CN115581966A - Production process and application of triglycerol monostearate - Google Patents
Production process and application of triglycerol monostearate Download PDFInfo
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- CN115581966A CN115581966A CN202211253895.0A CN202211253895A CN115581966A CN 115581966 A CN115581966 A CN 115581966A CN 202211253895 A CN202211253895 A CN 202211253895A CN 115581966 A CN115581966 A CN 115581966A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D25/00—Filters formed by clamping together several filtering elements or parts of such elements
- B01D25/12—Filter presses, i.e. of the plate or plate and frame type
- B01D25/21—Plate and frame presses
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D25/00—Filters formed by clamping together several filtering elements or parts of such elements
- B01D25/32—Removal of the filter cakes
- B01D25/34—Removal of the filter cakes by moving, e.g. rotating, the filter elements
- B01D25/346—Removal of the filter cakes by moving, e.g. rotating, the filter elements by vibration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention relates to the technical field of food additives, in particular to a production process and application of triglycerol monostearate, wherein the process comprises the following specific steps: s1, mixing and heating glycerol and a compound mixed alkaline catalyst, and concentrating and dehydrating to obtain triglycerol; s2, circularly decoloring the triglycerin; s3, adding the triglycerin and the compound mixed alkaline catalyst into a reaction kettle, uniformly mixing, heating, continuously introducing nitrogen into the reaction kettle, adding the tristearate into the reaction kettle, heating and stirring, cooling after an esterification reaction, and cooling to obtain solid triglycerin monostearate; the method carries out multiple times of decolorization treatment on the triglycerin, can carry out continuous decolorization production, and improves the color of the product; in the stirring process, the raw materials at the bottom of the tank body enter the material stirring chamber, and the material stirring chamber is pushed to the top of the tank body through the movable baffle, so that the stirring is more uniform.
Description
Technical Field
The invention relates to the field of food additives, in particular to a production process and application of triglycerol monostearate.
Background
Triglycerol monostearate (PGFE) is a non-ionic surfactant, is a widely used food additive at present, has the functions of emulsification, thickening, fresh-keeping, food aging delaying and the like, has an HLB value of 5-8, and can be prepared into O/W and W/O emulsions. Triglycerol monostearate is an important food emulsifier and additive, and has wide application in the industries of food, pharmacy, plastics, textile, cosmetics, detergents and the like. In recent years, along with the improvement of living standard of people, the food monoglyceride cannot meet the requirement of some formulas to supplement and improve monoglyceride products due to excellent emulsifying property, and particularly cold drinks and ice creams cannot be compared with other emulsifying agents.
The production of common triglycerol monostearate is completed in two steps, the first step is to dehydrate and polymerize glycerin at high temperature to prepare triglycerol, and the second step is to esterify triglycerol directly to prepare triglycerol monostearate. The glycerol polymerization takes alkali as a catalyst, and the glycerol is condensed and dehydrated into triglycerol at about 260 ℃ under the protection of nitrogen. Trimerization glycerol alcoholization: alkali is used as a catalyst, and the triglycerin and the stearic acid are directly esterified at about 230 ℃ under the protection of nitrogen. In this preparation, about 4% of the total amount of material is produced, which requires energy consumption for removal, and stearic acid is expensive, thus increasing the production cost. Some manufacturers also use hardened oil and triglycerol as raw materials to prepare the triglycerol monostearate, but the problem of high cost cannot be solved.
The two methods both require the triglycerin to participate in the reaction, and the triglycerin needs to be decolored before the reaction with stearic acid or hardened oil, otherwise, the obtained triglycerin monostearate product has dark color and heavy smell, and the quality of the product is influenced. Therefore, it is highly desirable to improve the existing production process of triglycerol monostearate to improve the quality of the product.
Disclosure of Invention
The invention aims to provide triglycerol monostearate and a production process and application thereof, so as to solve the problems in the background technology.
The purpose of the invention can be realized by the following technical scheme:
a production process of triglycerol monostearate comprises the following steps:
s1, mixing and heating glycerol and a compound mixed alkaline catalyst, concentrating and dehydrating, and performing molecular distillation to obtain triglycerol;
s2, pouring the triglycerin and the water into a decoloring tank, uniformly mixing the triglycerin and the water through stirring, adding a decoloring agent through a decoloring agent inlet, decoloring, inputting the mixed solution into a plate-and-frame filter, filtering, sampling, observing, inputting the mixed solution into the decoloring tank again after the mixed solution is qualified, and heating and dehydrating;
and S3, mixing the decolorized triglycerin with a compound mixed alkaline catalyst, adding the mixture into a decolorizing tank, stirring and heating, introducing nitrogen into the decolorizing tank, adding tristearate into the decolorizing tank, heating, stirring and reacting, and cooling to normal temperature after the reaction is finished to obtain the solid triglycerin monostearate.
Further preferably, the specific steps of S2 are:
s2.1, putting the poly-triglycerin, the pure water and the decolorizing agent into a decolorizing tank, starting stirring, heating to 70-90 ℃, stirring for 20-40min, and turning the mixture at the bottom of the tank to the top of the tank through a movable baffle;
s2.2, conveying the stirred mixture to a reserved tank through a connecting pipe;
s2.3, conveying the mixture into a filter plate through a feeding pipe by using the reserved tank, filtering the mixture, shaking off filtered residues onto the collecting plate through a movable filter screen, discharging liquid from a discharging pipe, sampling, observing, and returning to a decoloring tank continuously through a circulating pump until decoloring is completed;
and S2.4, returning the mixture after decolorization to a decolorization tank, starting a vacuum system through a vacuum tube to enable the vacuum system of the decolorization tank to reach-0.1-0.2 MPa, slowly heating to 90-100 ℃, and dehydrating for 40-60 min.
Further preferably, in S2.1, turning over the mixture at the bottom of the tank to the top of the tank through the movable baffle is specifically:
the first movable sealing ring rotates to enable the first movable sealing ring to be communicated with the first through hole of the fixed sealing ring, the second movable sealing ring rotates to enable the second movable sealing ring to be communicated with the lifting sealing ring, and the mixture at the bottom can enter the material turning chamber from the first through hole and the second through hole;
the first movable sealing ring and the second movable sealing ring are rotated, so that the fixed baffle and the movable baffle are sealed again, and then the movable baffle slides upwards along the sliding rail, and the mixture in the stirring chamber can be moved to the top of the inner cavity of the tank body.
Further preferably, shaking off the residue in S2.3 onto the collecting plate by the movable filter screen specifically comprises:
after the clamping plates on the two sides of the filter frame are opened, the cam is rotated to push the movable filter screen to move towards the center, and then the movable filter screen is pulled back through the return spring to form reciprocating motion to shake off residues.
Further preferably, the compound mixed alkaline catalyst is Na 2 CO 3 NaOH, and Ca (OH) 2 With NaH 2 PO 2 To (2)And (3) mixing a compound, wherein the compound mixed alkaline catalyst added in the step S1 accounts for 0.5-1% of the total mass of the glycerol.
Further preferably, the decolorizing agent is a compound mixture of diatomite and at least one of activated clay, activated carbon and attapulgite clay.
Further preferably, the molar ratio of the triglycerol, the tristearate and the compounded mixed alkaline catalyst in the step S3 is 1:1:0.01 to 0.02.
The application of the triglycerol monostearate in the emulsion composition is characterized in that the triglycerol monostearate is prepared by the production process, the emulsion composition consists of the triglycerol monostearate and propylene glycol monostearate, and the mass ratio of the triglycerol monostearate to the propylene glycol monostearate is 1:1 to 1.5.
The invention has the beneficial effects that:
1. the method is provided with the decolorizing tank and the plate-and-frame filter, firstly, the mixture is decolorized in the decolorizing tank and then conveyed into the plate-and-frame filter for filtration, if the mixture is unqualified, the mixture in the plate-and-frame filter can be returned to the decolorizing tank by the circulating pump for continuous decolorization, and the triglycerin is repeatedly decolorized by the circulating decolorizing equipment, so that continuous decolorization production can be carried out, and the color of the product is improved;
2. according to the invention, the stirring chamber and the material turning chamber are arranged in the decolorizing tank, when raw materials such as triglycerin and the like are added, the raw materials are firstly added into the stirring chamber, in the stirring process, the fixed baffle and the movable baffle are opened, so that the raw materials at the bottom of the tank body enter the material turning chamber from the through hole between the fixed baffle and the movable baffle, then the fixed baffle and the movable baffle are sealed, and the material turning chamber is pushed to the top of the tank body through the movable baffle, so that the stirring is more uniform;
3. according to the invention, the movable filter screen is arranged in the plate-and-frame filter, when filter residues are required to be treated, the clamping plates on the two sides of the filter frame are firstly opened, then the cam rotates, when the protruding end of the cam moves to the movable filter screen, the movable filter screen is pushed to move towards the direction of the fixed filter screen, and when the protruding end of the cam is far away from the movable filter screen, the movable filter screen moves back under the elastic action of the reset spring to form reciprocating motion, so that vibration is generated, and the filter residues on the surface of the filter screen are shaken off.
Drawings
In order to more clearly illustrate the embodiments or technical solutions in the prior art of the present invention, the drawings used in the description of the embodiments or prior art will be briefly described below, and it is obvious for those skilled in the art to obtain other drawings without creative efforts;
FIG. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 is a schematic view of the construction of the decolorizing tank of the present invention;
FIG. 3 is a schematic view of the internal structure of the can body of the present invention;
FIG. 4 is a schematic view of the attachment of the retainer plate to the tank of the present invention;
FIG. 5 is a schematic structural view of a retainer plate according to the present invention;
FIG. 6 is a schematic view of the structure of a plate and frame filter of the present invention;
FIG. 7 is a schematic view of the structure of a filter plate according to the present invention;
fig. 8 is a schematic structural diagram of the movable filter screen of the present invention.
The reference numbers in the figures are as follows:
1. a decolorizing tank; 11. a tank body; 111. a stirring chamber; 112. a temperature control chamber; 113. a material turning chamber; 114. a temperature control oil pipe; 115. fixing a baffle plate; 1151. fixing a sealing ring; 1152. a first movable seal ring; 1153. a first through hole; 116. a movable baffle; 1161. lifting the sealing ring; 1162. a second movable seal ring; 1163. a second through hole; 1164. a first notch; 1165. a second notch; 117. a slide rail; 12. a stirring motor; 13. a stirring rod; 14. a stirring paddle; 15. a polyglycerol inlet; 16. a pure water inlet; 17. a decolorizing agent inlet; 18. a vacuum tube; 19. a fixed mount; 2. a plate and frame filter; 21. a frame; 22. a slide bar; 23. a stress plate; 24. pressing a plate; 25. a hydraulic cylinder; 26. a filter plate; 261. a filter frame; 262. a feed inlet; 263. a discharge port; 264. fixing the filter screen; 265. a movable filter screen; 266. a splint; 267. a cam; 268. a return spring; 27. a collection plate; 28. a feed pipe; 29. a discharge pipe; 3. reserving a tank; 31. a connecting pipe; 32. a polyglycerol outlet; 4. a circulation pump; 5. a circulation pipe.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the embodiment of the invention, tristearate is purchased from Kaiwen food Co., ltd, triglycerol is purchased from Kaiwen food Co., ltd, glycerol is purchased from Hua Long glycerol products Co., ltd, hydrogenated oil and stearic acid are purchased from Kaita chemical technology Co., ltd, and the used catalyst is purchased from Tianjin chemical reagent II.
A production process of triglycerol monostearate comprises the following steps:
s1, mixing and heating glycerol and a compound mixed alkaline catalyst, concentrating and dehydrating, and performing molecular distillation to obtain triglycerol;
s2, pouring the triglycerin and the water into the decoloring tank (1), uniformly mixing the triglycerin and the water through stirring, adding a decoloring agent through a decoloring agent inlet (17), decoloring, inputting the mixed solution into the plate and frame type filter (2), filtering, sampling, observing, inputting the mixed solution into the decoloring tank (1) again after the mixed solution is qualified, and heating and dehydrating;
and S3, mixing the decolorized triglycerin with a compound mixed alkaline catalyst, adding the mixture into a decolorizing tank (1), stirring and heating, introducing nitrogen into the decolorizing tank (1), adding tristearate into the decolorizing tank (1), heating, stirring and reacting, and cooling to normal temperature after the reaction is finished to obtain the solid triglycerin monostearate.
As shown in figures 1-8, in order to ensure that the triglycerin can be continuously decolorized and finally the triglycerin with small smell and colorless to light color can be produced, a recyclable decolorization device is particularly used, the device comprises a decolorization tank 1, a plate-and-frame filter 2 is arranged at the rear end of the decolorization tank 1, a reserved tank 3 is also arranged between the decolorization tank 1 and the plate-and-frame filter 2, the triglycerin is decolorized by the decolorization tank 1, then the mixture in the decolorization tank 1 is transferred into the reserved tank 3 through a connecting pipe 31 and then is conveyed to the plate-and-frame filter 2, the mixture is filtered, and whether the triglycerin reaches the standard or not is observed, if the triglycerin does not reach the standard, the mixture in the light filter 2 is conveyed back to the decolorization tank 1 from a circulating pipe 5 through a circulating pipe 4, the decolorization is continuously carried out, the circulation is carried out until the triglycerin is qualified, and then the triglycerin is conveyed to the decolorization tank 1 for subsequent operation.
As shown in fig. 2, the specific structure of the decoloring tank 1 further includes a tank 11, a plurality of material inlets capable of conveying different raw materials are disposed at the top of the tank 11, which are respectively a polyglycerol inlet 15, a pure water inlet 16, a decoloring agent inlet 17, and a vacuum tube 18 for providing a vacuum environment in the tank 11 when the final dehydration is performed, when the decoloring is performed, each raw material enters the tank 11 from the corresponding inlet, then the stirring motor 12 is started, and the stirring paddle 14 is driven by the stirring rod 13 to rotate, so as to stir the mixture in the tank 11, so that the mixture is uniformly mixed.
And because triglycerin is comparatively sticky, in the in-process of stirring, difficult mobile, though the mixture in the coplanar can carry out effective stirring through stirring rake 14, but the difference of jar body 11 top and bottom is too big, leads to the not identical degree of stirring of upper and lower mixture, consequently, just need in jar body 11, be provided with the mechanism that can turn over the material from top to bottom.
As shown in fig. 3 and 4, firstly, the tank 11 is divided into a plurality of cavities, the innermost is a stirring chamber 111, the raw materials are directly poured into the stirring chamber 111, then a temperature control chamber 112 is further formed in the side wall of the stirring chamber 111, a temperature control oil pipe 114 is wound in the temperature control chamber 112 for controlling the temperature of the whole tank 11, then the outermost material turning chamber 113 is formed, a fixed baffle plate 115 and a movable baffle plate 116 are arranged at the bottom of the material turning chamber 113, the fixed baffle plate 115 is used for blocking the material turning chamber 113 from the stirring chamber 111, the fixed baffle plate 115 and the movable baffle plate 116 are openable, when the mixture at the bottom needs to be conveyed to the top, the mixture can be opened, and then the mixture is pushed upwards to the top through the movable baffle plate 116.
As shown in fig. 5, the fixed baffle 115 includes a fixed sealing ring 1151 and a first movable sealing ring 1152, the movable baffle 116 includes a lifting sealing ring 1161 and a second movable sealing ring 1162, the same first through holes 1153 are formed on the surfaces of the fixed sealing ring 1151 and the first movable sealing ring 1152, the same second through holes 1163 are formed on the surfaces of the lifting sealing ring 1161 and the second movable sealing ring 1162, when the first through holes 1153 of the upper and lower sealing rings are staggered, a sealed state is formed, the stirring chamber 111 is separated from the stirring chamber 113, and when the first through holes 1153 are communicated with the second through holes 1163, the mixture at the bottom of the stirring chamber 111 enters the stirring chamber 113, and then the two through holes are staggered, so that the fixed baffle 115 blocks the two cavities, and then the mixture in the stirring chamber 113 can be pushed to move to the top of the stirring chamber 111 by moving up the movable baffle 116.
As shown in fig. 6, after the decoloring in the decoloring tank 1 is completed, the mixture is transferred to the reserve tank 3 and then conveyed to the plate and frame filter 2;
the plate-and-frame filter 2 comprises a frame 21, two opposite slide rods 22 are arranged in the frame 21, a stress plate 23 is fixed at one end of each slide rod 22, a pressing plate 24 is connected at the other end of each slide rod 22 in a sliding manner, a plurality of filter plates 26 are distributed between the stress plate 23 and the pressing plate 24 in an array manner, a hydraulic cylinder 25 is arranged at the rear end of the pressing plate 24, the hydraulic cylinder 25 pushes the pressing plate 24 to compact the filter plates 26, a collecting plate 27 is arranged at the bottom of each filter plate 26, the collecting plate 27 can be drawn out of the frame 21 and is convenient for collecting residues on the filter plates 26, a feeding pipe 28 is arranged on one side of the stress plate 23, one end of the feeding pipe 28 is connected with the reserved tank 3, the feeding pipe 28 penetrates through all the filter plates 26, a discharging pipe 29 is arranged on the other side of the stress plate 23, and the discharging pipe 29 also penetrates through all the filter plates 26.
As shown in fig. 7, the filter plate 26 includes a filter frame 261, a feed inlet 262 is disposed on the top and right side of the filter frame 261, the mixture enters the filter frame 261 from the feed inlet 262, a discharge outlet 263 is disposed on the bottom and left side of the filter frame 261, the mixture is discharged from the discharge outlet 263 after being filtered, a movable filter screen 265 which is movable up and down is disposed in the filter frame 261, a fixed filter screen 264 is disposed in the middle of the filter frame 261, when the filter screen needs to be cleaned, clamping plates 266 on both sides are opened first, and then the movable filter screen 265 is vibrated up and down, so that the residue on the surface of the filter screen is shaken off.
As shown in fig. 8, the rotating cams 267 are disposed in the upper and lower frames of the filter frame 261, the arc edges of the cams 267 are tightly attached to the surface of the movable filter screen 264, when the protruding ends of the cams 267 rotate to the surface attached to the movable filter screen 264, the movable filter screen 264 is pushed to move toward the center of the filter frame 261, and when the protruding ends are far away, the movable filter screen 264 moves back under the elastic force of the return spring 268, so as to form a reciprocating motion, and residues on the surface of the filter screen can be shaken off.
Based on the above equipment, the specific steps of S2 in the production process of the triglycerol monostearate are as follows:
s2.1, putting the poly-triglycerin, the pure water and the decolorizing agent into a decolorizing tank 1 according to a specified proportion, starting stirring, heating to 70-90 ℃, stirring for 20-40min, and overturning the mixture at the bottom of the tank body 11 to the top of the tank body 11 through a movable baffle 116;
wherein, turning over the mixture at the bottom of the tank body 11 to the top of the tank body 11 through the movable baffle 116 is specifically as follows:
the first movable sealing ring 1152 rotates, so that the first movable sealing ring 1152 is communicated with the first through hole 1153 of the fixed sealing ring 1151, the second movable sealing ring 1162 is rotated, so that the second movable sealing ring 1162 is communicated with the lifting sealing ring 1161, and the mixture at the bottom enters the material stirring chamber 113 from the first through hole 1153 and the second through hole 1163;
the first movable sealing ring 1152 and the second movable sealing ring 1162 are rotated to make the fixed baffle 115 and the movable baffle 116 to seal again, and then the movable baffle 116 slides upwards along the sliding rail 117, so that the mixture in the stirring chamber 113 is moved to the top of the inner cavity of the tank 11.
S2.2, conveying the stirred mixture into a reserved tank 3 through a connecting pipe 31;
s2.3, conveying the mixture into a filter plate 26 through a feeding pipe 28 by the reserved tank 3, filtering the mixture, shaking off filtered residues onto a collecting plate 27 through a movable filter screen 265, discharging liquid from a discharging pipe 29, sampling, observing, and returning to the decoloring tank 1 continuously through a circulating pump 4 until decoloring is finished;
wherein the shaking off of the residue onto the collecting plate 27 by the movable filter screen 265 is specifically:
after the clamps 266 on both sides of the filter frame 261 are opened, the cam 267 is rotated, and the cam 267 pushes the movable filter 265 to move toward the center, and then the movable filter is pulled back by the return spring 268 to reciprocate, so that the residue is shaken off.
And S2.4, returning the decolored mixture to the decoloring tank 1, starting a vacuum system through a vacuum tube 18 to enable the vacuum system of the decoloring tank 1 to reach-0.1-0.2 MPa, slowly heating to 90-100 ℃, and dehydrating for 40-60 min.
Wherein the compound mixed alkaline catalyst is Na 2 CO 3 NaOH, and Ca (OH) 2 With NaH 2 PO 2 The compound mixture of (1) is added with a compound mixed alkaline catalyst accounting for 0.5-1% of the total mass of the glycerol; the decolorizing agent is a compound mixture of diatomite and at least one of activated clay, activated carbon and attapulgite clay; the tristearate is at least one of tristearate or tripalmitin; in the step S3, the mol ratio of the triglycerol to the tristearate to the compound mixed alkaline catalyst is 1:1:0.01 to 0.02.
Example 1
A production process of triglycerol monostearate comprises the following steps:
s1, mixing and heating glycerol and a compound mixed alkaline catalyst accounting for 0.5 percent of the weight of the glycerol to 250 ℃ under the pressure of-0.1 MPa, concentrating and dehydrating the mixture, and obtaining triglycerol by molecular distillation, wherein the compound mixed alkaline catalyst is prepared from NaOH and NaH 2 PO 2 Mixing according to the mass ratio of 1:1;
s2.1, putting the polyglycerol, the pure water and the decolorizing agent into a decolorizing tank 1 according to the mass ratio of 1:4:1, mixing;
s2.2, conveying the stirred mixture into a reserved tank 3 through a connecting pipe 31;
s2.3, conveying the mixture into a filter plate 26 through a feeding pipe 28 by the reserved tank 3, filtering the mixture, shaking off filtered residues onto a collecting plate 27 through a movable filter screen 265, discharging liquid from a discharging pipe 29, sampling, observing, and returning to the decoloring tank 1 continuously through a circulating pump 4 until decoloring is finished;
s2.4, returning the decolored mixture to the decoloring tank 1, starting a vacuum system through a vacuum tube 18 to enable the vacuum system of the decoloring tank 1 to reach-0.1 MPa, slowly heating to 90 ℃, and dehydrating for 60min;
and S3, mixing 10mol of decolored triglycerin with 0.1mol of compound mixed alkaline catalyst, adding the mixture into a decoloring tank 1, stirring and heating the mixture to 100 ℃, introducing nitrogen into the decoloring tank 1, adding 6mol of tristearate into the decoloring tank 1, heating the mixture to 200 ℃, stirring the mixture, carrying out esterification reaction for 6 hours, and cooling the mixture to normal temperature after the reaction is finished to obtain the solid triglycerin monostearate.
Example 2
A production process of triglycerol monostearate comprises the following steps:
s1, mixing and heating glycerol and a compound mixed alkaline catalyst accounting for 0.8 percent of the weight of the glycerol to 260 ℃ under the pressure of 0.02MPa, concentrating and dehydrating the mixture, obtaining triglycerol through molecular distillation, and carrying out compound mixed alkaline catalysisThe agent consists of NaOH and NaH 2 PO 2 Mixing according to the mass ratio of 1:1;
s2.1, putting the polyglycerol, the pure water and the decolorizing agent into a decolorizing tank 1 according to a mass ratio of 1:2:1, mixing;
s2.2, conveying the stirred mixture into a reserved tank 3 through a connecting pipe 31;
s2.3, conveying the mixture into a filter plate 26 through a feeding pipe 28 by the reserved tank 3, filtering the mixture, shaking off filtered residues onto a collecting plate 27 through a movable filter screen 265, discharging liquid from a discharging pipe 29, sampling, observing, and returning to the decoloring tank 1 continuously through a circulating pump 4 until decoloring is finished;
s2.4, returning the decolored mixture to the decoloring tank 1, starting a vacuum system through a vacuum tube 18 to enable the vacuum system of the decoloring tank 1 to reach 0.02MPa, slowly heating to 80 ℃, and dehydrating for 60min;
s3, mixing 8mol of decolored triglycerin with 0.12mol of compound mixed alkaline catalyst, adding the mixture into a decoloring tank 1, stirring and heating the mixture to 100 ℃, introducing nitrogen into the decoloring tank 1, adding 8mol of tristearate into the decoloring tank 1, heating the mixture to 220 ℃, stirring the mixture, carrying out esterification reaction for 4 hours, and cooling the mixture to normal temperature after the reaction is finished to obtain the solid triglycerin monostearate.
Example 3
A production process of triglycerol monostearate comprises the following steps:
s1, mixing and heating glycerol and a compound mixed alkaline catalyst accounting for 1 percent of the weight of the glycerol to 255 ℃ under the pressure of 0.01MPa, concentrating and dehydrating the mixture, and obtaining triglycerol by molecular distillation, wherein the compound mixed alkaline catalyst is prepared from NaOH and NaH 2 PO 2 Mixing according to the mass ratio of 1:1;
s2.1, putting the polyglycerol, the pure water and the decolorizing agent into a decolorizing tank 1 according to the mass ratio of 1:1, mixing;
s2.2, conveying the stirred mixture into a reserved tank 3 through a connecting pipe 31;
s2.3, conveying the mixture into a filter plate 26 through a feeding pipe 28 by the reserved tank 3, filtering the mixture, shaking off filtered residues onto a collecting plate 27 through a movable filter screen 265, discharging liquid from a discharging pipe 29, sampling, observing, and returning to the decoloring tank 1 continuously through a circulating pump 4 until decoloring is finished;
s2.4, returning the decolored mixture to the decoloring tank 1, starting a vacuum system through a vacuum tube 18 to enable the vacuum system of the decoloring tank 1 to reach 0.01MPa, slowly heating to 95 ℃, and dehydrating for 50min;
and S3, mixing 10mol of decolored triglycerin with 0.15mol of compound mixed alkaline catalyst, adding the mixture into a decoloring tank 1, stirring and heating the mixture to 90 ℃, introducing nitrogen into the decoloring tank 1, adding 10mol of tristearate into the decoloring tank 1, heating the mixture to 260 ℃, stirring the mixture, carrying out esterification reaction for 3 hours, and cooling the mixture to normal temperature after the reaction is finished to obtain the solid triglycerin monostearate.
In comparative examples 1 and 2 of the present invention, a conventional decoloring process is employed, i.e., triglycerol, pure water, and a decoloring agent are mixed and stirred for a period of time, and then the decoloring agent is removed by filtration.
Comparative example 1
A production process of triglycerol monostearate comprises the following steps:
s1, mixing and heating glycerol and a compound mixed alkaline catalyst accounting for 0.8 percent of the weight of the glycerol to 260 ℃ under the pressure of 0.01MPa, concentrating and dehydrating the mixture, and obtaining triglycerol by molecular distillation, wherein the compound mixed alkaline catalyst is prepared from NaOH and NaH 2 PO 2 Mixing according to the mass ratio of 1:1;
s2, putting the polyglycerol, the pure water and the decolorizing agent into a stirring tank according to the mass ratio of 1:2:1, mixing, then conveying the mixture to a filter, filtering the mixture to obtain filtrate, and finishing decolorization;
and S3, mixing 8mol of decolorized triglycerin with 0.12mol of compounded mixed alkaline catalyst, adding the mixture into a reaction kettle, stirring and heating to 90 ℃, introducing nitrogen into the reaction kettle, adding 8mol of hydrogenated oil into the reaction kettle, heating to 220 ℃, stirring, carrying out esterification reaction for 4 hours, and cooling to normal temperature after the reaction is finished to obtain the solid triglycerin monostearate.
Comparative example 2
A production process of triglycerol monostearate comprises the following steps:
s1, mixing and heating glycerol and a compound mixed alkaline catalyst accounting for 0.8 percent of the weight of the glycerol to 260 ℃ under the pressure of 0.01MPa, concentrating and dehydrating the mixture, and obtaining triglycerol by molecular distillation, wherein the compound mixed alkaline catalyst is prepared from NaOH and NaH 2 PO 2 Mixing according to the mass ratio of 1:1;
s2, putting the polyglycerol, the pure water and the decolorizing agent into a stirring tank according to the mass ratio of 1:2:1, mixing, then conveying the mixture to a filter, filtering the mixture to obtain filtrate, and finishing decolorization;
s3, mixing 8mol of decolored triglycerin with 0.12mol of compound mixed alkaline catalyst, adding the mixture into a reaction kettle, stirring and heating the mixture to 90 ℃, introducing nitrogen into the reaction kettle, adding 8mol of stearic acid into the reaction kettle, heating the mixture to 220 ℃, stirring the mixture, carrying out esterification reaction for 4 hours, and cooling the mixture to normal temperature after the reaction is finished to obtain solid triglycerin monostearate.
Performance detection
Indexes of the initial products of triglycerol monostearate obtained in examples 1 to 3 and comparative examples 1 to 2 were measured according to GB 1886.178-2016, and the data are shown in Table 1 below.
TABLE 1 measurement of the Properties of Triglycerol monostearate
As can be seen from the experimental results of the examples 1-3 and the comparative examples 1-2, the continuous decoloring production can be carried out in the examples 1-3 by adopting the decoloring process of the invention, and the triglycerol monostearate prepared by using the decolored triglycerol has good color and smell, so that the product quality is improved.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (8)
1. A production process of triglycerol monostearate is characterized by comprising the following steps:
s1, mixing and heating glycerol and a compound mixed alkaline catalyst, concentrating and dehydrating, and performing molecular distillation to obtain triglycerol;
s2, pouring the triglycerin and the water into the decoloring tank (1), uniformly mixing the triglycerin and the water through stirring, adding a decoloring agent through a decoloring agent inlet (17), decoloring, inputting the mixed solution into the plate-and-frame filter (2), filtering, sampling, observing, inputting the mixed solution into the decoloring tank (1) again after the mixed solution is qualified, and heating and dehydrating;
and S3, mixing the decolorized triglycerin with a compound mixed alkaline catalyst, adding the mixture into a decolorizing tank (1), stirring and heating, introducing nitrogen into the decolorizing tank (1), adding tristearate into the decolorizing tank (1), heating, stirring and reacting, and cooling to normal temperature after the reaction is finished to obtain the solid triglycerin monostearate.
2. The process for producing triglycerol monostearate according to claim 1, wherein the specific steps of S2 are:
s2.1, putting the poly-triglycerin, the pure water and the decolorizing agent into a decolorizing tank (1), starting stirring, heating to 70-90 ℃, stirring for 20-40min, and overturning the mixture at the bottom of the tank body (11) to the top of the tank body (11) through a movable baffle (116);
s2.2, conveying the stirred mixture into a reserved tank (3) through a connecting pipe (31);
s2.3, conveying the mixture into a filter plate (26) through a feeding pipe (28) by the reserved tank (3), filtering the mixture, shaking off filtered residues onto a collecting plate (27) through a movable filter screen (265), discharging liquid from a discharging pipe (29), sampling, observing, and continuously returning to the decoloring tank (1) through a circulating pump (4), and decoloring until decoloring is completed;
and S2.4, returning the mixture after decolorization to the decolorizing tank (1), starting a vacuum system through a vacuum tube (18) to enable the vacuum system of the decolorizing tank (1) to reach-0.1-0.2 MPa, slowly heating to 90-100 ℃, and dehydrating for 40-60 min.
3. The process for the production of triglycerol monostearate according to claim 2, wherein in S2.1 the overturning of the mixture at the bottom of the tank (11) to the top of the tank (11) through the mobile baffle (116) is in particular:
the first movable sealing ring (1152) rotates to enable the first movable sealing ring (1152) to be communicated with the first through hole (1153) of the fixed sealing ring (1151), the second movable sealing ring (1162) is rotated to enable the second movable sealing ring (1162) to be communicated with the lifting sealing ring (1161), and the mixture at the bottom enters the material stirring chamber (113) from the first through hole (1153) and the second through hole (1163);
the first movable sealing ring (1152) and the second movable sealing ring (1162) are rotated, so that the fixed baffle (115) and the movable baffle (116) are sealed again, and then the movable baffle (116) slides upwards along the sliding rail (117), so that the mixture in the stirring chamber (113) is moved to the top of the inner cavity of the tank body (11).
4. The process for the production of triglycerol monostearate according to claim 2, characterized in that the shaking off of the residues in S2.3 on the collection plate (27) by means of a mobile strainer (265) is in particular:
after the clamping plates (266) at the two sides of the filter frame (261) are opened, the cam (267) is rotated, the cam (267) pushes the movable filter screen (265) to move towards the center, and then the movable filter screen is pulled back through the return spring (268) to form reciprocating motion, so that residues are shaken off.
5. The process for producing triglycerol monostearate according to claim 1, wherein the compounded mixed alkaline catalyst is Na 2 CO 3 NaOH and Ca (OH) 2 With NaH 2 PO 2 The compound mixture of step S1 is added with a compound mixed alkaline catalyst accounting for 0.5-1% of the total mass of the glycerol.
6. The production process of triglycerol monostearate according to claim 1, wherein the decolorizing agent is a compounded mixture of at least one of activated clay, activated carbon, attapulgite clay and diatomaceous earth.
7. The process for producing triglycerol monostearate according to claim 1, wherein the molar ratio of triglycerol, tristearate and compounded mixed basic catalyst in step S3 is 1:1:0.01 to 0.02.
8. Use of triglycerol monostearate prepared by the process according to any one of claims 1 to 7 in an emulsifying composition consisting of triglycerol monostearate and propylene glycol monostearate in a mass ratio of 1:1 to 1.5.
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