CN115650259A - Preparation method and device of large-particle sodium bicarbonate - Google Patents
Preparation method and device of large-particle sodium bicarbonate Download PDFInfo
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- CN115650259A CN115650259A CN202211334387.5A CN202211334387A CN115650259A CN 115650259 A CN115650259 A CN 115650259A CN 202211334387 A CN202211334387 A CN 202211334387A CN 115650259 A CN115650259 A CN 115650259A
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- sodium bicarbonate
- crystallizer
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- carbon dioxide
- carbonization reactor
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- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 title claims abstract description 135
- 239000002245 particle Substances 0.000 title claims abstract description 73
- 235000017557 sodium bicarbonate Nutrition 0.000 title claims abstract description 67
- 229910000030 sodium bicarbonate Inorganic materials 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 48
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 43
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 24
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 24
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 230000014759 maintenance of location Effects 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000013078 crystal Substances 0.000 claims description 43
- 238000003763 carbonization Methods 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 25
- 230000008030 elimination Effects 0.000 claims description 19
- 238000003379 elimination reaction Methods 0.000 claims description 19
- 238000003860 storage Methods 0.000 claims description 18
- 239000006200 vaporizer Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 8
- 238000001631 haemodialysis Methods 0.000 abstract description 7
- 230000000322 hemodialysis Effects 0.000 abstract description 7
- 239000000243 solution Substances 0.000 description 21
- 235000017550 sodium carbonate Nutrition 0.000 description 15
- 238000009826 distribution Methods 0.000 description 8
- 238000000502 dialysis Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 206010014418 Electrolyte imbalance Diseases 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- -1 baking soda Chemical compound 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention belongs to the technical field of sodium bicarbonate preparation, and particularly relates to a preparation method and device of large-particle sodium bicarbonate. The preparation method of the large-particle sodium bicarbonate comprises the following steps: sodium carbonate and carbon dioxide are used as raw materials, sodium carbonate raw material liquid with a certain concentration is prepared and reacts with food-grade carbon dioxide, a certain reaction temperature is maintained in a reactor, materials are transferred into a crystallizer after a certain retention time, the crystallizer is kept at a certain temperature and is transferred into a centrifugal machine after a certain retention time for washing and centrifuging, and then the large-particle sodium bicarbonate product is obtained after drying. The large-particle sodium bicarbonate product prepared by the invention is fusiform and approximately spherical, has good fluidity, the particle content of particles in the particle size range of 180-425 mu m is more than 80%, the product quality meets the standard of Chinese pharmacopoeia, and the requirement of large-particle sodium bicarbonate for hemodialysis can be met.
Description
Technical Field
The invention belongs to the technical field of sodium bicarbonate preparation, and particularly relates to a preparation method and device of large-particle sodium bicarbonate.
Background
Sodium bicarbonate, namely baking soda, is an important inorganic chemical product, is widely applied to various industries and plays an important role in national economy. For the production of the traditional sodium bicarbonate, a considerable industrial scale is formed in China, but in recent years, the consumption structure of sodium bicarbonate products in China gradually changes, the demand for high-end sodium bicarbonate products rises rapidly, and the problem of shortage of high-end sodium bicarbonate products in China is highlighted.
Sodium bicarbonate for dialysis and injection is one of important varieties in baking soda series products, and is mainly applied to hemodialysis scenes. The dialysate is used as an important component of a hemodialysis system, and has the main functions of correcting electrolyte disturbance in the internal environment of a patient and maintaining acid-base balance. The hemodialysis concentrated solution can be divided into acidic dialysis concentrated solution (solution A) and alkaline dialysis concentrated solution (solution B), wherein the solution A is sodium chloride, potassium chloride, calcium chloride, magnesium chloride and glacial acetic acid solution, and the solution B is sodium bicarbonate solution. In a specific use scene, the B liquid can be prepared in two ways, one is prepared for use on site, concentrated sodium bicarbonate dry powder is dissolved for use, and the other is prepared by filling granular sodium bicarbonate into a column or a bag and realizing continuous preparation of the B liquid on a dialysis machine. The sodium bicarbonate solution may be decomposed to a certain degree in the storage and transportation processes, the liquid is inconvenient to store and transport and the risk of biological hazard exists, and for the reasons, the continuous preparation of the solution B by adopting the granular sodium bicarbonate on the machine is more and more popular in the market. However, the method has high requirements on sodium bicarbonate particles, the powdery sodium bicarbonate particles are small, the powdery sodium bicarbonate particles are easy to agglomerate when dissolved, the flowability is poor, the sodium bicarbonate is not beneficial to quick dissolution, a conduit is extremely easy to block in a dialysis process, the particle size of the product produced by the domestic medical sodium bicarbonate manufacturer is small at present and cannot reach the on-machine standard, and the domestic large-particle sodium bicarbonate for hemodialysis is an imported product, so that the blank of large-particle sodium bicarbonate products for dialysis in the domestic market is filled.
CN206428008U utilizes recrystallization method to prepare raw material liquid with certain composition at 90 deg.C, and then crystallize at 30-40 deg.C, the particle size of large particle product is in the range of 180-425 μm, but there is no mention about product morphology and particle size distribution.
In patent CN206428007U, soda ash and food-grade carbon dioxide are used as raw materials, the raw materials are reacted in a crystallizer, the constant temperature in the reaction and crystallization processes is 25 ℃, fine crystals in a system are discharged every 40 minutes, the reaction time is 6 hours, and a product is taken out after reaction liquid is retained for 24 hours. The product proportion of the obtained product in the range of 180-425 mu m can reach 60%, but the large-particle sodium bicarbonate product for hemodialysis needs to have a regular shape and has certain requirements on particle accumulation performance, but the shape of the product is not given in the patent.
Patent CN105819471B discloses a method for producing baking soda with large particle size, which is based on soda ash carbonization, and adopts innovative design of reaction crystallizer of key equipment in the process, and combines the modes of fine crystal elimination and seed crystal addition to obtain a product with satisfactory particle size distribution, wherein the particle size is larger than 180 mu m and accounts for more than 75%, but the particle appearance is long rod-shaped, and the problems of small bulk density and poor operation effect can be caused when the method is different from similar spherical and fusiform particle products.
Disclosure of Invention
The technical problem solved by the invention is as follows: the product is in a fusiform shape, is approximately spherical, has good fluidity, has the particle size of 180-425 mu m accounting for more than 80 percent, meets the relevant standards of medicinal sodium bicarbonate in Chinese pharmacopoeia, and simultaneously meets the clinical requirements of the sodium bicarbonate for hemodialysis; the invention also provides a preparation method of the composition.
The preparation method of the large-particle sodium bicarbonate comprises the following steps:
preparing a sodium carbonate solution with a certain concentration, filtering, pumping into a carbonization reactor, introducing carbon dioxide, carrying out gas-liquid two-phase reaction at 70-90 ℃, transferring the material into a crystallizer after a certain retention time, cooling and crystallizing at 20-70 ℃, simultaneously adopting a fine grain elimination tank to extract and dissolve fine grains in the crystallizer, returning the fine grains to the crystallizer, transferring the material into a centrifuge after a certain retention time, washing, centrifuging, and drying to obtain a large-particle sodium bicarbonate product.
In the invention, the concentration of the sodium carbonate solution is 10-20wt%.
In the present invention, the carbon dioxide is preferably food grade carbon dioxide.
In the invention, the material retention time in the carbonization reactor is 0.2-3h.
In the carbonization process, certain crystals are separated out, and the part of crystals can be used as seed crystals in the crystallizer.
In the invention, the retention time of the materials in the crystallizer is 2-8h.
In the invention, the temperature in the fine grain elimination tank is 75-85 ℃.
In the crystallizer, when the crystal nucleates and grows, a fine crystal elimination mode is adopted, fine crystals smaller than 180 mu m are extracted, and the fine crystals are quickly dissolved in a fine crystal elimination tank at a high temperature and then return to the crystallizer for crystallization, so that the granularity of the crystal in the system is reformed and optimized.
In the invention, the prepared large-particle sodium bicarbonate crystal is in a fusiform or spheroid shape, the proportion of particles with the particle size of 180-425 mu m is more than 80%, the fluidity is good, and the large-particle sodium bicarbonate crystal has certain particle strength.
The device used in the preparation method of the large-particle sodium bicarbonate comprises a food-grade carbon dioxide storage tank, a sodium carbonate solution storage tank, a carbonization reactor, a crystallizer and a fine grain elimination tank, wherein a feed inlet of the carbonization reactor is connected with the food-grade carbon dioxide storage tank and the sodium carbonate solution storage tank, a discharge outlet of the carbonization reactor is connected with a feed inlet of the crystallizer, the top of the crystallizer is circularly connected with the fine grain elimination tank, and a discharge outlet at the bottom of the crystallizer is sequentially connected with a centrifugal machine and an air flow dryer.
The crystallizer and the fine grain elimination tank are provided with jackets and are controlled in temperature through public works.
And a carbon dioxide vaporizer is arranged between the food-grade carbon dioxide storage tank and the carbonization reactor.
Wherein the reaction temperature in the carbonization reactor is controlled by the feeding temperature, and the fine crystal elimination tank and the crystallizer are maintained in a constant temperature state by public works.
Compared with the prior art, the invention has the following beneficial effects:
(1) The granular sodium bicarbonate is prepared based on a soda carbonization method, basic particles with proper morphology and distribution are obtained through a carbonization reaction by adopting a basic idea of separating a carbonization process and a crystallization process, and the basic particles are further transferred to a crystallizer for growth, so that the granular sodium bicarbonate is prepared;
(2) The shape, the particle size distribution and the crystal strength of the large-particle sodium bicarbonate prepared by the invention meet the requirements of a granular sodium bicarbonate product for dialysis, no additive is required to be added in the process, and the product quality meets the basic requirements of the national pharmacopoeia on pharmaceutical-grade sodium bicarbonate;
(3) The method has simple process steps, is effective and reliable in preparing the large-particle sodium bicarbonate, has certain production efficiency, and can be used for further production in an enlarged scale.
Drawings
FIG. 1 is an SEM image of sodium bicarbonate crystals prepared in example 1 of the present invention;
FIG. 2 is an SEM photograph of sodium bicarbonate crystals prepared according to example 2 of the present invention;
FIG. 3 is a graph of the particle size distribution of sodium bicarbonate crystals prepared in example 1 of the present invention;
FIG. 4 is a graph of the particle size distribution of sodium bicarbonate crystals prepared in example 2 of the present invention;
FIG. 5 is an SEM image of commercially available sodium bicarbonate crystals;
FIG. 6 is a schematic structural diagram of a device for preparing large-particle sodium bicarbonate according to the present invention;
in the figure: 1. a food-grade carbon dioxide storage tank; 2. a sodium carbonate solution storage tank; 3. a carbonization reactor; 4. a crystallizer; 5. a fine grain elimination tank; 6, a centrifuge; 7. an air flow dryer; 8. a carbon dioxide vaporizer.
Detailed Description
The present invention will be further illustrated by the following examples, wherein the starting materials used in the examples are, unless otherwise specified, commercially available conventional starting materials; the processes used in the examples, unless otherwise specified, are conventional in the art.
Example 1
As shown in fig. 6, a preparation device of large-particle sodium bicarbonate comprises a food-grade carbon dioxide storage tank 1, a sodium carbonate solution storage tank 2, a carbonization reactor 3, a crystallizer 4 and a fine-grain elimination tank 5, wherein a feed inlet of the carbonization reactor 3 is connected with the food-grade carbon dioxide storage tank 1 and the sodium carbonate solution storage tank 2, a discharge outlet of the carbonization reactor 3 is connected with a feed inlet of the crystallizer 4, the top of the crystallizer 4 is circularly connected with the fine-grain elimination tank 5, and a discharge outlet at the bottom of the crystallizer 4 is sequentially connected with a centrifuge 6 and an airflow dryer 7.
The crystallizer 4 and the fine grain elimination tank 5 are both provided with jackets and are controlled by public works.
And a carbon dioxide vaporizer 8 is arranged between the food-grade carbon dioxide storage tank 1 and the carbonization reactor 3.
Wherein, the reaction temperature in the carbonization reactor 3 is controlled by the feeding temperature, and the fine crystal elimination tank 5 and the crystallizer 4 are maintained in a constant temperature state by public works.
Example 2
Large particles of sodium bicarbonate were prepared using the apparatus described in example 1, with the following steps:
sodium carbonate is used as raw material, sodium carbonate solution with the concentration of 12wt% is prepared and filtered, and the concentration is 0.6m 3 At a rate of 60.8 Nm/h, while food grade carbon dioxide is fed into the carbonization reactor 3 The reaction temperature in the carbonization reactor is kept at 70 ℃, the materials are transferred into a crystallizer after staying in the carbonization reactor for 1.5 hours, the temperature in the crystallizer is kept at 20 ℃ for crystallization, a fine crystal elimination tank is adopted to extract and dissolve crystallization crystals with the grain diameter of less than 180 mu m in the crystallizer (the dissolution temperature is 75 ℃) and then return to the crystallizer, the materials are transferred into a centrifuge after staying in the crystallizer for 4 hours, and then washing and centrifuging are carried out, and then drying are carried out to obtain a large-particle sodium bicarbonate product.
The microscopic morphology of the prepared large-particle sodium bicarbonate crystals is shown in figure 1, the particle size distribution of the crystals is shown in figure 3, and the prepared large-particle sodium bicarbonate crystals are in a fusiform or spheroid shape, and the proportion of particles with the particle size of 180-425 mu m is 87.9%.
Example 3
Large particles of sodium bicarbonate were prepared using the apparatus described in example 1, with the following steps:
sodium carbonate is used as raw material, sodium carbonate solution with the concentration of 15wt% is prepared and filtered, and the concentration is 0.6m 3 At a rate of 57.0 Nm/h, while food grade carbon dioxide is passed into the carbonation reactor 3 Introducing the mixture into a carbonization reactor at a speed of/h, keeping the reaction temperature in the carbonization reactor at 80 ℃, standing the material in the carbonization reactor for 0.2h, transferring the material into a crystallizer, keeping the temperature in the crystallizer at 50 ℃, crystallizing, simultaneously adopting a fine crystal elimination tank to extract and dissolve (the dissolution temperature is 60 ℃) crystals with the grain diameter of less than 180 mu m in the crystallizer, returning the crystals to the crystallizer, standing the material in the crystallizer for 2h, transferring the materials into a centrifuge, washing, centrifuging, and drying to obtain a large-particle sodium bicarbonate product.
The microscopic morphology of the prepared large-particle sodium bicarbonate crystals is shown in FIG. 2, the particle size distribution of the crystals is shown in FIG. 4, and the prepared large-particle sodium bicarbonate crystals are in the shape of spindle or spheroid, and the proportion of particles with the particle size of 180-425 μm is 88.1%.
Example 4
Large particles of sodium bicarbonate were prepared using the apparatus described in example 1, with the following steps:
sodium carbonate is used as raw material, sodium carbonate solution with the concentration of 20wt% is prepared and filtered, and the concentration is 0.6m 3 At a rate of 50.6 Nm/h, while food grade carbon dioxide is fed into the carbonization reactor 3 Introducing the mixture into a carbonization reactor at a speed of/h, keeping the reaction temperature in the carbonization reactor at 90 ℃, keeping the material in the carbonization reactor for 3 hours, transferring the material into a crystallizer, keeping the temperature in the crystallizer at 70 ℃, crystallizing, simultaneously adopting a fine crystal elimination tank to extract and dissolve (the dissolution temperature is 80 ℃) crystals with the grain diameter of less than 180 mu m in the crystallizer, returning the materials to the crystallizer, and putting the materials in the crystallizerAfter the mixture stays for 8 hours, the mixture is transferred into a centrifuge for washing and centrifugation, and then the product of large-particle sodium bicarbonate is obtained after drying.
The prepared large-particle sodium bicarbonate crystals are spindle-shaped or spheroid in shape, and the proportion of particles with the particle size of 180-425 mu m is 87.2%.
Comparative example 1
Sodium bicarbonate is commercially available.
The microscopic morphology of the sodium bicarbonate crystals on the market is shown in fig. 5, and it can be seen that the crystal morphology is irregular, the particle size uniformity is poor, and the fine particle content is high.
Claims (9)
1. The preparation method of the large-particle sodium bicarbonate is characterized by comprising the following steps:
preparing a sodium carbonate solution with a certain concentration, filtering, pumping into a carbonization reactor, introducing carbon dioxide, carrying out gas-liquid two-phase reaction at 70-90 ℃, transferring the material into a crystallizer after a certain retention time, cooling and crystallizing at 20-70 ℃, simultaneously extracting and dissolving fine crystals in the crystallizer by using a fine crystal elimination tank, returning the fine crystals back to the crystallizer, transferring the material into a centrifuge after a certain retention time, washing, centrifuging, and drying to obtain a large-particle sodium bicarbonate product.
2. The method of claim 1, wherein the method comprises the steps of: the concentration of the sodium carbonate solution is 10-20wt%.
3. The method of claim 1, wherein the method comprises the steps of: the material retention time in the carbonization reactor is 0.2-3h.
4. The method of claim 1, wherein the method comprises the steps of: the retention time of the materials in the crystallizer is 2-8h.
5. The method of claim 1, wherein the method comprises the steps of: the temperature in the fine crystal eliminating tank is 75-85 ℃.
6. The method of claim 1, wherein the method comprises the steps of: the prepared large-particle sodium bicarbonate crystal is in a fusiform or spheroidal shape, and the proportion of particles with the particle size of 180-425 mu m is more than 80%.
7. A device for preparing large-particle sodium bicarbonate according to any one of claims 1 to 6, wherein the device comprises: jar (5) are eliminated including food level carbon dioxide storage tank (1), sodium carbonate solution storage tank (2), carbonization reactor (3), crystallizer (4) and fine grain, food level carbon dioxide storage tank (1) and sodium carbonate solution storage tank (2) are connected to the feed inlet of carbonization reactor (3), the feed inlet of crystallizer (4) is connected to the discharge gate of carbonization reactor (3), the top and the fine grain of crystallizer (4) are eliminated jar (5) and are circulated continuously, and centrifuge (6) and air dryer (7) are connected in proper order to the bottom discharge gate of crystallizer (4).
8. The apparatus for preparing large particle sodium bicarbonate according to claim 7, wherein: the crystallizer (4) and the fine grain elimination tank (5) are both provided with jackets and are controlled in temperature by public works.
9. The apparatus for preparing large particle sodium bicarbonate according to claim 7, wherein: a carbon dioxide vaporizer (8) is arranged between the food-grade carbon dioxide storage tank (1) and the carbonization reactor (3).
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| CN208413873U (en) * | 2018-03-07 | 2019-01-22 | 武汉德泽环保科技有限公司 | A kind of device producing sodium bicarbonate |
| CN111994923A (en) * | 2020-08-28 | 2020-11-27 | 新兴凌云医药化工有限公司 | Production medicine level large granule sodium bicarbonate crystal system |
| CN113230688A (en) * | 2021-07-13 | 2021-08-10 | 天津乐科节能科技有限公司 | Large-particle nickel sulfate continuous crystallization system and method |
| CN114920270A (en) * | 2022-05-18 | 2022-08-19 | 天津大学 | Multistage continuous crystallization method of baking soda |
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