CN114538478A - Preparation method of sodium bicarbonate particles - Google Patents
Preparation method of sodium bicarbonate particles Download PDFInfo
- Publication number
- CN114538478A CN114538478A CN202210252870.2A CN202210252870A CN114538478A CN 114538478 A CN114538478 A CN 114538478A CN 202210252870 A CN202210252870 A CN 202210252870A CN 114538478 A CN114538478 A CN 114538478A
- Authority
- CN
- China
- Prior art keywords
- reaction
- sodium bicarbonate
- concentration
- sodium
- additive
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 title claims abstract description 92
- 239000002245 particle Substances 0.000 title claims abstract description 58
- 229910000030 sodium bicarbonate Inorganic materials 0.000 title claims abstract description 46
- 235000017557 sodium bicarbonate Nutrition 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 48
- 239000000654 additive Substances 0.000 claims abstract description 40
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 32
- 230000000996 additive effect Effects 0.000 claims abstract description 29
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 21
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 239000012528 membrane Substances 0.000 claims abstract description 15
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 13
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 13
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 12
- 238000001728 nano-filtration Methods 0.000 claims abstract description 9
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 6
- 238000011033 desalting Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 5
- 239000012266 salt solution Substances 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 229920001467 poly(styrenesulfonates) Polymers 0.000 claims description 4
- 229940006186 sodium polystyrene sulfonate Drugs 0.000 claims description 3
- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 claims description 2
- JSYPRLVDJYQMAI-ODZAUARKSA-N (z)-but-2-enedioic acid;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)\C=C/C(O)=O JSYPRLVDJYQMAI-ODZAUARKSA-N 0.000 claims description 2
- UXYAJXBVMZFRMS-UHFFFAOYSA-N 2-hydroxy-1,3,2$l^{5}-dioxaphosphepane 2-oxide Chemical compound OP1(=O)OCCCCO1 UXYAJXBVMZFRMS-UHFFFAOYSA-N 0.000 claims description 2
- 229920002126 Acrylic acid copolymer Polymers 0.000 claims description 2
- 229920002197 Sodium polyaspartate Polymers 0.000 claims description 2
- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 0.000 claims description 2
- YDONNITUKPKTIG-UHFFFAOYSA-N [Nitrilotris(methylene)]trisphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CP(O)(O)=O YDONNITUKPKTIG-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 229940090960 diethylenetriamine pentamethylene phosphonic acid Drugs 0.000 claims description 2
- DUYCTCQXNHFCSJ-UHFFFAOYSA-N dtpmp Chemical compound OP(=O)(O)CN(CP(O)(O)=O)CCN(CP(O)(=O)O)CCN(CP(O)(O)=O)CP(O)(O)=O DUYCTCQXNHFCSJ-UHFFFAOYSA-N 0.000 claims description 2
- BEGBSFPALGFMJI-UHFFFAOYSA-N ethene;sodium Chemical group [Na].C=C BEGBSFPALGFMJI-UHFFFAOYSA-N 0.000 claims description 2
- 229920000141 poly(maleic anhydride) Polymers 0.000 claims description 2
- 229920001529 polyepoxysuccinic acid Polymers 0.000 claims description 2
- 159000000000 sodium salts Chemical class 0.000 claims description 2
- PDAVHEOHZSVBQQ-UHFFFAOYSA-J tetrasodium;2,2-diphosphonatoethanol Chemical compound [Na+].[Na+].[Na+].[Na+].OCC(P([O-])([O-])=O)P([O-])([O-])=O PDAVHEOHZSVBQQ-UHFFFAOYSA-J 0.000 claims description 2
- GYBINGQBXROMRS-UHFFFAOYSA-J tetrasodium;2-(1,2-dicarboxylatoethylamino)butanedioate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CC(C([O-])=O)NC(C([O-])=O)CC([O-])=O GYBINGQBXROMRS-UHFFFAOYSA-J 0.000 claims description 2
- 238000005374 membrane filtration Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 35
- 238000001514 detection method Methods 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 description 19
- 238000003756 stirring Methods 0.000 description 19
- 238000009826 distribution Methods 0.000 description 10
- 238000009776 industrial production Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000006477 desulfuration reaction Methods 0.000 description 2
- 230000023556 desulfurization Effects 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000008235 industrial water Substances 0.000 description 2
- -1 light industry Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/38—Preparation in the form of granules, pieces or other shaped products
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/10—Preparation of bicarbonates from carbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
Abstract
The invention relates to a preparation method of sodium bicarbonate particles, which comprises the following steps: s1, adding one or more additives into a mixed solution of sodium carbonate and sodium bicarbonate; s2, raising the temperature of the mixed solution to 50-80 ℃, continuously introducing carbon dioxide gas with the flow rate of 10-40 mL/min for reaction, filtering after 6-10 h of reaction to obtain reaction liquid and reaction products, and drying the reaction products at 40 ℃ for 12 hours to obtain sodium bicarbonate particles; s3, desalting the reaction liquid obtained by filtering after the reaction in the step S2 by using a nanofiltration membrane or an ultrafiltration membrane, and analyzing the concentration of the additive in the solution after the reaction by using an ultraviolet-visible spectrophotometry; s4, adding additives and sodium carbonate into the residual filtered reaction liquid to reach the required concentration, and then repeating the step S2 to continue the reaction to prepare sodium bicarbonate particles; in the process of preparing the sodium bicarbonate particles, the concentration of the additive can be rapidly determined, and the detection method is simple, accurate, rapid and good in practicability.
Description
Technical Field
The invention belongs to the technical field of sodium bicarbonate preparation, and particularly relates to a preparation method of sodium bicarbonate particles.
Background
Sodium bicarbonate is an important green chemical, is also an industrial chemical, has low toxicity, and is widely applied to foods, medicines, pesticides, light industry, additives and detergents. Different application fields have different requirements on the particle size. For example, in the production of certain products, it is desirable that the sodium bicarbonate crystals have a larger size to reduce the energy consumption of the filtration separation and drying processes and to reduce the caking of the product. When sodium bicarbonate is used as the desulfurization catalyst, it is desirable to have a smaller crystal grain size to enhance the catalytic desulfurization effect.
In order to adjust the particle size of sodium bicarbonate, patent WO2014/207120 discloses a method for preparing large-particle alkali metal bicarbonate particles by adding an additive such as sodium polyacrylate, and the like, although the crystal size can be controlled, the amount of the added material cannot be controlled, and the method cannot be industrially carried out in a circulating column. Journal of Crystal Growth 270(2004)573-581 discloses a method for increasing the particle size of sodium bicarbonate by adding sodium polystyrene sulfonate with different molecular weights, and the optimal concentration range of the additive is narrow and is not suitable for industrialization. Journal of Crystal Growth 275(2005)1333-1339 report Ca2+Has certain effect on increasing the particle size of the sodium bicarbonate, but the effect is not obvious, and the factory solution already contains a small amount of Ca2+Impurities, the amount of which cannot be controlled. And the experimental results obtained by the method are from laboratory bench tests and are not reported industrially.
In the preparation process of sodium bicarbonate particles, certain additives are required to adjust the particle size of the sodium bicarbonate particles, but the concentration of the additives is difficult to detect in the industrial production process. Several methods for measuring the concentration of additives are disclosed in the prior art, for example, the method for measuring trace polyacrylic acid in industrial circulating water by using a turbidity method is reported by the Limb-swallow method (industrial water treatment, 2014,34 (4): 76-78), but the method can only be used in the field of industrial water, and the NaCl content in the water is less than 400ppm, so that the method cannot be used for detecting high-salt solution.
Disclosure of Invention
The invention aims to provide a preparation method of sodium bicarbonate particles on the basis of the prior art, which can monitor the concentration of an additive in real time in the industrial production process so as to obtain sodium bicarbonate particles with expected particle size, and the detection method of the concentration of the additive is simple, accurate, rapid and good in practicability, and can be widely used in the industrial production process.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for preparing sodium bicarbonate particles, comprising the steps of:
s1, adding one or more additives into a mixed solution of sodium carbonate and sodium bicarbonate to obtain a salt solution;
s2, raising the temperature of the salt solution to 50-80 ℃, continuously introducing carbon dioxide gas with the flow rate of 10-40 mL/min for reaction, filtering after 6-10 h of reaction to obtain reaction liquid and reaction products, and drying the reaction products for 12 hours at 40 ℃ to obtain sodium bicarbonate particles;
s3, filtering the reaction solution obtained after the reaction in the step S2, taking 1ml of water, diluting to 100ml, desalting by using a nanofiltration membrane or an ultrafiltration membrane, and analyzing the concentration of the additive in the reaction solution after the reaction by using an ultraviolet-visible spectrophotometry.
S4, adding additives and sodium carbonate into the residual filtered reaction liquid to reach the required concentration, and then repeating the step S2 to continue the reaction to prepare sodium bicarbonate particles.
Further, the concentration of the sodium carbonate in the mixed solution in the step S1 is less than or equal to 160g/Kg, and the concentration of the sodium bicarbonate in the mixed solution is less than or equal to 90 g/Kg.
In step S4, the concentration of sodium carbonate in the supplemented solution is less than or equal to 160 g/Kg.
Further, the additive in step S1 is one or more of hydrolyzed polymaleic anhydride (HPMA), polyepoxysuccinic acid, sodium polystyrene sulfonate (NaPSS), acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer, 2-phosphonobutane-1, 2, 4-tricarboxylic acid, hydroxyethylidene diphosphonic acid tetrasodium salt, maleic acid acrylic acid copolymer sodium salt, aminotrimethylene phosphonic acid, sodium polyaspartate, iminodisuccinic acid tetrasodium salt, hydroxyethylidene diphosphonic acid, sodium ethylene diamine tetra methylene phosphate, or diethylenetriamine pentamethylene phosphonic acid.
Preferably, the additive is HPMA, NaPSS.
Further, the concentration of the additive in the salt solution in the step S1 is 5 mg/L-100 mg/L.
In step S4, the concentration of the additive in the solution after being supplemented is 5 mg/L-100 mg/L.
Further, the method for detecting the concentration of the additive in the reaction solution in the step S3 includes the following steps:
(1) preparing additive solutions with different concentrations by using ultrapure water, measuring the absorbance of the additive solutions with different concentrations by using an ultraviolet-visible spectrophotometer, determining the optimal wavelength, and drawing a standard curve by taking the concentration of the additive as a horizontal coordinate and the absorbance as a vertical coordinate.
(2) The reaction liquid is filtered by a nanofiltration membrane or an ultrafiltration membrane according to different additives, the molecular weight cut-off of the filtration membrane is 150-20000Dal, the filtration pressure is 1-3MPa, and the filtration time is 1-6 hours. And then measuring the absorbance of the filtrate by using an ultraviolet-visible spectrophotometer, and calculating the concentration of the filtrate according to a standard curve.
Compared with the prior art, the invention has the following advantages and beneficial effects:
in the preparation process of the sodium bicarbonate, sodium bicarbonate particles with different particle sizes are obtained by controlling the concentration of the additive. Because the concentration of the additive in the salt solution to be measured is low, the additive is gradually lost in the industrial production process, and the concentration of the additive is difficult to monitor in real time, so that the sodium bicarbonate particles with expected particle size are obtained. Aiming at the problem that the concentration of an additive is too low to be monitored in real time in the prior art, the invention provides the preparation method of the sodium bicarbonate particles, which can monitor the concentration of the additive in real time in the industrial production process so as to obtain the sodium bicarbonate particles with expected particle size; the method can rapidly determine the concentration of the additive in the process of preparing the sodium bicarbonate particles, has simple, accurate and rapid detection method and good practicability, and can be widely applied to the industrial production process.
Drawings
FIG. 1 is a scanning electron micrograph (a) and a corresponding particle size distribution (b) of sodium bicarbonate particles obtained in example 1;
FIG. 2 is a scanning electron micrograph (a) and a corresponding particle size distribution (b) of sodium bicarbonate particles obtained in example 2;
FIG. 3 is a scanning electron micrograph (a) and a corresponding particle size distribution (b) of sodium bicarbonate particles obtained in example 3;
FIG. 4 is a scanning electron micrograph (a) and a corresponding particle size distribution (b) of sodium bicarbonate particles obtained in example 4;
fig. 5 is a scanning electron micrograph (a) and a corresponding particle size distribution (b) of the sodium bicarbonate particles obtained in comparative example 1.
Detailed Description
The technical solutions provided by the present invention will be described in detail below with reference to specific examples, and it should be understood that the following specific embodiments are only illustrative of the present invention and are not intended to limit the scope of the present invention.
Example 1
To 100g of water were added 15.9g of sodium carbonate and 9g of sodium bicarbonate to give salt solution I.
Adding HPMA into 200mL of salt solution I, uniformly stirring to ensure that the concentration of the HPMA in the salt solution I is 20ppm, then stirring the salt solution I containing the HPMA at a stirring speed of 500r/min, heating to 60 ℃ while stirring, continuously introducing carbon dioxide gas at a flow rate of 10mL/min for 8h, stopping introducing the carbon dioxide gas after the reaction is finished, filtering the obtained reaction solution while the reaction solution is hot, and collecting crystals. Taking out 1ml of the filtered reaction solution, adding water to dilute the reaction solution to 100ml, desalting the reaction solution by using a nanofiltration membrane (with the molecular weight cutoff of 150Dal), and measuring the concentration of the additive in the solution by using an ultraviolet-visible spectrophotometry. Then adding HPMA to 20ppm in the residual reaction liquid, adding sodium carbonate to 15.9g/100g of water, continuing to perform crystallization reaction, and continuing to collect crystals. The crystals were washed with absolute ethanol and dried at 40 ℃ for 12 hours to obtain sodium bicarbonate particles having an average particle diameter of 47um and a particle size distribution as shown in FIG. 1.
Example 2
To 100g of water were added 14.5g of sodium carbonate and 8.5g of sodium bicarbonate, after complete dissolution, as salt solution II.
HPMA was added to 200ml of the salt solution II, and after stirring to uniformity, the concentration of HPMA in the salt solution II was made 60ppm as a salt solution III. And then stirring the salt solution III at a stirring speed of 500r/min, heating to 60 ℃ while stirring, continuously introducing carbon dioxide gas with the flow rate of 40mL/min, introducing the carbon dioxide gas for 8h, stopping introducing the gas after the reaction is finished, filtering the obtained reaction solution while the reaction solution is hot, collecting crystals, taking out 1mL of the filtered reaction solution, adding water to dilute the reaction solution to 100mL, desalting by using a nanofiltration membrane (the molecular weight cut-off is 150Dal), and determining the concentration of the additive in the solution by using an ultraviolet-visible spectrophotometry. Then adding HPMA to 60ppm in the residual reaction liquid, adding sodium carbonate to 14.5g/100g of water, continuing to perform crystallization reaction and collecting crystals. The crystals were washed with absolute ethanol and dried at 40 ℃ for 12 hours to obtain sodium bicarbonate particles having an average particle diameter of 31um and a particle size distribution as shown in FIG. 2.
Example 3
To 100g of water were added 15.9g of sodium carbonate and 9g of sodium bicarbonate to give salt solution I.
Adding NaPSS into 200mL of salt solution I, uniformly stirring to ensure that the concentration of NaPSS in the salt solution I is 5ppm, then stirring the salt solution I containing NaPSS at a stirring speed of 500r/min, heating to 60 ℃ while stirring, continuously introducing carbon dioxide gas with the flow rate of 10mL/min into the salt solution I, introducing the carbon dioxide gas for 8 hours, stopping introducing the gas after the reaction is finished, filtering the obtained reaction solution while the reaction solution is hot, collecting crystals, taking 1mL of the filtered reaction solution out, adding water to dilute the reaction solution to 100mL, removing salt by using a nanofiltration membrane (the molecular weight cutoff is 20000Dal), and determining the concentration of an additive in the solution by using an ultraviolet-visible spectrophotometry. And then, adding NaPSS to 5ppm in the residual reaction solution, adding sodium carbonate to 15.9g/100g of water, continuing to perform crystallization reaction and collecting crystals. The collected crystals were washed with anhydrous ethanol and dried at 40 ℃ for 12 hours to obtain sodium bicarbonate particles having an average particle diameter of 38um and a particle size distribution as shown in FIG. 3.
Example 4
To 100g of water were added 15.9g of sodium carbonate and 9g of sodium bicarbonate to give salt solution I.
Adding NaPSS into 200mL of salt solution I, uniformly stirring to ensure that the concentration of NaPSS in the salt solution I is 100ppm, then stirring the salt solution I containing PSS at a stirring speed of 500r/min, heating to 60 ℃ while stirring, continuously introducing carbon dioxide gas with the flow rate of 10mL/min into the salt solution I, introducing the carbon dioxide gas for 8 hours, stopping introducing the gas after the reaction is finished, filtering the obtained reaction solution while the reaction solution is hot, collecting crystals, taking 1mL of the filtered reaction solution out, adding water to dilute the reaction solution to 100mL, removing salt by using a nanofiltration membrane (the molecular weight cutoff is 20000Dal), and determining the concentration of an additive in the solution by using an ultraviolet-visible spectrophotometry method. And then, adding NaPSS to 100ppm in the residual reaction solution, adding sodium carbonate to 15.9g/100g of water, continuing to perform crystallization reaction and collecting crystals. The collected crystals were washed with anhydrous ethanol and dried at 40 ℃ for 12 hours to obtain sodium bicarbonate particles having an average particle diameter of 42um and a particle size distribution as shown in FIG. 4.
Comparative example 1
Taking 200mL of the salt solution I prepared in the example 2, stirring at a stirring speed of 500r/min, heating to 60 ℃ while stirring, continuously introducing carbon dioxide gas at a flow rate of 10mL/min for 8h, stopping introducing the carbon dioxide gas after the reaction is finished, filtering the obtained reaction solution while the reaction solution is hot, collecting crystals, washing the collected crystals with absolute ethyl alcohol, and drying at 40 ℃ for 12h to obtain sodium bicarbonate particles with an average particle size of 19um and a particle size distribution shown in figure 5.
The technical means disclosed in the invention scheme are not limited to the technical means disclosed in the above embodiments, but also include the technical scheme formed by any combination of the above technical features. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and such improvements and modifications are also considered to be within the scope of the present invention.
Claims (5)
1. A method for preparing sodium bicarbonate particles is characterized by comprising the following steps:
s1, adding one or more additives into a mixed solution of sodium carbonate and sodium bicarbonate to obtain a salt solution;
s2, raising the temperature of the salt solution to 50-80 ℃, continuously introducing carbon dioxide gas with the flow rate of 10-40 mL/min for reaction, filtering after 6-10 h of reaction to obtain reaction liquid and reaction products, and drying the reaction products for 12 hours at 40 ℃ to obtain sodium bicarbonate particles;
s3, in the reaction liquid obtained by filtering after the reaction in the step S2, 1ml of water is taken and diluted to 100ml, a nanofiltration membrane or an ultrafiltration membrane is used for desalting, and then the concentration of the additive in the reaction liquid after the reaction is analyzed by an ultraviolet-visible spectrophotometry.
S4, adding additives and sodium carbonate into the residual filtered reaction liquid to reach the required concentration, and then repeating the step S2 to continue the reaction to prepare sodium bicarbonate particles.
2. The method of claim 1, wherein the concentration of sodium bicarbonate in the mixed solution of step S1 is less than or equal to 160g/Kg, and the concentration of sodium bicarbonate in the mixed solution is less than or equal to 90 g/Kg.
3. The method of claim 1, wherein the additive in steps S1 and S3 is one or more of hydrolyzed polymaleic anhydride, polyepoxysuccinic acid, sodium polystyrene sulfonate, acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer, 2-phosphonobutane-1, 2, 4-tricarboxylic acid, hydroxyethylidene diphosphonic acid tetrasodium salt, maleic acid acrylic acid copolymer sodium salt, aminotrimethylene phosphonic acid, sodium polyaspartate, iminodisuccinic acid tetrasodium salt, hydroxyethylidene diphosphonic acid, sodium ethylene diamine tetra methylene phosphate, or diethylenetriamine pentamethylene phosphonic acid.
4. The method of claim 1, wherein the concentration of the additive in the salt solution in step S1 is 5mg/L to 100 mg/L.
5. The method as claimed in claim 1, wherein the molecular weight cut-off of the nanofiltration membrane or ultrafiltration membrane in step S3 is 150-.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210252870.2A CN114538478A (en) | 2022-03-15 | 2022-03-15 | Preparation method of sodium bicarbonate particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210252870.2A CN114538478A (en) | 2022-03-15 | 2022-03-15 | Preparation method of sodium bicarbonate particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114538478A true CN114538478A (en) | 2022-05-27 |
Family
ID=81664286
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210252870.2A Pending CN114538478A (en) | 2022-03-15 | 2022-03-15 | Preparation method of sodium bicarbonate particles |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114538478A (en) |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1207238A (en) * | 1967-08-29 | 1970-09-30 | Kalk Chemische Fabrik Gmbh | Method of producing sodium bicarbonate |
| JPH05339005A (en) * | 1992-06-08 | 1993-12-21 | Tokuyama Soda Co Ltd | Production of sodium bicarbonate |
| CN102252985A (en) * | 2011-06-10 | 2011-11-23 | 同济大学 | Method for measuring polyepoxysuccinic acid content of circulating cooling water by pinacyanol chloride spectrophotometric method |
| US20140348738A1 (en) * | 2011-12-21 | 2014-11-27 | Solvay Sa | Process for preparing sodium bicarbonate particles |
| US20150037583A1 (en) * | 2011-12-23 | 2015-02-05 | Solvay Sa | Process for the joint production of sodium carbonate and sodium bicarbonate |
| CN107364878A (en) * | 2016-05-11 | 2017-11-21 | 江苏井神盐化股份有限公司 | A kind of high-purity soda ash of low calcium and its production method by the production of sodium sulfate type ore deposit halogen |
| US20180230018A1 (en) * | 2015-09-23 | 2018-08-16 | Solvay Sa | Production of crystalline sodium bicarbonate |
| CN109337941A (en) * | 2018-09-29 | 2019-02-15 | 宿州学院 | A kind of the Quality Control production method and its application of L-Aspartic acid |
| CN109675518A (en) * | 2018-11-12 | 2019-04-26 | 天津大学 | The nano zero valence iron nickel bimetal compound of montmorillonite load and preparation method thereof for removing heavy metals in industrial wastewater ion |
| CN110261335A (en) * | 2019-06-24 | 2019-09-20 | 陕西省石油化工研究设计院 | A method of measurement poly-epoxy succinic acid content |
| CN111634928A (en) * | 2020-05-14 | 2020-09-08 | 山东海天生物化工有限公司 | Method for preparing large-particle baking soda by secondary carbonization method and baking soda obtained by method |
| CN111943234A (en) * | 2020-08-13 | 2020-11-17 | 河北华晨药业有限公司 | Method for preparing medicinal sterile sodium bicarbonate granules with large particle size |
-
2022
- 2022-03-15 CN CN202210252870.2A patent/CN114538478A/en active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1207238A (en) * | 1967-08-29 | 1970-09-30 | Kalk Chemische Fabrik Gmbh | Method of producing sodium bicarbonate |
| JPH05339005A (en) * | 1992-06-08 | 1993-12-21 | Tokuyama Soda Co Ltd | Production of sodium bicarbonate |
| CN102252985A (en) * | 2011-06-10 | 2011-11-23 | 同济大学 | Method for measuring polyepoxysuccinic acid content of circulating cooling water by pinacyanol chloride spectrophotometric method |
| US20140348738A1 (en) * | 2011-12-21 | 2014-11-27 | Solvay Sa | Process for preparing sodium bicarbonate particles |
| US20150037583A1 (en) * | 2011-12-23 | 2015-02-05 | Solvay Sa | Process for the joint production of sodium carbonate and sodium bicarbonate |
| US20180230018A1 (en) * | 2015-09-23 | 2018-08-16 | Solvay Sa | Production of crystalline sodium bicarbonate |
| CN107364878A (en) * | 2016-05-11 | 2017-11-21 | 江苏井神盐化股份有限公司 | A kind of high-purity soda ash of low calcium and its production method by the production of sodium sulfate type ore deposit halogen |
| CN109337941A (en) * | 2018-09-29 | 2019-02-15 | 宿州学院 | A kind of the Quality Control production method and its application of L-Aspartic acid |
| CN109675518A (en) * | 2018-11-12 | 2019-04-26 | 天津大学 | The nano zero valence iron nickel bimetal compound of montmorillonite load and preparation method thereof for removing heavy metals in industrial wastewater ion |
| CN110261335A (en) * | 2019-06-24 | 2019-09-20 | 陕西省石油化工研究设计院 | A method of measurement poly-epoxy succinic acid content |
| CN111634928A (en) * | 2020-05-14 | 2020-09-08 | 山东海天生物化工有限公司 | Method for preparing large-particle baking soda by secondary carbonization method and baking soda obtained by method |
| CN111943234A (en) * | 2020-08-13 | 2020-11-17 | 河北华晨药业有限公司 | Method for preparing medicinal sterile sodium bicarbonate granules with large particle size |
Non-Patent Citations (5)
| Title |
|---|
| 中国建材检验认证集团股份有限公司，国家水泥质量监督检验中心: "水泥化学分析检验技术", 北京：中国建材工业出版社, pages: 125 - 128 * |
| 中矢圭一 , 佐藤邦夫 , 段胜莉: "碳酸氢钠的制造方法", 纯碱工业, no. 03 * |
| 刘婕, 尚红霞: "饲料添加剂――阿散酸的分光光度法测定", 粮食与饲料工业, no. 01 * |
| 徐海莹: "烷基苯磺酸盐与聚丙烯酰胺混合水溶液的测定", 西南石油学院学报, no. 04 * |
| 潘梅荣;任慧萍;杨君梅;: "紫外分光光度法测定反萃液、结晶母液、铼酸铵中铼含量", 中国金属通报, no. 05 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TWI537211B (en) | Method of purifying strong acids or strongly acidic media to remove di- and higher valent metal ions | |
| US11746023B2 (en) | Basic copper chloride particulate matter and preparation method therefor | |
| TWI630241B (en) | Modulation method of phycocyanin | |
| CN111634925A (en) | Method for separating mixed salt containing sodium chloride and sodium sulfate of organic matters after carbonization | |
| CN105399867A (en) | Preparation method for heparin sodium | |
| JPH04262786A (en) | Method for production of powdery citric acid and its salt | |
| CN114538478A (en) | Preparation method of sodium bicarbonate particles | |
| CN112694511B (en) | Preparation method and quality control method of polysaccharide-iron compound and capsule preparation | |
| CN106349057B (en) | A kind of sodium citrate mother liquor deferrization purification process technique | |
| CN103864604B (en) | A kind of sodium citrate mother liquor deferrization purification process technique | |
| CN111689605A (en) | Method for treating wastewater containing tungsten and vanadium in regeneration process of waste SCR catalyst | |
| CN111320202A (en) | Deep iron removal method for zinc sulfate solution and preparation method of zinc sulfate | |
| CN109761800A (en) | The method of continuous crystallisation removing oxalic acid in glyoxalic acid production process | |
| CN112110830B (en) | Material pretreatment method for preparing tea theanine | |
| JPH10137771A (en) | Method for removing water-soluble high molecular compound | |
| US9534078B2 (en) | Method for measuring the thermal stability of a succinic acid crystal intended for the production of polymers | |
| US7166645B2 (en) | Process for the alkaline saponification of crosslinked acrylonitrile bead polymers | |
| CN112239413A (en) | Purification and closed production method of glycine | |
| CN108676926B (en) | Production method of white granulated sugar | |
| CN102731294B (en) | Preparation method of sodium citrate | |
| CN103145188B (en) | A kind of purification process of manganese sulfate monohydrate | |
| CN105329871B (en) | A kind of production method of Instant calgon | |
| CN104497176A (en) | Preparation method of low-haze polyvinyl butyral resin | |
| Saiful et al. | Forward osmosis membrane to produce water energy drink from seawater | |
| CN109406507A (en) | The preparation and application of the stabilisation probe of silver ion in a kind of colorimetric detection seawater |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |