CN115650259B - 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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- CN115650259B CN115650259B CN202211334387.5A CN202211334387A CN115650259B CN 115650259 B CN115650259 B CN 115650259B CN 202211334387 A CN202211334387 A CN 202211334387A CN 115650259 B CN115650259 B CN 115650259B
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- sodium bicarbonate
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- carbon dioxide
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- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 title claims abstract description 119
- 229910000030 sodium bicarbonate Inorganic materials 0.000 title claims abstract description 59
- 235000017557 sodium bicarbonate Nutrition 0.000 title claims abstract description 59
- 239000002245 particle Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 41
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 20
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 20
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000013078 crystal Substances 0.000 claims description 49
- 238000003763 carbonization Methods 0.000 claims description 31
- 230000014759 maintenance of location Effects 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 10
- 238000001631 haemodialysis Methods 0.000 abstract description 7
- 230000000322 hemodialysis Effects 0.000 abstract description 7
- 239000000243 solution Substances 0.000 description 27
- 238000003860 storage Methods 0.000 description 14
- 238000000034 method Methods 0.000 description 10
- 230000008030 elimination Effects 0.000 description 9
- 238000003379 elimination reaction Methods 0.000 description 9
- 238000002425 crystallisation Methods 0.000 description 8
- 230000008025 crystallization Effects 0.000 description 8
- 238000009826 distribution Methods 0.000 description 8
- 238000000502 dialysis Methods 0.000 description 7
- 235000013339 cereals Nutrition 0.000 description 6
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000012141 concentrate Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000006200 vaporizer Substances 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
- 235000013305 food Nutrition 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 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
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation 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
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 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
- 235000011868 grain product Nutrition 0.000 description 1
- 239000008187 granular material 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
- 238000011068 loading method Methods 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005457 optimization Methods 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
- 238000002407 reforming 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
Classifications
-
- 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 to prepare sodium carbonate raw material liquid with certain concentration, the sodium carbonate raw material liquid reacts with food-grade carbon dioxide, a certain reaction temperature is maintained in a reactor, the material is transferred into a crystallizer after a certain residence time, the material is kept at a certain temperature in the crystallizer, and the material is transferred into a centrifuge for washing and centrifuging after a certain residence time, and then a large-particle sodium bicarbonate product is obtained by drying. The large-particle sodium bicarbonate product prepared by the invention is fusiform and approximately spherical, has good fluidity, and the particle ratio of particles in the particle size range of 180-425 μm is more than 80%, so that the quality of the product meets the standard of Chinese pharmacopoeia, and can meet the requirement of large-particle sodium bicarbonate for hemodialysis.
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 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 faster, and the problem of production shortage of the high-end sodium bicarbonate products in China is increasingly outstanding.
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 the disturbance of the electrolyte in the environment of a patient and maintaining the acid-base balance. Hemodialysis concentrate can be divided into acidic dialysis concentrate (solution A) and alkaline dialysis concentrate (solution B), wherein solution A is sodium chloride, potassium chloride, calcium chloride, magnesium chloride, glacial acetic acid solution, and solution B is sodium bicarbonate solution. In a specific use scene, the solution B can be prepared in two ways, one is prepared at present, concentrated sodium bicarbonate dry powder is dissolved and then used, and the other is prepared by filling granular sodium bicarbonate into a column or a bag, so that the solution B is continuously prepared on a dialysis machine. The sodium bicarbonate solution may be decomposed to a certain extent during storage and transportation, liquid storage and transportation are inconvenient and risk of biological hazards exists, and for the above reasons, continuous preparation of the B solution by adopting granular sodium bicarbonate during on-line is increasingly favored by the market. However, the method has higher requirements on sodium bicarbonate particles, small powdery sodium bicarbonate particles, easy agglomeration during dissolution and poor fluidity, is not beneficial to the rapid dissolution of sodium bicarbonate, is extremely easy to block a conduit in the dialysis process, has smaller product granularity and can not meet the on-machine standard, and large-particle sodium bicarbonate for domestic hemodialysis is an imported product, so that the blank of the large-particle sodium bicarbonate product for domestic market dialysis is filled.
The patent CN206428008U utilizes a recrystallization method to prepare a raw material liquid with a certain composition at 90 ℃, and then performs crystallization at 30-40 ℃, wherein the granularity of a large-particle product is in the range of 180-425 mu m, but the morphology and granularity distribution of the product are not mentioned.
Patent CN206428007U takes sodium carbonate and food-grade carbon dioxide as raw materials, and takes out the product after the reaction liquid is retained for 24 hours by reacting in a crystallizer, wherein the constant temperature of the reaction and crystallization process is 25 ℃, fine crystals in the system are discharged every 40 minutes, and the reaction time is 6 hours. The ratio of the product accounting for 60% of the product in the range of 180-425 mu m is obtained, but the large-particle sodium bicarbonate product for hemodialysis needs to have a regular morphology, and certain requirements on particle stacking performance are met, but the morphology of the product is not shown in the patent.
Patent CN105819471B discloses a method for producing sodium bicarbonate with large granularity, which takes soda carbonization as a basis, innovatively designs a reaction crystallizer of key equipment in the process, and obtains a product with satisfactory granularity distribution by combining fine crystal elimination and seed crystal addition, wherein the grain diameter is more than 180 μm and accounts for more than 75%, but the grain morphology is in a long rod shape, which is different from a nearly spherical and fusiform grain product, and the problems of smaller bulk density and poorer loading effect can be generated.
Disclosure of Invention
The invention solves the technical problems that: the preparation method of the large-particle sodium bicarbonate is provided, the product is fusiform and approximately spherical, the fluidity is good, the particle size of 180-425 mu m accounts for more than 80%, the related standard of medicinal sodium bicarbonate in Chinese pharmacopoeia is met, and the clinical requirement of sodium bicarbonate for hemodialysis is met; the invention also provides a preparation method of the composite.
The preparation method of the large-particle sodium bicarbonate comprises the following steps:
preparing sodium carbonate solution with a certain concentration, filtering, pumping into a carbonization reactor, introducing carbon dioxide, performing gas-liquid two-phase reaction at 70-90 ℃, transferring the material into a crystallizer after a certain residence time, cooling and crystallizing at 20-70 ℃, simultaneously adopting a fine crystal elimination tank to extract and dissolve fine crystals in the crystallizer, returning the dissolved fine crystals to the crystallizer, transferring the material into a centrifuge after a certain residence 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 retention time of the materials in the carbonization reactor is 0.2-3h.
During carbonization, certain crystals are separated out, and the part of crystals can be used as seed crystals in a crystallizer.
In the invention, the retention time of the materials in the crystallizer is 2-8h.
In the invention, the temperature in the fine crystal eliminating tank is 75-85 ℃.
In the crystallizer, fine crystals smaller than 180 mu m are extracted by adopting a fine crystal elimination mode while crystals are nucleated and grown, and after being rapidly dissolved at a higher temperature in a fine crystal elimination tank, the crystals are returned to the crystallizer for crystallization, so that the granularity reforming optimization of crystals in a system is carried out.
In the invention, the prepared large-particle sodium bicarbonate crystal has the shape of a shuttle or spheroid, the particle with the granularity of 180-425 μm accounts for more than 80%, the fluidity is good, and the large-particle sodium bicarbonate crystal has certain particle strength.
The device comprises a food-grade carbon dioxide storage tank, a sodium carbonate solution storage tank, a carbonization reactor, a crystallizer and a fine crystal eliminating 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 crystal eliminating tank, and a discharge outlet at the bottom of the crystallizer is sequentially connected with a centrifuge and an airflow dryer.
The crystallizer and the fine crystal eliminating tank are both provided with jackets, and the temperature is controlled through public engineering.
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 eliminating tank and the crystallizer are maintained in a constant temperature state by public engineering.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention is based on the basic thought of separating the carbonization process from the crystallization process, and obtains basic particles with proper morphology and distribution through carbonization reaction, and the basic particles are further transferred into a crystallizer for growth, thereby preparing the granular sodium bicarbonate;
(2) The morphology, the particle size distribution and the crystal strength of the large-particle sodium bicarbonate prepared by the invention meet the requirements of a dialysis particle sodium bicarbonate product, no additive is needed to be added in the process, and the quality of the product meets the basic requirements of national formulary on pharmaceutical grade sodium bicarbonate;
(3) The process has simple steps, is effective and reliable in preparing the large-particle sodium bicarbonate, has certain production efficiency, and can be used for further amplified production.
Drawings
FIG. 1 is an SEM image of sodium bicarbonate crystals prepared in example 1 of the present invention;
FIG. 2 is an SEM image of sodium bicarbonate crystals prepared in example 2 of the present invention;
FIG. 3 is a graph showing the particle size distribution of sodium bicarbonate crystals prepared in example 1 of the present invention;
FIG. 4 is a graph showing 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 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 crystal eliminating tank; 6, a centrifugal machine; 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 raw materials used in the examples are commercially available conventional raw materials unless otherwise specified; the process used in the examples, unless otherwise specified, is conventional in the art.
Example 1
As shown in fig. 6, a preparation facilities of large granule sodium bicarbonate, including food-grade carbon dioxide storage tank 1, sodium carbonate solution storage tank 2, carbonization reactor 3, crystallizer 4 and fine grain elimination jar 5, food-grade carbon dioxide storage tank 1 and sodium carbonate solution storage tank 2 are connected to carbonization reactor 3's feed inlet, crystallizer 4's feed inlet is connected to carbonization reactor 3's discharge gate, crystallizer 4's top links to each other with fine grain elimination jar 5 circulation, and centrifuge 6 and pneumatic dryer 7 are connected gradually to crystallizer 4's bottom discharge gate.
The crystallizer 4 and the fine crystal eliminating tank 5 are both provided with jackets, and the temperature is controlled by public engineering.
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 eliminating tank 5 and the crystallizer 4 are maintained in a constant temperature state by public engineering.
Example 2
Large particle sodium bicarbonate was prepared using the apparatus described in example 1, as follows:
sodium carbonate is used as raw material to prepare sodium carbonate solution with concentration of 12wt percent, and the solution is filtered to obtain the sodium carbonate solution with concentration of 0.6m 3 At a rate of/h, into a carbonization reactor, while feeding food-grade carbon dioxide at 60.8Nm 3 Introducing the rate of/h into a carbonization reactor, keeping the reaction temperature in the carbonization reactor at 70 ℃, transferring the materials into a crystallizer after staying for 1.5h in the carbonization reactor, keeping the temperature in the crystallizer at 20 ℃, crystallizing, simultaneously adopting a fine crystal elimination tank to extract and dissolve crystallization with the grain diameter smaller than 180 mu m in the crystallizer (the dissolution temperature is 75 ℃) and returning the crystallization, transferring the materials into a centrifuge after staying for 4h in the crystallizer, washing and centrifuging, and drying to obtain the large-particle sodium bicarbonate product.
The microscopic morphology of the prepared large-particle sodium bicarbonate crystals is shown in figure 1, the crystal size distribution is shown in figure 3, and the prepared large-particle sodium bicarbonate crystals are shuttle-shaped or spheroid, and the proportion of particles with the particle size of 180-425 μm is 87.9%.
Example 3
Large particle sodium bicarbonate was prepared using the apparatus described in example 1, as follows:
sodium carbonate is used as raw material to prepare sodium carbonate solution with concentration of 15wt percent, and the solution is filtered to obtain the sodium carbonate solution with concentration of 0.6m 3 The rate of/h is introduced into the carbonization reactor, whileFood grade carbon dioxide at 57.0Nm 3 Introducing the solution into a carbonization reactor at the rate of/h, keeping the reaction temperature in the carbonization reactor at 80 ℃, transferring the material into a crystallizer after staying for 0.2h in the carbonization reactor, keeping the temperature in the crystallizer at 50 ℃, crystallizing, simultaneously adopting a fine crystal elimination tank to extract and dissolve crystals with the particle size smaller than 180 mu m in the crystallizer (the dissolution temperature is 60 ℃) and returning the crystals to the crystallizer, transferring the material into a centrifuge after staying for 2h in the crystallizer, washing and centrifuging, and drying to obtain the large-particle sodium bicarbonate product.
The microscopic morphology of the prepared large-particle sodium bicarbonate crystals is shown in fig. 2, the crystal size distribution is shown in fig. 4, and the prepared large-particle sodium bicarbonate crystals are in the shape of a fusiform or spheroid, and the proportion of particles with the particle size of 180-425 μm is 88.1%.
Example 4
Large particle sodium bicarbonate was prepared using the apparatus described in example 1, as follows:
sodium carbonate is used as raw material to prepare sodium carbonate solution with concentration of 20wt percent, and the solution is filtered to obtain the solution with concentration of 0.6m 3 At a rate of/h, into a carbonization reactor, while feeding food grade carbon dioxide at 50.6Nm 3 Introducing the rate of/h into a carbonization reactor, keeping the reaction temperature in the carbonization reactor at 90 ℃, transferring the materials into a crystallizer after staying for 3h in the carbonization reactor, keeping the temperature in the crystallizer at 70 ℃, crystallizing, simultaneously adopting a fine crystal elimination tank to extract and dissolve crystallization with the grain diameter smaller than 180 mu m in the crystallizer (the dissolution temperature is 80 ℃) and returning the crystallization, transferring the materials into a centrifuge after staying for 8h in the crystallizer, washing and centrifuging, and drying to obtain the large-particle sodium bicarbonate product.
The prepared large-particle sodium bicarbonate crystal has a fusiform or spheroid shape, and the particle size of 180-425 μm accounts for 87.2%.
Comparative example 1
Sodium bicarbonate is commercially available.
The microscopic morphology of the commercial sodium bicarbonate crystals is shown in fig. 5, and it can be seen that the crystal morphology is irregular, the uniformity of particle size is poor, and the content of fine particles is high.
Claims (1)
1. The preparation method of the large-particle sodium bicarbonate is characterized by comprising the following steps of:
preparing sodium carbonate solution with the concentration of 10-20wt% and 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 residence time, cooling and crystallizing at 20-70 ℃, simultaneously extracting and dissolving fine crystals in the crystallizer by using a fine crystal eliminating tank, returning the material to the crystallizer after a certain residence time, transferring the material into a centrifuge, washing, centrifuging and drying to obtain a large-particle sodium bicarbonate product;
the retention time of the materials in the carbonization reactor is 0.2-3h;
the retention time of the materials in the crystallizer is 2-8h;
the temperature in the fine crystal eliminating tank is 75-85 ℃;
the morphology of the prepared large-particle sodium bicarbonate crystals is shuttle-shaped or spheroid, and the particle ratio of particles with the granularity of 180-425 μm is more than 80%.
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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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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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