CN112299993B - Device and method for producing tributyrin - Google Patents
Device and method for producing tributyrin Download PDFInfo
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- CN112299993B CN112299993B CN202011190407.7A CN202011190407A CN112299993B CN 112299993 B CN112299993 B CN 112299993B CN 202011190407 A CN202011190407 A CN 202011190407A CN 112299993 B CN112299993 B CN 112299993B
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
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- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
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Abstract
The invention discloses a device for producing tributyrin, which comprises: the device comprises a glycerol storage tank, a butyric acid storage tank, a synthesis reaction kettle, a synthesis flash tank, a synthesis flash heater, a condenser and a rectifying device; the glycerol storage tank and the butyric acid storage tank are both arranged at the top end of the synthesis reaction kettle; the top end of the synthesis reaction kettle is also provided with a catalyst inlet and a fractionating column; the top end of the synthesis reaction kettle is also connected with a synthesis flash tank, a synthesis flash heater, a condenser and a rectifying device in sequence. The device is simple, and the glycerol storage tank is arranged to save energy and recycle waste; in addition, the rectification device is arranged in the invention to obtain the product with high purity.
Description
Technical Field
The invention relates to the technical field of chemical synthesis, in particular to a device and a method for producing tributyrin.
Background
The biodiesel byproduct glycerol is used for producing tributyrin, so that the extension of the industrial chain of downstream products of biodiesel products can be increased, and products with higher added values can be produced by utilizing the byproducts.
Tributyrin has wide application in animal husbandry cultivation, tributyrin is not decomposed in gastric juice, and is slowly released into butyric acid and glycerol under the action of pancreatic lipase, so that small intestinal villi is repaired, harmful bacteria in intestinal tracts are inhibited, and absorption and utilization of nutrient substances are promoted. The tributyrin is used on young animals, and has the effects of reducing diarrhea of young animals after weaning, reducing weaning stress, increasing survival rate and increasing daily gain. The main uses in animal husbandry can be summarized as follows:
1. full gastric-100% gastric;
2. enteritis-preventing-effective absorption of at least 100ppm butyric acid by the hindgut, prevention of nutritional diarrhea and proliferative ileitis in the colon segment;
3. the mucous membrane is protected, namely, three points of the foregut, the midgut and the hindgut are uniformly absorbed, so that the damage of the intestinal mucous membrane is effectively repaired, and the intestinal mucous membrane is comprehensively protected;
4. promoting lactation, namely promoting feed intake of sows and promoting lactation of sows;
5. quick energy supply-quick energy supply for intestinal mucosa cells, and quick growth and development of the intestinal mucosa are promoted;
6. growth uniformity-promoting weaned pigs to eat, improving nutrient absorption and remarkably improving uniformity of pig groups.
It can be seen that tributyrin has potential application value, however, no method for producing tributyrin by using biodiesel byproducts is currently adopted.
Therefore, how to provide a device and a method for producing tributyrin with simple device, high efficiency and energy saving are the problems to be solved by the person skilled in the art.
Disclosure of Invention
In view of the above, the invention provides a device and a method for producing tributyrin, which are simple in device, high in efficiency and energy-saving, and the produced tributyrin has excellent comprehensive performance and high purity.
In order to achieve the above purpose, the present invention adopts the following technical scheme: an apparatus for producing tributyrin, comprising: the device comprises a glycerol storage tank, a butyric acid storage tank, a synthesis reaction kettle, a synthesis flash tank, a synthesis flash heater, a condenser and a rectifying device;
the glycerol storage tank and the butyric acid storage tank are both arranged at the top end of the synthesis reaction kettle; the top end of the synthesis reaction kettle is also provided with a catalyst inlet and a fractionating column;
the top end of the synthesis reaction kettle is also connected with the synthesis flash tank, the synthesis flash heater, the condenser and the rectifying device in sequence.
The invention has the beneficial effects that: the device is simple, and the glycerol storage tank is arranged to save energy and recycle waste; in addition, the rectification device is arranged in the invention to obtain the product with high purity.
Preferably, the method further comprises: a synthesis reaction pump, a synthesis flash pump and a filter;
one end of the synthesis reaction pump is connected with the bottom end of the synthesis reaction kettle, and the other end of the synthesis reaction pump is connected with the top end of the synthesis reaction kettle; one end of the synthetic flash pump is connected with the bottom end of the synthetic flash tank, and the other end of the synthetic flash pump is connected with the bottom end of the synthetic flash heater; the filter is respectively connected with the condenser and the rectifying device.
The beneficial effect of adopting above-mentioned scheme: the purpose of the pump is to provide pressure for the materials in the synthesis reaction kettle and the synthesis flash tank and pump the materials into all needed components; the filter is provided for further removal of impurities.
Preferably, the rectifying device comprises a rectifying tower, a first falling film heater, a first cooler, a first temporary storage tank and a byproduct recovery device;
the filter is sequentially connected with the first falling film heater and the bottom of the rectifying tower; the middle part of the rectifying tower is sequentially connected with the first cooler, the first temporary storage tank and the tributyrin storage tank; the top of the rectifying tower is connected with the byproduct recovery device.
The beneficial effect of adopting above-mentioned scheme: the byproduct recovery device is arranged to store the obtained byproducts (monobutyric anhydride grease and dibutyric glyceride) and supply the byproducts to the synthesis reaction kettle. The energy loss is reduced by recycling.
Preferably, the method further comprises: and the second falling film heater is arranged at the bottom of the rectifying tower.
Preferably, the byproduct recovering device comprises a second cooler, a second temporary storage tank and a byproduct storage tank;
the top of the rectifying tower is sequentially connected with the second cooler, the second temporary storage tank and the byproduct storage tank.
Preferably, the rectification apparatus further comprises: the bottom residual liquid storage tank is connected with the bottom end of the rectifying tower; circulation pumps are arranged between the bottom of the rectifying tower and the second falling film heater, between the first temporary storage tank and the glyceride storage tank at the three top ends, between the top of the rectifying tower and the second temporary storage tank, and between the second temporary storage tank and the byproduct storage tank.
The beneficial effect of adopting above-mentioned scheme: the arrangement of the residual liquid storage tank at the bottom of the tower avoids environmental pollution caused by waste, thereby achieving the effect of environmental protection.
The invention also provides a method for producing tributyrin, which is characterized by comprising the following steps:
(1) Pumping glycerol in a glycerol storage tank and part of butyric acid in a butyric acid storage tank into a synthesis reaction kettle under the protection of nitrogen, heating to 60-100 ℃, starting stirring and mixing uniformly, adding p-toluenesulfonic acid serving as a catalyst into the synthesis reaction kettle through a catalyst inlet, heating the synthesis reaction kettle to 120-180 ℃, controlling the temperature of a distillation head of a fractionating column to be 100-120 ℃, reacting, pumping the rest butyric acid into the synthesis reaction kettle, controlling the temperature to be 120-180 ℃, and reacting for 3-10 hours to obtain a mixture A;
(2) Pumping the mixture A into a synthesis flash tank, heating and flashing by a synthesis flash heater, pumping the product into a condenser to reduce the temperature to below 80 ℃, and pumping the product into a rectifying device to obtain refined tributyrin.
The preparation method provided by the invention has the advantages that the steps are tightly connected, and the preparation method is used for preparing the tributyrin with high purity and good performance. According to the invention, the butyric acid is thoroughly removed after flash evaporation, so that the high purity of the product is ensured; the distillation head is adopted to control the temperature, the water is controlled to be distilled out, and the butyric acid flows back to the reaction kettle for continuous reaction, so that the consumption of the butyric acid is reduced.
Preferably, in the step (1), the mass ratio of the glycerin to the butyric acid is 1: (3-5.8), wherein the mass ratio of the part of butyric acid to the glycerol is (2.0-3.0): 1, a step of; the addition amount of the p-toluenesulfonic acid is 0.1-1.0% of the total weight of the glycerin and the butyric acid; the stirring speed is 60-80r/min.
Preferably, in the step (2), the heating flash time is 2-3h, and the temperature is 100-160 ℃.
Preferably, in the step (2), the rectification temperature is 100-200 ℃, and the reflux ratio is controlled to be 1: (0.8-2).
Compared with the prior art, the device and the method for producing the tributyrin are provided, and the device is simple, low in cost, energy-saving and environment-friendly; the tributyrin obtained by adopting the device and the process has high purity, high yield and excellent comprehensive performance, can improve animal production performance, is an optimal substitute for antibiotics growth promoters, and can be widely applied to animal cultivation and the like; the glycerol adopted in the invention is a byproduct of biodiesel, has the advantages of raw material and low cost, prolongs the industrial chain of biodiesel, and improves economic benefit; the content of tributyrin is improved by rectification, the tributyrin content of the company reaches more than 99 percent, and the content of high-purity tributyrin in the current market is generally more than 9 percent. .
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a flash process according to the present invention;
FIG. 2 is a schematic diagram of the rectification process according to the present invention;
the device comprises a 1-glycerin storage tank, a 2-synthesis reaction kettle, a 3-synthesis flash heater, a 4-condenser, a 5-rectifying device, a 6-filter, a 7-synthesis reaction pump, an 8-synthesis flash pump, a 9-butyric acid recovery system, a 10-butyric acid storage tank, a 11-synthesis flash tank, a 12-catalyst inlet, a 51-rectifying tower, a 52-first falling film heater, a 53-first cooler, a 54-first temporary storage tank, a 55-tributyrin storage tank, a 56-second falling film heater, a 57-second cooler, a 58-second temporary storage tank, a 59-byproduct storage tank, a 60-tower bottom residual liquid storage tank, a 61-circulating pump I, a 62-circulating pump II, a 63-circulating pump III, a 64-circulating pump VI and a 65-circulating pump V.
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. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The embodiment of the invention discloses a device for producing tributyrin, which comprises: a glycerin storage tank 1, a butyric acid storage tank 10, a synthesis reaction kettle 2, a synthesis flash tank 11, a synthesis flash heater 3, a condenser 4 and a rectifying device 5;
the glycerin storage tank 1 and the butyric acid storage tank 10 are both arranged at the top end of the synthesis reaction kettle 2; the top end of the synthesis reaction kettle 2 is also provided with a catalyst inlet 12 and a fractionating column;
the top end of the synthesis reaction kettle 2 is also connected with a synthesis flash tank 11, a synthesis flash heater 3, a condenser 4 and a rectifying device 5 in sequence.
The device is simple, and the glycerol storage tank 1 is arranged to save energy and recycle waste; in addition, the rectification device 5 is arranged in the invention to obtain a product with high purity.
In one embodiment, further comprising: a synthesis reaction pump 7, a synthesis flash pump 8 and a filter 6;
one end of the synthesis reaction pump 7 is connected with the bottom end of the synthesis reaction kettle 2, and the other end is connected with the top end of the synthesis reaction kettle 2; one end of the synthetic flash pump 8 is connected with the bottom end of the synthetic flash tank 11, and the other end is connected with the bottom end of the synthetic flash heater 3; the filters 6 are connected to the condenser 4 and the rectifying device 5, respectively.
The purpose of the pump is to provide pressure to the materials in the synthesis reaction kettle 2 and the synthesis flash tank 11 and pump the materials into all the required components; the filter 6 is provided for further removal of impurities.
In one embodiment, the rectifying device 5 includes a rectifying column 51, a first falling film heater 52, a first cooler 53, a first temporary storage tank 54, a tributyrin storage tank 55, and a byproduct recovery device;
the filter 6 is connected with the first falling film heater 52 and the bottom of the rectifying tower 51 in sequence; the middle part of the rectifying tower 51 is sequentially connected with a first cooler 53, a first temporary storage tank 54 and a tributyrin storage tank 55; the top of the rectifying column 51 is connected to a byproduct recovery apparatus.
The byproduct recovery device is provided to store the obtained byproducts (monobutyraldehyde anhydride oil and dibutyraldehyde glyceride) and supply the same to the synthesis reaction kettle 2. The energy loss is reduced by recycling.
In one embodiment, further comprising: the second falling film heater 56, the second falling film heater 56 is installed at the bottom of the rectifying tower 51.
In one embodiment, the byproduct recovery apparatus includes a second cooler 57, a second temporary storage tank 58, and a byproduct storage tank 59;
the top of the rectifying tower 51 is connected to a second cooler 57, a second temporary storage tank 58, and a byproduct storage tank 59 in this order.
In one embodiment, the rectifying device 5 further comprises: a bottom raffinate storage tank 60 and a plurality of circulating pumps, wherein the bottom raffinate storage tank 60 is connected with the bottom end of the rectifying tower 51; circulation pumps are arranged between the bottom of the rectifying tower 51 and the second falling film heater 56, between the first temporary storage tank 54 and the triglyceride storage tank at the three top ends, between the top of the rectifying tower 51 and the second temporary storage tank 58, and between the second temporary storage tank 58 and the byproduct storage tank 59. The arrangement of the residual liquid storage tank 60 at the bottom of the tower avoids the environmental pollution caused by waste, thereby achieving the effect of protecting the environment.
Example 1
The method for producing tributyrin by adopting the device comprises the following steps:
(1) Under the protection of nitrogen, firstly, glycerin containing glycerin in a glycerin storage tank 1 and butyric acid in a butyric acid storage tank 10 are mixed according to the mass ratio of 1:2.0 pumping into a synthesis reaction kettle 2, heating to 60 ℃, starting stirring, uniformly mixing at the speed of 60r/min, adding p-toluenesulfonic acid serving as a catalyst into the synthesis reaction kettle 2 through a catalyst inlet 12, heating the synthesis reaction kettle 2 to 120 ℃, controlling the temperature of a distillation head of a fractionating column at 100 ℃, reacting for 1h, and steaming out water generated by the reaction; then the mass ratio of the butyric acid to the glycerol is 1:1, pumping the mixture into a synthesis reaction kettle 2, controlling the temperature to be 120 ℃, and reacting for 3 hours, wherein when the water discharged from a distillation head is 55% of the weight of glycerol, the mixture A is obtained after the reaction; wherein the mass ratio of glycerin to total butyric acid is 3:1, the adding amount of the p-toluenesulfonic acid is 0.1% of the total weight of the glycerin and the butyric acid;
(2) Pumping the mixture A into a synthesis flash evaporation heater 3 through a synthesis reaction pump 7 and a synthesis flash evaporation pump 8, then entering a synthesis flash evaporation tank 11, controlling the synthesis flash evaporation tank 11 to heat and flash at 100 ℃ under vacuum of-0.1 MPa for 2 hours, pumping the product into a condenser 4 to cool to 80 ℃, pumping the product into a filter 6, and filtering to remove trace impurities to obtain crude tributyrin; the residual butyric acid in the synthesis flash tank 11 enters the butyric acid recovery system 9 for recovery;
(3) The crude tributyrin was passed through the first falling film heater 52 to a vacuum of 50Pa, and the reflux ratio was controlled at 1:0.8, controlling the temperature in the rectifying tower 51 to be 150 ℃ through the second falling film heater 56, controlling the tower top temperature to be 100 ℃ and providing power for the second falling film heater 56 through the circulating pump I61; the tributyrin distilled by the crude tributyrin in the rectifying tower 51 is cooled to 30 ℃ by a first cooler 53, and then enters a refined tributyrin storage tank 55 for storage through a first temporary storage tank 54 and a circulating pump II 62;
the byproducts pass through the top of the rectifying tower 51, enter the second cooler 57 through the circulating pump III 63 to be cooled to 30 ℃, and enter the byproduct storage tank 59 through the second temporary storage tank 58 and the circulating pump VI 64 for standby;
the residual liquid at the bottom of the rectifying tower 51 is pumped into a residual liquid storage tank 60 at the bottom of the tower through a circulating pump V65 for recovery, thereby avoiding environmental pollution.
Example 2
The method for producing tributyrin by adopting the device comprises the following steps:
(1) Under the protection of nitrogen, firstly, glycerin containing glycerin in a glycerin storage tank 1 and butyric acid in a butyric acid storage tank 10 are mixed according to the mass ratio of 1:3.0 pumping into a synthesis reaction kettle 2, heating to 100 ℃, starting stirring, uniformly mixing at the speed of 80r/min, adding p-toluenesulfonic acid serving as a catalyst into the synthesis reaction kettle 2 through a catalyst inlet 12, heating the synthesis reaction kettle 2 to 180 ℃, controlling the temperature of a distillation head of a fractionating column at 120 ℃, reacting for 2 hours, and steaming out water generated by the reaction; then the mass ratio of the butyric acid to the glycerol is 2.8:1, pumping the mixture into a synthesis reaction kettle 2, controlling the temperature to be 180 ℃, reacting for 10 hours, and obtaining a mixture A after the reaction is finished when the water discharged from a distillation head is 70% of the weight of glycerol; wherein the mass ratio of glycerin to butyric acid is 1:5.8, the adding amount of the p-toluenesulfonic acid is 1.0% of the total weight of the glycerin and the butyric acid;
(2) Pumping the mixture A into a synthesis flash evaporation heater 3 through a synthesis reaction pump 7 and a synthesis flash evaporation pump 8, then entering a synthesis flash evaporation tank 11, controlling the synthesis flash evaporation tank 11 to heat and flash at 160 ℃ under vacuum of-0.1 MPa for 3 hours, pumping the product into a condenser 4 to cool to 75 ℃, pumping the product into a filter 6, and filtering to remove trace impurities to obtain crude tributyrin; the residual butyric acid in the synthesis flash tank 11 enters the butyric acid recovery system 9 for recovery;
(3) The crude tributyrin was passed through the first falling film heater 52 to a vacuum of 200Pa, and the reflux ratio was controlled at 1:2, controlling the temperature in the rectifying tower 51 to be 200 ℃ through a second falling film heater 56, controlling the tower top temperature to be 150 ℃ and providing power for the second falling film heater 56 through a circulating pump I61; the tributyrin distilled by the crude tributyrin in the rectifying tower 51 is cooled to 40 ℃ by a first cooler 53, and then enters a refined tributyrin storage tank 55 for storage through a first temporary storage tank 54 and a circulating pump II 62;
the byproducts pass through the top of the rectifying tower 51, enter the second cooler 57 through the circulating pump III 63 to be cooled to 40 ℃, and enter the byproduct storage tank 59 through the second temporary storage tank 58 and the circulating pump VI 64 for standby;
the residual liquid at the bottom of the rectifying tower 51 is pumped into a residual liquid storage tank 60 at the bottom of the tower through a circulating pump V65 for recovery, thereby avoiding environmental pollution.
Example 3
The method for producing tributyrin by adopting the device comprises the following steps:
(1) Under the protection of nitrogen, firstly, glycerin containing glycerin in a glycerin storage tank 1 and butyric acid in a butyric acid storage tank 10 are mixed according to the mass ratio of 1:2.5 pumping the mixture into a synthesis reaction kettle 2 to raise the temperature to 80 ℃, starting stirring and uniformly mixing at the speed of 70r/min, adding p-toluenesulfonic acid serving as a catalyst into the synthesis reaction kettle 2 through a catalyst inlet 12, raising the temperature of the synthesis reaction kettle 2 to 150 ℃, controlling the temperature of a distillation head of a fractionating column at 110 ℃ for 1.5h, and steaming out water generated by the reaction; pumping the mixture into a synthesis reaction kettle 2 according to the mass ratio of butyric acid to glycerol of 1.9:1, controlling the temperature at 150 ℃ for reaction for 6 hours, and obtaining a mixture A after the reaction is finished when the water discharged from a distillation head is 65% of the weight of the glycerol; wherein the mass ratio of glycerin to butyric acid is 1:4.4, the adding amount of the p-toluenesulfonic acid is 0.5% of the total weight of the glycerin and the butyric acid;
(2) Pumping the mixture A into a synthesis flash evaporation heater 3 through a synthesis reaction pump 7 and a synthesis flash evaporation pump 8, then entering a synthesis flash evaporation tank 11, controlling the synthesis flash evaporation tank 11 to heat and flash at 130 ℃ under vacuum of-0.1 MPa for 2 hours, pumping the product into a condenser 4 to cool to 80 ℃, pumping the product into a filter 6, and filtering to remove trace impurities to obtain crude tributyrin; the residual butyric acid in the synthesis flash tank 11 enters the butyric acid recovery system 9 for recovery;
(3) The crude tributyrin was passed through the first falling film heater 52 to a vacuum of 100Pa, and the reflux ratio was controlled at 1:1.9, controlling the temperature in the rectifying tower 51 to be 170 ℃ through a second falling film heater 56, controlling the tower top temperature to be 130 ℃ and providing power for the second falling film heater 56 through a circulating pump I61; the tributyrin distilled by the crude tributyrin in the rectifying tower 51 is cooled to 50 ℃ by a first cooler 53, and then enters a refined tributyrin storage tank 55 for storage through a first temporary storage tank 54 and a circulating pump II 62;
the byproducts pass through the top of the rectifying tower 51, enter the second cooler 57 through the circulating pump III 63 to be cooled to 50 ℃, and enter the byproduct storage tank 59 through the second temporary storage tank 58 and the circulating pump VI 64 for standby;
the residual liquid at the bottom of the rectifying tower 51 is pumped into a residual liquid storage tank 60 at the bottom of the tower through a circulating pump V65 for recovery, thereby avoiding environmental pollution.
Performance testing
Determination of the purity and Properties of tributyrin obtained in examples 1 to 3 of the invention
As can be seen from the above table, the tributyrin obtained in the present invention has high purity, low acid value and outstanding properties.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. An apparatus for producing tributyrin, comprising: the device comprises a glycerol storage tank, a butyric acid storage tank, a synthesis reaction kettle, a synthesis flash tank, a synthesis flash heater, a condenser and a rectifying device;
the glycerol storage tank and the butyric acid storage tank are both arranged at the top end of the synthesis reaction kettle; the top end of the synthesis reaction kettle is also provided with a catalyst inlet and a fractionating column;
the top end of the synthesis reaction kettle is also connected with the synthesis flash tank, the synthesis flash heater, the condenser and the rectifying device in sequence;
further comprises: a synthesis reaction pump, a synthesis flash pump and a filter;
one end of the synthesis reaction pump is connected with the bottom end of the synthesis reaction kettle, and the other end of the synthesis reaction pump is connected with the top end of the synthesis reaction kettle; one end of the synthetic flash pump is connected with the bottom end of the synthetic flash tank, and the other end of the synthetic flash pump is connected with the bottom end of the synthetic flash heater; the filter is respectively connected with the condenser and the rectifying device;
the rectifying device comprises a rectifying tower, a first falling film heater, a first cooler, a first temporary storage tank, a tributyrin storage tank and a byproduct recovery device;
the filter is sequentially connected with the first falling film heater and the bottom of the rectifying tower; the middle part of the rectifying tower is sequentially connected with the first cooler, the first temporary storage tank and the tributyrin storage tank; the top of the rectifying tower is connected with the byproduct recovery device;
further comprises: and the second falling film heater is arranged at the bottom of the rectifying tower.
2. The apparatus for producing tributyrin according to claim 1, wherein said byproduct recovery apparatus comprises a second cooler, a second temporary storage tank, and a byproduct storage tank;
the top of the rectifying tower is sequentially connected with the second cooler, the second temporary storage tank and the byproduct storage tank.
3. The apparatus for producing tributyrin according to claim 2, wherein said rectifying apparatus further comprises: the bottom residual liquid storage tank is connected with the bottom end of the rectifying tower; circulation pumps are arranged between the bottom of the rectifying tower and the second falling film heater, between the first temporary storage tank and the tributyrin storage tank, between the top of the rectifying tower and the second temporary storage tank, and between the second temporary storage tank and the byproduct storage tank.
4. A method for producing tributyrin using the apparatus as claimed in any one of claims 1-3, comprising the steps of:
(1) Pumping glycerol in a glycerol storage tank and part of butyric acid in a butyric acid storage tank into a synthesis reaction kettle under the protection of nitrogen, heating to 60-100 ℃, starting stirring and mixing uniformly, adding p-toluenesulfonic acid serving as a catalyst into the synthesis reaction kettle through a catalyst inlet, heating the synthesis reaction kettle to 120-180 ℃, controlling the temperature of a distillation head of a fractionating column to be 100-120 ℃, reacting, pumping the rest butyric acid into the synthesis reaction kettle, controlling the temperature to be 120-180 ℃, and reacting for 3-10 hours to obtain a mixture A;
(2) Pumping the mixture A into a synthesis flash tank, heating and flashing by a synthesis flash heater, pumping the product into a condenser to reduce the temperature to below 80 ℃, and pumping the product into a rectifying device to obtain refined tributyrin.
5. The method for producing tributyrin according to claim 4, wherein in step (1), the mass ratio of glycerin to total butyric acid is 1: (3-5.8), the mass ratio of the part of butyric acid to the glycerol is (2.0-3.0): 1, a step of; the addition amount of the p-toluenesulfonic acid is 0.1-1.0% of the total weight of the glycerin and the butyric acid; the stirring speed is 60-80r/min.
6. The method for producing tributyrin according to claim 4, wherein in step (2), the heating flash time is 2 to 3 hours and the temperature is 100 to 160 ℃.
7. The method for producing tributyrin according to claim 4, wherein in step (2), the rectification temperature is 100 to 200 ℃, and the reflux ratio is controlled to be 1: (0.8-2).
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB729305A (en) * | 1951-05-16 | 1955-05-04 | Standard Oil Dev Co | Improvements in or relating to process for the manufacture of esters |
| CN101735049A (en) * | 2009-12-18 | 2010-06-16 | 沈阳工业大学 | Method and equipment for producing C4-C6 diacid low-carbon alcohol ester |
| CN104098469A (en) * | 2014-07-25 | 2014-10-15 | 安徽华业香料股份有限公司 | Device for synthesizing tricyclodecenyl propionate by adopting loaded solid acid catalyst |
| CN206318903U (en) * | 2016-12-14 | 2017-07-11 | 焦作大学 | A kind of synthesizer for being used to prepare glyceryl triacetate |
| CN107652180A (en) * | 2016-07-23 | 2018-02-02 | 天津晶林新材料科技有限公司 | The production method of tributyrin |
-
2020
- 2020-10-30 CN CN202011190407.7A patent/CN112299993B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB729305A (en) * | 1951-05-16 | 1955-05-04 | Standard Oil Dev Co | Improvements in or relating to process for the manufacture of esters |
| CN101735049A (en) * | 2009-12-18 | 2010-06-16 | 沈阳工业大学 | Method and equipment for producing C4-C6 diacid low-carbon alcohol ester |
| CN104098469A (en) * | 2014-07-25 | 2014-10-15 | 安徽华业香料股份有限公司 | Device for synthesizing tricyclodecenyl propionate by adopting loaded solid acid catalyst |
| CN107652180A (en) * | 2016-07-23 | 2018-02-02 | 天津晶林新材料科技有限公司 | The production method of tributyrin |
| CN206318903U (en) * | 2016-12-14 | 2017-07-11 | 焦作大学 | A kind of synthesizer for being used to prepare glyceryl triacetate |
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