CN112047836A - Preparation method and equipment of calcium L-threonate - Google Patents
Preparation method and equipment of calcium L-threonate Download PDFInfo
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- CN112047836A CN112047836A CN202010974278.4A CN202010974278A CN112047836A CN 112047836 A CN112047836 A CN 112047836A CN 202010974278 A CN202010974278 A CN 202010974278A CN 112047836 A CN112047836 A CN 112047836A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/01—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/96—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor in which the filtering elements are moved between filtering operations; Particular measures for removing or replacing the filtering elements; Transport systems for filters
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/07—Optical isomers
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- Engineering & Computer Science (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing calcium L-threonate and a device thereof, which has the technical proposal that the method comprises a washing device, the washing device also comprises a box body, a fixing device arranged in the box body, and a filter screen arranged below the fixing device, the filter screen is provided with a support frame, the outer side of the box body is provided with a motor, the motor is connected with the fixing device through a rotating shaft, the top of the tank body is provided with a flushing mechanism which comprises a water distribution pipe, a plurality of nozzles arranged on the water distribution pipe and a water inlet pipe connected with the water distribution pipe, the inner wall of the box body is provided with a guide rail matched with the filter screen, one side of the box body is provided with a box door, the cabinet door is provided with a first handle, the washing device is provided with a recycling circulation system, the purity of the calcium L-threonate product is effectively improved, the resource utilization rate is increased, and the production and processing cost is reduced.
Description
Technical Field
The invention belongs to the technical field of processing of calcium L-threonate, and particularly relates to a preparation method and equipment of calcium L-threonate.
Background
The children need to be continuously supplemented with calcium for growth, and the old need to be supplemented with calcium and other nutrients for overcoming osteoporosis. The L-threonic acid calcium is easy to be absorbed by human body, is a good nutriment for supplementing calcium to human body and treating osteoporosis, is widely applied to food additives, medical raw materials, health products, beverage food and fine chemical raw materials, and has wide application field. The existing calcium L-threonate product has low purity and is easy to influence the use of the calcium L-threonate.
Disclosure of Invention
The invention aims to solve the technical problems, and provides a method for effectively improving the purity of calcium L-threonate, increasing the resource utilization rate and reducing the production and processing cost.
The purpose of the invention is realized as follows: a preparation method of calcium L-threonate comprises the following steps of (1) dissolving Vc in water, heating to 22-24 ℃, stirring for dissolving, adding calcium carbonate, cooling to 15 ℃ under stirring, and dropwise adding 30% hydrogen peroxide;
(2) after the dropping of hydrogen peroxide is finished, keeping the temperature at 55min, heating to 50-55 ℃ after the temperature is finished, adding activated carbon, heating to 75 ℃, and decomposing excessive H2O 2;
(3) then filtering, distilling the filtrate at 53-57 ℃ in vacuum to remove water, concentrating, adding into methanol, cooling to-1-3 ℃ for crystallization, and filtering to obtain a filter cake;
(4) washing the filter cake with methanol, carrying out microwave drying after washing to obtain the product of calcium L-threonate, then weighing and detecting.
The invention is further configured to: in the step (1), the molar ratio of Vc to calcium carbonate is 1: 2-3: 5.
the invention is further configured to: the time for crystallization in step (3) was 15 hours.
The invention is further configured to: and (4) the microwave drying temperature in the step (4) is 95-100 ℃, the content of Vc calcium is detected by adopting an HPLC method, and the purity of the calcium L-threonate is calculated.
The invention also provides equipment for preparing the calcium L-threonate, which comprises a washing device, wherein the washing device further comprises a box body, a fixing device arranged in the box body, and a filter screen arranged below the fixing device, the filter screen is provided with a support frame, the outer side of the box body is provided with a motor, the motor is connected with the fixing device through a rotating shaft, the top of the box body is provided with a washing mechanism, the washing mechanism comprises a water distribution pipe, a plurality of spray heads arranged on the water distribution pipe, and a water inlet pipe connected with the water distribution pipe, the inner wall of the box body is provided with a guide rail matched with the filter screen, one side of the box body is provided with a box door, the box door is provided with a first handle.
By adopting the technical scheme, the washing device also comprises a box body, a fixing device arranged in the box body, and a filter screen arranged below the fixing device, wherein the box body has sealing performance and prevents the leakage of the washing liquid, the washing liquid adopts methanol or ethanol, the filter cake is fixed by the fixing device and is convenient to wash, smaller crystals washed off the filter cake are separated from the washing liquid by the filter screen, the loss of the L-threonic acid calcium is reduced, the washing liquid has certain potential energy when dropping from the fixing device, the filter screen is provided with a support frame, the structural strength of the filter screen is increased by the support frame, the service life of the filter screen is prolonged, the outer side of the box body is provided with a motor, the motor is connected with the fixing device through a rotating shaft, the motor drives the fixing device to rotate, the front side and the back side of the filter cake on the fixing device are fully, the purity of the L-threonic acid calcium is improved, a washing mechanism is arranged at the top of the box body, the washing mechanism comprises a water distribution pipe, a plurality of spray heads arranged on the water distribution pipe and a water inlet pipe connected with the water distribution pipe, filter cakes are washed by the washing mechanism, the filter cakes are uniformly and quickly washed and supplied by uniformly installing the spray heads on the water distribution pipe, a detergent is conveniently guided into the water distribution pipe through the water inlet pipe, a guide rail matched with the filter screen is arranged on the inner wall of the box body, the filter screen is conveniently and fixedly installed through the guide rail, a box door is arranged on one side of the box body, a first handle is arranged on the box door, the filter cakes are conveniently fixed on a fixing device through the box door, fine crystals on the filter screen are conveniently recovered, the box door is conveniently opened through the first handle, the resource utilization rate is increased, and the production and processing cost is reduced.
The invention is further configured to: the bottom surface of box is conical surface structure, and recovery circulation system includes evaporation plant and condensing equipment, be equipped with first circulating pump between the bottom surface of box and the evaporation plant, be equipped with the second circulating pump between condensing equipment and the inlet tube.
Through adopting above-mentioned technical scheme, the bottom surface of box is the conical surface structure, the flow of the detergent of being convenient for through the conical surface, recovery circulation system includes evaporation plant and condensing equipment, through the methyl alcohol evaporation of evaporation plant in will mixing the liquid, then with the methyl alcohol condensation through condensing equipment, be convenient for recycle, be provided with first circulating pump between the bottom surface of box and the evaporation plant, be convenient for through first circulating pump with the detergent in the box leading-in to evaporation plant fast, be provided with the second circulating pump between condensation plant and the inlet tube, pass through the leading-in box of inlet tube with the condensing agent in the condensing equipment through the second circulating pump, and wash the filter cake.
The invention is further configured to: fixing device includes upper fixing frame, lower fixed frame, arranges the upper filter screen on the upper fixing frame in, arranges the lower filter screen on the lower fixed frame in, arranges the fastener between upper fixing frame and the lower fixed frame in, one side inner wall of lower fixed frame is equipped with the grip block, be equipped with a plurality of springs between grip block and the lower fixed frame.
Through adopting the above technical scheme, fixing device includes the upper fixed frame, the lower fixed frame, arrange the last filter screen on the upper fixed frame in, arrange the lower filter screen on the lower fixed frame in, arrange the fastener between upper fixed frame and the lower fixed frame in, through arranging the filter cake between upper filter screen and the lower filter screen, prevent that the filter cake from dropping on the filter screen after cracked when washing, cause the impact to make the filter screen damaged to the filter screen, the upper fixed frame passes through the fastener with the lower fixed frame and is connected, be convenient for inseparable fixed connection, the pivot is installed on the lower fixed frame, the detergent passes the filter screen and washes the filter cake, one side inner wall of lower fixed frame is provided with the grip block, be provided with a plurality of springs between grip block and the lower fixed frame, it is fixed with the filter.
The invention is further configured to: the meshes of the upper filter screen and the lower filter screen are the same in size, and the meshes of the filter screens are smaller than those of the lower filter screen.
By adopting the technical scheme, the meshes of the upper filter screen and the lower filter screen are the same in size, the meshes of the filter screens are smaller than those of the lower filter screen, some fine crystals pass through the meshes of the upper filter screen and the lower filter screen under the washing of the detergent, and are filtered by the filter screens, so that the loss of the product of the calcium L-threonate is reduced.
The invention is further configured to: the filter screen is provided with a second handle arranged on one side close to the box door.
Through adopting above-mentioned technical scheme, the filter screen is provided with arranges the second handle that is close to chamber door one side in, is convenient for follow the guide rail dismouting with the filter screen through the second handle, prevents that the crystalline substance on the filter screen from dropping.
The invention has the beneficial effects that:
1. and washing the filter cake obtained by filtering after crystallization by using methanol, so that impurities in the filter cake are dissolved in the detergent, the impurities in the calcium L-threonate product are reduced, and the purity of the calcium L-threonate product is improved.
2. The filter cake is fixed by the fixing device, the fixing device is rotated by the motor, the upper surface and the lower surface of the filter cake can be washed by the detergent, the filter cake is fully washed, fine crystals which are flushed from the filter cake are added by the filter screen to be filtered, and the loss of the calcium L-threonate product is reduced.
3. The methanol is evaporated and condensed by the recycling circulation system, so that the recycling use of the methanol is increased, the utilization rate of resources is increased, and the production and processing cost is reduced.
Drawings
FIG. 1 is a schematic structural diagram of a washing apparatus according to an embodiment of the present invention;
FIG. 2 is a front view of an embodiment of the washing apparatus of the present invention;
FIG. 3 is a schematic structural view of an embodiment of a fixing device according to the present invention;
FIG. 4 is a schematic structural diagram of a filter according to an embodiment of the present invention;
reference numeral in the figure, 1, a washing device; 11. a box body; 111. a box door; 112. a first handle; 12. a fixing device; 121. an upper fixing frame; 122. a lower fixed frame; 123. a filter screen is arranged; 124. a lower filter screen, 125, a clamping plate; 126. a spring; 127. a fastener; 13. a filter screen; 131. a support frame; 132. a second handle; 2. a motor; 21. a rotating shaft; 3. a guide rail; 4. a flushing mechanism; 41. a water inlet pipe; 42. a water distribution pipe; 43. a spray head; 5. a recycling circulation system; 51. an evaporation device; 52. a condensing unit; 53. a first circulation pump; 54. and a second circulation pump.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the following description clearly and completely describes the technical solution in the embodiment of the present invention with reference to fig. 1 to 4:
a preparation method of calcium L-threonate comprises the following steps of (1) dissolving Vc in water, heating to 22-24 ℃, stirring for dissolving, adding calcium carbonate, cooling to 15 ℃ under stirring, and dropwise adding 30% hydrogen peroxide;
(2) after the dropping of hydrogen peroxide is finished, keeping the temperature at 55min, heating to 50-55 ℃ after the temperature is finished, adding activated carbon, heating to 75 ℃, and decomposing excessive H2O 2;
(3) then filtering, distilling the filtrate at 53-57 ℃ in vacuum to remove water, concentrating, adding into methanol, cooling to-1-3 ℃ for crystallization, and filtering to obtain a filter cake;
(4) washing the filter cake with methanol, carrying out microwave drying after washing to obtain the product of calcium L-threonate, then weighing and detecting.
In the step (1), the molar ratio of Vc to calcium carbonate is 1: 2-3: 5.
the time for crystallization in step (3) was 15 hours.
And (4) the microwave drying temperature in the step (4) is 95-100 ℃, the content of Vc calcium is detected by adopting an HPLC method, and the purity of the calcium L-threonate is calculated.
The filter cake obtained by filtering after crystallization is washed by using a methanol or ethanol solution to dissolve the calcium vitamin C in the filter cake, so that the purity of the calcium L-threonate product is improved. And (3) detecting the final dried finished product by an HPLC method, detecting the content of calcium vitamin C in the calcium L-threonate, and calculating the purity of the calcium L-threonate, so that the later-stage calculation of the calcium L-threonate is facilitated, the usage amount is more accurate, and the effect is more stable.
An apparatus for preparing L-threonic acid calcium comprises a washing device 1, the washing device 1 further comprises a box body 11, a fixing device 12 arranged in the box body 11, a filter screen 13 arranged below the fixing device 12, the box body 11 has sealing performance and prevents washing liquid from leaking, the washing liquid adopts methanol or ethanol, a filter cake is fixed by the fixing device 12 and is convenient to wash, smaller crystals which are washed from the filter cake are separated from the washing liquid by the filter screen 13, the loss of the L-threonic acid calcium is reduced, the washing liquid has certain potential energy when dropping from the fixing device 12, the filter screen 13 is provided with a support frame 131, the structural strength of the filter screen 13 is increased by the support frame 131, the service life of the filter screen 13 is prolonged, a motor 2 is arranged on the outer side of the box body 11, the motor 2 is connected with the fixing device 12 through a rotating shaft 21, the fixing, the front and back sides of the filter cake on the fixing device 12 are fully washed by the detergent, the content of calcium vitamin C in the calcium L-threonate is reduced, the purity of the calcium L-threonate is improved, the top of the box body 11 is provided with the washing mechanism 4, the washing mechanism 4 comprises a water distribution pipe 42, a plurality of spray heads 43 arranged on the water distribution pipe 42 and a water inlet pipe 41 connected with the water distribution pipe 42, the filter cake is washed by the washing mechanism 4, the spray heads 43 are uniformly arranged on the water distribution pipe 42 to ensure that the filter cake washing supply is uniform and quicker, the detergent is conveniently guided into the water distribution pipe 42 through the water inlet pipe 41, the inner wall of the box body 11 is provided with a guide rail 3 matched with the filter screen 13, the filter screen 13 is conveniently and fixedly arranged through the guide rail 3, one side of the box body 11 is provided with a box door 111, the box door 111 is provided with a, the fine crystals on the filter screen 13 can be conveniently recovered, the box door 111 can be conveniently opened through the first handle 112, the washing device 1 is provided with the recovery circulation system 5, and the recovery circulation system 5 is mainly used for recycling the detergent, so that the resource utilization rate is increased, and the production and processing cost is reduced.
The bottom surface of box 11 is the conical surface structure, be convenient for the flow of detergent through the conical surface, recycling system 5 includes evaporation plant 51 and condensing equipment 52, evaporate the methyl alcohol in the mixed liquid through evaporation plant 51, then through condensing equipment 52 with the methyl alcohol condensation, be convenient for recycle, be provided with first circulating pump 53 between the bottom surface of box 11 and evaporation plant 51, be convenient for through first circulating pump 53 with the detergent in the box 11 leading-in to evaporation plant 51 fast, be provided with second circulating pump 54 between condensing equipment 52 and the inlet tube 41, through second circulating pump 54 with the condensing agent in the condensing equipment 52 through the leading-in box 11 of inlet tube 41, and wash the filter cake.
The fixing device 12 includes an upper fixing frame 121, a lower fixing frame 122, an upper screen 123 disposed on the upper fixing frame 121, a lower screen 124 disposed on the lower fixing frame 122, a fastener 127 disposed between the upper fixing frame 121 and the lower fixing frame 122, by placing the filter cake between the upper screen 123 and the lower screen 124, the filter cake is prevented from falling onto the filter screen 13 after being broken during washing, the filter screen 13 is damaged by impact on the filter screen 13, the upper fixing frame 121 is connected with the lower fixing frame 122 through a fastening piece 127 so as to be tightly and fixedly connected, the rotating shaft 21 is installed on the lower fixing frame 122, a detergent passes through the filter screen 13 to wash filter cakes, a clamping plate 125 is arranged on the inner wall of one side of the lower fixing frame 122, a plurality of springs 126 are arranged between the clamping plate 125 and the lower fixing frame 122, the filter cake is fixed by the clamping plate 125 and the spring 126, so that the shaking of the filter cake when the fixing device 12 is turned over is reduced.
The mesh sizes of the upper filter screen 123 and the lower filter screen 124 are the same, the mesh size of the filter screen 13 is smaller than that of the lower filter screen 124, some fine crystals pass through the mesh sizes of the upper filter screen 123 and the lower filter screen 124 under the washing of detergent, and the crystals are filtered by the filter screen 13, so that the loss of the product of the calcium L-threonate is reduced.
The filter 13 is provided with a second handle 132 disposed at a side close to the door 111, and the filter 13 is easily detached from the guide rail 3 by the second handle 132, so as to prevent crystals on the filter 13 from falling.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and those skilled in the art should be able to make general changes and substitutions within the technical scope of the present invention.
Claims (9)
1. A preparation method of calcium L-threonate is characterized by comprising the following steps of (1) dissolving Vc in water, heating to 22-24 ℃, stirring to dissolve, adding calcium carbonate, cooling to 15 ℃ under stirring, and dropwise adding 30% hydrogen peroxide;
(2) keeping the temperature for 55min after the dropping of the hydrogen peroxide is finished, heating to 50-55 ℃, adding activated carbon, heating to 75 ℃ and decomposing excessive H2O 2;
(3) then filtering, distilling the filtrate at 53-57 ℃ in vacuum to remove water, concentrating, adding into methanol, cooling to-1-3 ℃ for crystallization, and filtering to obtain a filter cake;
(4) washing the filter cake with methanol, carrying out microwave drying after washing to obtain the product of calcium L-threonate, then weighing and detecting.
2. The method for preparing calcium L-threonate according to claim 1, wherein in step (1), the molar ratio of Vc to calcium carbonate is 1: 2-3: 5.
3. the process for the preparation of calcium L-threonate as claimed in claim 1, wherein the crystallization time in step (3) is 15 hours.
4. The method for preparing calcium L-threonate according to claim 1, wherein the temperature of microwave drying in step (4) is 95-100 ℃, and the purity of calcium L-threonate is calculated by detecting the content of Vc calcium by HPLC.
5. The equipment for preparing the calcium L-threonate comprises a washing device (1) and is characterized in that the washing device (1) further comprises a box body (11), a fixing device (12) arranged in the box body (11) and a filter screen (13) arranged below the fixing device (12), wherein a support frame (131) is arranged on the filter screen (13), a motor (2) is arranged on the outer side of the box body (11), the motor (2) is connected with the fixing device (12) through a rotating shaft (21), a washing mechanism (4) is installed at the top of the box body (11), the washing mechanism (4) comprises a water distribution pipe (42), a plurality of spray heads (43) arranged on the water distribution pipe (42) and a water inlet pipe (41) connected with the water distribution pipe (42), a guide rail (3) matched with the filter screen (13) is arranged on the inner wall of the box body (11), and a box door (111) is arranged on one side of the box, the box door (111) is provided with a first handle (112), and the washing device (1) is provided with a recycling circulation system (5).
6. The apparatus for preparing calcium L-threonate according to claim 5, characterized in that the bottom surface of the box (11) is a conical surface structure, the recycling system (5) comprises an evaporation device (51) and a condensation device (52), a first circulation pump (53) is arranged between the bottom surface of the box (11) and the evaporation device (51), and a second circulation pump (54) is arranged between the condensation device (52) and the water inlet pipe (41).
7. The apparatus for preparing calcium L-threonate according to claim 6, characterized in that said fixing device (12) comprises an upper fixing frame (121), a lower fixing frame (122), an upper filter screen (123) placed on the upper fixing frame (121), a lower filter screen (124) placed on the lower fixing frame (122), and a fastener (127) placed between the upper fixing frame (121) and the lower fixing frame (122), wherein a clamping plate (125) is provided on the inner wall of one side of the lower fixing frame (122), and a plurality of springs (126) are provided between the clamping plate (125) and the lower fixing frame (122).
8. The apparatus for preparing calcium L-threonate according to claim 7, characterized in that the upper screen (123) and the lower screen (124) have the same mesh size, and the mesh of the filter screen (13) is smaller than the mesh of the lower screen (124).
9. The apparatus for the preparation of calcium L-threonate according to claim 8, characterized in that said filter sieve (13) is provided with a second handle (132) placed on the side close to the chamber door (111).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010974278.4A CN112047836A (en) | 2020-09-16 | 2020-09-16 | Preparation method and equipment of calcium L-threonate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010974278.4A CN112047836A (en) | 2020-09-16 | 2020-09-16 | Preparation method and equipment of calcium L-threonate |
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| CN112047836A true CN112047836A (en) | 2020-12-08 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115436418A (en) * | 2021-06-01 | 2022-12-06 | 中国石油化工股份有限公司 | Shaft salt deposition simulation device and simulation method thereof |
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Application publication date: 20201208 |