CN114133328A - Production process and formula for preparing monoglyceride from grease - Google Patents
Production process and formula for preparing monoglyceride from grease Download PDFInfo
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- CN114133328A CN114133328A CN202111232218.6A CN202111232218A CN114133328A CN 114133328 A CN114133328 A CN 114133328A CN 202111232218 A CN202111232218 A CN 202111232218A CN 114133328 A CN114133328 A CN 114133328A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- 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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Abstract
The invention relates to a production process of monoglyceride, and discloses a production process for preparing monoglyceride from grease and a formula thereof, wherein the production process comprises the following operation steps: s1, preparation of grease hydrogenation: firstly, grease is put into a reaction kettle, copper accounting for 0 to 0.5 percent of the total mass of the grease, nickel accounting for 0 to 1 percent of the total mass of the grease, manganese accounting for 0 to 1 percent of the total mass of the grease and palladium accounting for 0 to 0.01 percent of the total mass of the grease are added into the reaction kettle, and then the mixture is stirred, continuously heating while stirring to ensure that the temperature is maintained at 50-300 ℃, controlling the temperature to be maintained, and ensuring that the stirring speed in the reaction kettle is 60-1200r/min, during hydrogenation, the bottom end of hydrogen is filled into the reaction kettle, and pressurization is also needed to ensure that the gas pressure in the reaction kettle is 0-1Mpa, the reaction lasts for about 7-10 hours, when the temperature is not changed drastically, the hydrogenated oil and the unhydrogenated oil are poured into a cooling tank to help the oil to be hydrogenated, the hydrogenated grease is directly used for preparing the monoglyceride, and the grease obtained through differential rotation has higher hydrogenation efficiency.
Description
Technical Field
The invention relates to the technical field of a production process of monoglyceride, and particularly relates to a production process for preparing monoglyceride from grease and a formula of the monoglyceride.
Background
Monoglycerides are frequently used as emulsifiers and additives for foods, as emulsifiers in cosmetic and pharmaceutical ointments, as emulsifiers for industrial silk-oils and lubricants for textiles, as anti-dripping agents and anti-fogging agents in plastic films, etc.
The traditional monoglyceride is produced by carrying out hydrolysis reaction on grease to obtain stearic acid and glycerol, but the traditional production method is not environment-friendly, and the traditional monoglyceride preparation method needs to be carried out and can not take waste vegetable grease as a raw material.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a production process for preparing monoglyceride from grease and a formula thereof, and the technical problems to be solved by the invention are as follows: a method for preparing monoglyceride by using waste vegetable oil and fat.
The invention provides the following technical scheme: a production process for preparing monoglyceride from grease and a formula thereof comprise the following operation steps:
s1, preparation of grease hydrogenation: firstly, filling oil into a reaction kettle, adding 0-0.5% of copper, 0-1% of nickel, 0-1% of manganese and 0-0.01% of palladium into the reaction kettle, stirring the oil, continuously heating the oil while stirring to ensure that the temperature is maintained at 50-300 ℃, controlling the temperature to maintain so that the stirring speed in the reaction kettle is 60-1200r/min, filling hydrogen into the reaction kettle at the bottom end during hydrogenation, pressurizing to ensure that the internal gas pressure is 0-1Mpa, reacting for about 7-10 hours, and pouring the hydrogenated oil and the unhydrogenated oil into a cooling tank until the temperature is not changed violently.
S2, cooling hydrogenated grease: pouring the grease in the cooling tank into water at 15-30 ℃ to solidify the hydrogenated grease in the water, wherein the grease which is not hydrogenated floats on the water surface as oil, and collecting the solidified hydrogenated grease;
s3, alcoholysis reaction of hydrogenated grease: removing water from the hydrogenated oil solidified block, adding the hydrogenated oil solidified block into a reaction kettle, adding 1-20 times of glycerol by mass of the hydrogenated oil into the reaction kettle, adding 0-1% of sodium hydroxide serving as a catalyst, maintaining the reaction temperature for 2-5 hours, and pouring liquid in the reaction kettle after alcoholysis into a cooling barrel after the reaction is finished;
s4, extracting monoglyceride: and (3) carrying out centrifugal separation after the temperature of the liquid in the cooling barrel is 50-100 ℃, cooling after the centrifugal separation, and collecting the solid at the top end to obtain the monoglyceride solidified block.
In a preferred embodiment, the metal copper nickel manganese palladium metal as a catalyst is mixed to account for 1.2% of the total mass of the grease when the grease is subjected to grease hydrogenation treatment by S1, so as to achieve the maximum catalytic effect while ensuring economic benefits.
In a preferred embodiment, the stirring speed of the reaction kettle of S1 is subjected to differential stirring when the reaction kettle rotates, and the stirring speed of the differential stirring is reduced or increased by 300r/min every minute, so that the stirring is more uniform.
S5, incorporation of bile salts: after the monoglyceride solidified block is melted, bile salt is added, the bile salt accounts for 0-5% of the total amount of the monoglyceride, and after the monoglyceride solidified block is uniformly stirred, the monoglyceride is solidified into a new solidified block through cooling treatment, so that the better emulsification effect of the monoglyceride can be provided.
In a preferred embodiment, the hydrogen purity of the hydrogen filled in the S1 is more than 98%, and the amount of the filled hydrogen is not 3-5 times of the total mass of the grease, so that the grease can be hydrogenated more thoroughly.
In a preferred embodiment, the grease in the cooling tank for pouring the S2 into the water falls into the water after passing through a 160-mesh screen to reduce the volume of the grease, so that the hydrogenated grease is not easy to wrap the unhydrogenated grease when the water bath is performed.
In a preferred embodiment, the collection of the S2 hydrogenated oil is performed after the solidified small hydrogenated oil ball passes through the water bath again, and the water bath is used for removing the unhydrogenated oil on the surface.
In a preferred embodiment, the oil floating on the water surface of the S3 is collected and dried, and then can be continuously used as the grease raw material of S1.
In a preferred embodiment, the oil liquid is recovered by the S4 to be used as the glycerol of S3, and the grease solidified at the bottom end of the S4 can be used as hydrogenated grease to be put into the S2.
The invention has the technical effects and advantages that:
1. the invention prepares the work through the hydrogenation of grease: firstly, grease is put into a reaction kettle, copper accounting for 0 to 0.5 percent of the total mass of the grease, nickel accounting for 0 to 1 percent of the total mass of the grease, manganese accounting for 0 to 1 percent of the total mass of the grease and palladium accounting for 0 to 0.01 percent of the total mass of the grease are added into the reaction kettle, and then the mixture is stirred, continuously heating while stirring to ensure that the temperature is maintained at 50-300 ℃, controlling the temperature to be maintained, ensuring that the stirring speed in the reaction kettle is 60-1200r/min, during hydrogenation, the bottom end of hydrogen is filled into the reaction kettle, and pressurization is also needed to ensure that the gas pressure in the reaction kettle is 0-1MPa, the reaction lasts for about 7-10 hours, pouring the hydrogenated oil and the unhydrogenated oil into a cooling tank until the temperature is not changed violently, so as to be helpful for hydrogenation of the oil, the hydrogenated grease is directly used for preparing monoglyceride, and the grease obtained through differential rotation has higher hydrogenation efficiency;
2. according to the invention, the grease in the cooling tank is poured into the water at the temperature of 15-30 ℃, so that the hydrogenated grease is solidified in the water, but the grease which is not hydrogenated floats on the water surface in the form of oil liquid, and the solidified hydrogenated grease is collected, so that the grease and the hydrogenated grease can be separated through a water bath, and the recovery is facilitated.
3. According to the invention, the liquid in the cooling barrel is centrifugally separated after the temperature is 50-100 ℃, the liquid is cooled after centrifugal separation, and the solid at the top end is collected to obtain the monoglyceride solidified block, so that the separation effect is better and the resource is saved.
4. The method is characterized in that the monoglyceride coagulated block is melted and added with bile salt, the bile salt accounts for 0-5% of the total amount of monoglyceride, the monoglyceride is coagulated into a new coagulated block by cooling treatment after being uniformly stirred, so that the powerful emulsification effect of the grease fat can be assisted by the bile salt, under the action of the bile salt, the contact area between the bile salt and molecules at positions of the monoglyceride and grease needing to be emulsified later and the like can be increased under various emulsification effects, the emulsification effect is increased, and meanwhile, in the actual use process, when the prepared monoglyceride raw material is used as edible grease for emulsification, the edible grease can be easier to digest due to the effect of the bile salt.
Detailed Description
The following will clearly and completely describe the technical solutions 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 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.
The invention provides a production process for preparing monoglyceride from grease and a formula thereof, which comprises the following operations:
s1, preparation of grease hydrogenation: firstly, filling grease into a reaction kettle, adding 0-0.5% of copper, 0-1% of nickel, 0-1% of manganese and 0-0.01% of palladium into the reaction kettle, stirring the grease, continuously heating the grease while stirring to ensure that the temperature is maintained at 50-300 ℃, controlling the temperature to maintain, ensuring that the stirring speed in the reaction kettle is 60-1200r/min, filling hydrogen into the reaction kettle at the bottom end during hydrogenation, pressurizing to ensure that the internal gas pressure is 0-1Mpa, reacting for about 7-10 hours, and pouring the hydrogenated grease and the unhydrogenated grease into a cooling tank until the temperature is not changed violently;
s2, cooling hydrogenated grease: pouring the grease in the cooling tank into water at 15-30 ℃ to solidify the hydrogenated grease in the water, wherein the grease which is not hydrogenated floats on the water surface as oil, and collecting the solidified hydrogenated grease;
s3, alcoholysis reaction of hydrogenated grease: removing water from the hydrogenated oil solidified block, adding the hydrogenated oil solidified block into a reaction kettle, adding 1-20 times of glycerol by mass of the hydrogenated oil into the reaction kettle, adding 0-1% of sodium hydroxide serving as a catalyst, maintaining the reaction temperature for 2-5 hours, and pouring liquid in the reaction kettle after alcoholysis into a cooling barrel after the reaction is finished;
s4, extracting monoglyceride: and (3) carrying out centrifugal separation after the temperature of the liquid in the cooling barrel is 50-100 ℃, cooling after the centrifugal separation, and collecting the solid at the top end to obtain the monoglyceride solidified block.
S5, incorporation of bile salts: the monoglyceride coagulation block is melted and then added with bile salt, the ratio of the bile salt accounts for 0-5% of the total amount of the monoglyceride, the monoglyceride is coagulated into a new coagulation block by cooling treatment after uniform stirring, so that the powerful emulsification effect of the grease fat can be assisted by the bile salt, the contact area between the bile salt and the monoglyceride and grease needing to be emulsified in the later period can be increased under various emulsification effects, and the emulsification effect is increased.
Further, in the step of hydrogenating the oil or fat in S1, the metal copper nickel manganese palladium metal as a catalyst is mixed in an amount of 1.2% by mass based on the total mass of the oil or fat.
Further, the reaction vessel of S1 was agitated at a differential stirring speed during the rotation, and the stirring speed was decreased or increased by 300r/min every minute by the differential stirring.
Furthermore, the purity of hydrogen filled in the S1 is more than 98%, and the amount of the filled hydrogen is not 3-5 times of the total mass of the grease.
Further, the grease in the cooling tank for pouring the grease into the water in the S2 falls into the water after passing through the 160-mesh screen, and the 160-mesh screen enables the oil to form small oil drops so as to reduce the amount of the non-hydrogenated grease mixed into the hydrogenated grease.
Further, the collection of the S2 hydrogenated oil is carried out after the solidified small hydrogenated oil ball passes through the water bath again.
Furthermore, the oil liquid floating on the water surface of the S3 can be continuously used as the oil raw material of the S1 after being collected and dried, so that the utilization rate of the unhydrogenated oil is improved.
Furthermore, the oil liquid is recovered as the glycerol of S3 by S4, and the oil solidified at the bottom end of S4 can be used as hydrogenated oil and put into S2, so that the hydrogenated oil and fat remained in the alcoholysis reaction can be used continuously.
The first embodiment is as follows:
s1, preparation of grease hydrogenation: firstly, oil is filled into a reaction kettle, copper, nickel, manganese and palladium are added into the reaction kettle, wherein the copper, the nickel, the manganese and the palladium are 0-0.5% of the total mass of the oil, the nickel, the manganese and the palladium are 0% of the total mass of the oil, the mixture is stirred, the temperature is kept between 50 and 300 ℃ by continuous heating while stirring, the temperature is controlled to be kept, the stirring speed in the reaction kettle is 60 to 1200r/min, the bottom end of hydrogen is firstly filled into the reaction kettle during hydrogenation, the internal pressure of the hydrogen is kept between 0 and 1MPa by pressurization, the reaction is carried out for about 7 to 10 hours, and the hydrogenated oil and the unhydrogenated oil are poured into a cooling tank until the temperature is not changed violently.
In conclusion, the catalytic effect of copper on the reaction of hydrogenated fats and oils can be directly obtained.
Example two:
s1, preparation of grease hydrogenation: firstly, loading oil into a reaction kettle, adding 0.3% of copper, 0-1% of nickel, 0% of manganese and 0% of palladium by the total mass of the oil into the reaction kettle, stirring the oil, continuously heating the oil while stirring to ensure that the temperature is maintained at 50-300 ℃, controlling the temperature to be maintained, so that the stirring speed in the reaction kettle is 60-1200r/min, filling hydrogen into the reaction kettle at the bottom end during hydrogenation, pressurizing the pressure in the reaction kettle to ensure that the pressure is 0-1MPa, and pouring the hydrogenated oil and the unhydrogenated oil into a cooling tank when the reaction is about 7-10 hours until the temperature is not changed violently.
In conclusion, the catalytic effect of nickel on the reaction of the hydrogenated grease can be directly obtained.
Example three:
s1, preparation of grease hydrogenation: firstly, oil is filled into a reaction kettle, copper, nickel, manganese and palladium are added into the reaction kettle, wherein the copper, the nickel, the manganese and the palladium are 0.3 percent, 0.6 percent, 0-1 percent and 0 percent of the total mass of the oil, the mixture is stirred, the temperature is kept between 50 and 300 ℃ by continuous heating while stirring, the temperature is controlled to be kept, the stirring speed in the reaction kettle is 60 to 1200r/min, the bottom end of hydrogen is filled into the reaction kettle during hydrogenation, the pressure is increased to ensure that the internal pressure is between 0 and 1MPa, the reaction is carried out for about 7 to 10 hours, and the hydrogenated oil and the unhydrogenated oil are poured into a cooling tank until the temperature is not changed violently.
In conclusion, the catalytic effect of manganese on the reaction of the hydrogenated grease can be directly obtained.
Example four:
s1, preparation of grease hydrogenation: firstly, loading oil into a reaction kettle, adding 0.3% of copper, 0.6% of nickel, 0.6% of manganese and 0-0.01% of palladium into the reaction kettle, stirring, continuously heating while stirring to ensure that the temperature is maintained at 50-300 ℃, controlling the temperature to be maintained, ensuring that the stirring speed in the reaction kettle is 60-1200r/min, filling hydrogen into the reaction kettle at the bottom end when hydrogenation is carried out, pressurizing while ensuring that the internal pressure is 0-1MPa, reacting for about 7-10 hours, and pouring the hydrogenated oil and the unhydrogenated oil into a cooling tank until the temperature is not changed violently.
From the above, the catalytic effect of palladium on the reaction of hydrogenated fats and oils can be directly obtained.
Example five:
s2, cooling hydrogenated grease: and pouring the grease in the cooling tank into water at 15-30 ℃ to solidify the hydrogenated grease in the water, wherein the grease which is not hydrogenated floats on the water surface as oil, and collecting the solidified hydrogenated grease.
In conclusion, it can be seen that the temperature of the water bath influences the collection of the hydrogenated fats.
Example six:
s3, alcoholysis reaction of hydrogenated grease: removing water from the hydrogenated oil solidified block, adding the hydrogenated oil solidified block into a reaction kettle, adding 1-20 times of glycerol by mass of the hydrogenated oil into the reaction kettle, adding 1% of sodium hydroxide serving as a catalyst, maintaining the reaction temperature for 2 hours, and pouring liquid in the reaction kettle after alcoholysis into a cooling barrel after the reaction is finished.
From the above, the effect of the total mass of glycerol on the yield of monoglycerides can be known.
Example seven:
s3, alcoholysis reaction of hydrogenated grease: removing water from the hydrogenated oil solidified block, adding the hydrogenated oil solidified block into a reaction kettle, adding glycerol which is 19 times of the mass of the hydrogenated oil into the reaction kettle, adding 0-1% of sodium hydroxide serving as a catalyst into the reaction kettle, maintaining the reaction temperature for 2 hours, and pouring liquid in the reaction kettle after alcoholysis into a cooling barrel after the reaction is finished.
Example eight:
s3, alcoholysis reaction of hydrogenated grease: removing water from the hydrogenated oil solidified block, adding the hydrogenated oil solidified block into a reaction kettle, adding glycerol which is 19 times of the mass of the hydrogenated oil into the reaction kettle, adding 0.6% of sodium hydroxide serving as a catalyst into the reaction kettle, maintaining the reaction temperature for 2-5 hours, and pouring liquid in the reaction kettle after alcoholysis into a cooling barrel after the reaction is finished.
From the above, it was found that the effect of the reaction time on the alcoholysis reaction was affected.
Example nine:
s5, incorporation of bile salts: melting monoglyceride coagulated block, adding bile salt in an amount of 0-5% of total amount of monoglyceride, stirring, and cooling to coagulate monoglyceride into new coagulated block.
In summary, the effect of bile salts on the post-emulsification effect of monoglyceride is described.
The points to be finally explained are: first, in the description of the present application, it should be noted that, unless otherwise specified and limited, the terms "mounted," "connected," and "connected" should be understood broadly, and may be a mechanical connection or an electrical connection, or a communication between two elements, and may be a direct connection, and "upper," "lower," "left," and "right" are only used to indicate a relative positional relationship, and when the absolute position of the object to be described is changed, the relative positional relationship may be changed;
secondly, the method comprises the following steps: in the disclosed embodiment of the invention, only the structures related to the disclosed embodiment are related, other structures can refer to common design, and the same embodiment and different embodiments of the invention can be combined with each other under the condition of no conflict;
and finally: the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that are within the spirit and principle of the present invention are intended to be included in the scope of the present invention.
Claims (8)
1. A production process for preparing monoglyceride from grease and a formula thereof are characterized by comprising the following operations:
s1, preparation of grease hydrogenation: firstly, filling oil into a reaction kettle, adding 0-0.5% of copper, 0-1% of nickel, 0-1% of manganese and 0-0.01% of palladium into the reaction kettle, stirring the oil, continuously heating the oil while stirring to ensure that the temperature is maintained at 50-300 ℃, controlling the temperature to maintain, ensuring that the stirring speed in the reaction kettle is 60-1200r/min, filling hydrogen into the reaction kettle at the bottom end during hydrogenation, pressurizing to ensure that the internal gas pressure is 0-1Mpa, reacting for about 7-10 hours, and pouring the hydrogenated oil and the unhydrogenated oil into a cooling tank until the temperature is not changed violently;
s2, cooling hydrogenated grease: pouring the grease in the cooling tank into water at 15-30 ℃ to solidify the hydrogenated grease in the water, wherein the grease which is not hydrogenated floats on the water surface as oil, and collecting the solidified hydrogenated grease;
s3, alcoholysis reaction of hydrogenated grease: removing water from the hydrogenated oil solidified block, adding the hydrogenated oil solidified block into a reaction kettle, adding 1-20 times of glycerol by mass of the hydrogenated oil into the reaction kettle, adding 0-1% of sodium hydroxide serving as a catalyst, maintaining the reaction temperature for 2-5 hours, and pouring liquid in the reaction kettle after alcoholysis into a cooling barrel after the reaction is finished;
s4, extracting monoglyceride: and (3) carrying out centrifugal separation after the temperature of the liquid in the cooling barrel is 50-100 ℃, cooling after the centrifugal separation, and collecting the solid at the top end to obtain the monoglyceride solidified block.
S5, incorporation of bile salts: melting monoglyceride coagulated block, adding bile salt in an amount of 0-5% of total amount of monoglyceride, stirring, and cooling to coagulate monoglyceride into new coagulated block.
2. The production process and the formula for preparing monoglyceride by using the grease as claimed in claim 1, wherein the production process comprises the following steps: and when the S1 is subjected to grease hydrogenation treatment, the metal Cu-Ni-Mn-Pd metal serving as a catalyst is mixed to account for 1.2% of the total mass of the grease.
3. The production process and the formula for preparing monoglyceride by using the grease as claimed in claim 1, wherein the production process comprises the following steps: when the reaction kettle of the S1 rotates, the stirring speed is subjected to differential stirring, and the stirring speed of the differential stirring is reduced or increased by 300r/min every minute.
4. The production process and the formula for preparing monoglyceride by using the grease as claimed in claim 1, wherein the production process comprises the following steps: the hydrogen purity of the hydrogen filled in the S1 is more than 98%, and the amount of the filled hydrogen is not 3-5 times of the total mass of the grease.
5. The production process and the formula for preparing monoglyceride by using the grease as claimed in claim 1, wherein the production process comprises the following steps: and the grease in the cooling tank poured into the water from the S2 falls into the water after passing through a 160-mesh screen.
6. The production process and the formula for preparing monoglyceride by using the grease as claimed in claim 1, wherein the production process comprises the following steps: and the S2 hydrogenated grease is collected after the solidified small hydrogenated grease balls pass through the water bath again.
7. The production process and the formula for preparing monoglyceride by using the grease as claimed in claim 1, wherein the production process comprises the following steps: and after the oil liquid floating on the water surface of the S3 is collected and dried, the oil liquid can be continuously used as the oil raw material of the S1.
8. The production process and the formula for preparing monoglyceride by using the grease as claimed in claim 1, wherein the production process comprises the following steps: the S4 recovers oil liquid as glycerol of S3, and the oil solidified at the bottom end of S4 can be used as hydrogenated oil and put into S2.
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| CN202111232218.6A CN114133328A (en) | 2021-10-22 | 2021-10-22 | Production process and formula for preparing monoglyceride from grease |
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