CN113893809A - Device and method for synthesizing and purifying macamide - Google Patents
Device and method for synthesizing and purifying macamide Download PDFInfo
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- CN113893809A CN113893809A CN202111196810.5A CN202111196810A CN113893809A CN 113893809 A CN113893809 A CN 113893809A CN 202111196810 A CN202111196810 A CN 202111196810A CN 113893809 A CN113893809 A CN 113893809A
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- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 51
- 238000000746 purification Methods 0.000 claims abstract description 50
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 36
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 35
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims description 57
- 241000220317 Rosa Species 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- 238000009434 installation Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 239000010865 sewage Substances 0.000 claims description 14
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
- WGQKYBSKWIADBV-UHFFFAOYSA-N benzylamine Chemical compound NCC1=CC=CC=C1 WGQKYBSKWIADBV-UHFFFAOYSA-N 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 5
- 239000000194 fatty acid Substances 0.000 claims description 5
- 229930195729 fatty acid Natural products 0.000 claims description 5
- 150000004665 fatty acids Chemical class 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 241000196324 Embryophyta Species 0.000 claims 1
- 238000002425 crystallisation Methods 0.000 abstract description 6
- 230000008025 crystallization Effects 0.000 abstract description 6
- 240000000759 Lepidium meyenii Species 0.000 description 24
- 235000000421 Lepidium meyenii Nutrition 0.000 description 24
- 235000012902 lepidium meyenii Nutrition 0.000 description 24
- 150000001408 amides Chemical class 0.000 description 19
- 230000005540 biological transmission Effects 0.000 description 5
- 238000009413 insulation Methods 0.000 description 4
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 210000003437 trachea Anatomy 0.000 description 2
- 241000219193 Brassicaceae Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000801118 Lepidium Species 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- -1 amide compounds Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0004—Crystallisation cooling by heat exchange
- B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00132—Controlling the temperature using electric heating or cooling elements
- B01J2219/00135—Electric resistance heaters
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a device and a method for synthesizing and purifying macamide, relates to the technical field of biological pharmacy, and aims to solve the problems that in the prior art, in the process of synthesizing macamide, macamide needs to be purified, cooled and crystallized, but at present, a natural cooling mode is often adopted for crystallization, the cooling speed is slow, and the crystallization efficiency is low. The upper part of the working bottom plate is fixedly provided with a supporting plate, the upper part of the supporting plate is fixedly provided with a synthesis box, the lower part of the synthesis box is provided with a filter box along one side of the supporting plate, the lower part of the filter box is provided with a purification box, the purification box is fixedly connected with the working bottom plate through bolts, a liquid scattering assembly is arranged inside the purification box and consists of an upper plate, a vertical plate and a lower plate, the upper plate is arranged above the vertical plate, and the vertical plate is arranged above the lower plate.
Description
Technical Field
The invention relates to the technical field of biological pharmacy, in particular to a device and a method for synthesizing and purifying macamide.
Background
The maca amide compounds are amide alkaloids with the lowest alkalinity in nitrogen-containing alkaloids, in maca, maca amide is formed by bioconversion of benzylamine and fatty acid molecules, has very long carbon chains and multiple unsaturation degrees, is in the genus of Lepidium in the family of Cruciferae, has the eating history and wide biological efficacy for thousands of years, but has strict requirements on the growth environment of maca, low yield, extremely low content of maca amide in maca and complex components in maca, so that the maca amide preparation method by using maca as a raw material through biochemical separation is limited in raw material source and incapable of large-scale preparation due to the difficulty in separation and purification, and the problems of raw material resource shortage and the like are solved by obtaining maca amide through a chemical synthesis mode.
In the process of synthesizing macamide, the macamide needs to be purified, cooled and crystallized, but at present, the macamide is often crystallized in a natural cooling mode, the cooling speed is slow, and the crystallization efficiency is low; therefore, the market is urgently in need of developing a device and a method for synthesizing and purifying macamides to help people solve the existing problems.
Disclosure of Invention
The invention aims to provide a device and a method for synthesizing and purifying macamide, which aim to solve the problems that in the process of synthesizing macamide, the macamide needs to be purified, cooled and crystallized, but at present, the macamide is often crystallized in a natural cooling mode, the cooling speed is slow, and the crystallization efficiency is low.
In order to achieve the purpose, the invention provides the following technical scheme: the utility model provides a device of synthesis and purification maca amide, includes the work bottom plate, the top fixed mounting of work bottom plate has the backup pad, the top fixed mounting of backup pad has synthetic case, the below of synthetic case is provided with the rose box along one side of backup pad, the below of rose box is provided with the purification case, and purification case and work bottom plate pass through bolt fixed connection, the inside of purification case is provided with spills the liquid subassembly, it comprises upper plate, riser and hypoplastron to spill the liquid subassembly, the upper plate sets up in the top of riser, the riser sets up in the top of hypoplastron, the inside of upper plate is provided with the through-liquid hole, the top of hypoplastron is provided with along one side of riser and divides the liquid cone, and divides the liquid cone and pass through bolt fixed connection with the hypoplastron.
Preferably, spill the top of liquid subassembly and install defeated hopper, and spill liquid subassembly and defeated hopper and pass through bolt fixed connection, spill the below of liquid subassembly and install the connecting seat, and spill liquid subassembly and pass through bolt fixed connection with the connecting seat, the below of connecting seat is provided with the installation base, and installs the base and pass through bolt fixed connection with the purification case, the internally mounted of installation base has the second motor, and the installation base passes through bolt fixed connection with the second motor.
Preferably, the inside of purification case is provided with the cold air chamber, one side of cold air chamber is provided with leads warm annular plate, and leads warm annular plate and pass through bolt fixed connection with the purification case, the cold air duct is installed to one side of purification case, and cold air duct and cold air chamber intercommunication, the blast pipe is installed to the opposite side of purification case, and blast pipe and cold air chamber intercommunication.
Preferably, the inside of purification case is provided with dirty liquid chamber along the below in air conditioning chamber, one side in dirty liquid chamber is provided with the annular filter plate, and the annular filter plate passes through bolt fixed connection with the purification case, the blow off pipe is installed to one side of purification case, and blow off pipe and dirty liquid chamber intercommunication.
Preferably, the inlet pipe is installed to the top of synthetic case, and synthetic case passes through bolt fixed connection with the inlet pipe, one side of inlet pipe is provided with first motor, and first motor passes through bolt fixed connection with synthetic case, one side of first motor is provided with the trachea that looses, and looses the trachea and pass through bolt fixed connection with synthetic case, the internally mounted of synthetic case has the heat preservation, and synthetic case passes through bolt fixed connection with the heat preservation, the inside of synthetic case is provided with the hybrid chamber.
Preferably, the below of hybrid chamber is provided with the discharge hole, and hybrid chamber and discharge hole intercommunication, the inside in discharge hole is provided with the bleeder valve, and bleeder valve and synthetic case fixed connection, the inside of hybrid chamber is provided with the center pin, and the center pin rotates with synthetic case to be connected, stirring leaf is installed in the outside of center pin, and center pin and stirring leaf fixed connection, the internally mounted of synthetic case has electric heater, and synthetic case passes through bolt fixed connection with electric heater.
Preferably, one side of electric heater is provided with the heat transfer board, and passes through bolt fixed connection with synthetic case through the heat transfer board, be provided with the connecting pipe between synthetic case and the rose box, and synthetic case and rose box all with connecting pipe fixed connection, the sliding door is installed to the top of rose box, and rose box and sliding door rotate to be connected.
Preferably, the conveyer pipe is installed to the below of rose box, and the rose box passes through bolt fixed connection with the conveyer pipe, defeated pipe is installed down to the below of conveyer pipe, and the conveyer pipe passes through bolt fixed connection with defeated pipe down, the internally mounted of rose box has the installation piece, and the rose box passes through bolt fixed connection with the installation piece, the filter is installed to one side of installation piece, and the installation piece passes through bolt fixed connection with the filter.
A method for synthesizing and purifying macamides, comprising the steps of:
s1: synthesizing macamide, mixing and stirring a certain amount of dichloromethane solution, fatty acid and benzylamine, and heating;
s2: uniformly mixing the raw materials, reacting until the reaction solution in the mixed solution is evaporated to dryness to obtain a macamide concentrated solution;
s3: then purifying, namely adding a certain amount of absolute ethyl alcohol into the macamide concentrated solution for mixing and washing;
s4: filtering the mixed macamide solution to remove impurities;
s5: and then cooling the macamide solution to separate out the macamide crystals.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, through the arrangement of the purification box, the liquid scattering component capable of rotating is arranged in the purification box, when a macamide solution is input into the liquid scattering component, the macamide solution flows around under the action of the liquid separating cone and then enters different areas separated by the vertical plates, under the rotation of the liquid scattering component, the macamide solution in the different areas separated by the vertical plates scatters in an arc shape under the action of the vertical plates, the contact area and the path of the macamide solution and air are increased, so that the heat in the macamide solution can be quickly volatilized into the air, the temperature of the macamide solution is reduced, the cooling and crystallization speed of the macamide solution is increased, meanwhile, the cold air cavity is arranged in the purification box, the scattered macamide solution can fall onto the inner wall of the heat conducting annular plate, and under the action of the cold air in the cold air cavity, the messenger flies to fall to leading the temperature ring board maca amide solution on the inner wall and can the rapid cooling, has further improved maca amide solution cooling rate, has increased maca amide solution crystallization efficiency.
2. According to the invention, through the arrangement of the central shaft and the stirring blades, four groups of stirring blades are arranged on the central shaft, and the stirring blades can be driven to rotate through the rotation of the central shaft, so that different raw materials can be stirred in the process of synthesizing macamides, the raw materials are mixed more uniformly, and the reaction speed of the macamides is increased.
3. According to the invention, through the arrangement of the filter box, the filter plate is arranged in the filter box, so that the macamide solution can be filtered, impurities in the macamide solution are filtered, the purity of the macamide solution is improved, the purity of the macamide is increased, and meanwhile, the sliding door is arranged above the filter box, so that the filter plate can be detached from the filter box and taken out, and the convenience of cleaning and replacing the filter plate is improved.
Drawings
FIG. 1 is a schematic view of an apparatus for the synthesis and purification of macamides according to the invention;
fig. 2 is a front view of an apparatus for synthesizing and purifying macamides according to the invention;
FIG. 3 is a cross-sectional view of a purification cassette of the present invention;
FIG. 4 is a cross-sectional view of the dispensing assembly of the present invention;
FIG. 5 is a top cross-sectional view of the dispensing assembly of the present invention;
FIG. 6 is a cross-sectional view of a synthesis box of the invention;
FIG. 7 is a cross-sectional view of a filtration tank of the present invention
In the figure: 1. a synthesis box; 2. a support plate; 3. a filter box; 4. a purification box; 5. a work base plate; 6. a feed pipe; 7. a first motor; 8. an air diffusing pipe; 9. a lower conveying pipe; 10. a connecting pipe; 11. a delivery pipe; 12. a material conveying hopper; 13. a cold air pipe; 14. a blow-off pipe; 15. an exhaust pipe; 16. a cold air chamber; 17. a heat conducting ring plate; 18. a liquid spreading assembly; 19. a connecting seat; 20. a waste liquid chamber; 21. an annular filter plate; 22. installing a base; 23. a second motor; 24. an upper plate; 25. a vertical plate; 26. a lower plate; 27. a liquid through hole; 28. a liquid separating cone; 29. a heat-insulating layer; 30. a mixing chamber; 31. an electric heater; 32. a heat transfer plate; 33. a central shaft; 34. stirring the blades; 35. a discharge hole; 36. a discharge valve; 37. sliding the door; 38. mounting blocks; 39. a filter plate.
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. 1-7, an embodiment of the present invention is shown: a device for synthesizing and purifying maca amide comprises a working bottom plate 5, wherein a support plate 2 is fixedly arranged above the working bottom plate 5, the number of the support plates 2 is two, the installation stability of a synthesis box 1 is improved, the synthesis box 1 is fixedly arranged above the support plate 2, a filter box 3 is arranged below the synthesis box 1 along one side of the support plate 2, a purification box 4 is arranged below the filter box 3, the purification box 4 is fixedly connected with the working bottom plate 5 through bolts, a liquid scattering component 18 is arranged inside the purification box 4, the liquid scattering component 18 comprises an upper plate 24, a vertical plate 25 and a lower plate 26, the upper plate 24 is arranged above the vertical plate 25, the upper plate 24 is fixedly connected with the vertical plate 25, the vertical plate 25 is arranged above the lower plate 26, the vertical plate 25 is fixedly connected with the lower plate 26, a liquid through hole 27 is arranged inside the upper plate 24, and the liquid through hole 27 is arranged, so that a solution can flow into the liquid scattering component 18 from a material conveying hopper 12, a liquid separating cone 28 is arranged above the lower plate 26 along one side of the vertical plate 25, the liquid separating cone 28 is fixedly connected with the lower plate 26 through bolts, the liquid separating cone 28 is arranged to enable a solution to flow around, a liquid conveying hopper 12 is arranged above the liquid scattering assembly 18, the liquid scattering assembly 18 is fixedly connected with the liquid conveying hopper 12 through bolts, a large-diameter opening is arranged at the upper end of the liquid conveying hopper 12 to prevent the solution from splashing, a connecting seat 19 is arranged below the liquid scattering assembly 18, the liquid scattering assembly 18 is fixedly connected with the connecting seat 19 through bolts, a mounting base 22 is arranged below the connecting seat 19, the mounting base 22 is fixedly connected with the purifying box 4 through bolts, a second motor 23 is arranged inside the mounting base 22, the mounting base 22 is fixedly connected with the second motor 23 through bolts, the second motor 23 is rotatably connected with the connecting seat 19 through a rotating shaft, so that the second motor 23 can drive the connecting seat 19 to rotate, a cold air cavity 16 is arranged inside the purification box 4, a temperature guide ring plate 17 is arranged on one side of the cold air cavity 16, the temperature guide ring plate 17 is fixedly connected with the purification box 4 through bolts, the temperature guide ring plate 17 is made of die-cast aluminum alloy, the temperature guide capability is improved, a cold air pipe 13 is arranged on one side of the purification box 4, the cold air pipe 13 is communicated with the cold air cavity 16, the cold air pipe 13 is externally connected with cold air supply equipment, the cold air pipe 13 can convey cold air, an exhaust pipe 15 is arranged on the other side of the purification box 4, the exhaust pipe 15 is communicated with the cold air cavity 16, a sewage cavity 20 is arranged inside the purification box 4 along the lower part of the cold air cavity 16, an annular filter plate 21 is arranged on one side of the sewage cavity 20, the annular filter plate 21 is fixedly connected with the purification box 4 through bolts, crystal outflow can be prevented due to the arrangement of the annular filter plate 21, a sewage discharge pipe 14 is arranged on one side of the purification box 4, and the sewage discharge pipe 14 is communicated with the sewage cavity 20, the sewage pipe 14 is externally connected with sewage treatment equipment, so that residual sewage can be treated.
Furthermore, a feeding pipe 6 is installed above the synthesis box 1, the synthesis box 1 is fixedly connected with the feeding pipe 6 through a bolt, a first motor 7 is arranged on one side of the feeding pipe 6, the first motor 7 is fixedly connected with the synthesis box 1 through a bolt, an air diffusing pipe 8 is arranged on one side of the first motor 7, the air diffusing pipe 8 is fixedly connected with the synthesis box 1 through a bolt, the air diffusing pipe 8 is arranged to enable steam in the solution evaporation process to flow out, a heat insulation layer 29 is installed inside the synthesis box 1, the synthesis box 1 is fixedly connected with the heat insulation layer 29 through a bolt, the heat insulation layer 29 is arranged to improve the heat insulation capability of the synthesis box 1 and reduce the loss of heat, a mixing cavity 30 is arranged inside the synthesis box 1, a discharge hole 35 is arranged below the mixing cavity 30, the mixing cavity 30 is communicated with the discharge hole 35, and a discharge valve 36 is arranged inside the discharge hole 35, the discharge valve 36 is fixedly connected with the synthesis box 1, the discharge valve 36 is an electromagnetic valve which can regulate and control the discharge of the solution in the mixing cavity 30, the center shaft 33 is arranged in the mixing cavity 30, the center shaft 33 is rotatably connected with the synthesis box 1, the center shaft 33 is rotatably connected with the first motor 7, so that the first motor 7 can drive the center shaft 33 to rotate, the stirring blades 34 are arranged outside the center shaft 33, the center shaft 33 is fixedly connected with the stirring blades 34, a plurality of through holes are arranged in the stirring blades 34, the liquid resistance on the stirring blades 34 during rotation can be reduced, the electric heater 31 is arranged in the synthesis box 1, the synthesis box 1 is fixedly connected with the electric heater 31 through bolts, the temperature transmission plate 32 is arranged on one side of the electric heater 31, the temperature transmission plate 32 is fixedly connected with the synthesis box 1 through bolts, the temperature transmission plate 32 is made of die-cast aluminum alloy, and the temperature conduction capability is improved, a connecting pipe 10 is arranged between the synthesis box 1 and the filter box 3, the synthesis box 1 and the filter box 3 are both fixedly connected with the connecting pipe 10, a sliding door 37 is arranged above the filter box 3, the filter box 3 is rotatably connected with the sliding door 37, the arrangement of the sliding door 37 improves the convenience of cleaning and replacing the filter plate 39, a conveying pipe 11 is arranged below the filter box 3, the filter box 3 is fixedly connected with the conveying pipe 11 through a bolt, a lower conveying pipe 9 is arranged below the conveying pipe 11, the conveying pipe 11 is fixedly connected with the lower conveying pipe 9 through a bolt, a mounting block 38 is arranged inside the filter box 3, the filter box 3 is fixedly connected with the mounting block 38 through a bolt, a filter plate 39 is arranged on one side of the mounting block 38, the mounting block 38 is fixedly connected with the filter plate 39 through a bolt, the filter plate 39 is arranged, the maca amide solution can be filtered, and impurities in the maca amide solution can be filtered, the purity of the macamide solution is improved.
A method for synthesizing and purifying macamides, comprising the steps of:
s1: synthesizing macamide, mixing and stirring a certain amount of dichloromethane solution, fatty acid and benzylamine, and heating;
s2: uniformly mixing the raw materials, reacting until the reaction solution in the mixed solution is evaporated to dryness to obtain a macamide concentrated solution;
s3: then purifying, namely adding a certain amount of absolute ethyl alcohol into the macamide concentrated solution for mixing and washing;
s4: filtering the mixed macamide solution to remove impurities;
s5: and then cooling the macamide solution to separate out the macamide crystals.
The working principle is as follows: when the maca amide solution synthesis device is used, a certain amount of dichloromethane solution, fatty acid and benzylamine are respectively and sequentially added into a mixing cavity 30 of a synthesis box 1 through a feeding pipe 6, then an electric heater 31 is electrified, the electric heater 31 generates a large amount of heat, the temperature transmission effect of a temperature transmission plate 32 is achieved, the mixed solution in the mixing cavity 30 is heated and heated, then a first motor 7 is started, a central shaft 33 drives an agitating blade 34 to rotate, the mixed solution is agitated, raw materials are uniformly mixed and react, until the reaction liquid in the mixed solution is evaporated to dryness, a maca amide concentrated solution is obtained, a certain amount of absolute ethyl alcohol is added into the maca amide concentrated solution through the feeding pipe 6 for washing, then a discharge valve 36 is opened, the maca amide solution flows into a filter box 3 through a connecting pipe 10, the maca amide solution is filtered under the effect of a filter plate 39, impurities in the maca amide solution are filtered, and then the maca amide solution flows into a conveying hopper 12 through a conveying pipe 11 and a lower conveying pipe 9, the second motor 23 is started to rotate the liquid spreading component 18, macamide solution flowing into the liquid spreading component 18 through the liquid conveying hopper 12 flows around under the action of the liquid separating cone 28 and then enters different areas separated by the plurality of vertical plates 25, under the rotation of the liquid spreading component 18, macamide solution in different areas separated by the plurality of vertical plates scatters in an arc shape under the action of the vertical plates 25 to increase the contact area and the path of the macamide solution and the air, so that heat in the macamide solution can be rapidly volatilized into the air, cold air is conveyed to the cold air cavity 16 through the cold air pipe 13, the scattered macamide solution falls onto the inner wall of the heat conducting annular plate 17, under the action of the cold air in the cold air cavity 16, the macamide solution flying onto the inner wall of the heat conducting annular plate 17 can be rapidly cooled, and the cooling speed of the macamide solution is further increased, the macamide in the solution is crystallized and separated out, and the residual sewage flows into the sewage cavity 20 through the annular filter plate 21 and is discharged through the sewage discharge pipe 14.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (9)
1. A device for synthesizing and purifying macamides, comprising a work base (5), characterized in that: a support plate (2) is fixedly arranged above the working bottom plate (5), a synthesis box (1) is fixedly arranged above the support plate (2), a filter box (3) is arranged below the synthesis box (1) along one side of the support plate (2), a purification box (4) is arranged below the filter box (3), the purification box (4) is fixedly connected with the working bottom plate (5) through bolts, a liquid scattering assembly (18) is arranged inside the purification box (4), the liquid scattering assembly (18) is composed of an upper plate (24), an upright plate (25) and a lower plate (26), the upper plate (24) is arranged above the upright plate (25), the upright plate (25) is arranged above the lower plate (26), a liquid through hole (27) is arranged inside the upper plate (24), and a liquid separating cone (28) is arranged above the lower plate (26) along one side of the upright plate (25), and the liquid separating cone (28) is fixedly connected with the lower plate (26) through bolts.
2. An apparatus for the synthesis and purification of macamides according to claim 1, wherein: spill the top of liquid subassembly (18) and install defeated hopper (12), and spill liquid subassembly (18) and defeated hopper (12) and pass through bolt fixed connection, spill the below of liquid subassembly (18) and install connecting seat (19), and spill liquid subassembly (18) and pass through bolt fixed connection with connecting seat (19), the below of connecting seat (19) is provided with installation base (22), and installation base (22) and purification case (4) pass through bolt fixed connection, the internally mounted of installation base (22) has second motor (23), and installation base (22) and second motor (23) pass through bolt fixed connection.
3. An apparatus for the synthesis and purification of macamides according to claim 1, wherein: the inside of purification case (4) is provided with cold air chamber (16), one side of cold air chamber (16) is provided with leads warm crown plate (17), and leads warm crown plate (17) and purification case (4) and pass through bolt fixed connection, cold air duct (13) are installed to one side of purification case (4), and cold air duct (13) and cold air chamber (16) intercommunication, blast pipe (15) are installed to the opposite side of purification case (4), and blast pipe (15) and cold air chamber (16) intercommunication.
4. A plant for the synthesis and purification of macamides according to claim 3, characterized in that: the inside of purification case (4) is provided with sewage chamber (20) along the below of cold air chamber (16), one side in sewage chamber (20) is provided with annular filter plate (21), and annular filter plate (21) pass through bolt fixed connection with purification case (4), blow off pipe (14) are installed to one side of purification case (4), and blow off pipe (14) and sewage chamber (20) intercommunication.
5. An apparatus for the synthesis and purification of macamides according to claim 1, wherein: inlet pipe (6) are installed to the top of synthetic case (1), and synthetic case (1) passes through bolt fixed connection with inlet pipe (6), one side of inlet pipe (6) is provided with first motor (7), and first motor (7) pass through bolt fixed connection with synthetic case (1), one side of first motor (7) is provided with air diffusing pipe (8), and air diffusing pipe (8) and synthetic case (1) pass through bolt fixed connection, the internally mounted of synthetic case (1) has heat preservation (29), and synthetic case (1) passes through bolt fixed connection with heat preservation (29), the inside of synthetic case (1) is provided with hybrid chamber (30).
6. An apparatus for the synthesis and purification of macamides according to claim 5, wherein: the below of hybrid chamber (30) is provided with discharge hole (35), and hybrid chamber (30) and discharge hole (35) intercommunication, the inside of discharge hole (35) is provided with bleeder valve (36), and bleeder valve (36) and synthetic case (1) fixed connection, the inside of hybrid chamber (30) is provided with center pin (33), and center pin (33) and synthetic case (1) rotate to be connected, stirring leaf (34) are installed in the outside of center pin (33), and center pin (33) and stirring leaf (34) fixed connection, the internally mounted of synthetic case (1) has electric heater (31), and synthetic case (1) passes through bolt fixed connection with electric heater (31).
7. An apparatus for the synthesis and purification of macamides according to claim 6, wherein: one side of electric heater (31) is provided with temperature transfer board (32), and temperature transfer board (32) and synthetic case (1) pass through bolt fixed connection, be provided with connecting pipe (10) between synthetic case (1) and rose box (3), and synthetic case (1) and rose box (3) all with connecting pipe (10) fixed connection, sliding door (37) are installed to the top of rose box (3), and rose box (3) rotate with sliding door (37) and are connected.
8. An apparatus for the synthesis and purification of macamides according to claim 1, wherein: conveyer pipe (11) are installed to the below of rose box (3), and rose box (3) and conveyer pipe (11) pass through bolt fixed connection, defeated pipe (9) are installed down to the below of conveyer pipe (11), and conveyer pipe (11) and defeated pipe (9) pass through bolt fixed connection down, the internally mounted of rose box (3) has installation piece (38), and rose box (3) and installation piece (38) pass through bolt fixed connection, filter (39) are installed to one side of installation piece (38), and install piece (38) and pass through bolt fixed connection with filter (39).
9. A method for synthesizing and purifying macamides, which is realized on the basis of the device for synthesizing and purifying macamides of any one of claims 1 to 8, and is characterized by comprising the following steps:
s1: synthesizing macamide, mixing and stirring a certain amount of dichloromethane solution, fatty acid and benzylamine, and heating;
s2: uniformly mixing the raw materials, reacting until the reaction solution in the mixed solution is evaporated to dryness to obtain a macamide concentrated solution;
s3: then purifying, namely adding a certain amount of absolute ethyl alcohol into the macamide concentrated solution for mixing and washing;
s4: filtering the mixed macamide solution to remove impurities;
s5: and then cooling the macamide solution to separate out the macamide crystals.
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