CN113000028A - Preparation method of adsorbent for recovering phosphoric acid in waste acid - Google Patents
Preparation method of adsorbent for recovering phosphoric acid in waste acid Download PDFInfo
- Publication number
- CN113000028A CN113000028A CN202110460831.7A CN202110460831A CN113000028A CN 113000028 A CN113000028 A CN 113000028A CN 202110460831 A CN202110460831 A CN 202110460831A CN 113000028 A CN113000028 A CN 113000028A
- Authority
- CN
- China
- Prior art keywords
- solution
- silica gel
- deionized water
- acid
- stirring
- 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
Images
Classifications
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
- C01B25/234—Purification; Stabilisation; Concentration
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
A preparation method of an adsorbent for recovering phosphoric acid in waste acid comprises the following steps: s1, activated silica gel: activating the silica gel microspheres for later use; s2, immersing the activated silica gel into an aminosilane solution, refluxing for a period of time, cleaning with an organic solvent and deionized water to remove residual silane, and drying; s3, soaking the material obtained in the step S2 in deionized water, then adding propylmalonic acid, and stirring uniformly at room temperature to obtain a solution A; preparing an aqueous solution of zirconium oxychloride octahydrate with a certain concentration, adding a small amount of ammonium persulfate serving as an initiator and N, N' -methylene bisacrylamide serving as a cross-linking agent, and uniformly stirring to obtain a solution B; and (3) bubbling the S4, the solution A and the solution B respectively by using N2 airflow, then dropwise adding the solution A into the solution B, magnetically stirring for a period of time under the atmosphere of N2, taking out, washing by using deionized water, and drying. The adsorbent has high adsorption capacity, high selectivity, easy regeneration capacity and high cyclicity, and is effectively used for treating the phosphorus-containing waste acid.
Description
Technical Field
The invention relates to the technical field of preparation of adsorbents for recovering phosphoric acid in waste acid.
Background
As is known, a large amount of phosphorus-containing waste acid is generated on the surface of an aluminum material after cleaning, and mainly comprises 10-40% of phosphoric acid, 5-20% of sulfuric acid, 1-5% of aluminum ions and a small amount of heavy metal ions, and if the waste acid is directly discharged, not only is environmental pollution caused, but also resource waste is caused. For the waste acid, the traditional treatment method is neutralization precipitation, i.e. neutralization precipitation is carried out by using calcium hydroxide or other precipitator. But not only can generate a large amount of sludge hazardous waste in the sedimentation process, but also causes huge waste of phosphorus resources; not only increases the post-treatment cost and the profit of the enterprise to be reduced, but also causes secondary pollution. There is therefore still a need for a more efficient method of treatment
The adsorption method is a green and environment-friendly process method, has the advantages of convenience in operation, simple equipment and the like, but the existing commercial phosphorus adsorbent generally has the problems of small adsorption capacity, low selectivity, difficulty in recycling, high cost and the like.
Disclosure of Invention
The invention aims to prepare an adsorbent for recovering phosphoric acid in waste acid, which has high adsorption capacity, high selectivity, easy regeneration capacity and high cyclicity, and can be effectively used for treating the phosphorus-containing waste acid.
A preparation method of an adsorbent for recovering phosphoric acid in waste acid comprises the following steps:
s1, activated silica gel: activating the silica gel microspheres for later use;
s2, immersing the activated silica gel obtained in the step S1 into aminosilane solution, refluxing for 0.5-6h, cleaning with an organic solvent and deionized water to remove residual silane, and drying;
s3, soaking the material obtained in the step S2 in deionized water, then adding propylmalonic acid, and stirring uniformly at room temperature to obtain a solution A; preparing 10-200 mass percent of zirconium oxychloride octahydrate aqueous solution, adding 0.1-10ml of ammonium persulfate serving as an initiator and N, N' -methylene bisacrylamide serving as a cross-linking agent, and uniformly stirring to obtain solution B;
s4, solution A and solution B are respectively N2The gas stream is bubbled and treatedThen adding the solution A into the solution B drop by drop at N2And magnetically stirring for 0.2-3h in the atmosphere, taking out, washing with deionized water, and drying.
Preferably, the aminosilane solution of the present invention is at least one of aminopropyl-3-methoxysilane, aminopropyl-triethoxysilane, N- (aminoethyl) - γ -aminopropylmethyltrimethoxysilane, N- (aminoethyl) - γ -aminopropylmethyldimethoxysilane or N- (aminoethyl) - γ -aminopropylmethyldiethoxysilane.
Preferably, the organic solvent of the present invention is at least one of ethanol, methanol, acetone, isopropanol or petroleum ether.
By adopting the technical scheme, compared with the prior art, the invention has the following advantages:
1. according to the invention, the porous silica gel microspheres are used as carriers, and the specific surface area of the porous silica gel microspheres is large, so that more adsorption sites can be formed, and the adsorption capacity of the adsorbent is increased; and the mechanical strength is high, the wear resistance and the acid resistance are good, and the service life is longer.
2. The invention prepares the adsorbing material by the bonding method, has stable property and is not easy to lose.
3. Nowadays, organic resin is used as a carrier in most cases, but the organic resin is a high molecular material, and the resin is difficult to recycle after being used and failed; the silica gel microspheres used in the invention are inorganic materials, so that the subsequent recovery treatment is more convenient.
Drawings
FIG. 1 is a schematic diagram showing the effect of interfering ions on phosphorus adsorption at different concentrations.
Detailed Description
A preparation method of an adsorbent for recovering phosphoric acid in waste acid comprises the following steps:
s1, activated silica gel: activating the silica gel microspheres for later use;
s2, immersing the activated silica gel obtained in the step S1 into aminosilane solution, refluxing for 0.5-6h, cleaning with an organic solvent and deionized water to remove residual silane, and drying;
s3, soaking the material obtained in the step S2 in deionized water, then adding propylmalonic acid, and stirring uniformly at room temperature to obtain a solution A; preparing 10-200 mass percent of zirconium oxychloride octahydrate aqueous solution, adding 0.1-10ml of ammonium persulfate serving as an initiator and N, N' -methylene bisacrylamide serving as a cross-linking agent, and uniformly stirring to obtain solution B;
s4, solution A and solution B are respectively N2A gas-flow bubbling treatment, and then dropwise adding the solution A into the solution B at N2And magnetically stirring for 0.2-3h in the atmosphere, taking out, washing with deionized water, and drying.
The aminosilane solution is at least one of aminopropyl-3-methoxysilane, aminopropyl-triethoxysilane, N- (aminoethyl) -gamma-aminopropyl methyl trimethoxysilane, N- (aminoethyl) -gamma-aminopropyl methyl dimethoxysilane or N- (aminoethyl) -gamma-aminopropyl methyl diethoxysilane.
The organic solvent is at least one of ethanol, methanol, acetone, isopropanol or petroleum ether.
Example 1
1. 10g of silica gel microspheres are taken and treated for 10h at 100 ℃ for activation.
2. Soaking the activated silica gel in 0.2% aminopropyl-3-methoxysilane/ethanol solution, refluxing at 60 deg.C for 12 hr, washing with ethanol and deionized water, and oven drying.
3. The material obtained in step 2 was immersed in 50ml of deionized water, followed by addition of 5g of propylmalonic acid and stirring at room temperature to obtain solution A. 100ml of 3 percent zirconium oxychloride octahydrate aqueous solution is prepared, 0.5g of ammonium persulfate serving as an initiator and 0.3g N, N' -methylene bisacrylamide serving as a cross-linking agent are added, and the mixture is uniformly stirred to obtain solution B.
4. Using N for solution A and solution B respectively2A gas-flow bubbling treatment, and then dropwise adding the solution A into the solution B at N2And magnetically stirring for a period of time in the atmosphere, taking out, washing with deionized water, and drying.
Example 2
1. 50g of silica gel microspheres are taken and activated for 5 hours in 5mol/L hydrochloric acid solution.
2. Soaking the activated silica gel in a 3% aminopropyl-3-methoxysilane/methanol solution, refluxing for 6h at 50 ℃, then respectively washing with ethanol and deionized water, and drying.
3. The material obtained in step 2 was immersed in 300ml of deionized water, followed by addition of 15g of propylmalonic acid and stirring at room temperature to obtain solution A. 100ml of 10 percent zirconium oxychloride octahydrate aqueous solution is prepared, 2.5g of ammonium persulfate serving as an initiator and 1g N, N' -methylene bisacrylamide serving as a cross-linking agent are added, and the mixture is uniformly stirred to obtain solution B.
4. Using N for solution A and solution B respectively2A gas-flow bubbling treatment, and then dropwise adding the solution A into the solution B at N2And magnetically stirring for a period of time in the atmosphere, taking out, washing with deionized water, and drying.
Example 3
1. Activating silica gel: 5g of silica gel microspheres were treated at 60 ℃ for 20h for activation.
2. Soaking the activated silica gel in a 5% aminopropyl-3-ethoxysilane/acetone solution, refluxing for 20h at room temperature, respectively washing with ethanol and deionized water, and drying.
3. The material obtained in step 2 was immersed in 50ml of deionized water, followed by addition of 2g of propylmalonic acid and stirring at room temperature to obtain solution A. 50ml of 3 percent zirconium oxychloride octahydrate aqueous solution is prepared, 0.2g of ammonium persulfate serving as an initiator and 0.1g N, N' -methylene bisacrylamide serving as a cross-linking agent are added, and the mixture is uniformly stirred to obtain solution B.
4. Using N for solution A and solution B respectively2A gas-flow bubbling treatment, and then dropwise adding the solution A into the solution B at N2And magnetically stirring for a period of time in the atmosphere, taking out, washing with deionized water, and drying.
Example 4
1. Activating silica gel: 20g of silica gel microspheres were treated at 130 ℃ for 6h for activation.
2. Soaking activated silica gel in 0.5% N- (aminoethyl) -gamma-aminopropyl methyl trimethoxy silane/petroleum ether solution, refluxing at room temperature for 20 hr, washing with ethanol and deionized water, and oven drying.
3. The material obtained in step 2 was immersed in 200ml of deionized water, followed by addition of 10g of propylmalonic acid and stirring at room temperature to obtain solution A. 50ml of 10 percent zirconium oxychloride octahydrate aqueous solution is prepared, 1g of ammonium persulfate serving as an initiator and 0.3g N, N' -methylene bisacrylamide serving as a cross-linking agent are added, and the mixture is uniformly stirred to obtain solution B.
4. Using N for solution A and solution B respectively2A gas-flow bubbling treatment, and then dropwise adding the solution A into the solution B at N2And magnetically stirring for a period of time in the atmosphere, taking out, washing with deionized water, and drying.
Example 5
1. Activating silica gel: 10g of silica gel microspheres are activated in 3mol/L hydrochloric acid solution for 1 hour.
2. Soaking activated silica gel in 5% N- (aminoethyl) -gamma-aminopropyl methyl diethoxy silane/isopropanol solution, refluxing at 50 deg.C for 12 hr, washing with ethanol and deionized water, and oven drying.
3. The material obtained in step 2 was immersed in 100ml of deionized water, followed by addition of 6g of propylmalonic acid and stirring at room temperature to obtain solution A. 50ml of 10 percent zirconium oxychloride octahydrate aqueous solution is prepared, 1g of ammonium persulfate serving as an initiator and 0.6g N, N' -methylene bisacrylamide serving as a cross-linking agent are added, and the mixture is uniformly stirred to obtain solution B.
4. Using N for solution A and solution B respectively2A gas-flow bubbling treatment, and then dropwise adding the solution A into the solution B at N2And magnetically stirring for a period of time in the atmosphere, taking out, washing with deionized water, and drying.
FIG. 1 is a schematic diagram showing the effect of interfering ions on phosphorus adsorption at different concentrations. The following table shows the statistical results of the adsorption capacities of different adsorbents for phosphorus.
Claims (3)
1. A preparation method of an adsorbent for recovering phosphoric acid in waste acid is characterized by comprising the following steps:
s1, activated silica gel: activating the silica gel microspheres for later use;
s2, immersing the activated silica gel obtained in the step S1 into aminosilane solution, refluxing for 0.5-6h, cleaning with an organic solvent and deionized water to remove residual silane, and drying;
s3, soaking the material obtained in the step S2 in deionized water, then adding propylmalonic acid, and stirring uniformly at room temperature to obtain a solution A; preparing 10-200 mass percent of zirconium oxychloride octahydrate aqueous solution, adding 0.1-10ml of ammonium persulfate serving as an initiator and N, N' -methylene bisacrylamide serving as a cross-linking agent, and uniformly stirring to obtain solution B;
s4, solution A and solution B are respectively N2A gas-flow bubbling treatment, and then dropwise adding the solution A into the solution B at N2And magnetically stirring for 0.2-3h in the atmosphere, taking out, washing with deionized water, and drying.
2. The method as claimed in claim 1, wherein the aminosilane solution is at least one selected from aminopropyl-3-methoxysilane, aminopropyl-triethoxysilane, N- (aminoethyl) - γ -aminopropylmethyltrimethoxysilane, N- (aminoethyl) - γ -aminopropylmethyldimethoxysilane and N- (aminoethyl) - γ -aminopropylmethyldiethoxysilane.
3. The method according to claim 1, wherein the organic solvent is at least one of ethanol, methanol, acetone, isopropanol, and petroleum ether.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110460831.7A CN113000028A (en) | 2021-04-27 | 2021-04-27 | Preparation method of adsorbent for recovering phosphoric acid in waste acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110460831.7A CN113000028A (en) | 2021-04-27 | 2021-04-27 | Preparation method of adsorbent for recovering phosphoric acid in waste acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113000028A true CN113000028A (en) | 2021-06-22 |
Family
ID=76380604
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110460831.7A Pending CN113000028A (en) | 2021-04-27 | 2021-04-27 | Preparation method of adsorbent for recovering phosphoric acid in waste acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113000028A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113893827A (en) * | 2021-11-18 | 2022-01-07 | 苏州博萃循环科技有限公司 | Fluorine adsorption material and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1354357A (en) * | 1970-05-22 | 1974-06-05 | Du Pont | Chromatographic packing with chemically bonded organic stationary phases |
| CN1817444A (en) * | 2006-01-06 | 2006-08-16 | 青岛科技大学 | Production of silica-gel carried dye affinity substrate and use thereof |
| CN103877941A (en) * | 2014-03-20 | 2014-06-25 | 浙江大学 | Spherical silicon-based organic-inorganic hybrid boron adsorbent and preparation method thereof |
| CN108079974A (en) * | 2017-12-26 | 2018-05-29 | 珠海健帆生物科技股份有限公司 | A kind of preparation method and adsorbent equipment of western blot polymeric sorbent |
| CN110339825A (en) * | 2019-07-25 | 2019-10-18 | 杭州电子科技大学 | A kind of adsorbent and preparation method thereof suitable for textile printing and dyeing wastewater processing |
-
2021
- 2021-04-27 CN CN202110460831.7A patent/CN113000028A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1354357A (en) * | 1970-05-22 | 1974-06-05 | Du Pont | Chromatographic packing with chemically bonded organic stationary phases |
| CN1817444A (en) * | 2006-01-06 | 2006-08-16 | 青岛科技大学 | Production of silica-gel carried dye affinity substrate and use thereof |
| CN103877941A (en) * | 2014-03-20 | 2014-06-25 | 浙江大学 | Spherical silicon-based organic-inorganic hybrid boron adsorbent and preparation method thereof |
| CN108079974A (en) * | 2017-12-26 | 2018-05-29 | 珠海健帆生物科技股份有限公司 | A kind of preparation method and adsorbent equipment of western blot polymeric sorbent |
| CN110339825A (en) * | 2019-07-25 | 2019-10-18 | 杭州电子科技大学 | A kind of adsorbent and preparation method thereof suitable for textile printing and dyeing wastewater processing |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113893827A (en) * | 2021-11-18 | 2022-01-07 | 苏州博萃循环科技有限公司 | Fluorine adsorption material and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107597071B (en) | Preparation method of grafted magnetic chitosan adsorbent | |
| CN108246269B (en) | Lithium ion adsorbent and preparation method and application thereof | |
| CN112755972B (en) | Preparation of silicon-based resin and application of silicon-based resin as defluorination adsorbent | |
| CN106914222B (en) | Adsorbent for removing liquid-phase mercury and preparation method and use method thereof | |
| CN103877943A (en) | Activated carbon supported nano copper desulfurizing agent and preparation method and application thereof | |
| CN111330553A (en) | Preparation method and application of MCS/SA @ PEI composite hydrogel ball | |
| CN113000028A (en) | Preparation method of adsorbent for recovering phosphoric acid in waste acid | |
| CN112516968A (en) | Preparation method of metal organic framework material loaded modified diatomite adsorbent | |
| CN109126743A (en) | A kind of preparation method of polyurethane foam adsorbent material | |
| CN114057193A (en) | Nitrogen-doped activated carbon-based desulfurizer as well as preparation method and application thereof | |
| CN103695654A (en) | Method for recovering rare earth from low-concentration rare-earth solution by using loaded chitosan | |
| CN111203197A (en) | Adsorbing material based on epoxy and amino crosslinking and preparation method thereof | |
| CN113877550B (en) | Preparation method of polymeric adsorbent for boron element in water phase | |
| CN111995025A (en) | Macromolecular heavy metal chelating agent for treating nickel-complex-containing wastewater and preparation method thereof | |
| CN102500338A (en) | PFOA (perfluorooctanoic acid) adsorbent and preparation method thereof | |
| CN104549172B (en) | Method for preparing sulfydryl-modified chitosan short hole microspheres | |
| CN112717892A (en) | Copper-removing adsorbent for purifying cobalt-nickel electrolyte and preparation method thereof | |
| CN113304730A (en) | Preparation method of special adsorbent for cobalt recovery in waste ternary batteries | |
| CN113134340A (en) | Chromium ion adsorbent, preparation method, application method and regeneration method thereof, and treatment method of chromium in leather tail water | |
| CN108940225B (en) | Preparation method and application of sodium alginate/amino mesoporous silica gel spheres for low-concentration uranium-containing wastewater treatment | |
| CN110732311A (en) | crosslinked chitosan coated MoS2Adsorbent, preparation method and application thereof | |
| CN109201015B (en) | Surface imprinting Fe3+ potassium tetratitanate whisker adsorbent and preparation method thereof | |
| CN109384872B (en) | Chelate resin and preparation method and application thereof | |
| CN114177898A (en) | Low-temperature thermal regeneration and solvent regeneration-ultrasonic wave/persulfate regeneration coupled powdered activated carbon composite regeneration method | |
| CN110201647B (en) | Poly-pyrrole-2, 5-di (polyalcohol methane) adsorbent and preparation method thereof |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210622 |
|
| RJ01 | Rejection of invention patent application after publication |