulic cylinder (11) is fixed on one side, far away from the rotating block (7), of the pushing block (10), the grinding blocks (12) are fixed on the opposite sides of the rotating block (7) and the pushing block (10) and are provided in a plurality, the grinding blocks (12) on the rotating block (7) and the grinding blocks (12) on the pushing block (10) work in a matched mode, and the output end of the feeding hopper (6) is located between the rotating block (7) and the pushing block (10).
3. The phloroglucinol preparation method according to claim 1, characterized in that the stirring component comprises a stepping motor (16), a rotating shaft (17) and a plurality of stirring rods (18), the stepping motor (16) is fixed on one side of the outside of the fermentation device (5) through screws, the rotating shaft (17) is connected to the output end of the stepping motor (16) in a transmission manner, one end of the rotating shaft (17) far away from the stepping motor (16) is rotatably connected to the inner wall of the left side of the fermentation device (5) through a bearing, the stirring rods (18) are fixed on two sides of the rotating shaft (17) inside the fermentation device (5) and are provided with a plurality of stirring rods (18), and the stirring rods (18) are rotatably sleeved inside the fermentation device (5).
4. The method for preparing phloroglucinol according to claim 1, wherein a discharge pipe (19) is installed at the bottom of the right side of the fermentation equipment (5), and a butterfly valve (20) is installed on the discharge pipe (19).
5. The phloroglucinol preparation method according to claim 2, wherein a rotary groove is formed in the left side of the crushing device (1), and the rotating shaft (9) is rotatably connected to the inside of the rotary groove.
6. The method for preparing phloroglucinol according to claim 3, wherein a rotating groove is formed in the right side of the fermentation equipment (5), and the rotating shaft (17) is rotatably connected to the inside of the rotating groove.
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