CN118062809A - Preparation method of sodium chlorite - Google Patents
Preparation method of sodium chlorite Download PDFInfo
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- CN118062809A CN118062809A CN202410479468.7A CN202410479468A CN118062809A CN 118062809 A CN118062809 A CN 118062809A CN 202410479468 A CN202410479468 A CN 202410479468A CN 118062809 A CN118062809 A CN 118062809A
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- sodium chlorite
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- sodium
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- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 title claims abstract description 87
- 229960002218 sodium chlorite Drugs 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title claims abstract description 69
- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 claims abstract description 86
- 239000000243 solution Substances 0.000 claims abstract description 74
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 65
- 238000010521 absorption reaction Methods 0.000 claims abstract description 52
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 51
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 48
- 239000007789 gas Substances 0.000 claims abstract description 48
- 239000004155 Chlorine dioxide Substances 0.000 claims abstract description 43
- 235000019398 chlorine dioxide Nutrition 0.000 claims abstract description 43
- 239000007864 aqueous solution Substances 0.000 claims abstract description 34
- 238000001035 drying Methods 0.000 claims abstract description 34
- 239000002250 absorbent Substances 0.000 claims abstract description 27
- 230000002745 absorbent Effects 0.000 claims abstract description 27
- 238000001914 filtration Methods 0.000 claims abstract description 22
- 239000000376 reactant Substances 0.000 claims abstract description 15
- 239000006228 supernatant Substances 0.000 claims abstract description 10
- 238000007599 discharging Methods 0.000 claims abstract description 7
- 238000011049 filling Methods 0.000 claims abstract description 3
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims description 50
- 238000003756 stirring Methods 0.000 claims description 44
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 42
- 239000000945 filler Substances 0.000 claims description 42
- 238000000034 method Methods 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 25
- 229910052799 carbon Inorganic materials 0.000 claims description 25
- 239000002202 Polyethylene glycol Substances 0.000 claims description 22
- 229920001223 polyethylene glycol Polymers 0.000 claims description 22
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 21
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 15
- 238000004090 dissolution Methods 0.000 claims description 15
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 12
- 125000000217 alkyl group Chemical group 0.000 claims description 12
- 229930182470 glycoside Natural products 0.000 claims description 12
- 150000002338 glycosides Chemical class 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000011780 sodium chloride Substances 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 9
- PFKFTWBEEFSNDU-UHFFFAOYSA-N carbonyldiimidazole Chemical compound C1=CN=CN1C(=O)N1C=CN=C1 PFKFTWBEEFSNDU-UHFFFAOYSA-N 0.000 claims description 8
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 7
- 230000021523 carboxylation Effects 0.000 claims description 7
- 238000006473 carboxylation reaction Methods 0.000 claims description 7
- 239000008103 glucose Substances 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 6
- -1 polypropylene Polymers 0.000 claims description 6
- 239000004743 Polypropylene Substances 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 229920001155 polypropylene Polymers 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 2
- QOSATHPSBFQAML-UHFFFAOYSA-N hydrogen peroxide;hydrate Chemical compound O.OO QOSATHPSBFQAML-UHFFFAOYSA-N 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims 2
- 230000001376 precipitating effect Effects 0.000 claims 2
- 239000000203 mixture Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000002244 precipitate Substances 0.000 description 32
- 238000006243 chemical reaction Methods 0.000 description 14
- 238000005406 washing Methods 0.000 description 14
- 235000011121 sodium hydroxide Nutrition 0.000 description 12
- 238000004064 recycling Methods 0.000 description 8
- 238000005119 centrifugation Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 description 5
- 229910000342 sodium bisulfate Inorganic materials 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 230000036632 reaction speed Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 2
- 230000020477 pH reduction Effects 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- XEMZLVDIUVCKGL-UHFFFAOYSA-N hydrogen peroxide;sulfuric acid Chemical compound OO.OS(O)(=O)=O XEMZLVDIUVCKGL-UHFFFAOYSA-N 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000003014 ion exchange membrane Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Treating Waste Gases (AREA)
Abstract
The invention discloses a preparation method of sodium chlorite, which belongs to the technical field of sodium chlorite preparation and comprises the following steps: dissolving, preparing chlorine dioxide, preparing sodium chlorite solution, concentrating, filtering and drying; introducing gas generated in the preparation of chlorine dioxide into an absorption tower from the bottom of the tower, filling hydrogen peroxide aqueous solution, sodium hydroxide aqueous solution and absorbent into the absorption tower, absorbing and discharging the gas at the top of the tower, centrifuging reactants in the absorption tower after the gas is introduced, and separating the obtained supernatant to obtain sodium chlorite solution; the preparation method of sodium chlorite can simplify the production flow, reduce the investment of equipment, reduce energy consumption, improve the utilization rate of the raw material of sulfuric acid in the preparation of chlorine dioxide and improve the yield in the preparation of sodium chlorite.
Description
Technical Field
The invention relates to the technical field of sodium chlorite preparation, in particular to a preparation method of sodium chlorite.
Background
Sodium chlorite is an inorganic compound that is used mainly as a bleaching agent, a decoloring agent, a disinfectant, a discharge agent, etc. Sodium chlorite has the chemical formula of NaClO 2, is white or slightly pale yellow amorphous crystal or powder, has strong oxidizing property, and is easy to gradually decompose in wet air. Sodium chlorite is easily dissolved in water and the aqueous solution is alkaline.
The preparation method of sodium chlorite mainly includes electrolytic method, chemical method and reduction method. The electrolysis method is to electrolyze sodium chloride aqueous solution in a three-chamber type electrolytic tank separated by an ion exchange membrane, continuously introducing gaseous chlorine dioxide into a negative chamber, and then spray-drying the sodium chlorite solution obtained by the reaction; the sodium chlorite obtained by the method has high purity, raw material saving and lower cost, but the investment in factory construction is large, and the production process and operation are complex. The chemical method is to react sodium chlorate with hydrochloric acid or sulfuric acid to obtain sodium chlorite and chlorine, wherein the pH value and the temperature need to be controlled in the reaction to ensure the yield and the purity of the sodium chlorite; the method has simple process and convenient operation, but generates a large amount of waste gas and waste water in the reaction process, thereby causing environmental pollution. The reduction method is to prepare chlorine dioxide by taking sodium chlorate as a raw material, then adding chlorine dioxide into an alkaline medium to react with a reducing agent to obtain sodium chlorite, wherein the common reducing agent comprises hydrogen peroxide, zinc powder, lead monoxide, carbonaceous materials and the like, and the most common reducing agent is hydrogen peroxide; the method is the most commonly used sodium chlorite preparation method, the purity of the obtained sodium chlorite is high, the yield is high, but the automation degree is low, and the reaction speed is slower and slower due to the existence of water generated by the reaction of chlorine dioxide and hydrogen peroxide.
In order to solve the problems existing in the reduction method, the applicant introduces an automatic production line of sodium chlorite, in particular to integrate a sodium chlorate dissolver, a generating reactor, an absorption system (comprising an absorption tower, a washing tower and an absorption tank), a concentrator, a filter and a dryer into one production line, and realize the automation of sodium chlorite production by a pumping and conveying mode, wherein the production process comprises the following steps: adding sodium chlorate into a sodium chlorate dissolver for dissolution, introducing the dissolved sodium chlorate, sulfuric acid with the concentration of 98wt% and hydrogen peroxide with the concentration of 27.5wt% into a generating reactor to generate gaseous chlorine dioxide and liquid sodium bisulfate products, then pumping hydrogen peroxide into an absorption tower, pumping liquid caustic soda into a washing tower, continuously circulating materials among the absorption tower, the washing tower and an absorption tank, introducing chlorine dioxide gas into the absorption tower, fully reacting the chlorine dioxide gas with the circulating liquid caustic soda and the hydrogen peroxide through the washing tower to generate sodium chlorite solution, wherein chlorine dioxide which does not participate in the reaction in the absorption process is photolyzed into reaction tail gas containing oxygen and chlorine, discharging after absorption, introducing the sodium chlorite solution into a concentrator for evaporation concentration, introducing the sodium chlorite solution into a filter for filtration, and drying in a dryer to obtain sodium chlorite. However, the following problems were found when the production was carried out according to the above production process: in the reaction of sodium chlorate, sulfuric acid with the concentration of 98wt% and hydrogen peroxide with the concentration of 27.5wt%, in order to promote the reaction, excessive sulfuric acid is required to be used to provide an acidic environment, so that the raw material utilization rate of the sulfuric acid is low; in order to perform full reaction, hydrogen peroxide and liquid alkali are required to be continuously circulated in an absorption tower and a washing tower respectively, so that the production flow is complex, more equipment is required in production, and energy consumption is high, but if the hydrogen peroxide and the liquid alkali are not circulated, the problem that the hydrogen peroxide and the liquid alkali cannot be fully mixed exists, and the yield of sodium chlorite is reduced.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a preparation method of sodium chlorite, which can simplify the production flow, reduce the investment of equipment, reduce energy consumption, improve the utilization rate of the raw material of sulfuric acid in the preparation of chlorine dioxide and improve the yield in the preparation of sodium chlorite.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the preparation method of the sodium chlorite comprises the following steps: dissolving, preparing chlorine dioxide, preparing sodium chlorite solution, concentrating, filtering and drying;
Adding sodium chlorate and water into a sodium chlorate dissolver, stirring until the sodium chlorate and the water are completely dissolved to obtain sodium chlorate aqueous solution, and introducing the obtained sodium chlorate aqueous solution into a generation reactor;
In the dissolution, the mass volume ratio of sodium chlorate to water is 200-210kg:400-450L;
the method comprises the steps of preparing chlorine dioxide, adding a filler into a generating reactor in advance, controlling the temperature of the generating reactor to 60-70 ℃ after sodium chlorate aqueous solution is introduced into the generating reactor, keeping stirring, wherein the stirring speed in stirring is 50-150rpm, adding concentrated sulfuric acid and hydrogen peroxide aqueous solution into the generating reactor, continuously generating gas in the stirring process, introducing the generated gas into an absorption tower of an absorption system, centrifuging the reactant in the generating reactor when no gas is generated any more, keeping the rotating speed in the centrifuge at 8000-9000rpm for 20-30min, drying the obtained precipitate, continuously adding the precipitate into the generating reactor as the filler for recycling, and separating the obtained supernatant to obtain sodium bisulfate byproducts;
the mass ratio of the sodium chlorate in the dissolution to the filler in the preparation of chlorine dioxide is 200-210:5-6;
the mass volume ratio of the sodium chlorate in the dissolution to the concentrated sulfuric acid in the preparation of the chlorine dioxide and the hydrogen peroxide water solution is 200-210kg:153-187L:127-139L;
the concentration of the concentrated sulfuric acid is 98wt%;
The concentration of the aqueous hydrogen peroxide solution is 27.5wt%;
The preparation method of the filler comprises the following steps: preparing hollow carbon spheres and carboxylating;
The preparation method comprises the steps of uniformly mixing citric acid, glucose, alkyl glycoside APG 1214 and water, adding into a hydrothermal kettle for hydrothermal reaction, wherein the temperature in the hydrothermal reaction is 220-240 ℃, the pressure is 1.5-2MPa, the time is 2-3h, centrifuging after the hydrothermal reaction is finished, the centrifugal speed is 8000-9000rpm, the time is 20-30min, washing the precipitate with water, and drying at 70-90 ℃ to obtain the hollow carbon spheres;
In the preparation of the hollow carbon sphere, the mass volume ratio of citric acid, glucose, alkyl glycoside APG 1214 and water is 5-5.5kg:5-6kg:1-1.5kg:25-30L;
the active content of the alkyl glycoside APG 1214 is 50wt%;
The carboxylation, hollow carbon sphere and mixed acid are mixed and then stirred and refluxed at 60-70 ℃, the rotation speed during stirring and refluxing is 50-300rpm, the time is 3-4h, the centrifugation is carried out after the stirring and refluxing is finished, the rotation speed during centrifugation is 8000-9000rpm, the time is 20-30min, the precipitate is washed by water, and the precipitate is dried at 70-90 ℃ to obtain the filler;
in the carboxylation, the mass volume ratio of the hollow carbon spheres to the mixed acid is 2.5-3kg:250-350L;
The mixed acid is a mixed solution of sulfuric acid and nitric acid, the concentration of sulfuric acid is 98wt%, the concentration of nitric acid is 70wt%, and the volume ratio of sulfuric acid to nitric acid is 3-4:1;
Introducing gas generated in the preparation of chlorine dioxide into an absorption tower from the bottom of the tower, regulating the flow rate of the gas by using a pump, absorbing the gas at the top of the absorption tower by using a hydrogen peroxide aqueous solution, a sodium hydroxide aqueous solution and an absorbent, discharging the gas after the gas is introduced, centrifuging reactants in the absorption tower after the gas is introduced, and drying the obtained precipitate at 7000-8000rpm for 15-20min, and then continuously adding the dried precipitate into the absorption tower to serve as the absorbent for recycling, and separating the obtained supernatant to obtain the sodium chlorite solution;
In the preparation of the sodium chlorite solution, the gas flow rate is 0.8-1m 3/min;
The mass ratio of the sodium chlorate in the dissolution to the absorbent in the sodium chlorite solution is 200-210:4-5;
The mass volume ratio of the sodium chlorate in the dissolution to the sodium hydroxide aqueous solution and the hydrogen peroxide aqueous solution in the preparation of the sodium chlorite solution is 200-210kg:121-133L:211-231L;
The concentration of the sodium hydroxide aqueous solution is 30wt%;
The concentration of the aqueous hydrogen peroxide solution is 27.5wt%;
The filler in the absorption tower is polypropylene pall ring filler;
The preparation method of the absorbent comprises the steps of mixing filler, N' -carbonyl diimidazole and tetrahydrofuran in the prepared chlorine dioxide under the protection of nitrogen, stirring at room temperature, wherein the stirring speed is 50-300rpm, the time is 10-20min, adding a tetrahydrofuran solution of polyethylene glycol 2000, continuing stirring at 30-35 ℃ for 10-12h after the addition, centrifuging, the centrifugal speed is 7000-8000rpm, the time is 15-20min, washing the precipitate with an ethanol water solution with the concentration of 50wt%, and drying at 70-90 ℃ to obtain the absorbent;
In the preparation of the absorbent, the mass volume ratio of the filling material, N' -carbonyl diimidazole, tetrahydrofuran and tetrahydrofuran solution of polyethylene glycol 2000 in the chlorine dioxide is 2.5-3kg:0.8-1kg:50-60L:10-13L;
the adding speed of the tetrahydrofuran solution of the polyethylene glycol 2000 is 400-500mL/min;
The concentration of the polyethylene glycol 2000 in the tetrahydrofuran solution of the polyethylene glycol 2000 is 15wt%;
Adding sodium chloride into the sodium chlorite solution obtained in the preparation of the sodium chlorite solution, uniformly mixing, evaporating and concentrating at 65-80 ℃ to obtain a suspension with the solid content of 30-35%, and obtaining a concentrated solution;
the mass ratio of the sodium chlorate in the dissolution to the sodium chloride in the concentration is 200-210:34-45;
The purity of the sodium chloride is 99.5wt%;
Filtering, namely filtering the concentrated solution, continuously concentrating and filtering the obtained filtrate, and drying the obtained filter residues;
and (3) drying, namely drying filter residues obtained in the filtering to obtain sodium chlorite.
Compared with the prior art, the invention has the beneficial effects that:
(1) The preparation method of sodium chlorite can simplify the production flow and omit the process of circulating the hydrogen peroxide aqueous solution and the sodium hydroxide aqueous solution in the preparation of sodium chlorite solution;
(2) According to the preparation method of sodium chlorite, disclosed by the invention, the contact area of chlorine dioxide and other reactants is promoted by adding the absorbent into the absorption tower used in the preparation of sodium chlorite solution, so that the investment of a washing tower and an absorption tank is reduced, and the energy consumption is reduced;
(3) The preparation method of sodium chlorite improves the utilization rate of the raw materials of sulfuric acid in the preparation of chlorine dioxide, and the yield of sodium chlorite can reach 95.8-96.8 percent (calculated by sodium chlorate) when the molar ratio of sodium chlorate to sulfuric acid is 1:1.55-1.75.
Detailed Description
Specific embodiments of the present invention will now be described in order to provide a clearer understanding of the technical features, objects and effects of the present invention.
Example 1
The preparation method of sodium chlorite comprises the following steps:
1. Dissolving: 200kg of sodium chlorate and 400L of water are added into a sodium chlorate dissolver, stirred until the sodium chlorate is completely dissolved, so as to obtain sodium chlorate aqueous solution, and the obtained sodium chlorate aqueous solution is introduced into a generating reactor;
2. Preparing chlorine dioxide: adding 5kg of filler into a generating reactor in advance, after the sodium chlorate aqueous solution obtained in the step 1 dissolution is introduced into the generating reactor, controlling the temperature of the generating reactor to 60 ℃, keeping stirring, wherein the stirring speed in stirring is 50rpm, adding 153L of concentrated sulfuric acid with the concentration of 98wt% and 127L of hydrogen peroxide aqueous solution with the concentration of 27.5wt% into the generating reactor, continuously generating gas in the stirring process, introducing the generated gas into an absorption tower of an absorption system, centrifuging the reactant in the generating reactor when no gas is generated any more, drying the obtained precipitate at the rotating speed of 8000rpm for 20min, continuously adding the obtained precipitate into the generating reactor as the filler for recycling, and separating the obtained supernatant to obtain sodium bisulfate byproducts;
The preparation method of the filler specifically comprises the following steps:
(1) Preparing hollow carbon spheres: uniformly mixing 5kg of citric acid, 5kg of glucose, 1kg of alkyl glycoside APG 1214 and 25L of water, adding into a hydrothermal kettle for hydrothermal reaction, wherein the temperature in the hydrothermal reaction is 220 ℃, the pressure is 1.5MPa, the time is 2 hours, centrifuging after the hydrothermal reaction is finished, the rotating speed in the centrifuge is 8000rpm, the time is 20 minutes, washing the precipitate with water, and drying at 70 ℃ to obtain hollow carbon spheres;
the active content of the alkyl glycoside APG 1214 is 50wt%;
(2) Carboxylation: 2.5kg of hollow carbon spheres and 250L of mixed acid are mixed and then are stirred and refluxed at 60 ℃, the rotation speed during stirring and refluxing is 50rpm, the time is 3 hours, the stirring and refluxing are finished, the centrifugation is carried out, the rotation speed in the centrifuge is 8000rpm, the time is 20 minutes, the precipitate is washed by water, and the precipitate is dried at 70 ℃ to obtain the filler;
the mixed acid is a mixed solution of sulfuric acid and nitric acid, the concentration of sulfuric acid is 98wt%, the concentration of nitric acid is 70wt%, and the volume ratio of sulfuric acid to nitric acid is 3:1;
3. Preparation of sodium chlorite solution: introducing the gas generated in the step 2 of preparing chlorine dioxide into an absorption tower from the bottom, regulating the gas flow rate by using a pump, wherein the gas flow rate is 0.8m 3/min, 121L of aqueous hydrogen peroxide solution with the concentration of 27.5wt%, 211L of aqueous sodium hydroxide solution with the concentration of 30wt% and 4kg of absorbent are filled in the absorption tower, introducing the gas at the top into 60L of aqueous sodium hydroxide solution with the concentration of 30wt% for absorption, discharging, centrifuging reactants in the absorption tower after the gas is introduced, drying the obtained precipitate for 15min at the rotating speed of 7000rpm, continuously adding the obtained precipitate into the absorption tower as the absorbent for recycling, and separating the obtained supernatant to obtain sodium chlorite solution;
The filler in the absorption tower is polypropylene pall ring filler;
The preparation method of the absorbent comprises the following steps: mixing 2.5kg of filler in the step 2 preparation of chlorine dioxide, 0.8kg of N, N' -carbonyldiimidazole and 50L of tetrahydrofuran under the protection of nitrogen, stirring at room temperature, wherein the stirring speed is 50rpm for 10min, slowly adding 10L of tetrahydrofuran solution of polyethylene glycol 2000, the adding speed is 400mL/min, continuing stirring at 30 ℃ for 10h after the adding is finished, centrifuging, the centrifugal rotating speed is 7000rpm, the centrifugal rotating speed is 15min, washing the precipitate with ethanol water solution with the concentration of 50wt%, and drying at 70 ℃ to obtain an absorbent;
The concentration of the polyethylene glycol 2000 in the tetrahydrofuran solution of the polyethylene glycol 2000 is 15wt%;
4. concentrating: adding 34kg of sodium chloride with the purity of 99.5wt% into the sodium chlorite solution obtained in the step 3, uniformly mixing, evaporating and concentrating at 65 ℃ to obtain a suspension with the solid content of 30%, and obtaining a concentrated solution;
5. And (3) filtering: cooling and crystallizing the concentrated solution, filtering, concentrating and filtering the obtained filtrate according to the step 4 concentration step, and drying the obtained filter residue;
6. And (3) drying: the filter residue obtained in the 5 th filtration was dried to obtain 203.4kg of sodium chlorite with a purity of 80wt% and a yield of 95.8% (based on sodium chlorate).
Example 2
The preparation method of sodium chlorite comprises the following steps:
1. Dissolving: adding 205kg of sodium chlorate and 420L of water into a sodium chlorate dissolver, stirring until the sodium chlorate is completely dissolved to obtain sodium chlorate aqueous solution, and introducing the obtained sodium chlorate aqueous solution into a generation reactor;
2. Preparing chlorine dioxide: adding 5.5kg of filler into a generating reactor in advance, after the sodium chlorate aqueous solution obtained in the step 1 is introduced into the generating reactor, controlling the temperature of the generating reactor to 65 ℃, keeping stirring, wherein the stirring speed in stirring is 100rpm, adding 168L of concentrated sulfuric acid with the concentration of 98wt% and 132L of hydrogen peroxide aqueous solution with the concentration of 27.5wt% into the generating reactor, continuously generating gas in the stirring process, introducing the generated gas into an absorption tower of an absorption system, centrifuging the reactant in the generating reactor when no gas is generated any more, drying the obtained precipitate at the rotating speed of 8500rpm for 25min, continuously adding the obtained precipitate into the generating reactor as the filler for recycling, and separating the obtained supernatant to obtain sodium bisulfate byproducts;
The preparation method of the filler specifically comprises the following steps:
(1) Preparing hollow carbon spheres: uniformly mixing 5.2kg of citric acid, 5.5kg of glucose and 1.2kg of alkyl glycoside APG 1214 and 28L of water, adding into a hydrothermal kettle for hydrothermal reaction, wherein the temperature in the hydrothermal reaction is 230 ℃, the pressure is 1.7MPa, the time is 2.5h, centrifuging after the hydrothermal reaction is finished, the centrifugal speed is 8500rpm, the time is 25min, washing the precipitate with water, and drying at 80 ℃ to obtain hollow carbon spheres;
the active content of the alkyl glycoside APG 1214 is 50wt%;
(2) Carboxylation: 2.7kg of hollow carbon spheres and 300L of mixed acid are mixed and then stirred and refluxed at 65 ℃, the rotation speed during stirring and refluxing is 200rpm, the time is 3.5h, the centrifugation is carried out after the stirring and refluxing is finished, the rotation speed during centrifugation is 8500rpm, the time is 25min, the precipitate is washed by water, and the precipitate is dried at 80 ℃ to obtain the filler;
The mixed acid is a mixed solution of sulfuric acid and nitric acid, the concentration of sulfuric acid is 98wt%, the concentration of nitric acid is 70wt%, and the volume ratio of sulfuric acid to nitric acid is 3.5:1;
3. Preparation of sodium chlorite solution: introducing the gas generated in the step 2 of preparing chlorine dioxide into an absorption tower from the bottom, regulating the gas flow rate by using a pump, wherein the gas flow rate is 0.9m 3/min, 127L of aqueous hydrogen peroxide solution with the concentration of 27.5wt%, 220L of aqueous sodium hydroxide solution with the concentration of 30wt% and 4.5kg of absorbent are filled in the absorption tower, introducing the gas at the top of the tower into 70L of aqueous sodium hydroxide solution with the concentration of 30wt% for absorption, discharging, centrifuging reactants in the absorption tower after the gas is introduced, drying the obtained precipitate for 17min at the rotating speed of 7500rpm, continuously adding the obtained precipitate into the absorption tower as the absorbent for recycling, and separating the obtained supernatant to obtain sodium chlorite solution;
The filler in the absorption tower is polypropylene pall ring filler;
The preparation method of the absorbent comprises the following steps: mixing 2.8kg of filler in the step 2 preparation of chlorine dioxide, 0.9kg of N, N' -carbonyldiimidazole and 55L of tetrahydrofuran under the protection of nitrogen, stirring at room temperature, wherein the rotation speed during stirring is 150rpm for 15min, slowly adding 12L of tetrahydrofuran solution of polyethylene glycol 2000, the adding speed is 450mL/min, continuing stirring at 32 ℃ for 11h after the adding is finished, centrifuging, the rotation speed during centrifugation is 7500rpm, the time is 18min, washing precipitate with ethanol water solution with the concentration of 50wt%, and drying at 80 ℃ to obtain an absorbent;
The concentration of the polyethylene glycol 2000 in the tetrahydrofuran solution of the polyethylene glycol 2000 is 15wt%;
4. Concentrating: adding 38kg of sodium chloride with the purity of 99.5wt% into the sodium chlorite solution obtained in the step 3, uniformly mixing, evaporating and concentrating at 75 ℃ to obtain a suspension with the solid content of 32%, and obtaining a concentrated solution;
5. And (3) filtering: cooling and crystallizing the concentrated solution, filtering, concentrating and filtering the obtained filtrate according to the step 4 concentration step, and drying the obtained filter residue;
6. And (3) drying: the filter residue obtained in the step 5 is dried to obtain 208.1kg of sodium chlorite with the purity of 81wt percent and the yield is 96.8 percent.
Example 3
The preparation method of sodium chlorite comprises the following steps:
1. dissolving: adding 210kg of sodium chlorate and 450L of water into a sodium chlorate dissolver, stirring until the sodium chlorate is completely dissolved to obtain sodium chlorate aqueous solution, and introducing the obtained sodium chlorate aqueous solution into a generation reactor;
2. Preparing chlorine dioxide: adding 6kg of filler into a generating reactor in advance, after the sodium chlorate aqueous solution obtained in the step 1 dissolution is introduced into the generating reactor, controlling the temperature of the generating reactor to 70 ℃, keeping stirring, wherein the stirring speed in stirring is 150rpm, adding 187L of concentrated sulfuric acid with the concentration of 98wt% and 139L of hydrogen peroxide aqueous solution with the concentration of 27.5wt% into the generating reactor, continuously generating gas in the stirring process, introducing the generated gas into an absorption tower of an absorption system, centrifuging the reactant in the generating reactor when no gas is generated any more, drying the obtained precipitate at the rotating speed of 9000rpm for 30min, continuously adding the precipitate into the generating reactor as the filler for recycling, and separating the obtained supernatant to obtain sodium bisulfate byproducts;
The preparation method of the filler specifically comprises the following steps:
(1) Preparing hollow carbon spheres: uniformly mixing 5.5kg of citric acid, 6kg of glucose, 1.5kg of alkyl glycoside APG 1214 and 30L of water, adding into a hydrothermal kettle for hydrothermal reaction, wherein the temperature in the hydrothermal reaction is 240 ℃, the pressure is 2MPa, the time is 3 hours, centrifuging after the hydrothermal reaction is finished, the centrifugal speed is 9000rpm, the time is 30 minutes, washing the precipitate with water, and drying at 90 ℃ to obtain hollow carbon spheres;
the active content of the alkyl glycoside APG 1214 is 50wt%;
(2) Carboxylation: 3kg of hollow carbon spheres and 350L of mixed acid are mixed and then are stirred and refluxed at 70 ℃, the rotation speed during stirring and refluxing is 300rpm, the time is 4 hours, the stirring and refluxing are finished, the centrifugation is carried out, the rotation speed in the centrifuge is 9000rpm, the time is 30 minutes, the precipitate is washed by water, and the precipitate is dried at 90 ℃ to obtain the filler;
The mixed acid is a mixed solution of sulfuric acid and nitric acid, the concentration of sulfuric acid is 98wt%, the concentration of nitric acid is 70wt%, and the volume ratio of sulfuric acid to nitric acid is 4:1;
3. Preparation of sodium chlorite solution: introducing the gas generated in the step 2 of preparing chlorine dioxide into an absorption tower from the bottom, regulating the gas flow rate by using a pump, wherein the gas flow rate is 1m 3/min, containing 133L of aqueous hydrogen peroxide solution with the concentration of 27.5wt%, 231L of aqueous sodium hydroxide solution with the concentration of 30wt% and 5kg of absorbent in the absorption tower, introducing the gas at the top into 80L of aqueous sodium hydroxide solution with the concentration of 30wt% for absorption, discharging, centrifuging the reactant in the absorption tower after the gas introduction is finished, keeping the rotating speed in the centrifuge at 8000rpm for 20min, drying the obtained precipitate, continuously adding the obtained precipitate into the absorption tower as the absorbent for recycling, and separating the obtained supernatant to obtain sodium chlorite solution;
The filler in the absorption tower is polypropylene pall ring filler;
The preparation method of the absorbent comprises the following steps: mixing 3kg of filler in the 2 nd step of preparation of chlorine dioxide, 1kg of N, N' -carbonyldiimidazole and 60L of tetrahydrofuran under the protection of nitrogen, stirring at room temperature, wherein the stirring speed is 300rpm, the time is 20min, slowly adding 13L of tetrahydrofuran solution of polyethylene glycol 2000, the adding speed is 500mL/min, continuing stirring at 35 ℃ for 12h after the adding is finished, centrifuging, the centrifugal speed is 8000rpm, the time is 20min, washing the precipitate with ethanol water solution with the concentration of 50wt%, and drying at 90 ℃ to obtain an absorbent;
The concentration of the polyethylene glycol 2000 in the tetrahydrofuran solution of the polyethylene glycol 2000 is 15wt%;
4. concentrating: adding 45kg of sodium chloride with the purity of 99.5wt% into the sodium chlorite solution obtained in the step 3, uniformly mixing, evaporating and concentrating at 80 ℃ to obtain a suspension with the solid content of 35%, and obtaining a concentrated solution;
5. And (3) filtering: cooling and crystallizing the concentrated solution, filtering, concentrating and filtering the obtained filtrate according to the step 4 concentration step, and drying the obtained filter residue;
6. And (3) drying: the filter residue obtained in the step 5 is dried to obtain 214.5kg of sodium chlorite with the purity of 80wt percent and the yield is 96.2 percent.
Comparative example 1
Based on the preparation method of example 2, the addition of filler was omitted in the preparation of chlorine dioxide in step 2, and 181.5kg of sodium chlorite with a purity of 81wt% was finally obtained with a yield of 84.4%.
In order to verify whether the addition of the filler can play a role in acidifying hydrogen peroxide and promoting the reaction to proceed, so that the consumption of sulfuric acid is reduced, and if the addition of the filler is omitted, the problem that the reaction is not thorough or side reaction is increased due to insufficient acidification because of too little sulfuric acid addition is solved, so that the consumption of concentrated sulfuric acid in the step 2 of preparing chlorine dioxide is multiplied by 1.5 times on the basis of the preparation method, namely, the consumption of the concentrated sulfuric acid with the concentration of 98wt% is increased from 168L to 252L; 207.6kg of sodium chlorite with a purity of 81wt% are obtained in a yield of 96.5%.
Comparative example 2
Based on the preparation method of example 2, the addition of the absorbent was omitted in the preparation of sodium chlorite solution in step 3, and finally 172.3kg of sodium chlorite with a purity of 80wt% was obtained with a yield of 79.1%.
In order to verify whether the addition of the absorbent can play a role in promoting the contact of reactants and the reaction, so that the difficulty of mixing the reactants is reduced, the gas flow rate in the sodium chlorite solution prepared in the step 3 is reduced to half of the original flow rate on the basis of the preparation method, namely, the gas flow rate is reduced to 0.45m 3/min; 207.1kg of sodium chlorite with a purity of 80% by weight were obtained in a yield of 95.1%.
As can be seen from the results of examples 1 to 3 and comparative examples 1 to 2, by adding the filler in the preparation of chlorine dioxide, the filler is carboxylated hollow carbon spheres, which have a large surface area and are light in weight, and by carboxylating, the surfaces and pores of the hollow carbon spheres are provided with carboxyl groups, not only can the adsorption of chlorine dioxide be reduced, but also the effect of providing hydrogen ions in the preparation of chlorine dioxide can be achieved, so that the effect of assisting the acidification of the durum sulfate hydrogen peroxide can be achieved, and in addition, the carboxylated hollow carbon spheres can promote the sufficient contact between reactants and provide more reaction sites due to the large surface area, so that the use of sulfuric acid is reduced, and the reaction speed is improved.
By adding the adsorbent into the sodium chlorite solution, the adsorbent is the hollow carbon sphere grafted with the polyethylene glycol 2000, the polyethylene glycol 2000 can improve the dispersibility of the hollow carbon sphere in water, and compared with carboxylated hollow carbon spheres, the polyethylene glycol 2000 can provide more reaction sites and promote the contact of chlorine dioxide and other reactants, thereby ensuring that high yield can be realized at a higher gas inlet speed, improving the reaction speed and shortening the reaction time.
The percentages used in the present invention are mass percentages unless otherwise indicated.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the sodium chlorite is characterized by comprising the following steps of: dissolving, preparing chlorine dioxide, preparing sodium chlorite solution, concentrating, filtering and drying;
The method comprises the steps of preparing chlorine dioxide, adding a filler into a generating reactor in advance, after introducing sodium chlorate aqueous solution into the generating reactor, controlling the temperature of the generating reactor to 60-70 ℃, keeping stirring, adding concentrated sulfuric acid and hydrogen peroxide aqueous solution into the generating reactor, and introducing generated gas into an absorption tower of an absorption system;
The preparation method of the filler comprises the following steps: preparing hollow carbon spheres and carboxylating;
The preparation method comprises the steps of uniformly mixing citric acid, glucose, alkyl glycoside APG 1214 and water, adding into a hydrothermal kettle for hydrothermal reaction, centrifuging after the hydrothermal reaction is finished, cleaning, drying and precipitating to obtain hollow carbon spheres;
The carboxylation, hollow carbon sphere and mixed acid are mixed and then stirred and refluxed at 60-70 ℃, and after stirring and refluxing are finished, the mixture is centrifuged, washed, dried and precipitated to obtain the filler;
Introducing gas generated in the preparation of chlorine dioxide into an absorption tower from the bottom of the tower, filling hydrogen peroxide aqueous solution, sodium hydroxide aqueous solution and absorbent into the absorption tower, absorbing and discharging the gas at the top of the tower, centrifuging reactants in the absorption tower after the gas is introduced, and separating the obtained supernatant to obtain sodium chlorite solution;
The preparation method of the absorbent comprises the steps of mixing the filler, N' -carbonyl diimidazole and tetrahydrofuran in the preparation of chlorine dioxide under the protection of nitrogen, stirring at room temperature, adding a tetrahydrofuran solution of polyethylene glycol 2000, continuously stirring at 30-35 ℃, centrifuging, cleaning, drying and precipitating to obtain the absorbent.
2. The method for preparing sodium chlorite according to claim 1, wherein the dissolution is carried out by adding sodium chlorate and water into a sodium chlorate dissolver, and stirring until completely dissolved to obtain sodium chlorate water solution.
3. The method for preparing sodium chlorite according to claim 2, wherein the mass-to-volume ratio of sodium chlorate to water in the dissolution is 200-210kg:400-450L;
the mass ratio of the sodium chlorate in the dissolution to the filler in the preparation of chlorine dioxide is 200-210:5-6;
the mass volume ratio of the sodium chlorate in the dissolution to the concentrated sulfuric acid in the preparation of the chlorine dioxide and the hydrogen peroxide water solution is 200-210kg:153-187L:127-139L;
the concentration of the concentrated sulfuric acid is 98wt%;
the concentration of the aqueous hydrogen peroxide solution was 27.5wt%.
4. The method for preparing sodium chlorite according to claim 1, wherein in the hollow carbon sphere preparation, the mass-volume ratio of citric acid, glucose, alkyl glycoside APG 1214 and water is 5-5.5kg:5-6kg:1-1.5kg:25-30L;
the active content of the alkyl glycoside APG 1214 is 50wt%;
the temperature in the hydrothermal reaction is 220-240 ℃, the pressure is 1.5-2MPa, and the time is 2-3h.
5. The method for preparing sodium chlorite according to claim 1, wherein in the carboxylation, the mass-volume ratio of the hollow carbon spheres to the mixed acid is 2.5-3kg:250-350L;
the mixed acid is a mixed solution of sulfuric acid and nitric acid, the concentration of sulfuric acid is 98wt%, the concentration of nitric acid is 70wt%, and the volume ratio of sulfuric acid to nitric acid is 3-4:1.
6. The method for preparing sodium chlorite according to claim 1, wherein the gas flow rate in the sodium chlorite solution is 0.8-1m 3/min.
7. The method for preparing sodium chlorite according to claim 1, wherein the mass ratio of sodium chlorate in solution to absorbent in the sodium chlorite solution is 200-210:4-5;
The mass volume ratio of the sodium chlorate in the dissolution to the sodium hydroxide aqueous solution and the hydrogen peroxide aqueous solution in the preparation of the sodium chlorite solution is 200-210kg:121-133L:211-231L;
In the preparation of the sodium chlorite solution, the concentration of the sodium hydroxide aqueous solution is 30wt%;
The concentration of the aqueous hydrogen peroxide solution is 27.5wt%;
the filler in the absorption tower is polypropylene pall ring filler.
8. The method for preparing sodium chlorite according to claim 1, wherein in the preparation of the absorbent, the mass volume ratio of the filler, the N, N' -carbonyldiimidazole, the tetrahydrofuran and the tetrahydrofuran solution of the polyethylene glycol 2000 in the chlorine dioxide is 2.5-3kg:0.8-1kg:50-60L:10-13L;
the adding speed of the tetrahydrofuran solution of the polyethylene glycol 2000 is 400-500mL/min;
The concentration of polyethylene glycol 2000 in the tetrahydrofuran solution of polyethylene glycol 2000 is 15wt%.
9. The method for preparing sodium chlorite according to claim 1, wherein sodium chloride is added into sodium chlorite solution obtained in the preparation of sodium chlorite solution, and after uniform mixing, the sodium chlorite solution is evaporated and concentrated at 65-80 ℃ to obtain a suspension with 30-35% of solid content by evaporation and concentration, so as to obtain a concentrated solution;
the mass ratio of the sodium chlorate in the dissolution to the sodium chloride in the concentration is 200-210:34-45;
The purity of the sodium chloride was 99.5wt%.
10. The method for preparing sodium chlorite according to claim 1, wherein the filtering is carried out by cooling and crystallizing the concentrated solution, filtering, concentrating the obtained filtrate, filtering, and drying the obtained filter residue;
and (3) drying, namely drying filter residues obtained in the filtering to obtain sodium chlorite.
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