CN210394392U - Esterification device of isooctyl palmitate - Google Patents
Esterification device of isooctyl palmitate Download PDFInfo
- Publication number
- CN210394392U CN210394392U CN201920608429.7U CN201920608429U CN210394392U CN 210394392 U CN210394392 U CN 210394392U CN 201920608429 U CN201920608429 U CN 201920608429U CN 210394392 U CN210394392 U CN 210394392U
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- tank
- esterification
- enzyme
- stirring
- interlayer
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- 238000005886 esterification reaction Methods 0.000 title claims abstract description 37
- 230000032050 esterification Effects 0.000 title claims abstract description 35
- AMUTYVGRCVFCCD-UHFFFAOYSA-N 5,6-diaminopyridine-3-carboxylic acid Chemical compound NC1=CC(C(O)=O)=CN=C1N AMUTYVGRCVFCCD-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 108090000790 Enzymes Proteins 0.000 claims abstract description 42
- 102000004190 Enzymes Human genes 0.000 claims abstract description 42
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000002156 mixing Methods 0.000 claims abstract description 21
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003208 petroleum Substances 0.000 claims abstract description 16
- 238000003860 storage Methods 0.000 claims abstract description 15
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims abstract description 14
- 235000021314 Palmitic acid Nutrition 0.000 claims abstract description 10
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004367 Lipase Substances 0.000 claims abstract description 8
- 102000004882 Lipase Human genes 0.000 claims abstract description 8
- 108090001060 Lipase Proteins 0.000 claims abstract description 8
- 235000019421 lipase Nutrition 0.000 claims abstract description 8
- 239000000919 ceramic Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 58
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 239000011229 interlayer Substances 0.000 claims description 21
- 238000000746 purification Methods 0.000 claims description 13
- -1 isooctyl ester Chemical class 0.000 claims description 5
- 238000011084 recovery Methods 0.000 claims description 5
- 108010093096 Immobilized Enzymes Proteins 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 12
- 238000000034 method Methods 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 5
- 239000012528 membrane Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- FLIACVVOZYBSBS-UHFFFAOYSA-N Methyl palmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC FLIACVVOZYBSBS-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011942 biocatalyst Substances 0.000 description 1
- 230000002210 biocatalytic effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
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- Apparatus Associated With Microorganisms And Enzymes (AREA)
Abstract
The utility model relates to an isooctyl palmitate production technical field, in particular to isooctyl palmitate's device of esterifying, including the device of esterifying, the device pan feeding mouth of esterifying passes through pipeline and blending tank intercommunication, the pan feeding mouth of blending tank communicates with palmitic acid storage tank, isooctanol storage tank, petroleum ether storage tank through the pipeline respectively, the inside (mixing) shaft that is equipped with of device of esterifying, be equipped with a plurality of enzyme loading board around the (mixing) shaft center on the (mixing) shaft, the enzyme loading board is porous ceramic plate, and the fixed lipase of surface attachment, it is equipped with vertical vertically agitator to lie in enzyme loading board below on the (mixing) shaft. The esterification rate of the reaction time of 12h of the utility model can reach 99 percent, and the esterification rate of 12h can still reach 94 percent after the immobilized enzyme is used for 36 batches.
Description
Technical Field
The utility model relates to an isooctyl palmitate production technical field, in particular to an esterification device of isooctyl palmitate.
Background
Most of the methods for producing isooctyl palmitate at home and abroad are chemical methods, i.e. palmitic acid and isopropanol/isooctyl alcohol react with a catalyst at high temperature and high pressure to synthesize isooctyl palmitate. However, the chemical synthesis method has the defects of large energy consumption, dark product color, more side reactions, large pollution and the like, and the conversion rate is generally 85-92%. The reaction apparatus for producing biotechnological products using biocatalysts is called a biocatalytic reactor. The place where the catalyst is used for carrying out biological reaction is an enzyme reactor. Enzyme reactors can be classified into free enzyme reactors, i.e., homogeneous enzyme reactors, according to the type of enzyme catalyst; another class is heterogeneous enzyme reactors, i.e.immobilized enzyme reactors, which are carried out using immobilized enzymes. At present, no production equipment for producing isooctyl palmitate by using industrial immobilized enzyme exists.
Disclosure of Invention
The to-be-solved technical problem of the utility model is to provide an esterification device of isooctyl palmitate, can generate high-purity isooctyl palmitate, reaction condition is mild, the product is single-purpose, green.
The technical scheme of the utility model is that:
an esterification device of isooctyl palmitate comprises an esterification device, wherein a feeding port of the esterification device is communicated with a mixing tank through a pipeline, the feeding port of the mixing tank is respectively communicated with a palmitic acid storage tank, an isooctanol storage tank and a petroleum ether storage tank through pipelines, a stirring shaft is arranged in the esterification device, a plurality of enzyme bearing plates are arranged on the stirring shaft around the center of the stirring shaft, the enzyme bearing plates are porous ceramic plates, lipase is attached and fixed on the surfaces of the enzyme bearing plates, a stirrer vertical to the longitudinal direction is arranged below the enzyme bearing plates on the stirring shaft, first stirring blades are uniformly distributed on the stirring blades, the esterification device forms a circulation loop with the mixing tank through a circulating pump through a pipeline, a discharge port of the esterification device is also communicated with a purification tank through a pipeline, a first interlayer and a second interlayer are respectively arranged on the tank walls of the esterification device and the purification tank, and the second interlayer is communicated through a pipeline steam generator, the second interlayer is communicated with the first interlayer through a pipeline.
Preferably, the top of the purification tank is communicated with the first condenser, the second condenser, the petroleum ether recovery tank, the third condenser, the oil-water separator and the vacuum pump in sequence through pipelines.
Further preferably, a buffer tank is arranged between the oil-water separator vacuum pumps, and a check valve is further arranged between the vacuum pumps.
Preferably, the mixing tank is provided with a stirring device.
Preferably, the bottom of the oil-water separator is provided with a water outlet pipe, and the upper part of the oil-water separator is provided with an isooctyl ester discharge pipe.
Preferably, a second stirring blade and a third stirring blade are uniformly distributed above and below each enzyme bearing plate, and the width and the thickness of the second stirring blade and the third stirring blade are larger than those of the enzyme bearing plates.
Preferably, each enzyme bearing plate is fixed around a cylinder, and the cylinder is sleeved on the stirring shaft and is in sliding fit with the stirring shaft.
The utility model discloses beneficial effect:
1. the utility model discloses use palmitic acid, isooctanol as the raw materials, lipase is the catalyst, and the esterification rate of reaction 12h can reach 99%, and after 36 batches of immobilized enzyme use, the esterification rate of 12h still can reach 94%. The preparation method adopts the biomembrane reaction, the reaction condition is mild, and the byproducts are few.
2. The utility model provides a realize the continuous production of iso-octyl palmitate utilization immobilized enzyme as the catalyst, the reaction is mild, has avoided the agitator to rotate too fast, causes the destruction of immobilized enzyme. Wherein the stirrer which is vertical to the longitudinal direction is arranged below the enzyme bearing plate on the stirring shaft, and the first stirring blades are uniformly distributed on the stirring blades, so that the shearing force generated in the stirring process can be prevented from damaging the structure of the enzyme bearing plate. Second stirring leaf, third stirring leaf have evenly distributed about every enzyme bearing board, and the width and the thickness of second stirring leaf and third stirring leaf all are greater than the enzyme bearing board, and such setting up guarantees that at the in-process of stirring, and the reaction liquid stirring flow mainly is that second stirring leaf and third stirring leaf drive, can reduce the striking of enzyme bearing board, makes the immobilized enzyme can stably catalyze the esterification reaction. So that the method is simple and convenient.
3. The mixing tank is provided with a stirring device, and the palmitic acid, the isooctyl alcohol and the petroleum ether are fully mixed and then enter the enzyme membrane reactor for reaction.
4. The enzyme membrane reactor and the purification tank are respectively provided with a first interlayer and a second interlayer on the tank walls, the reaction temperature of the enzyme membrane reactor needs to be controlled at 40-42 ℃, and the second interlayer is communicated with the first interlayer through a pipeline, so that the waste heat in a reaction system can be fully utilized, and the heat consumption of the system is reduced.
5. The top of the purification tank is sequentially communicated with a first condenser, a second condenser, a petroleum ether recovery tank, a third condenser, an oil-water separator and a vacuum pump through pipelines, reduced pressure distillation is carried out, the isooctyl palmitate crude product is purified by utilizing the different boiling points of petroleum ether, isooctanol and water, and the raw material is separated for recycling.
6. The buffer tank is arranged between the oil-water separator vacuum pumps, so that the problem that the service life of equipment is influenced when solution is sucked into the vacuum pumps in the vacuumizing process is solved, the buffer tank is arranged between the vacuum pumps, the buffer tank is also provided with a check valve, the sudden stop of the vacuum pumps can be avoided, the check valve can be opened, the system is ensured to be in a closed state, and the purifying effect is not influenced.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic diagram of a structure of an enzyme-bearing plate according to the present invention;
wherein: the device comprises an esterification device 1, a first interlayer 112, a stirring shaft 101, an enzyme bearing plate 102, a stirrer 103, a first stirring blade 104, a second stirring blade 105, a third stirring blade 106, a cylinder 107, a mixing tank 2, a stirring device 21, a palmitic acid storage tank 3, an isooctanol storage tank 4, a petroleum ether storage tank 5, a purification tank 6, a second interlayer 61, a steam generator 7, a first condenser 8, a second condenser 9, a petroleum ether recovery tank 10, a third condenser 11, an oil-water separator 12, a water outlet pipe 121, an isooctyl ester discharge pipe 122, a buffer tank 13, a vacuum pump 14 and a check valve 15.
Detailed Description
The invention is further illustrated by the following examples, but the scope of the invention as claimed is not limited to the scope of the examples.
Example 1
An esterification device of isooctyl palmitate comprises an esterification device 1, wherein a feeding port of the esterification device 1 is communicated with a mixing tank 2 through a pipeline, a feeding port of the mixing tank 2 is respectively communicated with a palmitic acid storage tank 3, an isooctanol storage tank 4 and a petroleum ether storage tank 5 through pipelines, a stirring shaft 101 is arranged inside the esterification device 1, a plurality of enzyme bearing plates 102 are arranged on the stirring shaft 101 around the center of the stirring shaft 101, the enzyme bearing plates 1 are porous ceramic plates, lipase is adhered and fixed on the surfaces of the porous ceramic plates, a stirrer 103 vertical to the longitudinal direction is arranged below the enzyme bearing plates 102 on the stirring shaft 101, first stirring blades 104 are uniformly distributed on the stirring blades 103, the esterification device 1 forms a circulation loop with the mixing tank 2 through a circulation pump through a pipeline, a discharge port of the esterification device 1 is also communicated with a purification tank 6 through a pipeline, and the tank walls of the esterification device 1 and the purification tank 6 are respectively provided with a first interlayer, A second interlayer 61, the second interlayer 61 communicating with the pipe steam generator 7, the second interlayer 61 communicating with the first interlayer 12 through a pipe.
Preferably, the top of the purification tank 6 is communicated with a first condenser 8, a second condenser 9, a petroleum ether recovery tank 10, a third condenser 11, an oil-water separator 12 and a vacuum pump 14 in sequence through pipelines.
Further preferably, a buffer tank 13 is disposed between the vacuum pumps 14 of the oil-water separator 12, and a check valve 15 is further disposed between the vacuum pumps 14 and the buffer tank 13.
Preferably, the mixing tank 2 is provided with stirring means 21.
Preferably, a water outlet pipe 121 is arranged at the bottom of the oil-water separator 12, and an isooctyl ester discharge pipe 122 is arranged above the oil-water separator.
Preferably, a second stirring blade 105 and a third stirring blade 106 are uniformly distributed above and below each enzyme bearing plate 102, and the width and thickness of the second stirring blade 105 and the third stirring blade 106 are larger than those of the enzyme bearing plate 102.
Preferably, each enzyme carrier plate 102 is fixed around a cylinder 107, and the cylinder 107 is sleeved on the stirring shaft 101 and is in sliding fit with the stirring shaft 101.
The utility model discloses during the use, at first add palmitic acid in the blending tank 2, isooctanol, petroleum ether, add fixed lipase in the immobilized enzyme rete 11 in the enzyme membrane reactor 1, the solid-to-liquid ratio of palmitic acid, isooctanol, petroleum ether, fixed lipase is 200-, and the steam generator 7 is communicated, petroleum ether is firstly evaporated at the temperature of 30-80 ℃, condensed by the first condenser 8 and recycled to the petroleum ether recycling tank 9, subsequent water vapor with residual isooctanol enters the third condenser 11 to be cooled into aqueous solution, the aqueous solution containing the isooctanol flows into the oil-water separator 12 to be collected, and is separated by the water outlet pipe 121 and the isooctyl ester discharge pipe 122.
Firstly, putting reaction substrates of methyl palmitate and isooctyl alcohol into a bioreactor for preheating, then adding the adsorbent and lipase, controlling the temperature of an enzyme catalysis system and the operation condition of the reactor, completing the catalytic reaction for 1-4 hours under the condition of no other solvent, and performing gas phase detection analysis on a sample to obtain the isooctyl palmitate with the yield of more than 99 percent and the highest 99.65 percent.
Claims (7)
1. An esterification device of isooctyl palmitate, which comprises an esterification device (1) and is characterized in that a feeding port of the esterification device (1) is communicated with a mixing tank (2) through a pipeline, the feeding port of the mixing tank (2) is respectively communicated with a palmitic acid storage tank (3), an isooctanol storage tank (4) and a petroleum ether storage tank (5) through pipelines, a stirring shaft (101) is arranged inside the esterification device (1), a plurality of enzyme bearing plates (102) are arranged on the stirring shaft (101) around the center of the stirring shaft (101), the enzyme bearing plates (102) are porous ceramic plates, lipase is fixedly attached to the surfaces of the enzyme bearing plates, stirring blades (103) which are vertical to the longitudinal direction are arranged below the enzyme bearing plates (102) on the stirring shaft (101), first stirring blades (104) are uniformly distributed on the stirring blades (103), and the esterification device (1) forms a circulation loop with the mixing tank (2) through a pipeline and a circulating pump, the device for purifying the esterification reaction comprises an esterification device (1) and a purification tank (6), wherein a discharge hole of the esterification device (1) is communicated with the purification tank (6) through a pipeline, a first interlayer (112) and a second interlayer (61) are respectively arranged on tank walls of the esterification device (1) and the purification tank (6), the second interlayer (61) is communicated with a pipeline steam generator (7), and the second interlayer (61) is communicated with the first interlayer (112) through a pipeline.
2. The apparatus for esterification of isooctyl palmitate according to claim 1, wherein the top of said purification tank (6) is connected in series via piping to a first condenser (8), a second condenser (9), a petroleum ether recovery tank (10), a third condenser (11), an oil-water separator (12) and a vacuum pump (14).
3. The apparatus for esterifying isooctyl palmitate according to claim 2, wherein a buffer tank (13) is provided between the vacuum pumps (14) of the oil-water separator (12), and a check valve (15) is further provided between the vacuum pumps (14) and the buffer tank (13).
4. The apparatus for the esterification of isooctyl palmitate according to claim 3, wherein said mixing tank (2) is provided with a stirring device (21).
5. The apparatus for esterifying isooctyl palmitate according to claim 3, wherein said oil-water separator (12) has a water outlet pipe (121) at the bottom and an isooctyl ester outlet pipe (122) at the top.
6. The esterification apparatus according to claim 1, wherein the second stirring blade (105) and the third stirring blade (106) are uniformly distributed above and below each enzyme carrying plate (102), and the width and thickness of the second stirring blade (105) and the third stirring blade (106) are larger than those of the enzyme carrying plate (102).
7. The apparatus for the esterification of isooctyl palmitate according to claim 1, wherein each of said enzyme carrying plates (102) is fixed around a cylinder (107), the cylinder (107) being fitted over the stirring shaft (101) in sliding engagement with the stirring shaft (101).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920608429.7U CN210394392U (en) | 2019-04-29 | 2019-04-29 | Esterification device of isooctyl palmitate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920608429.7U CN210394392U (en) | 2019-04-29 | 2019-04-29 | Esterification device of isooctyl palmitate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN210394392U true CN210394392U (en) | 2020-04-24 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201920608429.7U Expired - Fee Related CN210394392U (en) | 2019-04-29 | 2019-04-29 | Esterification device of isooctyl palmitate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN210394392U (en) |
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2019
- 2019-04-29 CN CN201920608429.7U patent/CN210394392U/en not_active Expired - Fee Related
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| GR01 | Patent grant | ||
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
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Granted publication date: 20200424 |