CN110229060B - Preparation method of food-grade sodium diacetate - Google Patents
Preparation method of food-grade sodium diacetate Download PDFInfo
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- CN110229060B CN110229060B CN201910560421.2A CN201910560421A CN110229060B CN 110229060 B CN110229060 B CN 110229060B CN 201910560421 A CN201910560421 A CN 201910560421A CN 110229060 B CN110229060 B CN 110229060B
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Abstract
The invention provides a preparation method of food-grade sodium diacetate, which comprises the following operation steps: s1, putting the sodium carbonate into the reactor at one time, adding glacial acetic acid 2.32 times of the weight of the sodium carbonate into the reactor, controlling the reaction temperature to be 80-90 ℃, and controlling the reaction time to be 2-2.5 hours; under stirring, glacial acetic acid and sodium carbonate are fully chemically reacted to synthesize sodium diacetate; s2, then curing for 1-1.5 hours at 80-90 ℃, and drying at 100-105 ℃; s3, cooling, and cooling the material to 40-45 ℃ to obtain the finished product of sodium diacetate. The reactor is a multifunctional rake reactor, comprising: support frame, transmission, bearing seal device, harrow material device, feeding device, ware body, rotary joint and heat transfer device. The invention realizes the preparation method of the food-grade sodium diacetate by utilizing the self-developed multifunctional rake reactor, has simpler production process, less equipment investment and easy operation, and is more beneficial to industrialized and automatic operation.
Description
Technical Field
The invention relates to the field of food additive production, and in particular relates to a preparation method of food-grade sodium diacetate.
Background
Sodium diacetate is a molecular complex of acetic acid and sodium acetate and appears as a white crystalline powder. Slightly smelling acetic acid, easy to dissolve in water and alcohol, its melting point is 95 deg.C, its decomposition temp. is 150 deg.C, it can be burnt, and after it is burnt, it can be acidified to form foam. Sodium diacetate is a highly effective antiseptic, mildew-proof safener. The new food additive is also approved by the Ministry of health of China in the middle of the 90 th year of the 20 th century to be used as a new food additive variety, and is one of 14 kinds of food, feed and grain mildewproof agents approved by the nation.
The existing method for synthesizing sodium diacetate mainly comprises the following steps: acetic acid and sodium acetate liquid phase method, acetic acid and sodium carbonate liquid phase method, acetic acid and sodium acetate gas phase reaction method and acetic acid and caustic soda liquid phase synthesis method. The acetic acid and sodium acetate liquid phase method uses acetic acid and sodium acetate as raw materials and ethanol or water as a solvent to synthesize sodium diacetate. The acetic acid and sodium carbonate liquid phase method takes acetic acid and sodium carbonate solution as raw materials, and the reaction is carried out under the condition of the existence of a solvent. The gas phase reaction method of acetic acid and sodium acetate is difficult to popularize due to high energy consumption and harsh reaction conditions. The acetic acid and caustic soda liquid phase synthesis method is characterized in that acetic acid and caustic soda are used as raw materials, liquid phase synthesis is carried out at a higher temperature, and the production cost is higher.
Disclosure of Invention
The invention aims to solve the technical problem that aiming at the defects of the prior production technology of sodium diacetate, the preparation method of food-grade sodium diacetate is realized by utilizing a self-developed multifunctional rake reactor, the production process is simpler, the equipment investment is less, the operation is easy, and the industrial and automatic operation is more facilitated.
In order to achieve the purpose, the invention is realized by the following scheme:
the invention provides a preparation method of food-grade sodium diacetate, which comprises the following operation steps:
s1, putting the sodium carbonate into the reactor at one time, adding glacial acetic acid 2.32 times of the weight of the sodium carbonate into the reactor, controlling the reaction temperature to be 80-90 ℃, and controlling the reaction time to be 2-2.5 hours; under stirring, glacial acetic acid and sodium carbonate are fully chemically reacted to synthesize sodium diacetate;
s2, then curing for 1-1.5 hours at 80-90 ℃, and drying at 100-105 ℃;
s3, cooling, and cooling the material to 40-45 ℃ to obtain the finished product of sodium diacetate.
Further, the drying time is 2 to 2.5 hours.
Further, the reactor is a multifunctional rake reactor comprising: the device body is fixedly arranged above the supporting frame, the driving device is fixedly arranged on the supporting frame on the left side of the device body, an air suction port, a feeding port and a manhole are arranged at the top of the device body, a discharge port is arranged in the middle of the bottom of the device body and is connected with a discharge valve, the raking device is arranged inside the device body, two ends of the raking device penetrate through the device body, the raking device and the device body are sealed through a shaft sealing device, two ends of the raking device are rotatably connected with a bearing seat through a rotor bearing, the bearing seat at the left end of the raking device is fixedly arranged on a base, the bearing seat at the right end of the raking device is fixed on the outer wall of the device body and is rotatably connected with the device body through the rotor bearing, the left end of the raking device is connected with the driving device, the right end of the raking device is connected with the rotary joint, the upper half part of the device body is rectangular, the lower half part of the device body is semicircular, and the outer wall of the lower half part of the device body is fixedly provided with a heat exchange device.
Further, the raking device comprises a hollow shaft, a raking device and a cold and hot medium guide pipe, the right end of the hollow shaft is connected with a rotary joint, the cold and hot medium guide pipe is installed inside the hollow shaft and comprises a straight pipe and a plurality of guide pipes, one end of the straight pipe is closed, the other end of the straight pipe is open, the open end of the straight pipe is connected with the rotary joint, the guide pipes are in one-to-one correspondence with rake rods, the raking device comprises rake rods and rake teeth, each rake rod is a hollow pipe, one end of each rake rod is connected with the hollow shaft, the other end of each rake rod is connected with the rake teeth, and the rake teeth are divided into straight teeth and oblique teeth.
Furthermore, the transmission device consists of a motor, a belt pulley, a transmission belt, a speed reducer and a coupling, wherein an output shaft of the motor is connected with the speed reducer through the belt pulley and the belt, the speed reducer is connected with the right side coupling, and the coupling is connected with the left end of the raking device.
Furthermore, a cold and heat medium inlet and a cold and heat medium outlet are arranged on the rotary joint, the cold and heat medium inlet is connected with a cold and heat medium pipe water inlet end in the hollow shaft, and the cold and heat medium outlet is connected with a cold and heat medium pipe water outlet end in the hollow shaft.
Furthermore, the feeding device consists of a transverse pipe and a vertical pipe, the lower part of the transverse pipe is provided with a plurality of small holes, one end of the vertical pipe is provided with a flange and is connected with the glacial acetic acid high-level metering tank, the other end of the vertical pipe is connected with the transverse pipe, the vertical pipe is welded with the device body, and the transverse pipe is arranged inside the device body.
Furthermore, the heat exchange device is a cold and hot medium guide pipe which is coiled at the lower part of the welding device body, the upper part of the guide pipe is provided with a heat medium inlet and a cold medium outlet, and the lower part of the guide pipe is provided with a heat medium outlet and a cold medium inlet.
Furthermore, the extraction opening is externally connected with an alkali absorption tower.
The invention has the beneficial effects that:
the invention takes the sodium carbonate and the glacial acetic acid as raw materials, does not need solvent, and the reaction, the curing, the drying and the cooling in the production process of the sodium diacetate are completed in one reactor.
The invention adopts a self-developed multifunctional rake reactor, which comprises a reactor body, a transmission device, a raking device (with the double functions of heat exchange and raking), a feeding device, a heat exchange device, a rotary joint, a supporting device, a shaft seal device and other parts, has multiple functions of stirring, heating and cooling, and can completely meet the requirement of a preparation method of food-grade sodium diacetate; the gas discharged in the reaction process is absorbed by the alkali absorption tower, and the absorption liquid is reused for producing sodium acetate, so that the atmospheric pollution can be effectively prevented, and the utilization rate of the raw materials is improved.
Drawings
FIG. 1 is a schematic structural view of a multifunctional rake reactor according to the present invention;
FIG. 2 is a schematic diagram of the side view of the multifunctional rake reactor of the present invention.
In the figure:
1-support frame, 2-transmission device, 3-shaft seal device, 4-raking device, 5-feeding device, 6-device body, 7-rotary joint and 8-heat exchange device.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood 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
The reactor is a multifunctional rake reactor, as shown in fig. 1-2, and comprises: the device comprises a support frame 1, a transmission device 2, a shaft seal device 3, a raking device 4, a feeding device 5, a device body 6, a rotary joint 7 and a heat exchange device 8, wherein the device body 6 is fixedly arranged above the support frame 1, the transmission device 2 is fixedly arranged on the support frame 1 on the left side of the device body 6, an air exhaust port, a feeding port and a manhole are arranged at the top of the device body 6, a discharge port is arranged in the middle of the bottom of the device body 6 and is connected with a discharge valve, the raking device 4 is arranged in the device body 6, two ends of the raking device 4 penetrate through the device body 6, the raking device 4 and the device body 6 are sealed through a shaft sealing device 3, two ends of the raking device 4 are rotatably connected with bearing seats through rotor bearings, the bearing seat at the left end of the raking device 4 is fixedly arranged on a base 1, the bearing seat at the right end of the raking device 4 is fixed on the outer wall of the device body 6 and is rotatably connected with the device body 6 through the rotor bearings, the left end of the raking device 4 is connected with the transmission device 2, the right end of the raking device 4 is connected with a rotary joint 7, the upper half part of the device body 6 is rectangular, the lower half part of the device body 6 is semicircular, and a heat exchange device 8 is fixedly arranged on the outer wall of the lower half part of the device body 6.
The raking device 4 comprises a hollow shaft, a raking device and a cold and hot medium guide pipe, the right end of the hollow shaft is connected with a rotary joint 7, the cold and hot medium guide pipe is installed inside the hollow shaft and comprises a straight pipe and a plurality of guide pipes, one end of the straight pipe is closed, the other end of the straight pipe is open, the open end of the straight pipe is connected with the rotary joint 7, the guide pipes correspond to rake rods one to one, the raking device comprises rake rods and rake teeth, the rake rods are hollow pipes, one end of each rake rod is connected with the hollow shaft, the other end of each rake rod is connected with the rake teeth, and the rake teeth are divided into straight teeth and oblique teeth.
The transmission device 2 consists of a motor, a belt pulley, a transmission belt, a speed reducer and a coupler, wherein an output shaft of the motor is connected with the speed reducer through the belt pulley and the belt, the speed reducer is connected with the right coupler, and the coupler is connected with the left end of the raking device 4.
The rotary joint 7 is provided with a cold and heat medium inlet and a cold and heat medium outlet, the cold and heat medium inlet is connected with the cold and heat medium pipe water inlet end in the hollow shaft, and the cold and heat medium outlet is connected with the cold and heat medium pipe water outlet end in the hollow shaft.
The feeding device 5 consists of a transverse pipe and a vertical pipe, the lower part of the transverse pipe is provided with a plurality of small holes, one end of the vertical pipe is provided with a flange and is connected with the glacial acetic acid high-level metering tank, the other end of the vertical pipe is connected with the transverse pipe, the vertical pipe is welded with the device body, and the transverse pipe is arranged inside the device body 6.
The heat exchange device 8 is a cold and hot medium guide pipe which is coiled at the lower part of the welding device body 6, the upper part of the guide pipe is provided with a hot medium inlet and a cold medium outlet, and the lower part of the guide pipe is provided with a hot medium outlet and a cold medium inlet.
The extraction opening is externally connected with an alkali absorption tower.
The working principle is as follows:
the raw material sodium carbonate is added into the rake reactor through a feeding port, and the raw material glacial acetic acid is uniformly distributed in the reactor body 6 through a feeding device 5. The two materials are fully chemically reacted under the stirring of the raking device 4 to synthesize sodium diacetate; controlling the reaction temperature within a specified range by controlling the adding speed of the glacial acetic acid; after the reaction is finished, introducing reduced-temperature and reduced-pressure steam into the raking device 4 and the heat exchange device 5, curing and drying, after the drying is finished, introducing cooling water into the raking device 4 and the heat exchange device 8, and cooling the product to a specified temperature to obtain sodium diacetate; gas generated by the reaction is discharged from the gas extraction opening and is discharged after passing through the alkali absorption tower.
Example 2
In the present embodiment, the raw materials of soda ash and glacial acetic acid are both food grade, and the reactor in the present embodiment is the multifunctional rake reactor in example 1.
A preparation method of food-grade sodium diacetate comprises the following specific steps:
s1, adding 500kg of soda ash into a rake reactor, starting a rake device of the multifunctional rake reactor, slowly adding 1160kg of glacial acetic acid into the reactor, uniformly distributing the glacial acetic acid in the reactor by a feeding device, controlling the reaction temperature at 80 ℃, controlling the reaction time at 2 hours, and fully performing chemical reaction on the glacial acetic acid and sodium carbonate under the stirring of the rake device to synthesize sodium diacetate;
s2, introducing 110 ℃ temperature-reducing and pressure-reducing steam into the heat exchange device and the raking device of the multifunctional rake reactor, curing at 90 ℃ for 1 hour, and drying at 105 ℃ for 2 hours;
s3, closing the steam, introducing cooling water into the heat exchange device, and cooling the material to 40 ℃ to obtain the finished product sodium diacetate.
The results of the actual measurement of the food additive sodium diacetate (GB25538-2010) according to the national food safety standard are shown in the following table 1:
TABLE 1 sodium diacetate detection results I
Example 3
In this example, the raw materials of soda ash and glacial acetic acid are both food grade, and the rake reactor in this example is the multifunctional rake reactor in example 1.
A preparation method of food-grade sodium diacetate comprises the following specific steps:
s1, adding 800kg of soda ash into a rake reactor, starting a rake device 4 of the multifunctional rake reactor, slowly adding 1856kg of glacial acetic acid into the reactor, controlling the reaction temperature at 85 ℃ and the reaction time at 2.2 hours, and fully performing chemical reaction on the glacial acetic acid and sodium carbonate under the stirring of the rake device to synthesize sodium diacetate;
s2, introducing reduced-temperature and reduced-pressure steam at 112 ℃ into a heat exchange device and a raking device of the multifunctional rake reactor, curing at 85 ℃ for 1.2 hours, and drying at 102 ℃ for 2 hours;
s3, closing the steam, introducing cooling water into the heat exchange device, and cooling the material to 42 ℃ to obtain the finished product sodium diacetate.
The results of the actual measurement of the food additive sodium diacetate (GB25538-2010) according to the national food safety standard are shown in the following table 2:
TABLE 2 sodium diacetate detection results II
Example 4
In this example, the raw materials of soda ash and glacial acetic acid are both food grade, and the rake reactor in this example is the multifunctional rake reactor in example 1.
A preparation method of food-grade sodium diacetate comprises the following specific steps:
s1, adding 1000kg of soda ash into the rake reactor, and starting a rake device 4 of the multifunctional rake reactor; 2320kg of glacial acetic acid was slowly added to the reactor. The reaction temperature was controlled at 90 ℃ and the reaction time was controlled at 2.5 hours. Under the stirring of the raking device, glacial acetic acid and sodium carbonate fully carry out chemical reaction to synthesize sodium diacetate;
s2, introducing reduced-temperature and reduced-pressure steam at 115 ℃ into a heat exchange device and a raking device of the multifunctional rake reactor, curing at 90 ℃ for 1 hour, and drying at 105 ℃ for 2.5 hours;
s3, closing the steam, introducing cooling water into the heat exchange device, and cooling the material to 45 ℃ to obtain the finished product sodium diacetate.
The results of the actual measurement of the food additive sodium diacetate (GB25538-2010) according to the national food safety standard are shown in the following table 3:
TABLE 3 sodium diacetate detection results III
As can be seen from tables 2-4, the sodium diacetate prepared by the invention meets the national food safety standard, and the preparation method of the food-grade sodium diacetate is realized by utilizing the self-developed multifunctional rake reactor, so that the preparation method has the advantages of less equipment, simple process, no solvent, low production cost and convenient realization of industrialization and automation.
In the description herein, references to the description of "one embodiment," "an example," "a specific example," etc., 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 preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise forms disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (3)
1. A preparation method of food-grade sodium diacetate is characterized by comprising the following operation steps:
s1, putting the sodium carbonate into the reactor at one time, adding glacial acetic acid 2.32 times of the weight of the sodium carbonate into the reactor, controlling the reaction temperature to be 80-90 ℃, and controlling the reaction time to be 2-2.5 hours; under stirring, glacial acetic acid and sodium carbonate are fully chemically reacted to synthesize sodium diacetate;
the reactor is a multifunctional rake reactor comprising: the device comprises a support frame (1), a transmission device (2), a shaft seal device (3), a raking device (4), a feeding device (5), a device body (6), a rotary joint (7) and a heat exchange device (8), wherein the device body (6) is fixedly arranged above the support frame (1), the transmission device (2) is fixedly arranged on the support frame (1) on the left side of the device body (6), the top of the device body (6) is provided with an air suction port, a feeding port and a manhole, the middle of the bottom of the device body (6) is provided with a discharging port, the discharging port is connected with a discharging valve, the raking device (4) is arranged inside the device body (6), two ends of the raking device (4) penetrate through the device body (6), the raking device (4) and the device body (6) are sealed through the shaft seal device (3), two ends of the raking device (4) are rotatably connected with a bearing seat through a rotor bearing, the bearing seat at the left end of the raking device (4) is fixedly arranged on a base (1), a bearing seat at the right end of the raking device (4) is fixed on the outer wall of the device body (6) and is rotationally connected with the device body (6) through a rotor bearing, the left end of the raking device (4) is connected with the transmission device (2), the right end of the raking device (4) is connected with a rotary joint (7), the upper half part of the device body (6) is rectangular, the lower half part of the device body (6) is semicircular, and a heat exchange device (8) is fixedly installed on the outer wall of the lower half part of the device body (6);
the raking device (4) consists of a hollow shaft, a raking device and a cold and hot medium guide pipe, the right end of the hollow shaft is connected with a rotary joint (7), the cold and hot medium guide pipe is installed inside the hollow shaft and consists of a straight pipe and a plurality of guide pipes, one end of the straight pipe is closed, the other end of the straight pipe is open, the open end of the straight pipe is connected with the rotary joint (7), the guide pipes are in one-to-one correspondence with rake rods, the raking device consists of rake rods and rake teeth, each rake rod is a hollow pipe, one end of each rake rod is connected with the hollow shaft, the other end of each rake rod is connected with the rake teeth, and the rake teeth are divided into straight teeth and oblique teeth;
the transmission device (2) consists of a motor, a belt pulley, a transmission belt, a speed reducer and a coupling, wherein an output shaft of the motor is connected with the speed reducer through the belt pulley and the belt, the speed reducer is connected with the right side coupling, and the coupling is connected with the left end of the raking device (4);
the feeding device (5) consists of a transverse pipe and a vertical pipe, the lower part of the transverse pipe is provided with a plurality of small holes, one end of the vertical pipe is provided with a flange and is connected with the glacial acetic acid high-level metering tank, the other end of the vertical pipe is connected with the transverse pipe, the vertical pipe is welded with the device body, and the transverse pipe is arranged inside the device body (6);
the heat exchange device (8) is a cold and hot medium guide pipe which is coiled at the lower part of the welding device body (6), the upper part of the guide pipe is provided with a heat medium inlet and a refrigerant outlet, and the lower part of the guide pipe is provided with a heat medium outlet and a refrigerant inlet;
s2, then curing for 1-1.5 hours at 80-90 ℃, and drying at 100-105 ℃;
s3, cooling, and cooling the material to 40-45 ℃ to obtain the finished product of sodium diacetate.
2. A process for the preparation of a food grade sodium diacetate as claimed in claim 1 wherein the drying time is from 2 to 2.5 hours.
3. The method for preparing food grade sodium diacetate according to claim 1, wherein the extraction opening is externally connected with an alkali absorption tower.
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