CN113117680B - Nano ferrous metatitanate-silica gel particle Fenton catalyst, and preparation method and application method thereof - Google Patents
Nano ferrous metatitanate-silica gel particle Fenton catalyst, and preparation method and application method thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 41
- 239000002245 particle Substances 0.000 title claims abstract description 41
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000000741 silica gel Substances 0.000 title claims abstract description 37
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 13
- 239000002253 acid Substances 0.000 claims abstract description 66
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 21
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 21
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 21
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 21
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 17
- 239000010865 sewage Substances 0.000 claims abstract description 12
- 230000007935 neutral effect Effects 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000002378 acidificating effect Effects 0.000 claims abstract description 4
- 239000000725 suspension Substances 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 22
- 230000035484 reaction time Effects 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 229960001866 silicon dioxide Drugs 0.000 claims 7
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002244 precipitate Substances 0.000 claims 1
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 239000002351 wastewater Substances 0.000 abstract description 17
- 239000010802 sludge Substances 0.000 abstract description 9
- 238000001556 precipitation Methods 0.000 abstract description 7
- 238000000926 separation method Methods 0.000 abstract description 7
- 239000003513 alkali Substances 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000004408 titanium dioxide Substances 0.000 description 4
- 238000006386 neutralization reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011973 solid acid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B01J35/50—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
Abstract
The invention relates to a nano ferrous metatitanate-silica gel particle Fenton catalyst, a preparation method and a using method thereof, wherein the method comprises the following steps: under the acidic condition, the nano metatitanic acid and the sodium silicate solution are subjected to a silica gel reaction to obtain the nano ferrous metatitanic acid-silica gel particle Fenton catalyst. The using method comprises the following steps: the nano ferrous metatitanic acid-silica gel particle Fenton catalyst and hydrogen peroxide are added into the sewage to treat the sewage. The invention has the advantages of nanoscale high specific surface area and catalytic activity, and hydrogen peroxide is directly added without adjusting the pH of wastewater when in use. The nano ferrous metatitanate-silica gel particle Fenton catalyst has high catalytic activity under the condition of neutral wastewater, has high precipitation separation speed and good repeated use stability performance, does not need to add acid, alkali liquor, ferrous sulfate and PAM, does not generate sludge, and has obvious economic benefit and social benefit.
Description
Technical Field
The invention relates to a nano ferrous metatitanate-silica gel particle Fenton catalyst, a preparation method and a use method thereof, and belongs to the technical field of Fenton catalysts.
Background
In the prior art, Fe is adopted in Fenton2+/Fe3+As a catalyst, hydrogen peroxide in the wastewater is firstly promoted to be decomposed to generate OH, and then the OH attacks refractory organic macromolecules in the wastewater, the OH annihilation speed is extremely high, the organic matter content in the wastewater is low, the capture and cracking efficiency is low, and meanwhile, the salinity is increased due to acid-base adjustment, the sludge yield is high, and the operation cost is high.
The novel Fenton catalyst adopts a certain process method, selects nano metatitanic acid as a raw material, firstly prepares nano ferrous metatitanic acid, and then generates a silica gel reaction with a silica gel solution under an acidic condition to generate the silica gel particle Fenton catalyst coated by the nano ferrous metatitanic acid with certain particle strength.
Disclosure of Invention
The invention provides a nano ferrous metatitanic acid-silica gel particle Fenton catalyst and a preparation method and a using method thereof, aiming at the problems, the nano ferrous metatitanic acid and sodium silicate with a certain modulus are subjected to a silica gel reaction under an acidic condition, and the nano ferrous metatitanic acid-silica gel particle Fenton catalyst is formed under a stirring state. The invention has obvious acid and alkali resistance, large specific surface area and excellent precipitation separation effect. The technical scheme of the invention is as follows:
a preparation method of a nano ferrous metatitanate-silica gel particle Fenton catalyst comprises the following specific steps:
(1) preparation of suspension of metatitanic acid (hydrated titanium dioxide)
Adding nano metatitanic acid with the particle size of 20-40nm into water to prepare metatitanic acid suspension with the mass concentration of 10-30%; preferably, the nano metatitanic acid with the particle size of 30nm is added into water to prepare metatitanic acid suspension with the mass concentration of 20%.
(2) Adding 10-30% ferrous sulfate solution into metatitanic acid suspension, wherein the molar ratio of nano metatitanic acid to ferrous sulfate is 0.1-1:1, the reaction time is 1-30min under the stirring condition that the stirring speed is 50-100 r/min, and the solution is neutral after the reaction to generate nano metatitanic acid suspension; preferably, 20% ferrous sulfate solution is added into the metatitanic acid suspension, the molar ratio of the nano metatitanic acid to the ferrous sulfate is 0.5:1, and the reaction time is 15min under the stirring condition that the stirring speed is 50 r/min.
(3) Under the stirring condition that the rotating speed is 20-200 revolutions per minute, simultaneously adding an acid solution and a sodium silicate solution with the modulus of 1.1-4 into the metatitanic acid suspension obtained in the step (2), wherein the molar ratio of the metatitanic acid solution to the sodium silicate solution is 1.5-3:1, the reaction time is 10-300min, and after reaction, carrying out precipitation separation to finally obtain the nano ferrous metatitanic acid-silica gel particle Fenton catalyst; preferably, an acid solution and a sodium silicate solution with the modulus of 2.5 are simultaneously added into the metatitanic acid suspension in the step (2), the molar ratio of the metatitanic acid solution to the sodium silicate solution is 2:1, the reaction time is 100min, and precipitation separation is carried out after the reaction to finally obtain the nano ferrous metatitanic acid-silica gel particle Fenton catalyst.
The use method of the invention comprises the following steps:
adding the nano ferrous metatitanate-silica gel particle Fenton catalyst and hydrogen peroxide into sewage to treat the sewage; preferably, the mass ratio of COD, the nano ferrous metatitanate-silica gel particle Fenton catalyst and 30% hydrogen peroxide in the wastewater is 1: 2-10: 1.2-1.5.
Compared with the prior art, the invention has the following advantages:
the invention has high specific surface area and catalytic activity in nanometer level, and can complete the catalytic oxidation effect of solid acid by directly adding hydrogen peroxide without adjusting the pH of the wastewater. Has obvious stability and repeated use performance, and reduces the cost.
Drawings
Fig. 1 is a biochemical sewage treatment diagram, wherein 1A is biochemical sewage before treatment, 1B is water treated in a neutralization tank of a fenton device, and 1C is water treated by adding ferrous sulfate and hydrogen peroxide while using the nano ferrous metatitanate-silica gel particle fenton catalyst of the present invention.
Detailed Description
The invention will be further described with reference to specific embodiments, and the advantages and features of the invention will become apparent as the description proceeds. The examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.
Example 1: a preparation method of a nano ferrous metatitanate-silica gel particle Fenton catalyst comprises the following specific steps:
(1) preparation of suspension of metatitanic acid (hydrated titanium dioxide)
Adding nano metatitanic acid with the particle size of 30nm into water to prepare metatitanic acid suspension with the mass concentration of 20%;
(2) adding 10% ferrous sulfate solution into metatitanic acid suspension, wherein the molar ratio of nano metatitanic acid to ferrous sulfate is 0.5:1, the reaction time is 5min under the stirring condition that the stirring speed is 50 r/min, and the solution is neutral after the reaction to generate nano metatitanic acid suspension;
(3) and (3) under the stirring condition that the rotating speed is 30 revolutions per minute, simultaneously adding an acid solution and a sodium silicate solution with the modulus of 1.5 into the metatitanic acid suspension obtained in the step (2), wherein the molar ratio of the metatitanic acid solution to the sodium silicate solution is 1.5:1, the reaction time is 10min, and after the reaction, carrying out precipitation separation to obtain the nano ferrous metatitanic acid-silica gel particle Fenton catalyst.
Example 2: a preparation method of a nano ferrous metatitanate-silica gel particle Fenton catalyst comprises the following specific steps:
(1) preparation of suspension of metatitanic acid (hydrated titanium dioxide)
Adding nano metatitanic acid with the particle size of 25nm into water to prepare metatitanic acid suspension with the mass concentration of 15%;
(2) adding 20% ferrous sulfate solution into the metatitanic acid suspension, wherein the molar ratio of the nano metatitanic acid to the ferrous sulfate is 0.1:1, the reaction time is 5min under the stirring condition that the stirring speed is 50 revolutions per minute, and the solution is neutral after the reaction to generate nano metatitanic acid suspension;
(3) and (3) under the stirring condition that the rotating speed is 60 revolutions per minute, simultaneously adding an acid solution and a sodium silicate solution with the modulus of 2.5 into the metatitanic acid suspension obtained in the step (2), wherein the molar ratio of the metatitanic acid solution to the sodium silicate solution is 2:1, the reaction time is 100min, and after reaction, carrying out precipitation separation to obtain the nano ferrous metatitanic acid-silica gel particle Fenton catalyst.
Example 3: a preparation method of a nano ferrous metatitanate-silica gel particle Fenton catalyst comprises the following specific steps:
(1) preparation of suspension of metatitanic acid (hydrated titanium dioxide)
Adding nano metatitanic acid with the particle size of 40nm into water to prepare metatitanic acid suspension with the mass concentration of 30%;
(2) adding 30% ferrous sulfate solution into the metatitanic acid suspension, wherein the molar ratio of the nano metatitanic acid to the ferrous sulfate is 1:1, the reaction time is 30min under the stirring condition that the stirring speed is 100 revolutions per minute, and the solution is neutral after the reaction to generate the nano metatitanic acid suspension;
(3) and (3) under the stirring condition that the rotating speed is 30 revolutions per minute, simultaneously adding an acid solution and a sodium silicate solution with the modulus of 3.0 into the metatitanic acid suspension obtained in the step (2), wherein the molar ratio of the metatitanic acid solution to the sodium silicate solution is 5:1, the reaction time is 100min, and after the reaction, carrying out precipitation separation to obtain the nano ferrous metatitanic acid-silica gel particle Fenton catalyst.
Test example:
test example 1: after wastewater is treated by using the nano ferrous metatitanate-silica gel particle Fenton catalyst, the treatment conditions are shown in Table 1, wherein 1A is biochemical sewage before treatment, 1B is water treated by a neutralization tank of a conventional Fenton device (effluent of the neutralization tank of the Fenton pilot plant), and 1C is water treated by using the nano ferrous metatitanate-silica gel particle Fenton catalyst and adding hydrogen peroxide (the catalyst is repeatedly used). The COD detection data in the effluent is shown in Table 1:
TABLE 1
Case 1 Synthesis of pharmaceutical and chemical wastewater
A sewage treatment plant of a pharmaceutical chemical industry park of Hebei Shizhuang (sewage treatment plant of pharmaceutical chemical industry park, 70% of wastewater is pharmaceutical chemical industry wastewater): the Fenton fluidized bed advanced oxidation section improves the Fenton oxidation efficiency and reduces sludge discharge, before oxidation, the COD of the biochemical wastewater is 250-300mg/L, and the original Fenton fluidized bed process conditions are as follows: the dosage of the 98 percent sulfuric acid is 1.2kg/m3The dosage of the ferrous sulfate is 4kg/m3The dosage of the hydrogen peroxide is 5.25kg/m3The dosage of the liquid caustic soda is 10kg/m30.2% PAM solution 10L/m3The COD of the effluent index is 80mg/L, the chroma is 16 times, and the yield of Fenton sludge is 200g of absolute dry sludge; by adopting the catalyst, the mass ratio of COD in the wastewater to the nano ferrous metatitanate-silica gel particle Fenton catalyst is 1:10, 30% of hydrogen peroxide is added in a stirring state, the mass ratio of the COD in the wastewater to the 30% of hydrogen peroxide is 1:1.5, the recovery rate of the catalyst is 100%, sulfuric acid, ferrous sulfate, liquid alkali and PAM are not required to be added, the COD of an effluent index is 70mg/L, the chroma is 8 times, and no sludge is generated.
Case 2-synthetic wastewater treatment plant of certain dye park in Shandong
COD of biochemical wastewater before oxidation in a conventional Fenton advanced oxidation section is 150-: the dosage of the 98 percent sulfuric acid is 1.0kg/m3The dosage of the ferrous sulfate is 3kg/m3Hydrogen peroxide solutionThe dosage is 3kg/m3The dosage of the liquid caustic soda is 5.5kg/m30.2% PAM solution 10L/m3The COD of the effluent index is 50mg/L, the chroma is 16 times, and the yield of Fenton sludge is 200g of absolute dry sludge; by adopting the catalyst, the mass ratio of COD in the wastewater to the nano ferrous metatitanate-silica gel particle Fenton catalyst is 1:5, 30% of hydrogen peroxide is added in a stirring state, the mass ratio of the COD in the wastewater to the 30% of hydrogen peroxide is 1:1.2, the recovery rate of the catalyst is 100%, sulfuric acid, ferrous sulfate, liquid alkali and PAM are not required to be added, the COD of an effluent index is 40mg/L, the chroma is 8 times, and no sludge is generated.
Claims (8)
1. A preparation method of a nano ferrous metatitanate-silica gel particle Fenton catalyst is characterized by comprising the following steps: preparing nano metatitanic acid into suspension, adding a ferrous sulfate solution into the suspension, and then carrying out a silicagel reaction with a sodium silicate solution under an acidic condition to obtain the nano ferrous metatitanic acid-silica gel particle Fenton catalyst.
2. The preparation method according to claim 1, comprising the following steps:
(1) preparation of metatitanic acid suspension
Adding nano metatitanic acid with the particle size of 20-40nm into water to prepare metatitanic acid suspension with the mass concentration of 10-30%;
(2) adding 10-30% ferrous sulfate solution into metatitanic acid suspension, wherein the molar ratio of nano metatitanic acid to ferrous sulfate is 0.1-1:1, the reaction time is 1-30min under the stirring condition that the stirring speed is 50-100 r/min, and the solution is neutral after the reaction to generate nano metatitanic acid suspension;
(3) and (3) under the stirring condition that the rotating speed is 20-200 revolutions per minute, simultaneously adding an acid solution and a sodium silicate solution with the modulus of 1.1-4 into the nano ferrous metatitanate suspension obtained in the step (2), wherein the molar ratio of the ferrous metatitanate solution to the sodium silicate solution is 1.5-3:1, the reaction time is 10-300min, and the solution is neutral after the reaction, so that the nano ferrous metatitanate-silica particle Fenton catalyst is obtained.
3. The production method according to claim 2, wherein in the step (1), the nano metatitanic acid having a particle size of 30nm is added to water to produce a suspension of metatitanic acid having a mass concentration of 20%.
4. The preparation method according to claim 2, wherein in the step (2), a 20% ferrous sulfate solution is added to the metatitanic acid suspension, the molar ratio of the nano-metatitanic acid to the ferrous sulfate is 0.5:1, the reaction time is 15min under the stirring condition that the stirring speed is 50 r/min, and the solution is neutral after the reaction, so that the nano-metatitanic acid suspension is generated.
5. The preparation method according to claim 2, wherein an acid solution and a sodium silicate solution with a modulus of 2.5 are simultaneously added to the metatitanic acid suspension of step (2) in step (3), the molar ratio of the metatitanic acid solution to the sodium silicate solution is 2:1, the reaction time is 100min, and the precipitate is separated after the reaction.
6. The nano ferrous metatitanate-silica gel particle Fenton catalyst obtained by the preparation method according to any one of claims 1 to 5.
7. The method of using the nano ferrous metatitanate-silica gel particle Fenton catalyst according to claim 6, wherein the nano ferrous metatitanate-silica gel particle Fenton catalyst and hydrogen peroxide are added into the sewage to treat the sewage.
8. The use method according to claim 7, wherein the mass ratio of COD in the sewage, the nano ferrous metatitanate-silica gel particle Fenton catalyst and 30% hydrogen peroxide is 1: 2-10: 1.2-1.5.
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| EP2698196A1 (en) * | 2011-03-30 | 2014-02-19 | Kolesnik, Viktor Grigorjevich | Method for obtaining silicon and titanium by generating electromagnetic interactions between sio2 and fetio3 particles and magnetic waves |
| WO2018095124A1 (en) * | 2016-11-25 | 2018-05-31 | 中冶赛迪工程技术股份有限公司 | Method and system for decarbonization, decolorization, and decyanation in deep treatment of coking wastewater |
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| US4289655A (en) * | 1980-05-27 | 1981-09-15 | Exxon Research & Engineering Co. | Magnetic catalysts and their preparation |
| EP1924525A1 (en) * | 2005-09-15 | 2008-05-28 | Battelle Memorial Institute | Photolytic generation of hydrogen peroxide |
| CN100560517C (en) * | 2007-08-10 | 2009-11-18 | 南京大学 | A kind of method of preprocessing coking wastewater by electrochemical oxidation flocculating composite technique |
| CN102626627A (en) * | 2012-03-26 | 2012-08-08 | 南京大学 | Preparation method of activated carbon supported ferrous heterogeneous Fenton's reagent oxidation catalyst |
| CN108404914B (en) * | 2018-04-13 | 2019-08-23 | 哈尔滨工业大学 | A kind of redox graphene cladding iron titanate composite catalyzing material and its preparation method and application |
| CN110075819B (en) * | 2019-01-22 | 2022-03-18 | 成都千砺金科技创新有限公司 | Production method of self-fitting nano catalytic sewage treatment agent |
| US11638911B2 (en) * | 2019-02-19 | 2023-05-02 | University Of Connecticut | Mesoporous metal titanates as multifunctional catalysts |
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| EP2698196A1 (en) * | 2011-03-30 | 2014-02-19 | Kolesnik, Viktor Grigorjevich | Method for obtaining silicon and titanium by generating electromagnetic interactions between sio2 and fetio3 particles and magnetic waves |
| WO2018095124A1 (en) * | 2016-11-25 | 2018-05-31 | 中冶赛迪工程技术股份有限公司 | Method and system for decarbonization, decolorization, and decyanation in deep treatment of coking wastewater |
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