CN112029805B - Preparation method of phloroglucinol - Google Patents
Preparation method of phloroglucinol Download PDFInfo
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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 high preparation cost of the existing phloroglucinol. The invention can simply and conveniently prepare the phloroglucinol, has the advantages of simple raw material acquisition, low production cost and convenient operation, can improve the purity of the phloroglucinol, can improve the production speed of the phloroglucinol, has a simple and reasonable structure, and is convenient to use.
Description
Technical Field
The invention relates to the technical field of phloroglucinol processing, in particular to a preparation method of phloroglucinol.
Background
The 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, and 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 and performing amination and hydrolysis, such as a haloaniline method, taking halobenzene or aminobenzene as the raw material, has high price and difficult raw material source, is inconvenient to use by using production equipment, and has high preparation cost, so the preparation method of the phloroglucinol is provided.
Disclosure of Invention
The preparation method of phloroglucinol solves the problem of high preparation cost of phloroglucinol.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the preparation method of the 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 arranged at the top of the crushing equipment, crushing parts are arranged in the crushing equipment, a liquid outlet pipe is arranged at the bottom of the crushing equipment, a receiving container is arranged at one side of the crushing equipment and is matched with the liquid outlet pipe, a filter screen is fixed in the crushing equipment and is positioned between the crushing parts and the liquid outlet pipe, and stirring parts are arranged in the fermentation equipment;
the preparation method of phloroglucinol also comprises the following purification steps:
s1, pouring cleaned brown algae into a charging hopper, conveying the brown algae into a crushing device through the charging hopper, crushing the brown algae through a crushing component in the crushing device, filtering brown algae residues through a filter screen, and collecting the filtered brown algae extract through a receiving container through a liquid outlet pipe;
s2, placing the brown algae extract extracted in the crushing equipment 1 in the step S1 into the microwave processing equipment 2, adding sodium bicarbonate solution at the moment, extracting for one hour by microwaves at the temperature of 50 ℃, centrifuging the extracted liquid, and collecting the supernatant after treatment;
s3, placing the solution obtained in the step S2 into the distillation equipment 3, evaporating the filtrate by the distillation equipment 3 at the moment, 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 the extraction equipment 4, adding chloroform solution with the volume of 12 times of the filtrate at the moment, extracting the mixed solution by the extraction equipment 4 at the moment, and collecting extract extracted by the extraction equipment 4;
s5, placing the extract obtained in the step S4 into distillation equipment 3, and evaporating the extract by the distillation equipment 3 to obtain brown algae polyphenol extract;
s6, placing the brown algae polyphenol extract obtained in the step S5 into the fermentation equipment 5, at the moment, injecting water with the amount of 8 times of the brown algae polyphenol extract into the fermentation equipment 5, at the moment, adding aspergillus into the fermentation equipment 5, at the moment, fermenting materials in the fermentation equipment 5 through the aspergillus, and at the same time, stirring the materials in the fermentation equipment 5 through a stirring component arranged in the fermentation equipment 5, so as to improve the fermentation rate of the materials in the fermentation equipment 5;
s7, after fermentation of the materials in the fermentation equipment 5 is finished, collecting fermentation extracting solution at the moment, adjusting the PH of the collected fermentation extracting solution at the moment, and obtaining extracting solution containing phloroglucinol monomers at the moment when the PH of the fermentation extracting solution is 5-5.5;
and S8, placing the extracting solution containing the phloroglucinol monomer obtained in the step S7 into the distillation equipment 3, evaporating the extracting solution by the distillation equipment 3, heating the extracting solution in the distillation equipment 3 to 331 ℃, and collecting the evaporated liquid to obtain the phloroglucinol liquid.
Preferably, the crushing part comprises a rotating block, a driving motor, a rotating shaft, a pushing block, a hydraulic cylinder and a grinding block, wherein the rotating block is rotationally connected to the inside of the crushing device, the driving motor is fixed to one side of the outside of the crushing device, the rotating shaft is in transmission connection with the output end of the driving motor, one end of the rotating shaft, which is far away from the driving motor, is rotationally connected to one side, which is close to the driving motor, of the rotating block through a bearing, the pushing block is located on one side, which is far away from the driving motor, of the rotating block, the pushing block is in sliding connection with the inner wall of the crushing device, the hydraulic cylinder is fixed to the inner wall of the right side two ends of the crushing device, the piston end of the hydraulic cylinder is fixed to one side, which is far away from the rotating block, of the grinding block is fixed to the opposite side of the rotating block, a plurality of grinding blocks located on the rotating block and the grinding block are matched to work, and the output end of the feeding hopper is located between the rotating block and the pushing block.
Preferably, the stirring part comprises a stepping motor, a rotating shaft and stirring rods, wherein the stepping motor is fixed on one side of the outer part of the fermentation equipment through screws, the rotating shaft is in transmission connection with the output end of the stepping motor, one end, far away from the stepping motor, of the rotating shaft is rotationally connected to the left inner wall of the fermentation equipment through a bearing, the stirring rods are fixed on two sides of the rotating shaft positioned in the fermentation equipment and are provided with a plurality of stirring rods, and the stirring rods are rotationally sleeved in the fermentation equipment.
Preferably, a discharge pipe is arranged at the bottom of the right side of the fermentation equipment, and a butterfly valve is arranged on the discharge pipe.
Preferably, a rotary groove is formed in the left side of the crushing equipment, and the rotary shaft is rotationally 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 rotationally connected to the inside of the rotating groove.
In the invention, the following components are added:
1. through the cooperation work of crushing equipment, microwave processing equipment, distillation plant, extraction equipment, fermentation equipment, feeding hopper, filter screen, drain pipe and receiving vessel, can be simple and convenient prepare the phloroglucinol, and raw and other materials obtain simply, manufacturing cost is less, and the operation is comparatively convenient.
2. The device comprises a rotating block, a driving motor, a rotating shaft, a pushing block, a hydraulic cylinder, a grinding block, a stepping motor, a rotating shaft, a stirring rod, a discharge pipe and a butterfly valve, wherein the raw materials of the phloroglucinol can be rapidly and efficiently crushed, raw material extracting solutions of the crushed raw materials can be filtered, so that the purity of the phloroglucinol is improved, the raw materials of the phloroglucinol can be effectively stirred, the fermentation rate of the raw materials of the phloroglucinol is improved, the production speed of the phloroglucinol is further improved, and the device is high in working performance.
Drawings
Fig. 1 is a schematic structural diagram of a preparation method of phloroglucinol.
Reference numerals in the drawings: 1. a crushing device; 2. microwave processing equipment; 3. distillation equipment; 4. extraction equipment; 5. a fermentation device; 6. a charging hopper; 7. a rotating block; 8. a driving motor; 9. a rotating shaft; 10. a pushing block; 11. a hydraulic cylinder; 12. grinding the 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 valve.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
Referring to fig. 1, a preparation method of phloroglucinol 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 arranged at the top of the crushing device 1, crushing components are arranged in the crushing device 1, a liquid outlet pipe 14 is arranged 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 are matched for working, a filter screen 13 is fixed in the crushing device 1, the filter screen 13 is positioned between the crushing components and the liquid outlet pipe 14, and stirring components are arranged in the fermentation device 5.
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, wherein the rotating block 7 is rotationally connected to the inside of the crushing device 1, the driving motor 8 is fixed to 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, which is far away from the driving motor 8, is rotationally connected to one side, which is close to the driving motor 8, of the rotating block 7 through a bearing, the pushing block 10 is located at one side, which is far away from the driving motor 8, of the rotating block 7, the pushing block 10 is in sliding connection with the inner wall of the crushing device 1, the hydraulic cylinder 11 is fixed to the inner wall at two ends of the right side of the crushing device 1, the piston end of the hydraulic cylinder 11 is fixed to one side, which is far away from the rotating block 7, of the grinding block 12 is fixed to the opposite sides of the rotating block 7 and the pushing block 10, and a plurality of grinding blocks 12 located on the rotating block 7 are matched with the grinding block 12 located on the pushing block 10, and the output end of the feeding hopper 6 is located between the rotating block 7 and the pushing block 10.
The stirring part comprises a stepping motor 16, a rotating shaft 17 and stirring rods 18, wherein the stepping motor 16 is fixed on one side of the outer part of the fermentation equipment 5 through screws, the rotating shaft 17 is in transmission connection with the output end of the stepping motor 16, one end of the rotating shaft 17, which is far away from the stepping motor 16, is rotationally connected to the inner wall of the left side of the fermentation equipment 5 through a bearing, the stirring rods 18 are fixed on two sides of the rotating shaft 17 positioned in the fermentation equipment 5 and are provided with a plurality of stirring rods 18, the stirring rods 18 are rotationally sleeved in the fermentation equipment 5, a discharge pipe 19 is installed at the bottom of the right side of the fermentation equipment 5, a butterfly valve 20 is installed on the discharge pipe 19, and extracting solution of the fermentation equipment can be discharged through the discharge pipe 19.
The left side of crushing equipment 1 has seted up the change groove, and pivot 9 rotates the inside of connecting at the change groove, through the change groove, pivot 9 can carry out nimble rotation.
The right side of the fermentation equipment 5 is provided with a rotating groove, the rotating shaft 17 is rotationally connected in the rotating groove, and the rotating shaft 17 can flexibly rotate through the rotating groove.
The preparation method of phloroglucinol also comprises the following purification steps:
s1, pouring cleaned brown algae into a charging hopper 6, conveying the brown algae into a crushing device 1 through the charging hopper 6, crushing the brown algae through a crushing component in the crushing device 1, filtering brown algae residues through a filter screen 13, and collecting the filtered brown algae extract through a receiving container 15 through a liquid outlet pipe 14, wherein the crushed brown algae extract is filtered through the filter screen 13;
s2, placing the brown algae extract extracted in the crushing equipment 1 in the step S1 into the microwave processing equipment 2, adding sodium bicarbonate solution at the moment, extracting for one hour by microwaves at the temperature of 50 ℃, centrifuging the extracted liquid, and collecting the supernatant after treatment;
s3, placing the solution obtained in the step S2 into the distillation equipment 3, evaporating the filtrate by the distillation equipment 3 at the moment, 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 the extraction equipment 4, adding chloroform solution with the volume of 12 times of the filtrate at the moment, extracting the mixed solution by the extraction equipment 4 at the moment, and collecting extract extracted by the extraction equipment 4;
s5, placing the extract obtained in the step S4 into distillation equipment 3, and evaporating the extract by the distillation equipment 3 to obtain brown algae polyphenol extract;
s6, placing the brown algae polyphenol extract obtained in the step S5 into the fermentation equipment 5, at the moment, injecting water with the amount of 8 times of the brown algae polyphenol extract into the fermentation equipment 5, at the moment, adding aspergillus into the fermentation equipment 5, at the moment, fermenting materials in the fermentation equipment 5 through the aspergillus, and at the same time, stirring the materials in the fermentation equipment 5 through a stirring component arranged in the fermentation equipment 5, so as to improve the fermentation rate of the materials in the fermentation equipment 5;
s7, after fermentation of the materials in the fermentation equipment 5 is finished, collecting fermentation extracting solution at the moment, adjusting the PH of the collected fermentation extracting solution at the moment, and obtaining extracting solution containing phloroglucinol monomers at the moment when the PH of the fermentation extracting solution is 5-5.5;
and S8, placing the extracting solution containing the phloroglucinol monomer obtained in the step S7 into the distillation equipment 3, evaporating the extracting solution by the distillation equipment 3, heating the extracting solution in the distillation equipment 3 to 331 ℃, and collecting the evaporated liquid to obtain the phloroglucinol liquid.
Working principle: when phloroglucinol needs to be prepared, the cleaned brown algae can be poured into the charging hopper 6, the brown algae is conveyed into the crushing equipment 1 through the charging 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, 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 is driven to horizontally displace through the operation of the hydraulic cylinder 11, the brown algae is pushed to horizontally displace through the pushing block 10 which horizontally displaces, when the brown algae is contacted with the rotating block 7, the brown algae can be effectively crushed through the grinding block 12, the crushed brown algae can fall on the filter screen 13, the brown algae extracting solution which is crushed at the moment can be filtered through the filter screen 13, and 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 is placed in the microwave processing equipment 2, sodium bicarbonate solution is added, the microwave extraction is performed for one hour at 50 ℃, the liquid after the extraction is centrifuged, the supernatant after the treatment is collected, the filtrate is placed in the distillation equipment 3, the filtrate is evaporated by the distillation equipment 3, when the filtrate in the distillation equipment 3 is one-ninth of the original volume, the obtained filtrate is collected, the obtained filtrate is placed in the extraction equipment 4, chloroform solution with the volume of 12 times of the filtrate is added, the mixed solution is extracted by the extraction equipment 4, then collecting the extract liquid extracted by the extraction equipment 4, placing the obtained extract liquid into the extraction equipment 4, evaporating the extract liquid by the distillation equipment 3, obtaining brown algae polyphenol extract, placing the obtained brown algae polyphenol extract into the fermentation equipment 5, injecting water with the amount of 8 times of brown algae polyphenol extract into the fermentation equipment 5, adding aspergillus into the fermentation equipment 5, fermenting the material in the fermentation equipment 5 by aspergillus, driving the rotating shaft 17 to rotate by the operation of the stepping motor 16, driving the stirring rod 18 to rotate by the rotating shaft 17, stirring the material in the fermentation equipment 5 by the rotating stirring rod 18, therefore, the fermentation rate of the materials in the fermentation equipment 5 is effectively improved, when the fermentation of the materials in the fermentation equipment 5 is finished, a user can open the butterfly valve 20, fermentation liquid in the fermentation equipment 5 can be discharged through the discharge pipe 19, fermentation extracting solution can be collected, the PH of the collected fermentation extracting solution can be adjusted, when the PH of the fermentation extracting solution is 5-5.5, extracting solution containing phloroglucinol monomers can be obtained, the obtained extracting solution containing phloroglucinol monomers can be placed in the distillation equipment 3, the extracting solution can be evaporated through the distillation equipment 3, the extracting solution in the distillation equipment 3 is heated to 331 ℃, evaporated liquid can be collected, and phloroglucinol liquid can be obtained.
In the description of the present invention, it should 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", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the apparatus or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (1)
1. The preparation method of the phloroglucinol comprises a preparation assembly line, and is characterized by comprising a crushing device (1), a microwave processing device (2), a distillation device (3), an extraction device (4) and a fermentation device (5), wherein a feeding hopper (6) is arranged at the top of the crushing device (1), a crushing part is arranged in the crushing device (1), a liquid outlet pipe (14) is arranged at the bottom of the crushing device (1), a receiving container (15) is arranged at one side of the crushing device (1), the receiving container (15) is matched with the liquid outlet pipe (14), a filter screen (13) is fixed in the crushing device (1), the filter screen (13) is positioned between the crushing part and the liquid outlet pipe (14), and a stirring part is arranged in the fermentation device (5);
the preparation method of phloroglucinol also comprises the following purification steps:
s1, pouring cleaned brown algae into a feeding hopper (6), conveying the brown algae into a crushing device (1) through the feeding hopper (6), crushing the brown algae through a crushing component in the crushing device (1), filtering brown algae residues through a filter screen (13) by using a brown algae extracting solution subjected to crushing at the moment, and collecting the brown algae extracting solution through a receiving container (15) by using a liquid outlet pipe (14), wherein the filtered brown algae extracting solution enters the receiving container (15);
s2, placing the brown algae extract extracted in the crushing equipment (1) in the step S1 into the microwave processing equipment (2), adding sodium bicarbonate solution at the moment, performing microwave extraction at the temperature of 50 ℃ for one hour, centrifuging the extracted liquid, and collecting the supernatant after treatment;
s3, placing the solution obtained in the step S2 into distillation equipment (3), evaporating the filtrate through the distillation equipment (3), and collecting the 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 chloroform solution with the volume of 12 times of the filtrate at the moment, performing extraction treatment on the mixed solution through the extraction equipment (4), and then collecting extract extracted by the extraction equipment (4);
s5, placing the extract obtained in the step S4 into distillation equipment (3), and performing evaporation treatment on the extract by the distillation equipment (3) at the moment to obtain brown algae polyphenol extract at the moment;
s6, placing the brown algae polyphenol extract obtained in the step S5 into fermentation equipment (5), at the moment, injecting water with the amount of 8 times of the brown algae polyphenol extract into the fermentation equipment (5), at the moment, adding aspergillus into the fermentation equipment (5), at the moment, fermenting materials in the fermentation equipment (5) through the aspergillus, and at the same time, stirring the materials in the fermentation equipment (5) through stirring components arranged in the fermentation equipment (5), so as to improve the fermentation rate of the materials in the fermentation equipment (5);
s7, after the fermentation of the materials in the fermentation equipment (5) is finished, collecting fermentation extracting solution at the moment, adjusting the PH of the collected fermentation extracting solution at the moment, and obtaining extracting solution containing phloroglucinol monomers at the moment when the PH of the fermentation extracting solution is 5-5.5;
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 ℃, and collecting the evaporated liquid to obtain phloroglucinol liquid;
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), wherein the rotating block (7) is rotationally connected to the inside of the crushing equipment (1), the driving motor (8) is fixed on one side of the outside of the crushing equipment (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 rotationally connected to 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 equipment (1), the hydraulic cylinder (11) is fixed on the inner wall at two ends of the right side of the crushing equipment (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 one side of the rotating block (7) and the opposite side of the pushing block (10) is provided with a plurality of grinding blocks (12) which are positioned on the corresponding grinding block (12), the output end of the feeding hopper (6) is positioned between the rotating block (7) and the pushing block (10), the stirring component comprises a stepping motor (16), a rotating shaft (17) and a stirring rod (18), the stepping motor (16) is fixed on one side of the outer part of the fermentation equipment (5) through screws, the rotating shaft (17) is connected to the output end of the stepping motor (16) in a transmission way, one end of the rotating shaft (17) far away from the stepping motor (16) is connected to the inner wall of the left side of the fermentation equipment (5) through a bearing in a rotating way, the utility model discloses a fermentation equipment, including fermentation equipment (5), puddler (18), discharge pipe (19) are installed to the bottom of puddler (18), rotation axis (17) both sides that are located fermentation equipment (5) inside are fixed to be equipped with a plurality of, puddler (18) rotate the cover and establish the inside at fermentation equipment (5), discharge pipe (19) are installed to the bottom on fermentation equipment (5) right side, butterfly valve (20) are installed on discharge pipe (19), the change groove has been seted up in the left side of crushing equipment (1), rotation axis (9) rotate the inside of connecting at the change groove, the change groove has been seted up on the right side of fermentation equipment (5), rotation axis (17) rotate the inside of connecting at the change groove.
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