CN113416132A - Production process for distilling low-glycerol glycerin monostearate - Google Patents
Production process for distilling low-glycerol glycerin monostearate Download PDFInfo
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- CN113416132A CN113416132A CN202110903526.0A CN202110903526A CN113416132A CN 113416132 A CN113416132 A CN 113416132A CN 202110903526 A CN202110903526 A CN 202110903526A CN 113416132 A CN113416132 A CN 113416132A
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- C07—ORGANIC CHEMISTRY
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- C07C67/00—Preparation of carboxylic acid esters
- C07C67/03—Preparation of carboxylic acid esters by reacting an ester group with a hydroxy group
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
Abstract
The invention discloses a production process for distilling glycerin monostearate from low glycerin, which comprises the following steps: s1: esterification reaction → S2: multi-stage distillation treatment: purification by primary, secondary and tertiary distillation of monoglycerides → S3: and (3) recycling: opening a discharge pump of the ester finished product after the first-stage distillation to recover the glycerol, opening a discharge pump of the ester finished product after the second-stage distillation to recover the glycerol and the fatty acid, and opening a discharge pump of the ester finished product after the second-stage distillation to recover the ditriester → S4: powder spraying and sieving → S5: and (6) metering and packaging. The invention adopts a three-stage distillation process, wherein the second stage is a half-short-distance evaporator, and the evaporation effect of the evaporator is improved by controlling the vacuum, the temperature of heat-conducting oil, the temperature of medium-temperature water and the like, so that the redundant glycerin is prevented from reaching the third stage distillation, the problem that the glycerin cannot be removed by the third stage distillation is avoided, and the content of the finished glycerin is effectively reduced.
Description
Technical Field
The invention relates to the technical field of food additive production, in particular to a production process for distilling low-glycerol glycerin monostearate.
Background
Distilled glyceryl monostearate produced by taking natural vegetable oil as a raw material, named monoglyceride for short, is purified by a molecular distillation technology to obtain the effective component of more than 90 percent, and is also named as molecular distilled monoglyceride, the distilled glyceryl monostearate is an emulsifier and an additive of food, and is used as an emulsifier in cosmetics and medical ointments to enable the ointments to be fine and smooth, and is used as an emulsifier of industrial silk oil agents and a lubricant of textiles, as an antistatic agent, a dripping agent and an antifogging agent in plastic films, as a lubricant, a plasticizer, an anti-shrinking agent and an antistatic agent in plastic processing, and can be used as an antifoaming agent, a dispersing agent, a thickening agent and a wetting agent in other aspects;
the oil-water separation phenomenon often occurs in food processing, the emulsion stabilizer is added to enable the mixed phase to form uniform emulsion, the phenomena of oil-water separation, delamination and precipitation of food and beverage are avoided and prevented, the product quality is improved, the shelf life is prolonged, the molecular distillation monoglyceride can form a complex with protein and starch, and an insoluble complex with amylose can prevent starch from being recrystallized after cooling and prevent starch from aging and retrogradation, so that foods rich in starch such as bread, cakes and potato products can be kept fresh for a long time, the pinofine molecular distillation monoglyceride can be directionally arranged on the surface of grease, the effect of controlling and stabilizing grease crystallization is achieved, particularly grease products such as artificial butter and the like can achieve the effects of improving plasticity and ductility and preventing bleeding and delamination.
The prior art has the following defects:
1. the distilled glyceryl monostearate has high glycerol content, the finished product is easy to agglomerate, the distilled glyceryl monostearate can not play the roles of a plasticizer and an anti-shrinking agent in the processing of a plastic foaming product, the effect of an internal lubricant is reduced in the production of a PVC product, the glycerol is easy to separate out, the monoglyceride content is low, the content of the triglyceride is increased, and the emulsifying effect is influenced when the distilled glyceryl monostearate is used in the food industry;
2. the traditional process adopts a four-stage distillation process, wherein a first-stage long-range evaporator extracts glycerol, a second-stage short-range evaporator extracts glycerol and a small amount of fatty acid, a third-stage short-range evaporator extracts fatty acid, a fourth-stage short-range evaporator extracts ditriester, and the rest is finished distilled monoglyceride.
Disclosure of Invention
The invention provides a production process for distilling glycerin monostearate by low glycerin, which adopts a three-stage distillation process, wherein a second stage is a half-short-distance evaporator, and the evaporation effect of the evaporator is improved by controlling vacuum, temperature of heat-conducting oil, temperature of medium-temperature water and the like, so that the excessive glycerin is prevented from reaching a third stage distillation, the problem that the glycerin cannot be removed by the third stage distillation is avoided, the content of finished glycerin is effectively reduced, and the problems in the background art are solved.
In order to achieve the purpose, the invention provides the following technical scheme: a production process for distilling glycerin monostearate from low glycerin comprises the following steps:
s1: esterification reaction
Preparing hydrogenated oil and glycerol materials, then feeding the materials into an esterification kettle, starting a heat conduction oil control system, heating the materials to a set temperature by using heat conduction oil in a vacuum state, continuously stirring the materials during heating, quenching the reacted materials through a cooler after the esterification reaction is finished, and feeding the cooled materials into a crude ester turnover tank for distillation;
s2: multistage distillation process
A. Primary distillation: opening a discharge valve of the crude ester turnover tank and a distillation feed pump, and opening a stirring and discharging ball valve when a material flows down at a discharge sight glass of the primary distillation long-range evaporator;
B. secondary distillation: starting a stirring and discharging ball valve of the second-stage half short-range evaporator, and observing the discharging condition of each material at a discharging sight glass;
C. and (3) three-stage distillation: starting a stirring and discharging ball valve of the three-stage short-distance evaporator, and observing the blanking condition of each material at a discharging sight glass;
s3: recycling and reusing
Opening a finished ester product discharging pump to recover glycerol after primary distillation, opening the finished ester product discharging pump to recover glycerol and fatty acid after secondary distillation, opening the finished ester product discharging pump to recover ditriester after secondary distillation, and returning the recovered glycerol, fatty acid and ditriester to the esterification kettle for recycling through a circulating system;
s4: powder spraying and sieving
Conveying the finished product to a powder spraying tower through a guide pipe, spraying powder to a vibrating screen by the powder spraying tower, performing vibrating screening treatment on the finished product by the vibrating screen, and freezing the screened finished product by a refrigerator;
s5: metering package
And (4) placing the screened finished product powder into an automatic packaging machine for automatic metering and packaging.
In a preferred embodiment, in step S1, a preparation tool before the esterification reaction is used to determine the water inlet and outlet valves of each circulating water and the water inlet and outlet valves of the cold trap, open the circulating water pump, observe whether the water pressure gauge and the cooling tower return water are normal, open the steam valves of the branch cylinders, pay attention to checking whether the steam in the steam pipelines of each path of material is smooth, open the screw vacuum pump, check whether the vacuum display of the esterification kettle is normal, the produced molecular distillation monoglyceride is liquid and forms powder after spray granulation, the melting point of the distilled monoglyceride is very low, which is only 65 degrees, because the glycerin content of monoglyceride is high, and the monoglyceride has a chemical process of crystal transformation after being produced, the monoglyceride can release heat during the process of crystal transformation, so that the packaged monoglyceride is agglomerated after lamination, thereby seriously affecting the use, and generally enhancing ventilation during storage, the stacking height is reduced, or the packaging is sieved again after being stored for a period of time, so that the warehouse pressure and the labor cost are increased.
In a preferred embodiment, in the step S1, the vacuum pressure of the esterification kettle is-0.05 ± 0.01MPa, the reaction temperature is 235 ± 5 ℃, the reaction time is 1.5-2h, the holding time is 0.5-1h, the content of monoglyceride glycerin is high, and the monoglyceride glycerin is contained together with the foaming agent, so that the uniform and fine foam structure and the shrinkage of small bubbles are affected, especially the shrinkage resistance is reduced when the temperature is low in winter, the brightness and smoothness of the product are reduced, and the foamed product is shrunk.
In a preferred embodiment, in step S1, the hydrogenated oil and glycerin material are formulated according to a formulation table control system, a hydrogenated oil and glycerin feed valve is opened, a hydrogenated oil and glycerin gear pump is opened, the feed rate is automatically controlled by a mass flow meter, the catalyst is formulated according to an automatic weighing system, the feed time and the feed rate are set, a start button is opened, the precision of the mass flow meter is 1kg, the automatic weighing system comprises an electronic scale, the precision of the electronic scale is ± 5g, before PVC plasticization, the polar group of the internal lubricant monoglyceride has a certain affinity with the polar node of the PVC resin to form a complex with strong bond energy, thereby weakening or eliminating the attraction force among particles of PVC layers, allowing the intertwined chain segments of PVC to be easily diffused, the boundary between the molecular groups to easily disappear, promoting PVC resin plasticization, when the PVC processing temperature reaches a certain temperature, monoglyceride glycerin is easy to separate out, so that the flowability of PVC resin is poor, the viscosity of a melt is increased, and the monoglyceride glycerin cannot play a role in internal lubrication.
In a preferred embodiment, in the step S2, the control requirements of the long-range evaporator are that the vacuum degree is less than 200Pa, the temperature of the heat transfer oil is 160 ± 5 ℃ and the temperature of the circulating water is 25 ± 5 ℃, the control requirements of the half short-range evaporator are that the vacuum degree is less than 100Pa, the temperature of the heat transfer oil is 175 ± 5 ℃ and the temperature of the circulating water is 65 ± 5 ℃, and the control requirements of the short-range evaporator are that the vacuum degree is less than 50Pa, the temperature of the heat transfer oil is 190 ± 5 ℃ and the temperature of the circulating water is 65 ± 5 ℃.
In a preferred embodiment, in step S2, the preparation before distillation is performed to determine the water inlet and outlet valves of each circulating water and the water inlet and outlet valves of the cold trap, start the circulating water pump, observe whether the water return of the water pressure gauge and the cooling tower is normal, start the steam valves of the branch cylinders, check whether the steam in the steam pipelines of each path of material is smooth, fill the water in the intermediate temperature water tank, start the steam preheating to a set temperature, close the steam valves, start the intermediate temperature water pump, start the screw vacuum pump, the roots pump set and the oil diffusion booster pump, check whether the vacuum display of each evaporator is normal, start the heat transfer oil pump, set the temperature of each evaporator according to the requirement, and open the automatic heat transfer oil regulating valve of each evaporator.
In a preferred embodiment, the preparation before distillation further comprises filling the medium-temperature water tank with water, starting steam to preheat to a set temperature, closing a steam valve, starting a medium-temperature water pump, starting a screw vacuum pump, a roots pump unit and an oil diffusion booster pump, checking whether vacuum display of each evaporator is normal, starting a heat conduction oil pump, setting the temperature of each evaporator according to requirements, and opening a heat conduction oil automatic regulating valve of each evaporator.
In a preferred embodiment, in the step S4, the feeding temperature of the powder spraying tower is less than or equal to 90 ℃, the temperature of the freezer is less than or equal to 10 ℃, and the fineness of the finished product powder after being screened by the vibrating screen is less than or equal to 20 meshes.
In a preferred embodiment, in step S5, the workshop where the automatic packaging machine is located is a clean workshop, the workshop and the production facility need to be hygienically controlled, the staff enters the workshop after washing hands and sterilizing, the workshop needs to be sterilized after the work is finished, and the electronic scale is calibrated by a standard weight of 25kg before the packaging, wherein the net content deviation is +/-1%.
In a preferred embodiment, in step S5, the packaged finished product is subjected to gold inspection by an automatic online all-digital intelligent metal foreign matter inspection machine, the quality inspection unit performs sampling inspection, the inspection result is compared with the product production inspection index requirement, the qualified finished product is put in storage, if the inspection is not qualified, the qualified product enters an unqualified product control program, the online all-digital intelligent metal foreign matter inspection machine is calibrated by a test block (iron phi is less than or equal to 2.0mm, stainless steel phi is less than or equal to 2.5 mm) before use, a standard test block is used every 2h during the inspection process, the product inspection standard is that the acid value is less than or equal to 2.0%, the free glycerol is less than or equal to 1.0%, and the monoglyceride content is greater than or equal to 95%.
The invention has the technical effects and advantages that:
1. according to the invention, a three-stage distillation process is adopted, wherein the second stage is a half-short-distance evaporator, and the evaporation effect of the evaporator is improved by controlling the vacuum, the temperature of the heat-conducting oil, the temperature of the medium-temperature water and the like, so that the excessive glycerol is prevented from reaching the third stage distillation, the problem that the glycerol cannot be removed by the third stage distillation is avoided, and the content of the finished glycerol is effectively reduced;
2. the invention adopts a three-stage distillation process, which not only reduces the glycerol content of the finished product, but also improves the yield of the finished product by 10-12%, and improves the process from four-stage distillation to three-stage distillation, thereby reducing one evaporator, reducing the equipment investment cost, and simultaneously reducing the equipment maintenance cost.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive effort.
FIG. 1 is a flow chart of the operation of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. The components of the embodiments of the present application, generally described and illustrated in the figures herein, can be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present application, presented in the accompanying drawings, is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. 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 application.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the embodiments of the present application, it should be noted that the indication of the orientation or positional relationship is based on the orientation or positional relationship shown in the drawings, or the orientation or positional relationship which is usually placed when the product of the application is used, or the orientation or positional relationship which is conventionally understood by those skilled in the art, or the orientation or positional relationship which is usually placed when the product of the application is used, and is only for the convenience of describing the application and simplifying the description, but does not indicate or imply that a kind of prefabricated house or element which is indicated must have a specific orientation, be constructed in a specific orientation, and be operated, and therefore, cannot be construed as limiting the application. Furthermore, the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
In the description of the embodiments of the present application, it should also be noted that, unless otherwise explicitly stated or limited, the terms "disposed," "mounted," and "connected" are to be construed broadly, and may for example be fixedly connected, detachably connected, or integrally connected; may be directly connected or indirectly connected through an intermediate. The specific meaning of the above terms in the present application can be understood in a specific case by those of ordinary skill in the art.
Referring to the attached figure 1 of the specification, the invention provides a production process for distilling low-glycerol glycerin monostearate, which comprises the following steps:
s1: esterification reaction
Preparing hydrogenated oil and glycerol materials, then feeding the materials into an esterification kettle, starting a heat conduction oil control system, heating the materials to a set temperature by using heat conduction oil in a vacuum state, continuously stirring the materials during heating, quenching the reacted materials through a cooler after the esterification reaction is finished, and feeding the cooled materials into a crude ester turnover tank for distillation;
s2: multistage distillation process
Primary distillation: opening a discharge valve of the crude ester turnover tank and a distillation feed pump, and opening a stirring and discharging ball valve when a material flows down at a discharge sight glass of the primary distillation long-range evaporator;
secondary distillation: starting a stirring and discharging ball valve of the second-stage half short-range evaporator, and observing the discharging condition of each material at a discharging sight glass;
and (3) three-stage distillation: starting a stirring and discharging ball valve of the three-stage short-distance evaporator, and observing the blanking condition of each material at a discharging sight glass;
s3: recycling and reusing
Opening a finished ester product discharging pump to recover glycerol after primary distillation, opening the finished ester product discharging pump to recover glycerol and fatty acid after secondary distillation, opening the finished ester product discharging pump to recover ditriester after secondary distillation, and returning the recovered glycerol, fatty acid and ditriester to the esterification kettle for recycling through a circulating system;
s4: powder spraying and sieving
Conveying the finished product to a powder spraying tower through a guide pipe, spraying powder to a vibrating screen by the powder spraying tower, performing vibrating screening treatment on the finished product by the vibrating screen, freezing the screened finished product by a refrigerator, wherein the feeding temperature of the powder spraying tower is less than or equal to 90 ℃, the temperature of the refrigerator is less than or equal to 10 ℃, the fineness of the powder screened by the vibrating screen is less than or equal to 20 meshes, periodically checking the screen mesh state of the vibrating screen, and sampling and detecting the powder fineness by a quality inspection part;
s5: metering package
The screened finished product powder is put into an automatic packaging machine for automatic metering and packaging, the workshop where the automatic packaging machine is located is a clean workshop, the workshop and production facilities need sanitary control, staff enter the clean workshop after washing hands and sterilizing in a changing room, the workshop needs to be cleaned and sterilized after the work is finished, a 25kg standard weight is used for calibrating an electronic scale before packaging, the net content deviation is +/-1%, the packaged finished product is subjected to gold detection by an automatic online all-digital intelligent metal foreign matter detector, a quality detection part performs sampling detection, the detection result is compared with the product output inspection index requirement, the qualified finished product is put in storage, if the detection is unqualified, a unqualified product control program is entered, the online all-digital intelligent metal foreign matter detector is calibrated by a test block (iron phi is less than or equal to 2.0mm, stainless steel phi is less than or equal to 2.5 mm) before use, the standard test block is used every 2 hours in the detection process, the product detection standard is that the acid value is less than or equal to 2.0%, free glycerol is less than or equal to 1.0%, the content of monoglyceride is more than or equal to 95 percent.
Example 1
The molecular distillation monoglyceride is insoluble in cold water, can be dissolved in hot water, is emulsified after strong oscillation, is a water-in-oil emulsifier, the HLB value of common 40 percent monoglyceride is 2.5-3.9, the HLB value of the molecular distillation monoglyceride is 3.9-5.3, and has better emulsification and expansion effects, the molecular distillation monoglyceride contains more than 90 percent of monoester and other ditriesters, the monoester plays an emulsification and expansion effect, and the ditriesters play a role in counteracting the emulsification and expansion effect and are main components of a defoaming agent, so the higher the monoester content, the less the ditriester content, the better the emulsification and expansion effect, the higher the emulsification and expansion effect can be achieved by adding a small amount, the molecular distillation monoglyceride content is up to more than 95 percent, and the product cost performance is higher.
Further, in step S1, before the esterification, a preparation task is performed to determine the water inlet and outlet valves of each circulating water and the water inlet and outlet valves of the cold trap, start the circulating water pump, observe whether the water pressure gauge and the cooling tower return water are normal, start the steam valves of the branch cylinders, pay attention to check whether the steam in the steam pipelines of each path of material is smooth, start the screw vacuum pump, check whether the vacuum display of the esterification kettle is normal, the vacuum pressure of the esterification kettle is-0.05 ± 0.01MPa, the reaction temperature is 235 ± 5 ℃, the reaction time is 1.5-2h, the heat preservation time is 0.5-1h, the feeding of the hydrogenated oil and the glycerol controls the speed of the gear pump through a mass flow meter, and the precision of the flow meter is 1 kg. The catalyst is automatically added once within 30min according to an automatic weighing system, the adding amount of each time is added according to the set amount, and the error of an electronic scale is +/-5 g.
Further, in step S1, the hydrogenated oil and glycerol material are set according to a formula table control system, a hydrogenated oil and glycerol feed valve is opened, a hydrogenated oil and glycerol gear pump is opened, the feed amount is automatically controlled through a mass flow meter, the catalyst is set with the feed time and feed amount according to an automatic weighing system, a start button is started, the precision of the mass flow meter is 1kg, the automatic weighing system comprises an electronic scale, the precision of the electronic scale is +/-5 g, the vacuumizing pressure is controlled to be-0.05 +/-0.01 MPa under the vacuum state, the catalyst is heated to 160 ℃ -180 ℃ by utilizing heat conducting oil, continuous stirring is carried out during heating, the water yield of a cold trap is larger, continuous heating and stirring are carried out, the reaction temperature is 235 +/-5 ℃, the reaction time is about 1.5-2h, the heat preservation stage is carried out, the time is 0.5-1h, the solution is gradually transparent, and the esterification reaction is finished, sampling and detecting the crude ester of the process product.
Further, in step S2, the control requirements of the long-range evaporator are that the vacuum degree is less than 200Pa, the temperature of the heat transfer oil is 160 ± 5 ℃ and the temperature of the circulating water is 25 ± 5 ℃, the control requirements of the half short-range evaporator are that the vacuum degree is less than 100Pa, the temperature of the heat transfer oil is 175 ± 5 ℃ and the temperature of the circulating water is 65 ± 5 ℃, and the control requirements of the short-range evaporator are that the vacuum degree is less than 50Pa, the temperature of the heat transfer oil is 190 ± 5 ℃ and the temperature of the circulating water is 65 ± 5 ℃.
Further, in step S2, the pre-distillation preparation tool determines the water inlet and outlet valves of each circulating water and the water inlet and outlet valves of the cold trap, opens the circulating water pump, observes whether the backwater of the water pressure gauge and the cooling tower is normal, opens the steam valves of the branch cylinders, checks whether the steam in the steam pipelines of each path of material is smooth, fills the water in the intermediate temperature water tank, opens the steam valve after preheating the steam to a set temperature, opens the intermediate temperature water pump, opens the screw vacuum pump, the roots pump set and the oil diffusion booster pump, checks whether the vacuum display of each evaporator is normal, opens the heat conduction oil pump, sets the temperature of each evaporator according to the requirement, opens the automatic heat conduction oil regulating valve of each evaporator, the pre-distillation preparation tool further includes filling the water in the intermediate temperature water tank, opens the steam after preheating the steam to a set temperature, closes the steam valve, opens the intermediate temperature water pump, opens the screw vacuum pump, the roots pump set and the oil diffusion booster pump, checking whether the vacuum display of each evaporator is normal or not, starting a heat-conducting oil pump, setting the temperature of each evaporator according to requirements, and opening a heat-conducting oil automatic regulating valve of each evaporator.
Example 2
The long-range evaporator controls the vacuum degree to be less than or equal to 200Pa by using a screw vacuum pump and a roots pump unit, the temperature of a heat conduction oil automatic valve is controlled to be 160 +/-5 ℃, the temperature of circulating water is controlled to be 25 +/-5 ℃, the glycerol recovered by a cold trap is normally discharged, the glycerol is clear and transparent, the key indexes of the working procedure are mainly controlled to release the glycerol and the water, and the monoglyceride after primary distillation is extracted and detected.
Example 3
The semi-short-range evaporator controls the vacuum degree to be less than or equal to 100Pa by using a screw vacuum pump and a Roots pump unit, the temperature of a heat conduction oil automatic valve is controlled to be 175 +/-5 ℃, the temperature of medium-temperature water is controlled to be 65 +/-5 ℃, the glycerol recovered by a cold trap is normally discharged, the glycerol is semitransparent, the fatty acid discharged by the evaporator is normally discharged, the fatty acid is light brown, the key indexes of free glycerol and the acid value are mainly controlled in the working procedure, and the monoglyceride after secondary distillation is extracted and detected.
Example 4
The short-range evaporator controls the vacuum degree to be less than or equal to 50Pa by utilizing a screw vacuum pump, a Roots pump unit and an oil diffusion booster pump, the temperature of a heat conduction oil automatic valve is controlled to be 190 +/-5 ℃, the temperature of medium-temperature water is controlled to be 65 +/-5 ℃, under the condition, the evaporation ester discharge of the evaporator is normal, the evaporation ester is clear and transparent, the evaporation triglyceride discharge of the evaporator is normal, the triglyceride is in a dark brown shape, the working procedure mainly controls the key index of total monoglyceride, and the monoglyceride after tertiary distillation is extracted and detected.
The following table was prepared according to the results of the monoglyceride extraction tests of examples 2-4:
as can be seen from the above table, the monoglyceride total monoglyceride fatty acid ester obtained by the three-time distillation treatment
The content of the glycerol reaches the peak value (96.77 percent), the contents of water (0.30 w/%), free glycerol (0.54 w/%), an acid value (0.54 mg/g), soap (0.03 w/%) and lead (0.016 mg/kg) are far lower than the international standard, a three-stage distillation process is adopted, wherein the second stage is a half-short-range evaporator, and the vacuum, the temperature of heat-conducting oil, the temperature of water and the like are controlled, so that the evaporation effect of the evaporator is improved, the excessive glycerol is prevented from reaching the third stage distillation, the problem that the glycerol cannot be removed by the third stage distillation is avoided, and the content of the finished glycerol is effectively reduced.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (10)
1. A production process for distilling glycerin monostearate from low glycerin is characterized by comprising the following steps: the production process comprises the following steps:
s1: esterification reaction
Preparing hydrogenated oil and glycerol materials, then feeding the materials into an esterification kettle, starting a heat conduction oil control system, heating the materials to a set temperature by using heat conduction oil in a vacuum state, continuously stirring the materials during heating, quenching the reacted materials through a cooler after the esterification reaction is finished, and feeding the cooled materials into a crude ester turnover tank for distillation;
s2: multistage distillation process
Primary distillation: opening a discharge valve of the crude ester turnover tank and a distillation feed pump, and opening a stirring and discharging ball valve when a material flows down at a discharge sight glass of the primary distillation long-range evaporator;
secondary distillation: starting a stirring and discharging ball valve of the second-stage half short-range evaporator, and observing the discharging condition of each material at a discharging sight glass;
and (3) three-stage distillation: starting a stirring and discharging ball valve of the three-stage short-distance evaporator, and observing the blanking condition of each material at a discharging sight glass;
s3: recycling and reusing
Opening a finished ester product discharging pump to recover glycerol after primary distillation, opening the finished ester product discharging pump to recover glycerol and fatty acid after secondary distillation, opening the finished ester product discharging pump to recover ditriester after secondary distillation, and returning the recovered glycerol, fatty acid and ditriester to the esterification kettle for recycling through a circulating system;
s4: powder spraying and sieving
Conveying the finished product to a powder spraying tower through a guide pipe, spraying powder to a vibrating screen by the powder spraying tower, performing vibrating screening treatment on the finished product by the vibrating screen, and freezing the screened finished product by a refrigerator;
s5: metering package
And (4) placing the screened finished product powder into an automatic packaging machine for automatic metering and packaging.
2. The process for producing distilled glycerin monostearate of low glycerin according to claim 1, wherein: in step S1, the preparation task before the esterification reaction is to determine the water inlet and outlet valves of each circulating water and the water inlet and outlet valves of the cold trap, start the circulating water pump, observe whether the backwater of the water pressure gauge and the cooling tower is normal, start the steam valves of the systems of the gas-distributing cylinders, pay attention to check whether the steam in the steam pipelines of each material is smooth, start the screw vacuum pump, and check whether the vacuum display of the esterification reactor is normal.
3. The process for producing distilled glycerin monostearate of low glycerin according to claim 1, wherein: in the step S1, the vacuum pressure of the esterification kettle is-0.05 +/-0.01 MPa, the reaction temperature is 235 +/-5 ℃, the reaction time is 1.5-2h, and the heat preservation time is 0.5-1 h.
4. The process for producing distilled glycerin monostearate of low glycerin according to claim 1, wherein: in the step S1, the formula of the hydrogenated oil and the glycerol material is set according to a formula table control system, a hydrogenated oil and glycerol feeding valve is opened, a hydrogenated oil and glycerol gear pump is opened, the feeding amount is automatically controlled through a mass flow meter, the catalyst sets the feeding time and the feeding amount according to an automatic weighing system, a starting button is started, the precision of the mass flow meter is 1kg, the automatic weighing system comprises an electronic scale, and the precision of the electronic scale is +/-5 g.
5. The process for producing distilled glycerin monostearate of low glycerin according to claim 1, wherein: in the step S2, the control requirements of the long-range evaporator are that the vacuum degree is less than 200Pa, the temperature of the heat transfer oil is 160 ± 5 ℃ and the temperature of the circulating water is 25 ± 5 ℃, the control requirements of the half short-range evaporator are that the vacuum degree is less than 100Pa, the temperature of the heat transfer oil is 175 ± 5 ℃ and the temperature of the circulating water is 65 ± 5 ℃, and the control requirements of the short-range evaporator are that the vacuum degree is less than 50Pa, the temperature of the heat transfer oil is 190 ± 5 ℃ and the temperature of the circulating water is 65 ± 5 ℃.
6. The process for producing distilled glycerin monostearate of low glycerin according to claim 1, wherein: in the step S2, the preparation tool before distillation is used to determine the water inlet and outlet valves of each circulating water and the water inlet and outlet valves of the cold trap, start the circulating water pump, observe whether the backwater of the water pressure gauge and the cooling tower is normal, start the steam valves of each system of the gas-distributing cylinder, check whether the steam in the steam pipelines of each path of material is smooth, fill the water in the intermediate temperature water pool, start the steam preheating to a set temperature, close the steam valve, start the intermediate temperature water pump, start the screw vacuum pump, the roots pump set and the oil diffusion booster pump, check whether the vacuum display of each evaporator is normal, start the heat conduction oil pump, set the temperature of each evaporator according to requirements, and open the automatic heat conduction oil regulating valve of each evaporator.
7. The process according to claim 6, wherein the glycerol monostearate is prepared by distilling glycerol monostearate with low glycerol, and the process comprises the following steps: the preparation work before distillation also comprises the steps of filling water in the medium-temperature water tank, starting steam to preheat to a set temperature, closing a steam valve, starting a medium-temperature water pump, starting a screw vacuum pump, a roots pump unit and an oil diffusion booster pump, checking whether the vacuum display of each evaporator is normal or not, starting a heat conduction oil pump, setting the temperature of each evaporator according to requirements, and opening a heat conduction oil automatic regulating valve of each evaporator.
8. The process for producing distilled glycerin monostearate of low glycerin according to claim 1, wherein: in the step S4, the feeding temperature of the powder spraying tower is less than or equal to 90 ℃, the temperature of the refrigerating machine is less than or equal to 10 ℃, and the fineness of the powder after the finished product powder is screened by the vibrating screen is less than or equal to 20 meshes.
9. The process for producing distilled glycerin monostearate of low glycerin according to claim 1, wherein: in the step S5, the workshop where the automatic packaging machine is located is a clean workshop, the workshop and production facilities need sanitary control, staff enter the clean workshop after washing hands and sterilizing through a changing room, the workshop needs to be cleaned and sterilized after the work is finished, an electronic scale is calibrated by using a 25kg standard weight before packaging, and the net content deviation is +/-1%.
10. The process for producing distilled glycerin monostearate of low glycerin according to claim 1, wherein: in the step S5, the packaged finished product is subjected to gold detection by an automatic online all-digital intelligent metal foreign matter detector, a quality detection part performs sampling detection, the detection result is compared with the product output inspection index requirement, the qualified finished product is put in storage, if the detection is unqualified, an unqualified product control program is entered, the online all-digital intelligent metal foreign matter detector is calibrated by a test block (iron phi is less than or equal to 2.0mm, stainless steel phi is less than or equal to 2.5 mm) before use, a standard test block detector is used every 2h in the detection process, the product detection standard is that the acid value is less than or equal to 2.0%, the free glycerol is less than or equal to 1.0%, and the monoglyceride content is greater than or equal to 95%.
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| CN114015510A (en) * | 2021-11-26 | 2022-02-08 | 浙江金棕榈科技股份有限公司 | Glyceryl monostearate and glyceryl distearate composition and preparation process thereof |
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