CN118184994A - Deodorization lift pipe for ester synthesis and deodorization method for ester synthesis - Google Patents
Deodorization lift pipe for ester synthesis and deodorization method for ester synthesis Download PDFInfo
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- CN118184994A CN118184994A CN202410319909.7A CN202410319909A CN118184994A CN 118184994 A CN118184994 A CN 118184994A CN 202410319909 A CN202410319909 A CN 202410319909A CN 118184994 A CN118184994 A CN 118184994A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/34—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a deodorizing riser for ester synthesis and a deodorizing method for ester synthesis, belonging to the technical field of chemical treatment. The deodorizing method for ester synthesis provided by the invention comprises the following steps: the synthesis reaction of the polyglycerol ester is carried out in the reaction kettle in a sectional heating mode; in the later stage of the reaction, the vacuum degree in the reaction kettle is regulated to be-0.06-0.099 MPa; the deodorizing riser for ester synthesis of the present invention is used in exhausting and recovering partial material and eliminating unpleasant smell via the tray set with deodorizing riser. The invention solves the problem of unpleasant odor generated in the production process of the polyglycerol ester, and protects the environment and human body safety to a certain extent; solves the problem that the distillate distilled in the synthesis process of the polyglycerol ester is recycled, and reduces the water consumption and the water discharge.
Description
The application relates to a divisional application of a deodorizing method in ester synthesis, which has the application date of 2018, 12, 29, the application number of CN 201811636741.3.
Technical Field
The invention belongs to the technical field of chemical treatment, and particularly relates to a deodorizing riser for ester synthesis and a deodorizing method for ester synthesis.
Background
The polyglycerol fatty acid ester is called polyglycerol ester for short, and is a novel, efficient and excellent-performance polyhydroxy ester nonionic surfactant. Because they have good multiple surface properties such as emulsification, dispersion, wetting, stability, etc., they can be decomposed in the metabolic process of human body, thus participating in metabolism, being utilized by human body, having high safety and very wide application field. In particular, in the food industry, food sanitation and safety are becoming more and more interesting today, and the development of nontoxic and environment-friendly surfactants is becoming an important content in the research of the field of food additives, and polyglycerin fatty acid esters are an additive which is recognized by people in terms of excellent safety and excellent surface activity. The FDA/WHO food additive expert Committee has confirmed that 30 or more polyglyceryl fatty acid esters food emulsifiers, which have been approved in the United states, japan, europe, china, etc., are used as food emulsifiers. At the same time, it is widely applied to medical products daily chemical industry and material auxiliary agent and the like. Compared with other polyhydroxy fatty acid esters, the modified fatty acid ester not only has strong salt resistance, acid resistance and heat resistance, but also has outstanding surface application performance. The polyglycerol fatty acid ester is a safe and environment-friendly surfactant, has wide HLB value distribution due to different structures, and therefore has a very wide application range. The existing polyglycerol ester preparation process is generally carried out in two steps: firstly, preparing polyglycerol by condensation reaction of glycerol or addition reaction of glyceride and glycerol; the second polyglycerol is obtained by direct esterification with fatty acids, which is one of the most widely used methods in industry today, or transesterification with triglycerides. The key point of the production of polyglycerol ester is that the polyglycerol polymerization is carried out at high temperature, the reaction time is prolonged continuously along with the larger polymerization degree of the polyglycerol, the color of the product is deepened continuously, and serious side reaction is accompanied, so that the odor of the polymerized product is increased. The prior production of the polyglycerol ester cannot avoid that the polyglycerol ester can generate unpleasant smell in the high-temperature synthesis process, and seriously influence the application and popularization of the polyglycerol ester. Therefore, improving the production process and improving the product quality has important significance, and is also helpful for promoting the development of other application fields such as food, medicine, cosmetics and the like.
Disclosure of Invention
In view of the above, the invention provides a deodorizing riser for ester synthesis and a deodorizing method for ester synthesis, which solve the problem of unpleasant odor generated in the production process of polyglycerol ester and protect the environment and human personal safety to a certain extent; solves the problem that the distillate distilled in the synthesis process of the polyglycerol ester is recycled, and reduces the water consumption and the water discharge.
The technical scheme of the invention is as follows:
The deodorizing lift pipe for ester synthesis comprises a pipe body (1), wherein a support column (2) is arranged in the central area of the pipe body, and tower plate groups (3) are symmetrically arranged in the pipe body by the support column; the column plate group (3) comprises a plurality of first column plates (31) and a plurality of second column plates (32), and the first column plates (31) and the second column plates (32) are arranged in a staggered manner;
the horizontal section of the first tower plate (31) is semicircular; the middle part of the first tower plate (31) is provided with a mounting groove (311), and the mounting groove (311) is connected with the support column (2) in a matching way;
The first tower plate (31) is symmetrically provided with liquid dropping holes (312), the first tower plate (31) is of a hollow structure, and an adsorption layer (313) is arranged inside the first tower plate;
The second tower plate (32) is identical to the first tower plate (31) in structure.
Preferably, the adsorption layer (313) is an activated carbon layer or a molecular sieve layer.
Preferably, the molecular sieve layer is an A-type molecular sieve, a Y-type molecular sieve or an X-type molecular sieve.
Preferably, the upper part of the deodorizing lift pipe used in the synthesis of esters is connected with a vacuum pipeline.
The invention also provides a deodorizing method in the synthesis of esters, which comprises the following steps:
s1, performing a synthesis reaction of polyglycerol ester in a reaction kettle in a sectional heating mode;
S2, in the later reaction period, regulating the vacuum degree in the reaction kettle to be-0.06-0.099 MPa;
s3, in the exhaust stage, the deodorizing riser used in the ester synthesis is used for exhausting and recycling part of materials;
in step S3, unpleasant odors are removed by a tray group (3) provided with a deodorizing riser for use in ester synthesis;
Substances with boiling points of 100-800 ℃ and moisture and volatile gases can be discharged through a vacuum pipeline at the upper part of a deodorizing riser used in ester synthesis after being separated by a tower plate group (3); the substances with the boiling point of 800-2000 ℃ are left in the reaction kettle.
Preferably, in the step S2, the vacuum degree is-0.01-0.06 MPa.
Preferably, in step S1, the processing manner of the sectional heating is as follows: adding polyglycerol into a reaction kettle, heating to 50-105 ℃, adding an alkaline catalyst, stirring and heating to 80-180 ℃, adding fatty acid for reaction when the temperature is 60-130 ℃, heating to 180-230 ℃, keeping the temperature for 0.5-1 h, slowly lifting the temperature to 240-298 ℃ for quick reaction, regulating the vacuum degree in the reaction kettle to minus 0.08-0.099 MPa, ending the reaction after the water yield reaches 80% of a preset value, and keeping the reaction temperature to 240-298 ℃.
Preferably, in step S3, the step of exhausting is performed by distilling unreacted raw materials in the material under vacuum condition to recover the unreacted raw materials, and the remainder is separated into polyglycerol ester by molecular distillation.
The invention provides a deodorizing riser used in ester synthesis, which can discharge substances, moisture and volatile gases with boiling points of 100-800 ℃ through a vacuum pipeline at the upper part of the deodorizing riser used in ester synthesis after being separated by a tower plate in the deodorizing riser used in ester synthesis, and the substances with the boiling points of 800-2000 ℃ are remained in a reaction kettle as much as possible.
The invention also provides a deodorizing method in the synthesis of esters, wherein the method firstly adopts sectional heating in the synthesis of polyglycerol ester, can reduce coking of materials, and then adopts high vacuum to remove odor generated by coking of partial materials. Because a part of materials can be taken away by high vacuum, the materials are separated by the tower plate group in the riser, and the partial materials taken away by vacuum can be recovered by increasing the contact area of the tower plate group and steam and the length of the riser by utilizing the boiling point difference of the materials; the invention solves unpleasant odor generated in the process of synthesizing polyglycerol ester by adopting the adsorption treatment of the active carbon layer/molecular sieve layer. The invention creatively adopts the tray separation technology and the organic combination of the adsorption layer arranged in the tray in the reaction kettle in the production process of the polyglycerol ester, thereby not only achieving the purpose of removing unpleasant odor, but also effectively recycling distilled distillate and achieving good process effect.
Through a large number of creative tests, the inventor of the application obtains the effect that the odor component in the product can be effectively controlled by adjusting the vacuum degree in the reaction kettle in the later period of reaction, and the good deodorizing effect is achieved.
The invention has the beneficial effects that:
1. the unpleasant odor generated in the production process of the polyglycerol ester is solved, and the environment and the personal safety of human bodies are protected to a certain extent;
2. Solves the problem that the distillate distilled in the synthesis process of the polyglycerol ester is recycled, and reduces the water consumption and the water discharge.
Drawings
FIG. 1 is a schematic diagram of a deodorizing riser for use in the synthesis of esters according to the present invention;
FIG. 2 is a schematic view of a partial structure of a deodorizing riser for use in the synthesis of esters according to the present invention;
FIG. 3 is a schematic view showing a partial structure of a deodorizing lift pipe for use in ester synthesis according to the present invention;
FIG. 4 is a schematic view showing a partial structure of a deodorizing lift pipe for use in the synthesis of esters according to the present invention.
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.
Example 1
A deodorizing method in ester synthesis, characterized by comprising the following steps:
s1, performing a synthesis reaction of polyglycerol ester in a reaction kettle in a sectional heating mode;
S2, in the later reaction period, regulating the vacuum degree in the reaction kettle to be-0.06-0.099 MPa;
s3, in the exhaust stage, exhausting through a riser and recycling part of materials;
In step S3, unpleasant odors are removed by a tray group provided in the riser.
Further, in step S2, the vacuum degree is-0.01 MPa.
Further, in step S1, the processing manner of the sectional heating is as follows: adding polyglycerol into a reaction kettle, heating to 50 ℃, adding an alkaline catalyst, stirring and heating to 80 ℃, adding fatty acid for reaction when the temperature is 60 ℃, heating to 180 ℃, keeping for 0.5 hour, slowly raising the temperature to 240 ℃ for quick reaction, adjusting the vacuum degree in the reaction kettle to-0.08 MPa, ending the reaction after the water yield reaches 80% of a preset value, and keeping the reaction temperature at 240 ℃.
In step S3, unreacted raw materials in the materials are distilled out under vacuum condition for recovery, and the distilled residue is subjected to molecular distillation to separate polyglycerol ester.
Further, the gas lift pipe comprises a pipe body 1, a supporting column 2 is arranged in the central area of the pipe body, and tower plate groups 3 are symmetrically arranged in the pipe body by the supporting column.
Further, the tray group comprises a first tray 31 and a second tray 32, and the first tray and the second tray are staggered.
Further, the horizontal section of the first column plate is semicircular, a mounting groove 311 is formed in the middle of the column plate, and the mounting groove is connected with the support column in a matched mode.
Further, the first tower plate is symmetrically provided with liquid-dropping holes 312, the first tower plate is of a hollow structure, and an adsorption layer 313 is arranged inside the first tower plate.
Further, the adsorption layer is a molecular sieve layer.
Furthermore, the molecular sieve layer adopts an A-type molecular sieve.
In the invention, the adopted active carbon layer or molecular sieve layer can be reused to a limited extent, and has strong purifying capability and good purifying effect.
Further, the second tray is structurally identical to the first tray.
In particular, the upper part of the draft tube is connected with a vacuum pipe (not labeled).
The gas riser of the invention can discharge substances, moisture and volatile gases with boiling points of 100-800 ℃ through the vacuum pipeline at the upper part of the gas riser after the separation of the tower plates, and the substances with boiling points of 800-2000 ℃ are remained in the reaction kettle as much as possible.
In the invention, the sectional heating is adopted in the synthesis of the polyglycerol ester, so that the coking of materials can be reduced, and the odor generated by the coking of partial materials is removed by adopting high vacuum. Because a part of materials can be taken away by high vacuum, the materials are separated by the tower plate group in the riser, and the partial materials taken away by vacuum can be recovered by increasing the contact area of the tower plate group and steam and the length of the riser by utilizing the boiling point difference of the materials; the invention solves unpleasant odor generated in the process of synthesizing polyglycerol ester by adopting the adsorption treatment of the active carbon layer/molecular sieve layer. The invention creatively adopts the tray separation technology and the organic combination of the adsorption layer arranged in the tray in the reaction kettle in the production process of the polyglycerol ester, thereby not only achieving the purpose of removing unpleasant odor, but also effectively recycling distilled distillate and achieving good process effect.
The invention has the beneficial effects that:
1. the unpleasant odor generated in the production process of the polyglycerol ester is solved, and the environment and the personal safety of human bodies are protected to a certain extent;
2. Solves the problem that the distillate distilled in the synthesis process of the polyglycerol ester is recycled, and reduces the water consumption and the water discharge.
Example 2
A deodorizing method in ester synthesis, characterized by comprising the following steps:
s1, performing a synthesis reaction of polyglycerol ester in a reaction kettle in a sectional heating mode;
S2, in the later reaction period, regulating the vacuum degree in the reaction kettle to be-0.06-0.099 MPa;
s3, in the exhaust stage, exhausting through a riser and recycling part of materials;
In step S3, unpleasant odors are removed by a tray group provided in the riser.
Further, in step S2, the vacuum degree is 0.06MPa.
Further, in step S1, the processing manner of the sectional heating is as follows: adding polyglycerol into a reaction kettle, heating to 105 ℃, adding an alkaline catalyst, stirring and heating to 180 ℃, adding fatty acid for reaction at 130 ℃, heating to 230 ℃ for 1h, slowly raising the temperature to 298 ℃ for rapid reaction, adjusting the vacuum degree in the reaction kettle to 0.099MPa, ending the reaction after the water yield reaches 80% of a preset value, and keeping the reaction temperature at 298 ℃.
In step S3, unreacted raw materials in the materials are distilled out under vacuum condition for recovery, and the distilled residue is subjected to molecular distillation to separate polyglycerol ester.
Further, the gas lift pipe comprises a pipe body 1, a supporting column 2 is arranged in the central area of the pipe body, and tower plate groups 3 are symmetrically arranged in the pipe body by the supporting column.
Further, the tray group comprises a first tray 31 and a second tray 32, and the first tray and the second tray are staggered.
Further, the horizontal section of the first column plate is semicircular, a mounting groove 311 is formed in the middle of the column plate, and the mounting groove is connected with the support column in a matched mode.
Further, the first tower plate is symmetrically provided with liquid-dropping holes 312, the first tower plate is of a hollow structure, and an adsorption layer 313 is arranged inside the first tower plate.
Further, the adsorption layer is an activated carbon layer.
Example 3
A deodorizing method in ester synthesis, characterized by comprising the following steps:
s1, performing a synthesis reaction of polyglycerol ester in a reaction kettle in a sectional heating mode;
S2, in the later reaction period, regulating the vacuum degree in the reaction kettle to be minus 0.06MPa;
s3, in the exhaust stage, exhausting through a riser and recycling part of materials;
In step S3, unpleasant odors are removed by a tray group provided in the riser.
Further, in step S1, the processing manner of the sectional heating is as follows: adding polyglycerol into a reaction kettle, heating to 65 ℃, adding an alkaline catalyst, stirring and heating to 95 ℃, adding fatty acid for reaction when the temperature is 75 ℃, heating to 195 ℃ and keeping for 0.6h, slowly raising the temperature to 260 ℃ for quick reaction, adjusting the vacuum degree in the reaction kettle to-0.01 MPa, ending the reaction after the water yield is metered to 80% of a preset value, and keeping the reaction temperature at 255 ℃.
In step S3, unreacted raw materials in the materials are distilled out under vacuum condition for recovery, and the distilled residue is subjected to molecular distillation to separate polyglycerol ester.
Further, the gas lift pipe comprises a pipe body 1, a supporting column 2 is arranged in the central area of the pipe body, and tower plate groups 3 are symmetrically arranged in the pipe body by the supporting column.
Further, the tray group comprises a first tray 31 and a second tray 32, and the first tray and the second tray are staggered.
Further, the horizontal section of the first column plate is semicircular, a mounting groove 311 is formed in the middle of the column plate, and the mounting groove is connected with the support column in a matched mode.
Further, the first tower plate is symmetrically provided with liquid-dropping holes 312, the first tower plate is of a hollow structure, and an adsorption layer 313 is arranged inside the first tower plate.
Further, the adsorption layer is a molecular sieve layer.
Further, the molecular sieve layer adopts a Y-type molecular sieve.
Example 4
A deodorizing method in ester synthesis, characterized by comprising the following steps:
s1, performing a synthesis reaction of polyglycerol ester in a reaction kettle in a sectional heating mode;
S2, in the later reaction period, regulating the vacuum degree in the reaction kettle to be 0.099MPa;
s3, in the exhaust stage, exhausting through a riser and recycling part of materials;
In step S3, unpleasant odors are removed by a tray group provided in the riser.
Further, in step S1, the processing manner of the sectional heating is as follows: adding polyglycerol into a reaction kettle, heating to 90 ℃, adding an alkaline catalyst, stirring and heating to 160 ℃, adding fatty acid for reaction when the temperature is 110 ℃, heating to 200 ℃, keeping for 0.8h, slowly raising the temperature to 275 ℃ for quick reaction, adjusting the vacuum degree in the reaction kettle to 0.06MPa, ending the reaction after the water yield reaches 80% of a preset value, and keeping the reaction temperature at 265 ℃.
In step S3, unreacted raw materials in the materials are distilled out under vacuum condition for recovery, and the distilled residue is subjected to molecular distillation to separate polyglycerol ester.
Further, the gas lift pipe comprises a pipe body 1, a supporting column 2 is arranged in the central area of the pipe body, and tower plate groups 3 are symmetrically arranged in the pipe body by the supporting column.
Further, the tray group comprises a first tray 31 and a second tray 32, and the first tray and the second tray are staggered.
Further, the horizontal section of the first column plate is semicircular, a mounting groove 311 is formed in the middle of the column plate, and the mounting groove is connected with the support column in a matched mode.
Further, the first tower plate is symmetrically provided with liquid-dropping holes 312, the first tower plate is of a hollow structure, and an adsorption layer 313 is arranged inside the first tower plate.
Further, the adsorption layer is a molecular sieve layer.
Furthermore, the molecular sieve layer adopts an X-type molecular sieve.
Example 5
A deodorizing method in ester synthesis, characterized by comprising the following steps:
s1, performing a synthesis reaction of polyglycerol ester in a reaction kettle in a sectional heating mode;
S2, in the later reaction period, regulating the vacuum degree in the reaction kettle to be 0.015MPa;
s3, in the exhaust stage, exhausting through a riser and recycling part of materials;
In step S3, unpleasant odors are removed by a tray group provided in the riser.
Further, in step S1, the processing manner of the sectional heating is as follows: adding polyglycerol into a reaction kettle, heating to 80 ℃, adding an alkaline catalyst, stirring and heating to 120 ℃, adding fatty acid for reaction at 90 ℃, heating to 190 ℃, keeping for 0.7h, slowly raising the temperature to 270 ℃ for quick reaction, adjusting the vacuum degree in the reaction kettle to 0.02MPa, ending the reaction after the water yield reaches 80% of a preset value, and keeping the reaction temperature at 260 ℃.
In step S3, unreacted raw materials in the materials are distilled out under vacuum condition for recovery, and the distilled residue is subjected to molecular distillation to separate polyglycerol ester.
Further, the gas lift pipe comprises a pipe body, a supporting column is arranged in the central area of the pipe body, and tower plate groups are symmetrically arranged in the pipe body by the supporting column.
Further, the column plate group comprises a first column plate and a second column plate, and the first column plate and the second column plate are arranged in a staggered mode.
Further, the horizontal section of the first column plate is semicircular, and the middle part of the column plate is provided with a mounting groove which is connected with the support column in a matched mode.
Further, the first column plate is symmetrically provided with liquid reducing holes, the first column plate is of a hollow structure, and an adsorption layer is arranged inside the first column plate.
Further, the adsorption layer is an activated carbon layer.
Further, the second tray is structurally identical to the first tray.
Example 6
A deodorizing method in ester synthesis, characterized by comprising the following steps:
s1, performing a synthesis reaction of polyglycerol ester in a reaction kettle in a sectional heating mode;
S2, in the later reaction period, regulating the vacuum degree in the reaction kettle to be 0.032MPa;
s3, in the exhaust stage, exhausting through a riser and recycling part of materials;
In step S3, unpleasant odors are removed by a tray group provided in the riser.
Further, in step S1, the processing manner of the sectional heating is as follows: adding polyglycerol into a reaction kettle, heating to 85 ℃, adding an alkaline catalyst, stirring and heating to 135 ℃, adding fatty acid for reaction when the temperature is 95 ℃, heating to 205 ℃, keeping for 0.75h, slowly raising the temperature to 280 ℃, carrying out quick reaction, adjusting the vacuum degree in the reaction kettle to 0.05MPa, ending the reaction after the water yield reaches 80% of a preset value, and keeping the reaction temperature at 255 ℃.
In step S3, unreacted raw materials in the materials are distilled out under vacuum condition for recovery, and the distilled residue is subjected to molecular distillation to separate polyglycerol ester.
Further, the gas lift pipe comprises a pipe body, a supporting column is arranged in the central area of the pipe body, and tower plate groups are symmetrically arranged in the pipe body by the supporting column.
Further, the column plate group comprises a first column plate and a second column plate, and the first column plate and the second column plate are arranged in a staggered mode.
Further, the horizontal section of the first column plate is semicircular, and the middle part of the column plate is provided with a mounting groove which is connected with the support column in a matched mode.
Further, the first column plate is symmetrically provided with liquid reducing holes, the first column plate is of a hollow structure, and an adsorption layer is arranged inside the first column plate.
Further, the adsorption layer is a molecular sieve layer.
Furthermore, the molecular sieve layer adopts an A-type molecular sieve.
Further, the second tray is structurally identical to the first tray.
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 characteristics 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.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art. It should be noted that technical features not described in detail in the present invention may be implemented by any prior art.
Claims (8)
1. The deodorizing lift pipe for the ester synthesis is characterized by comprising a pipe body (1), wherein a support column (2) is arranged in the central area of the pipe body, and tower plate groups (3) are symmetrically arranged in the pipe body by the support column; the tray group (3) comprises a plurality of first trays (31) and a plurality of second trays (32); the first tower plates (31) and the second tower plates (32) are arranged in a staggered manner;
the horizontal section of the first tower plate (31) is semicircular; the middle part of the first tower plate (31) is provided with a mounting groove (311), and the mounting groove (311) is connected with the support column (2) in a matching way;
The first tower plate (31) is symmetrically provided with liquid dropping holes (312), the first tower plate (31) is of a hollow structure, and an adsorption layer (313) is arranged inside the first tower plate;
The second tower plate (32) is identical to the first tower plate (31) in structure.
2. The deodorizing riser for use in the synthesis of esters according to claim 1, wherein said adsorption layer (313) is an activated carbon layer or a molecular sieve layer.
3. The deodorizing riser for use in the synthesis of esters according to claim 2, wherein said molecular sieve layer is a type a molecular sieve, a type Y molecular sieve or a type X molecular sieve.
4. A deodorizing riser for use in ester synthesis according to any one of claims 1 to 3, wherein a vacuum pipe is connected to the upper portion of the deodorizing riser for use in ester synthesis.
5. A deodorizing method in ester synthesis, characterized by comprising the following steps:
s1, performing a synthesis reaction of polyglycerol ester in a reaction kettle in a sectional heating mode;
S2, in the later reaction period, regulating the vacuum degree in the reaction kettle to be-0.06-0.099 MPa;
s3, in the exhaust stage, exhausting through the deodorizing lift pipe for use in the synthesis of esters according to any one of claims 1 to 4 and recycling part of materials;
in step S3, unpleasant odors are removed by a tray group (3) provided with a deodorizing riser for use in ester synthesis;
Substances with boiling points of 100-800 ℃ and moisture and volatile gases can be discharged through a vacuum pipeline at the upper part of a deodorizing riser used in ester synthesis after being separated by a tower plate group (3); the substances with the boiling point of 800-2000 ℃ are left in the reaction kettle.
6. The deodorizing method as set forth in claim 5, wherein in step S2, the vacuum degree is-0.01 to 0.06MPa.
7. The method for deodorizing in ester synthesis according to claim 5, wherein in step S1, the step of heating in stages is performed by: adding polyglycerol into a reaction kettle, heating to 50-105 ℃, adding an alkaline catalyst, stirring and heating to 80-180 ℃, adding fatty acid for reaction when the temperature is 60-130 ℃, heating to 180-230 ℃, keeping the temperature for 0.5-1 h, slowly lifting the temperature to 240-298 ℃ for quick reaction, regulating the vacuum degree in the reaction kettle to minus 0.08-0.099 MPa, ending the reaction after the water yield reaches 80% of a preset value, and keeping the reaction temperature to 240-298 ℃.
8. The method according to claim 5, wherein in step S3, the unreacted raw materials are distilled off under vacuum to recover the raw materials, and the residue is separated from the polyglycerol ester by molecular distillation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410319909.7A CN118184994A (en) | 2018-12-29 | 2018-12-29 | Deodorization lift pipe for ester synthesis and deodorization method for ester synthesis |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410319909.7A CN118184994A (en) | 2018-12-29 | 2018-12-29 | Deodorization lift pipe for ester synthesis and deodorization method for ester synthesis |
| CN201811636741.3A CN109762156A (en) | 2018-12-29 | 2018-12-29 | A kind of deodorizing methods in esters synthesis |
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| CN201811636741.3A Division CN109762156A (en) | 2018-12-29 | 2018-12-29 | A kind of deodorizing methods in esters synthesis |
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| CN118184994A true CN118184994A (en) | 2024-06-14 |
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| CN202410319909.7A Pending CN118184994A (en) | 2018-12-29 | 2018-12-29 | Deodorization lift pipe for ester synthesis and deodorization method for ester synthesis |
| CN201811636741.3A Pending CN109762156A (en) | 2018-12-29 | 2018-12-29 | A kind of deodorizing methods in esters synthesis |
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| CN113230985A (en) * | 2021-03-04 | 2021-08-10 | 佛山市银美联合科技有限公司 | Equipment for preparing polyglycerol n-fatty acid ester and operation method thereof |
| CN113145046A (en) * | 2021-03-04 | 2021-07-23 | 佛山市银美联合科技有限公司 | Equipment for preparing polyglycerol isomerous fatty acid ester and operation method thereof |
| CN114869828B (en) * | 2022-04-27 | 2024-05-07 | 广州禾力生物科技有限公司 | Pet deodorizing composition and application thereof |
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| CN104531365B (en) * | 2014-12-10 | 2018-01-16 | 柳州高通食品化工有限公司 | A kind of preparation method of polyglycerol ester |
| CN106084209B (en) * | 2016-07-22 | 2018-05-22 | 广州煌垅生物科技有限公司 | A kind of production technology of polyglyceryl fatty acid ester |
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