CN114015510A - Glyceryl monostearate and glyceryl distearate composition and preparation process thereof - Google Patents

Glyceryl monostearate and glyceryl distearate composition and preparation process thereof Download PDF

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Publication number
CN114015510A
CN114015510A CN202111421500.9A CN202111421500A CN114015510A CN 114015510 A CN114015510 A CN 114015510A CN 202111421500 A CN202111421500 A CN 202111421500A CN 114015510 A CN114015510 A CN 114015510A
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Prior art keywords
glycerin
glycerol
monostearate
feeding
distearate
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Chinese (zh)
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王�锋
吴海青
巴明建
何琴
赵玉东
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Hangzhou Fuchun Food Additive Co ltd
Zhejiang Golden Palm Technology Co ltd
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Hangzhou Fuchun Food Additive Co ltd
Zhejiang Golden Palm Technology Co ltd
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Priority to CN202111421500.9A priority Critical patent/CN114015510A/en
Publication of CN114015510A publication Critical patent/CN114015510A/en
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11CFATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
    • C11C3/00Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
    • C11C3/02Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fatty acids with glycerol
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/009Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a glycerin monostearate and glycerin distearate composition and a preparation process thereof, which relate to the field of monoglyceride.A transesterification reaction is carried out in a transesterification reaction kettle by taking stearic acid and glycerin as raw materials, sodium hydroxide is used as a catalyst, nitrogen is used as a protective gas, and after the reaction is finished, heat exchange is carried out on reaction materials to obtain high-quality coarse glycerin monostearate and glycerin distearate; by adopting secondary distillation, monoglyceride with low boiling point, glycerin and other components are removed, the glycerin content is effectively controlled, the acid value is effectively controlled, and the melting point of the glycerin monostearate and glycerin distearate composition is improved, so that the defect of low melting point of old products is overcome; the material is added into the evaporating pot in a rotational flow mode, so that the material can enter an evaporating surface, namely the inner wall of the evaporating pot, with pressure, the unit evaporation capacity of the evaporator is improved, and further the production cost is reduced.

Description

Glyceryl monostearate and glyceryl distearate composition and preparation process thereof
Technical Field
The invention relates to the field of monoglyceride, and in particular relates to a glycerin monostearate and glycerin distearate composition and a preparation process thereof.
Background
The glyceryl monostearate and the glyceryl distearate are additives and emulsifiers which are most widely applied and used in the grease chemical industry and the daily chemical industry, have the hydrophilic-lipophilic balance value of 3.6-4.2, belong to oil solubility, have the functions of precipitation, digestion, aging resistance and fatty acid coagulation control besides the emulsification function, are typical nonionic surfactants, have alpha isomers and beta isomers, and have good surface activity because the structures of the surfactants contain a lipophilic long fatty acid carbon chain and two hydrophilic hydroxyls;
monoglyceride is a yellowish waxy solid, is used as emulsifier and surfactant in food or cosmetics, is also used as lubricant and antistatic agent for transparent granules of polypropylene and polyvinyl chloride, and is insoluble in water and thermally soluble in oil, paraffin, ethanol, chloroform, acetone and diethyl ether;
polypropylene is a colorless, odorless, nontoxic and semitransparent solid substance, is a thermoplastic synthetic resin with excellent performance, is colorless and semitransparent thermoplastic light general-purpose plastic, has chemical resistance, heat resistance, electrical insulation, high-strength mechanical property, good high-wear-resistance processing property and the like, so that the polypropylene can be rapidly and widely developed and applied in various fields of machinery, automobiles, electronic appliances, buildings, textiles, packaging, agriculture, forestry, fishery, food industry and the like since the coming out, in recent years, with the rapid development of the industries of packaging, electronics, automobiles and the like in China, the development of the industries in China is greatly promoted, in addition, because the polypropylene material has plasticity, the polypropylene material gradually replaces wooden products, the high-strength toughness and the high-wear-resistance property gradually replace the mechanical function of metal, and in addition, the polypropylene has good grafting and compounding functions, the method has huge application space in the concrete, textile, packaging and agriculture, forestry and fishery fields;
the T40S type glyceryl monostearate and glyceryl distearate are mainly used for refining polypropylene in the refining industry of olefins such as medium and petrochemical industry and medium and petroleum industry as lubricants and antistatic agents, and the formula of an auxiliary agent bag used by domestic refining enterprises is provided by foreign enterprises, and has requirements on various indexes of monoglyceride in the auxiliary agent bag: the fatty acid composition is more than or equal to 42 percent, the total monoglyceride fatty acid ester is more than or equal to 45 percent, particularly the requirement of the initial melting point is more than 58 ℃, all indexes have high requirements, the raw materials of the auxiliary agent bag used by research and refining enterprises in China start late, the process is lagged behind, and the produced glyceryl monostearate and the produced glyceryl distearate are difficult to reach the standard;
therefore, a glycerin monostearate and glycerin distearate composition meeting the production requirement of polypropylene and reducing the production cost of polypropylene enterprises and a preparation process thereof are needed to solve the problems.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a glycerin monostearate and glycerin distearate composition and a preparation process thereof: stearic acid and glycerin are used as raw materials to carry out ester exchange reaction in an ester exchange reaction kettle, sodium hydroxide is used as a catalyst, nitrogen is used as protective gas, and after the reaction is finished, heat exchange is carried out on reaction materials to obtain high-quality T40S type crude ester of mono-and di-glyceryl monostearate; the method adopts secondary distillation to remove monoglyceride with low boiling point, glycerin and other components, and adds the materials into an evaporation tank in a rotational flow mode, so that the materials can enter an evaporation surface with pressure, namely the inner wall of the evaporation tank, the unit evaporation capacity of an evaporator is improved, and the problems that the existing process is lagged behind and the produced glyceryl monostearate and glyceryl distearate cannot reach the standard easily are solved.
The purpose of the invention can be realized by the following technical scheme:
the glyceryl monostearate and glyceryl distearate composition is prepared by using stearic acid and glycerin as raw materials, sodium hydroxide as a catalyst and nitrogen as protective gas and performing ester exchange reaction in an ester exchange reaction kettle;
the addition amount of the glycerol is 20-25% of the mass of the stearic acid, and the addition amount of the sodium hydroxide is 0.05-0.20% of the total mass of the stearic acid and the glycerol;
the glycerin monostearate and the glycerin distearate composition are prepared by the following steps:
the method comprises the following steps: weighing stearic acid, glycerol and sodium hydroxide according to the mass ratio for later use;
step two: adding stearic acid, glycerol and sodium hydroxide into an ester exchange reaction kettle for carrying out ester exchange reaction to obtain a reaction product;
step three: carrying out primary distillation and secondary distillation on the reaction product to obtain a distillation product;
step four: adding the distillation product into a powder spraying tower for spraying powder, and screening the powder through a vibrating screen to obtain composition powder;
step five: and packaging and gold-detecting the composition powder, and warehousing finished products after the inspection is qualified to obtain the glyceryl monostearate and glyceryl distearate composition.
As a further scheme of the invention: the evaporimeter of one-level distillation and second grade distillation includes the evaporating pot, connects the hopper, arranges the material pipe and carries the liquid pump, the bottom of evaporating pot is installed and is connect the hopper, connect one side of hopper to install driving motor, connect the bottom of hopper to install row material pipe, the mounting panel is installed to one side of evaporating pot, the liquid pump is installed at the top of mounting panel, the inlet pipe is installed to the output of carrying the liquid pump, the top of evaporating pot is run through to the one end of inlet pipe, the top of evaporating pot is provided with the gas outlet, the gas outlet communicates to the cold-trap through the pipeline.
As a further scheme of the invention: install the hot plate in the inner wall of evaporating pot, it is provided with and stirs the cage to rotate in the inner chamber of evaporating pot, stir the side of cage on the radian install a plurality of scrape the flitch, stir the top of cage and install feed mechanism, connect the inner chamber intercommunication of hopper and evaporating pot, the inner chamber middle part that connects the hopper is provided with the installation room, the bottom at the evaporating pot is installed to the installation room, rotate in the inner chamber of installation room and install the universal driving shaft, the top of universal driving shaft is connected to the bottom of stirring the cage.
As a further scheme of the invention: the feeding mechanism comprises a feeding box, an installation cylinder and a sliding block, the installation cylinder is installed at the bottom of the feeding box, the installation cylinder is installed at the top of the stirring cage, a feeding groove is formed in the top of the feeding box, a plurality of guide vanes are installed inside the feeding groove, a flow dividing groove is formed in the bottom of the feeding box, the feeding groove is communicated with the flow dividing groove, a placing bin is arranged inside the top end of the installation cylinder, a plurality of sliding blocks penetrate through the placing bin in an active mode, the sliding blocks and materials of scraping plates are made of polytetrafluoroethylene, a plurality of feeding holes are formed in the inner side of the placing bin of the installation cylinder, and the top end of each feeding hole is communicated into an inner cavity of the flow dividing groove.
As a further scheme of the invention: the driving bevel gear and the driven bevel gear are arranged in an inner cavity of the installation chamber and are arranged at right angles, the driving bevel gear and the driven bevel gear are meshed and connected, the driving bevel gear is sleeved on an output shaft of the driving motor, and the driven bevel gear is sleeved on the universal driving shaft.
As a further scheme of the invention: arrange the top one end of material pipe and seted up and connect the material mouth, install in the inner chamber of arranging the material pipe and carry the spiral leaf, the one end of carrying the spiral leaf is connected to on the output shaft of defeated material motor, defeated material motor is installed and is served at row material pipe.
As a further scheme of the invention: a preparation process of a glycerin monostearate and glycerin distearate composition comprises the following steps:
the method comprises the following steps: weighing stearic acid, glycerol and sodium hydroxide according to the mass ratio for later use;
step two: adding stearic acid, glycerol and sodium hydroxide into an ester exchange reaction kettle, introducing nitrogen for protection, and carrying out heat preservation reaction for 0.5-1h under the conditions that the pressure is-0.08 to-0.10 MPa and the reaction temperature is 230-240 ℃ to obtain a reaction product; wherein, the exhaust gas generated by the vacuum pump is incinerated in the boiler at high temperature;
step three: performing primary distillation and secondary distillation on the reaction product to obtain a distillation product, controlling the vacuum degree of an evaporator in the primary distillation to be 400Pa or below 400Pa and the temperature to be 150-170 ℃, and controlling the vacuum degree of the evaporator in the secondary distillation to be 300Pa or below 300Pa and the temperature to be 160-180 ℃;
step four: adding the distillation product into a powder spraying tower for spraying powder, controlling the feeding temperature to be 90 ℃ or below 90 ℃, and screening by using a vibrating screen after the powder spraying, wherein the aperture of a screen mesh of the vibrating screen is 20 meshes to obtain composition powder;
step five: and packaging and gold-detecting the composition powder, and warehousing finished products after the inspection is qualified to obtain the glyceryl monostearate and glyceryl distearate composition.
As a further scheme of the invention: and the packaging in the fifth step is realized by using a woven bag or a paper-plastic composite bag, the outer package is removed before entering a packaging room, the inner package is sterilized by ultraviolet rays, and the standard test block iron phi is less than or equal to 2.0mm and the stainless steel phi is less than or equal to 2.5mm in the gold detection process.
The invention has the following beneficial effects:
according to the glyceryl monostearate and the glyceryl distearate composition and the preparation process thereof, stearic acid and glycerol are taken as raw materials to carry out ester exchange reaction in an ester exchange reaction kettle, sodium hydroxide is taken as a catalyst, nitrogen is taken as a protective gas, and after the reaction is finished, heat exchange is carried out on reaction materials to obtain high-quality T40S type coarse glyceryl monostearate and distearate; adopting secondary distillation to remove monoglyceride with low boiling point, glycerin and other components, effectively controlling the content of glycerin to achieve that the free glycerin of a finished product is less than or equal to 3.0 percent, simultaneously effectively controlling the acid value to achieve that the acid value of the finished product is less than or equal to 3.0 percent, and improving the melting point of the glycerin monostearate and the glycerin distearate composition to enable the melting point to reach 58-70 ℃, thereby solving the defect of low melting point of old products; the material is added into the evaporating pot in a rotational flow mode, so that the material can enter an evaporating surface, namely the inner wall of the evaporating pot, with pressure, the unit evaporation capacity of the evaporator is improved, and further the production cost is reduced.
The preparation process improves the quality of T40S type mono-and di-glyceryl monostearate crude ester by using an evaporator, a driving motor runs through a driving bevel gear and a driven bevel gear to drive a universal driving shaft to rotate so as to drive a stirring cage and a feeding mechanism to rotate, a reaction product falls into a feeding groove of the feeding mechanism in an inclined direction, a guide vane in the feeding groove rotates, the rotation direction of the guide vane is the same as the feeding direction of the reaction product, under the synergistic action of the driving bevel gear and the driven bevel gear, the reaction product forms a rotational flow and enters a diversion groove at a high speed, then the reaction product flows out from a feeding hole at a high speed, and then is thrown onto the inner wall of an evaporation tank through the rotating stirring cage, so that the reaction product can be contacted with the inner wall of the high-temperature evaporation tank, then the reaction product is uniformly scraped onto the inner wall of the evaporation tank by using a scraper plate, and the evaporation efficiency of the reaction product is further improved, then sufficiently and quickly evaporating and discharging low boiling point substances in the glycerol monostearate, so that the remaining low boiling point substances in the distillation product are few, and factors influencing the melting point of the glycerol monostearate composition and the glycerol distearate composition are sufficiently removed, so that the glycerol monostearate and the glycerol distearate composition can reach the use standard of the glycerol monostearate composition and the glycerol distearate composition; the evaporator has high evaporation efficiency and good evaporation effect.
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a process flow diagram of a process for preparing a glycerol mono-and distearate composition of the present invention;
FIG. 2 is a schematic view of the evaporator according to the present invention;
FIG. 3 is a schematic view showing the internal structure of an evaporator according to the present invention;
FIG. 4 is a schematic view of the feed mechanism of the present invention;
FIG. 5 is a top view of the feed box of the present invention;
FIG. 6 is a bottom view of the mounting cartridge of the present invention;
FIG. 7 is a schematic view showing the internal structure of a discharge pipe in the present invention;
FIG. 8 is the connection view of the driving bevel gear, the driven bevel gear and the linkage shaft.
In the figure: 101. an evaporator tank; 102. a receiving hopper; 103. a discharge pipe; 104. a material conveying motor; 105. mounting a plate; 106. a liquid conveying pump; 107. a feed pipe; 108. a drive motor; 109. an installation chamber; 110. heating plates; 111. a scraping plate; 112. stirring a cage; 113. a feeding mechanism; 114. a feeding box; 115. a feed chute; 116. a shunt slot; 117. mounting the cylinder; 118. a slider; 119. a guide vane; 120. placing a bin; 121. a feed port; 122. conveying the spiral blade; 123. a material receiving port; 124. a driving bevel gear; 125. a driven helical gear; 126. a linkage shaft.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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.
Example 1:
referring to fig. 1, this embodiment is a process for preparing glycerol monostearate and glycerol distearate compositions, which comprises the following steps:
the method comprises the following steps: weighing stearic acid, glycerol and sodium hydroxide according to the mass ratio for later use;
step two: adding stearic acid, glycerol and sodium hydroxide into an ester exchange reaction kettle, introducing nitrogen for protection, and carrying out heat preservation reaction for 1h under the conditions that the pressure is-0.97 MPa and the reaction temperature is 220-240 ℃ to obtain a reaction product;
the specific process is as follows:
in a vacuum state, pumping sodium hydroxide into an ester exchange reaction kettle 1# by a gear pump through a flowmeter, heating and heating by utilizing heat conduction oil, continuously stirring when heating, heating to 220 ℃, filling nitrogen gas when reacting, starting a discharge pump of the ester exchange reaction kettle 1# when the liquid level of the ester exchange reaction kettle 1# reaches a discharge position, driving the material of the ester exchange reaction kettle 1# into the ester exchange reaction kettle 2# by the speed of the automatic liquid level control pump through the discharge pump, continuously heating, stirring and heating for reaction, heating to 240 ℃, filling nitrogen gas when reacting, wherein the nitrogen gas pressure is 0.08MPa, and finishing the ester exchange reaction when the solution becomes a transparent solution; when the liquid level of the transesterification reaction kettle No. 2 reaches a discharging position, a discharging pump of the transesterification reaction kettle No. 2 is started, the speed of the pump is automatically controlled by the discharging pump through the liquid level, the reacted materials enter a crude ester storage tank after heat exchange is carried out on the reacted materials through a cooler, and two-stage distillation is prepared;
step three: performing primary distillation and secondary distillation on the reaction product to obtain a distillation product, controlling the vacuum degree of an evaporator in the primary distillation to be 400Pa and the temperature to be 160 ℃, and controlling the vacuum degree of the evaporator in the secondary distillation to be 300Pa and the temperature to be 170 ℃;
the specific working process of the evaporator is as follows:
s31: starting the delivery liquid pump 106, wherein the delivery liquid pump 106 operates to deliver the reaction product into the inner cavity of the evaporation tank 101 through the feed pipe 107;
s32: the driving motor 108 is started, the driving motor 108 operates to drive the driving bevel gear 124 to rotate, and the driving bevel gear 124 and the driven bevel gear 125 are meshed and connected, so that the linkage shaft 126 is driven to rotate, and the stirring cage 112 and the feeding mechanism 113 are driven to rotate;
s33: reaction products fall into a feeding groove 115 of a feeding mechanism 113 in an inclined direction, a guide vane 119 in the feeding groove 115 rotates, the rotation direction of the guide vane 119 is the same as the feeding direction of the reaction products, so that the reaction products form a rotational flow and enter a diversion groove 116, then the reaction products flow out through a feeding hole 121 and are thrown onto the inner wall of an evaporation tank 101 through a rotating stirring cage 112, and the stirring cage 112 drives a sliding block 118 to move outwards when rotating and abuts against the inner wall of the evaporation tank 101, so that the thrown reaction products are prevented from overflowing upwards;
s34: starting the heating plate 110, heating the inner wall of the evaporation tank 101 by heat released by the heating plate 110, uniformly scraping reaction products onto the inner wall of the evaporation tank 101 through the scraper plate 111 when the stirring cage 112 rotates, heating and drying to evaporate low-boiling monoglyceride, glycerin and other components to form gas, communicating the gas from a gas outlet to a cold trap through a pipeline for condensation, and recycling the gas, wherein the rest reaction products rotate downwards along with the inner wall of the evaporation tank 101, then enter the receiving hopper 102, enter the discharging pipe 103 through the receiving port 123 to obtain distillation products, starting the material conveying motor 104, and driving the conveying spiral blades 122 to rotate by the operation of the material conveying motor 104 so as to output the distillation products;
step four: adding the distillation product into a powder spraying tower for spraying powder, controlling the feeding temperature to be 90 ℃, and screening the powder through a vibrating screen after the powder spraying, wherein the aperture of a screen mesh of the vibrating screen is 20 meshes to obtain composition powder;
step five: and packaging and gold-detecting the composition powder, and warehousing finished products after the inspection is qualified to obtain the glyceryl monostearate and glyceryl distearate composition.
The glyceryl monostearate and the glyceryl distearate composition are tested for 5 times and every 24 hours, and the test results are as follows:
Figure BDA0003377568120000081
Figure BDA0003377568120000091
referring to the data in the table, it can be found that the glyceryl monostearate and the glyceryl distearate composition both meet the standard according to the comparison between the new product trial index and the detection result.
Example 2:
referring to fig. 2-8, the present embodiment is an evaporator, including an evaporation tank 101, a receiving hopper 102, a discharging pipe 103 and a liquid conveying pump 106, the receiving hopper 102 is installed at the bottom of the evaporation tank 101, a driving motor 108 is installed at one side of the receiving hopper 102, the discharging pipe 103 is installed at the bottom of the receiving hopper 102, an installation plate 105 is installed at one side of the evaporation tank 101, the liquid conveying pump 106 is installed at the top of the installation plate 105, a feeding pipe 107 is installed at an output end of the liquid conveying pump 106, one end of the feeding pipe 107 penetrates through the top of the evaporation tank 101, a gas outlet is arranged at the top of the evaporation tank 101, and the gas outlet is communicated to a cold trap through a pipeline;
a heating plate 110 is installed in the inner wall of the evaporating pot 101, a stirring cage 112 is rotatably arranged in the inner cavity of the evaporating pot 101, a plurality of scraping plates 111 are installed on the side surface of the stirring cage 112 in an equal radian manner, a feeding mechanism 113 is installed at the top of the stirring cage 112, the receiving hopper 102 is communicated with the inner cavity of the evaporating pot 101, an installation chamber 109 is arranged in the middle of the inner cavity of the receiving hopper 102, the installation chamber 109 is installed at the bottom of the evaporating pot 101, a linkage shaft 126 is rotatably installed in the inner cavity of the installation chamber 109, and the top end of the linkage shaft 126 is connected to the bottom of the stirring cage 112;
the feeding mechanism 113 comprises a feeding box 114, an installation cylinder 117 and sliding blocks 118, the installation cylinder 117 is installed at the bottom of the feeding box 114, the installation cylinder 117 is installed at the top of the stirring cage 112, a feeding groove 115 is formed in the top of the feeding box 114, a plurality of guide vanes 119 are installed inside the feeding groove 115, a diversion groove 116 is formed in the bottom of the feeding box 114, the feeding groove 115 is communicated with the diversion groove 116, a placing bin 120 is arranged inside the top end of the installation cylinder 117, a plurality of sliding blocks 118 movably penetrate through the placing bin 120, the sliding blocks 118 and the scraping plate 111 are made of polytetrafluoroethylene, a plurality of feeding holes 121 are formed in the inner side of the placing bin 120 of the installation cylinder 117, and the top ends of the feeding holes 121 are communicated into the inner cavity of the diversion groove 116;
a driving bevel gear 124 and a driven bevel gear 125 are arranged in an inner cavity of the mounting chamber 109, the driving bevel gear 124 and the driven bevel gear 125 are arranged at a right angle, the driving bevel gear 124 and the driven bevel gear 125 are in meshed connection, the driving bevel gear 124 is sleeved on an output shaft of the driving motor 108, and the driven bevel gear 125 is sleeved on a universal driving shaft 126;
a material receiving port 123 is formed at one end of the top of the material discharging pipe 103, a conveying spiral blade 122 is installed in an inner cavity of the material discharging pipe 103, one end of the conveying spiral blade 122 is connected to an output shaft of the material conveying motor 104, and the material conveying motor 104 is installed at one end of the material discharging pipe 103.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.

Claims (8)

1. The glycerin monostearate and glycerin distearate composition is characterized in that stearic acid and glycerin are used as raw materials, sodium hydroxide is used as a catalyst, nitrogen is used as protective gas, and ester exchange reaction is carried out in an ester exchange reaction kettle to obtain the glycerin monostearate and glycerin distearate composition;
the addition amount of the glycerol is 20-25% of the mass of the stearic acid, and the addition amount of the sodium hydroxide is 0.05-0.20% of the total mass of the stearic acid and the glycerol;
the glycerin monostearate and the glycerin distearate composition are prepared by the following steps:
the method comprises the following steps: weighing stearic acid, glycerol and sodium hydroxide according to the mass ratio for later use;
step two: adding stearic acid, glycerol and sodium hydroxide into an ester exchange reaction kettle for carrying out ester exchange reaction to obtain a reaction product;
step three: carrying out primary distillation and secondary distillation on the reaction product to obtain a distillation product;
step four: adding the distillation product into a powder spraying tower for spraying powder, and screening the powder through a vibrating screen to obtain composition powder;
step five: and packaging and gold-detecting the composition powder, and warehousing finished products after the inspection is qualified to obtain the glyceryl monostearate and glyceryl distearate composition.
2. A glycerol mono-and distearate composition according to claim 1 wherein the evaporator of the primary distillation and of the secondary distillation comprises an evaporation tank (101), a receiving hopper (102), a discharge conduit (103) and a feed liquid pump (106), a receiving hopper (102) is arranged at the bottom of the evaporating pot (101), a driving motor (108) is arranged at one side of the receiving hopper (102), a discharge pipe (103) is arranged at the bottom of the receiving hopper (102), a mounting plate (105) is arranged at one side of the evaporating pot (101), the top of the mounting plate (105) is provided with a liquid conveying pump (106), the output end of the liquid conveying pump (106) is provided with a feeding pipe (107), the one end of inlet pipe (107) runs through the top of evaporating pot (101), the top of evaporating pot (101) is provided with the gas outlet, the gas outlet passes through the pipeline intercommunication to the cold-trap.
3. The glyceryl monostearate and the glyceryl distearate composition according to claim 2, wherein the heating plate (110) is mounted in the inner wall of the evaporation tank (101), the stirring cage (112) is rotatably disposed in the inner cavity of the evaporation tank (101), the plurality of scraping plates (111) are disposed on the side surface of the stirring cage (112) in an equal arc manner, the feeding mechanism (113) is mounted at the top of the stirring cage (112), the receiving hopper (102) is communicated with the inner cavity of the evaporation tank (101), the mounting chamber (109) is disposed in the middle of the inner cavity of the receiving hopper (102), the mounting chamber (109) is mounted at the bottom of the evaporation tank (101), the linkage shaft (126) is rotatably mounted in the inner cavity of the mounting chamber (109), and the top end of the linkage shaft (126) is connected to the bottom of the stirring cage (112).
4. The glyceryl monostearate and the glyceryl distearate composition according to claim 3, wherein the feeding mechanism (113) comprises a feeding box (114), a mounting cylinder (117) and a sliding block (118), the mounting cylinder (117) is mounted at the bottom of the feeding box (114), the mounting cylinder (117) is mounted at the top of the stirring cage (112), a feeding groove (115) is formed at the top of the feeding box (114), a plurality of guide vanes (119) are mounted inside the feeding groove (115), a diversion groove (116) is formed at the bottom of the feeding box (114), the feeding groove (115) is communicated with the diversion groove (116), a placing bin (120) is arranged inside the top end of the mounting cylinder (117), a plurality of sliding blocks (118) are movably penetrated through the placing bin (120), and the sliding blocks (118) and the scraping plate (111) are made of polytetrafluoroethylene, a plurality of feeding holes (121) are formed in the inner side of the placing bin (120) of the mounting cylinder (117), and the top ends of the feeding holes (121) are communicated to the inner cavity of the diversion channel (116).
5. The glycerol monostearate and the glycerol distearate composition according to claim 3, wherein the mounting chamber (109) is provided with a driving helical gear (124) and a driven helical gear (125) in the inner cavity thereof, the driving helical gear (124) and the driven helical gear (125) are arranged at a right angle to each other, the driving helical gear (124) and the driven helical gear (125) are engaged and connected, the driving helical gear (124) is sleeved on the output shaft of the driving motor (108), and the driven helical gear (125) is sleeved on the universal driving shaft (126).
6. A glycerol monostearate or distearate composition according to claim 2 wherein, a receiving opening (123) is provided at the top end of the discharge pipe (103), a conveying screw blade (122) is provided in the inner cavity of the discharge pipe (103), one end of the conveying screw blade (122) is connected to the output shaft of the conveying motor (104), and the conveying motor (104) is provided at one end of the discharge pipe (103).
7. The process for preparing glycerol monostearate or glycerol distearate composition according to claim 1, wherein the process comprises the steps of:
the method comprises the following steps: weighing stearic acid, glycerol and sodium hydroxide according to the mass ratio for later use;
step two: adding stearic acid, glycerol and sodium hydroxide into an ester exchange reaction kettle, introducing nitrogen for protection, and carrying out heat preservation reaction for 0.5-1h under the conditions that the pressure is-0.08 to-0.10 MPa and the reaction temperature is 230-240 ℃ to obtain a reaction product;
step three: performing primary distillation and secondary distillation on the reaction product to obtain a distillation product, controlling the vacuum degree of an evaporator in the primary distillation to be 400Pa or below 400Pa and the temperature to be 150-170 ℃, and controlling the vacuum degree of the evaporator in the secondary distillation to be 300Pa or below 300Pa and the temperature to be 160-180 ℃;
step four: adding the distillation product into a powder spraying tower for spraying powder, controlling the feeding temperature to be 90 ℃ or below 90 ℃, and screening by using a vibrating screen after the powder spraying, wherein the aperture of a screen mesh of the vibrating screen is 20 meshes to obtain composition powder;
step five: and packaging and gold-detecting the composition powder, and warehousing finished products after the inspection is qualified to obtain the glyceryl monostearate and glyceryl distearate composition.
8. The process for preparing glycerol monostearate or glycerol distearate composition according to claim 7, wherein the packaging in the fifth step is packaging by using a woven bag or a paper-plastic composite bag, the outer packaging is removed before entering the packaging room, the inner packaging is sterilized by ultraviolet rays, and the gold test process is carried out by using a standard test block with iron phi of not more than 2.0mm and stainless steel phi of not more than 2.5 mm.
CN202111421500.9A 2021-11-26 2021-11-26 Glyceryl monostearate and glyceryl distearate composition and preparation process thereof Pending CN114015510A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106565483A (en) * 2016-11-04 2017-04-19 杭州油脂化工有限公司 Two-step method of producing glyceryl monostearate and glyceryl distearate with low free glycerol
US20170233776A1 (en) * 2014-08-13 2017-08-17 Jinan University Method for preparing diglyceride using bubble column reactor
CN210874143U (en) * 2019-11-14 2020-06-30 杭州富春食品添加剂有限公司 Evaporator for producing high-purity low-glycerol molecular distillation monoglyceride
CN213254267U (en) * 2020-08-17 2021-05-25 单县龙宇生物科技有限公司 Compound acid mixer for furfural production
CN113416132A (en) * 2021-08-06 2021-09-21 杭州富春食品添加剂有限公司 Production process for distilling low-glycerol glycerin monostearate

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20170233776A1 (en) * 2014-08-13 2017-08-17 Jinan University Method for preparing diglyceride using bubble column reactor
CN106565483A (en) * 2016-11-04 2017-04-19 杭州油脂化工有限公司 Two-step method of producing glyceryl monostearate and glyceryl distearate with low free glycerol
CN210874143U (en) * 2019-11-14 2020-06-30 杭州富春食品添加剂有限公司 Evaporator for producing high-purity low-glycerol molecular distillation monoglyceride
CN213254267U (en) * 2020-08-17 2021-05-25 单县龙宇生物科技有限公司 Compound acid mixer for furfural production
CN113416132A (en) * 2021-08-06 2021-09-21 杭州富春食品添加剂有限公司 Production process for distilling low-glycerol glycerin monostearate

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