CN111333741A - High molecular compound dechlorinating agent and preparation method thereof - Google Patents
High molecular compound dechlorinating agent and preparation method thereof Download PDFInfo
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- CN111333741A CN111333741A CN202010139748.5A CN202010139748A CN111333741A CN 111333741 A CN111333741 A CN 111333741A CN 202010139748 A CN202010139748 A CN 202010139748A CN 111333741 A CN111333741 A CN 111333741A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/18—Oxidised starch
- C08B31/185—Derivatives of oxidised starch, e.g. crosslinked oxidised starch
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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
- 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
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
Abstract
The invention provides a preparation method of a metal aluminum complex dechlorinating agent, which comprises the following steps: s1 preparation of oxidized starch: heating starch and water in water for gelatinization, adding a catalyst, adding an oxidant for reaction, separating out a precipitate by using absolute ethyl alcohol after the reaction is finished, carrying out centrifugal filtration, and drying the obtained product for 24 hours to obtain oxidized starch; s2 preparation of oxidized starch metal complex dechlorinating agent: and (4) mixing the oxidized starch prepared in the step (S1) with aluminum sulfate, adding water to dissolve the mixture, adjusting the pH value, placing the solution in a water bath constant temperature oscillator to perform constant temperature reaction, and drying the mixture after the reaction is finished to obtain the dechlorinating agent. The dechlorinating agent prepared by the method utilizes the coordination of aluminum ions and compounds containing hydroxyl and carboxyl to form a stable polynuclear aluminum complex, and can greatly improve the removal efficiency of the chloride ions due to the positive charges.
Description
Technical Field
The invention belongs to the field of environment-friendly water treatment, and particularly relates to a high-molecular aluminum ion complex dechlorinating agent and a green preparation method thereof.
Background
Circulating water and produced wastewater in industrial production often contain chloride ions with negative charges, such as power plant desulfurization wastewater, polysilicon production wastewater, non-ferrous metal smelting production wastewater and the like all contain high-concentration chloride ions, the concentration of the chloride ions is even up to 5000-.
At present, with the stricter environmental protection requirements, in the major trends of continuously strengthening upgrading and reconstructing industrial technology and greatly advocating energy conservation and emission reduction, the traditional industrial wastewater dechlorination method comprises a chemical precipitation method, a membrane separation method, an electrochemical method, an ion exchange method, a traditional flocculation precipitation method and the like, but cannot meet the industrial requirements due to the easily generated secondary environmental pollution, high energy consumption, high cost and the like.
Because natural polymers are nontoxic, cheap, abundant and degradable, the flocculant is widely used in water treatment. However, when the method is applied to removing chloride ions, the removal efficiency is not high. The results of examining the dechlorination effect of the polymer dechlorinating agent mainly containing methoxyl, hydroxyl and carbonyl show that the dechlorinating agent has the dechlorinating rate of about 50 percent when the concentration of the chloride ions is 500mg/L and the dosage of the dechlorinating agent is 20 g/L; when the dosage of the dechlorinating agent is increased to 50g/L, the removal rate of the chloride ions is only 60% (CHENYU QING, Zhan Sheng Han, adsorption mechanism of the high-molecular dechlorinating agent to the chloride ions in water [ J ] chemical environmental protection, 2018,38 (2): 185-.
The complex formed by the modified natural polymer with long carbon chain and the metallic aluminum has multiple functions of bonding bridging, compressing double electric layers, electric neutralization and electrostatic clustering, is applied to dechlorination of industrial wastewater, has excellent adsorption effect on chloride ions, does not cause secondary environmental pollution, and can greatly reduce the treatment cost.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a metal aluminum complex dechlorinating agent and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: the metal aluminum complex dechlorination agent is characterized by being prepared from the following raw materials: the catalyst comprises starch, a catalyst, an oxidant and aluminum sulfate, wherein the mass ratio of the starch to the aluminum sulfate is 2-5: 1.
Preferably, the catalyst is ferrous sulfate, ferrous ammonium sulfate or ammonium metavanadate.
Preferably, the oxidant is hydrogen peroxide or concentrated nitric acid.
The invention also provides a preparation method of the metal aluminum complex dechlorinating agent, which comprises the following steps:
s1 preparation of oxidized starch: heating starch and water in water for gelatinization, adding a catalyst, adding an oxidant for reaction, separating out a precipitate by using absolute ethyl alcohol after the reaction is finished, carrying out centrifugal filtration, and drying the obtained product for 24 hours to obtain oxidized starch;
s2 preparation of oxidized starch metal complex dechlorinating agent: and (4) mixing the oxidized starch prepared in the step (S1) with aluminum sulfate, adding water to dissolve the mixture, adjusting the pH value, placing the solution in a water bath constant temperature oscillator to perform constant temperature reaction, and drying the mixture after the reaction is finished to obtain the dechlorinating agent.
Preferably, the mass ratio of the starch to the water is 1: 3-12.
Preferably, the gelatinization temperature in the step S1 is 30-70 ℃, and the gelatinization time is 0.5-1 h.
Preferably, the catalyst in step S1 is ferrous sulfate, ammonium ferrous sulfate or ammonium metavanadate; wherein when ferrous sulfate or ferrous sulfate is used, the dosage of the ferrous sulfate or ferrous sulfate is 1.8 percent of the starch; when ammonium metavanadate is used, the amount thereof is 0.15% of the starch.
Preferably, the oxidant in step S1 is hydrogen peroxide or concentrated nitric acid, wherein when hydrogen peroxide is used, the amount of hydrogen peroxide is 40% of that of starch; concentrated nitric acid was used in an amount of 1.4 times the mass of the starch.
Preferably, the mass ratio of the oxidized starch to the aluminum sulfate in the step S2 is 2-5: 1.
Compared with the prior art, the invention has the following beneficial effects:
1. the dechlorinating agent of the invention utilizes the coordination of aluminum ions and compounds containing hydroxyl and carboxyl to form stable polynuclear aluminum complexes, and can greatly improve the removal efficiency of the chloride ions due to the positive charges.
2. The dechlorinating agent has large adsorption capacity and high treatment efficiency, and is widely suitable for treating industrial wastewater and circulating water with various chloride ion concentrations: the adsorption capacity to chloride ions is up to 30-40mg/g, and the dosage can be adjusted according to the concentration of chloride ions in the wastewater and the treatment requirement.
3. The dechlorination agent disclosed by the invention is green and environment-friendly, and has the advantages of rich raw material sources and low cost. The dechlorinating agent is obtained by modifying natural polymers, is nontoxic and easy to degrade, and can reduce the difficulty of subsequent sludge treatment and reduce the cost of sludge treatment.
Drawings
FIG. 1 is a schematic diagram of an oxidized starch reaction.
FIG. 2 is a schematic diagram of the molecular formula of an alumina starch complex
Detailed Description
In order to more concisely and clearly demonstrate technical solutions, objects and advantages of the present invention, the present invention will be further described in detail with reference to specific embodiments.
Example 1
(1) Preparation of oxidized starch-carboxyl starch
Heating and stirring starch and water in a water bath according to a mass ratio of 1:10 for gelatinization, wherein the water bath heating gelatinization temperature is 70 ℃, and the gelatinization time is 0.5-1 h. Then adjusting the temperature of the water bath to 55 ℃, adding a catalyst ferrous sulfate or ferrous ammonium sulfate (the dosage is 1.8 percent of the starch), after stirring uniformly, slowly adding hydrogen peroxide (the dosage is 40 percent of the starch) to react for 1.5 hours. And (3) after the reaction is finished, precipitating with absolute ethyl alcohol, rinsing with absolute ethyl alcohol for 3-4 times, centrifuging, filtering, and drying the obtained product at 50-60 ℃ for 24 hours to obtain the oxidized starch.
(2) Preparation of chloride remover of oxidized starch metal complex
Putting the oxidized starch prepared in the step (1) and aluminum sulfate into a container according to the mass ratio of 3:1, adding a proper amount of water to fully dissolve the oxidized starch and the aluminum sulfate, and adjusting the pH of the solution to 2.5 by using diluted sulfuric acid; then placing the conical flask in a water bath constant temperature oscillator for constant temperature reaction at 30 ℃ for 24 hours; after the reaction is finished, transferring the reaction product to a rotary evaporator to be dried by distillation at 70 ℃, and drying the reaction product in a vacuum drying oven at 80 ℃ to obtain the dechlorinating agent.
NaCl is used for preparing a solution with the chloride ion concentration of 2000mg/L, the dechlorinating agent prepared in the embodiment is added according to the dosage of 50g/L, the solution is shaken at 150rpm and 30 ℃ in a constant temperature oscillator for 40mim, the chloride ion concentration in a water sample is determined to be 386mg/L by a silver nitrate method, and the removal rate of the chloride ions is 80.7 percent.
Example 2
(1) Preparation of oxidized starch-carboxyl starch
The starch and the water are heated and stirred in a water bath according to the mass ratio of 1:3 for gelatinization, the water bath heating gelatinization temperature is 30 ℃, and the gelatinization time is 0.5 h. Keeping the temperature unchanged, adding catalyst ammonium metavanadate (the dosage is 0.15 percent of the starch), after stirring uniformly, slowly adding oxidant concentrated nitric acid (the dosage is 1.4 times of the starch) for reacting for 8 hours. And (3) after the reaction is finished, precipitating with absolute ethyl alcohol, rinsing with absolute ethyl alcohol for 3-4 times, centrifuging, filtering, and drying the obtained product at 50-60 ℃ for 24 hours to obtain the oxidized starch.
(2) Preparation of chloride remover of oxidized starch metal complex
Putting the oxidized starch prepared in the step (1) and aluminum sulfate into a container according to the mass ratio of 3:1, adding a proper amount of water to fully dissolve the oxidized starch and the aluminum sulfate, and adjusting the pH of the solution to 2.5 by using diluted sulfuric acid; then placing the conical flask in a water bath constant temperature oscillator for constant temperature reaction at 30 ℃ for 24 hours; after the reaction is finished, transferring the reaction product to a rotary evaporator to be dried by distillation at 70 ℃, and drying the reaction product in a vacuum drying oven at 80 ℃ to obtain the dechlorinating agent.
NaCl is used for preparing a solution with the chloride ion concentration of 2000mg/L, the dechlorinating agent prepared in the embodiment is added according to the dosage of 50g/L, the solution is shaken at 150rpm and 30 ℃ in a constant temperature oscillator for 40mim, the chloride ion concentration in a water sample is measured to be 19mg/L by a silver nitrate method, and the removal rate of the chloride ions is 99.1 percent.
Example 3
(1) Preparation of oxidized starch-carboxyl starch
The starch and the water are heated and stirred in a water bath according to the mass ratio of 1:3 for gelatinization, the water bath heating gelatinization temperature is 30 ℃, and the gelatinization time is 0.5 h. Keeping the temperature unchanged, adding catalyst ammonium metavanadate (the dosage is 0.15 percent of the starch), after stirring uniformly, slowly adding oxidant concentrated nitric acid (the dosage is 1.4 times of the starch) for reacting for 8 hours. And (3) after the reaction is finished, precipitating with absolute ethyl alcohol, rinsing with absolute ethyl alcohol for 3-4 times, centrifuging, filtering, and drying the obtained product at 50-60 ℃ for 24 hours to obtain the oxidized starch.
(2) Preparation of chloride remover of oxidized starch metal complex
Putting the oxidized starch prepared in the step (1) and aluminum sulfate into a container according to the mass ratio of 2:1, adding a proper amount of water to fully dissolve the oxidized starch and the aluminum sulfate, and adjusting the pH of the solution to 2.5 by using diluted sulfuric acid; then placing the conical flask in a water bath constant temperature oscillator for constant temperature reaction at 30 ℃ for 24 hours; after the reaction is finished, transferring the reaction product to a rotary evaporator to be dried by distillation at 70 ℃, and drying the reaction product in a vacuum drying oven at 80 ℃ to obtain the dechlorinating agent.
NaCl is used for preparing a solution with the chloride ion concentration of 2000mg/L, the dechlorinating agent prepared in the embodiment is added according to the dosage of 50g/L, the solution is shaken at 150rpm and 30 ℃ in a constant temperature oscillator for 40mim, the chloride ion concentration in a water sample is measured to be 64mg/L by a silver nitrate method, and the removal rate of the chloride ions is 96.8 percent.
Example 4
(1) Preparation of oxidized starch-carboxyl starch
The starch and the water are heated and stirred in a water bath according to the mass ratio of 1:3 for gelatinization, the water bath heating gelatinization temperature is 30 ℃, and the gelatinization time is 0.5 h. Keeping the temperature unchanged, adding catalyst ammonium metavanadate (the dosage is 0.15 percent of the starch), after stirring uniformly, slowly adding oxidant concentrated nitric acid (the dosage is 1.4 times of the starch) for reacting for 8 hours. And (3) after the reaction is finished, precipitating with absolute ethyl alcohol, rinsing with absolute ethyl alcohol for 3-4 times, centrifuging, filtering, and drying the obtained product at 50-60 ℃ for 24 hours to obtain the oxidized starch.
(2) Preparation of chloride remover of oxidized starch metal complex
Putting the oxidized starch prepared in the step (1) and aluminum sulfate into a container according to the mass ratio of 5:1, adding a proper amount of water to fully dissolve the oxidized starch and the aluminum sulfate, and adjusting the pH of the solution to 2.5 by using diluted sulfuric acid; then placing the conical flask in a water bath constant temperature oscillator for constant temperature reaction at 30 ℃ for 24 hours; after the reaction is finished, transferring the reaction product to a rotary evaporator to be dried by distillation at 70 ℃, and drying the reaction product in a vacuum drying oven at 80 ℃ to obtain the dechlorinating agent.
NaCl is used for preparing a solution with the chloride ion concentration of 2000mg/L, the dechlorinating agent prepared in the embodiment is added according to the dosage of 50g/L, the solution is shaken at 150rpm and 30 ℃ in a constant temperature oscillator for 40mim, the chloride ion concentration in a water sample is measured by a silver nitrate method to be 220mg/L, and the removal rate of the chloride ions is 89%.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (9)
1. The metal aluminum complex dechlorination agent is characterized by being prepared from the following raw materials: the catalyst comprises starch, a catalyst, an oxidant and aluminum sulfate, wherein the mass ratio of the starch to the aluminum sulfate is 2-5: 1.
2. The metal aluminum complex dechlorination agent of claim 1 wherein the catalyst is ferrous sulfate, ferrous ammonium sulfate or ammonium metavanadate.
3. The metal aluminum complex dechlorination agent of claim 1, wherein the oxidant is hydrogen peroxide or concentrated nitric acid.
4. The preparation method of the metal aluminum complex dechlorinating agent is characterized by comprising the following steps of:
s1 preparation of oxidized starch: heating starch and water in a water bath for gelatinization, adding a catalyst, adding an oxidant for reaction, precipitating with absolute ethyl alcohol after the reaction is finished, performing centrifugal filtration, and drying the obtained product for 24 hours to obtain oxidized starch;
s2 preparation of oxidized starch metal complex dechlorinating agent: and (4) mixing the oxidized starch prepared in the step (S1) with aluminum sulfate, adding water to dissolve the mixture, adjusting the pH value, placing the solution in a water bath constant temperature oscillator to perform constant temperature reaction, and drying the mixture after the reaction is finished to obtain the dechlorinating agent.
5. The method according to claim 4, wherein the mass ratio of the starch to the water is 1: 3-12.
6. The method of claim 4, wherein the gelatinization temperature in step S1 is 30-70 ℃ and the gelatinization time is 0.5-1 h.
7. The method according to claim 4, wherein the catalyst in step S1 is ferrous sulfate, ammonium ferrous sulfate or ammonium metavanadate; wherein when ferrous sulfate or ferrous sulfate is used, the dosage of the ferrous sulfate or ferrous sulfate is 1.8 percent of the starch; when ammonium metavanadate is used, the amount thereof is 0.15% of the starch.
8. The preparation method according to claim 4, wherein the oxidant in step S1 is hydrogen peroxide or concentrated nitric acid, wherein the amount of hydrogen peroxide is 40% of the amount of starch when hydrogen peroxide is used; concentrated nitric acid was used in an amount of 1.4 times the mass of the starch.
9. The method according to claim 4, wherein the mass ratio of the oxidized starch to the aluminum sulfate in the step S2 is 2-5: 1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114349779A (en) * | 2021-12-29 | 2022-04-15 | 杜彪 | Modified silicon dioxide particle dechlorinating agent and preparation method and application thereof |
| CN114349887A (en) * | 2021-12-29 | 2022-04-15 | 杜彪 | Epoxy resin dechlorinating agent and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114349779A (en) * | 2021-12-29 | 2022-04-15 | 杜彪 | Modified silicon dioxide particle dechlorinating agent and preparation method and application thereof |
| CN114349887A (en) * | 2021-12-29 | 2022-04-15 | 杜彪 | Epoxy resin dechlorinating agent and preparation method and application thereof |
| CN114349887B (en) * | 2021-12-29 | 2023-06-13 | 智仑超纯环氧树脂(西安)有限公司 | Epoxy resin chlorine removing agent and preparation method and application thereof |
| CN114349779B (en) * | 2021-12-29 | 2023-09-26 | 智仑超纯环氧树脂(西安)有限公司 | Modified silicon dioxide particle chlorine removing agent and preparation method and application thereof |
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Address after: 510665 Guangzhou, Guangdong, Tianhe District Province Road West, No. 318 Patentee after: Institute of chemical engineering, Guangdong Academy of Sciences Address before: 510665 Guangzhou, Guangdong, Tianhe District Province Road West, No. 318 Patentee before: GUANGDONG RESEARCH INSTITITUTE OF PETROCHEMICAL AND FINE CHEMICAL ENGINEERING |