CN110975830A - AlO in aluminum profile processing wastewater2-Process for producing adsorbent for treatment - Google Patents
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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Abstract
The invention discloses AlO in aluminum profile processing wastewater2 ‑The preparation method of the adsorbent for treatment comprises the following specific preparation processes: adding the quaternized fibers into water, adding the modified diatomite into the quaternized fibers, uniformly stirring, adding p-toluenesulfonic acid into the quaternized fibers, heating to 250-260 ℃, performing reflux reaction for 14-15 hours, filtering, washing and drying to obtain the adsorbent. The adsorbent is prepared to adsorb metaaluminate ions in the wastewater, the adsorbent adsorbs the metaaluminate ions through physical adsorption and chemical adsorption, and the metaaluminate ions can be efficiently adsorbed and are efficiently adsorbed through the combined action of the adsorbent and the adsorbentThe adsorption capacity of the radical ions reaches 93.5mg/g, and after the metaaluminate radical ions are adsorbed, the residual sodium hydroxide in the wastewater can be reused, acid is not needed for neutralization, so that the cost is saved, the waste liquid is not needed to be discharged after neutralization, and the environmental pollution is avoided.
Description
Technical Field
The invention belongs to the field of wastewater treatment, and relates toAlO in aluminum profile processing wastewater2 -A preparation method of the adsorbent for treatment.
Background
In the aluminum profile processing process, a high-concentration sodium hydroxide solution is generally used for cleaning the aluminum alloy in the processing die cavity, metaaluminate ions are generated after the sodium hydroxide reacts with the aluminum in the aluminum alloy, the aluminum alloy is dissolved, further, the die is cleaned, the cleaned wastewater contains a large amount of sodium hydroxide and sodium metaaluminate, concentrated sulfuric acid is generally used for neutralization reaction with the sodium hydroxide in the waste liquid in the prior art, a high-concentration salt solution is formed and then discharged, the environmental pollution is easily caused, and the generation cost is increased by adding a large amount of acid.
Disclosure of Invention
The invention aims to provide AlO in aluminum profile processing wastewater2 -The preparation method of the treating adsorbent realizes the adsorption of metaaluminate ions in the wastewater by preparing the adsorbent, and the residual sodium hydroxide in the wastewater can be reused after the metaaluminate ions are adsorbed without neutralizing by acid, so that the cost is saved, and the waste liquid is discharged without neutralizing, thereby avoiding the environmental pollution.
The purpose of the invention can be realized by the following technical scheme:
AlO in aluminum profile processing wastewater2 -The preparation method of the adsorbent for treatment comprises the following specific preparation processes:
firstly, weighing a certain amount of diatomite and water, simultaneously adding the diatomite and the water into a reaction kettle, stirring to form a suspension, then adding an active coupling agent into the suspension, heating to 80-85 ℃, stirring to react for 3-4h, and then filtering, washing and drying to obtain modified diatomite; wherein, 0.13 to 0.15g of active coupling agent is added into each gram of diatomite; because the active coupling agent contains the oxysilane, the active coupling agent can react with hydroxyl on the surface of the diatomite, so that the active coupling agent is grafted on the surface of the diatomite, and a large amount of anhydride groups are introduced into the surface of the diatomite;
the preparation process of the active coupling agent is as follows: adding maleic anhydride and water into a reaction kettle simultaneously, adding azobisisobutyronitrile, heating to 80-90 ℃, stirring for reaction for 30-40min, dropwise adding 3-trimethoxy silane acrylic acid propyl ester, heating to 120-130 ℃ after complete dropwise addition, carrying out reflux reaction for 5-6h, and carrying out reduced pressure distillation to obtain an active coupling agent; wherein the ratio of the maleic anhydride to the 3-trimethoxy silane acrylic ester is 1: 1, and simultaneously adding 1.2-1.3g of azobisisobutyronitrile into each mole of 3-trimethoxy silane acrylic ester; the olefin group in the maleic anhydride and the olefin group in the 3-trimethoxy silane acrylic ester can carry out free radical polymerization reaction under the action of an initiator azodiisobutyronitrile, so that the prepared product contains both an oxysilane bond and an anhydride group;
step two, firstly, boiling cotton fibers in boiling water for 15-30min, then soaking the cotton fibers in a sodium hydroxide solution with the mass concentration of 15-18% for 2h, then washing the cotton fibers to be neutral, and then drying and storing the cotton fibers in the air to obtain pretreated cotton fibers;
step three, simultaneously adding diethylamine and epichlorohydrin into a reaction vessel, carrying out reflux reaction for 4-5h at 60-70 ℃, then adding pretreated cotton fiber and sodium hydroxide, heating to 100 ℃ and 110 ℃, carrying out reflux reaction for 9-10h, then washing to neutrality, and drying to obtain tertiary aminated cotton fiber; wherein the diethylamine and the epichlorohydrin are mixed according to the mass ratio of 1: 1, simultaneously adding 0.24-0.28g of ethylenediamine into each gram of pretreated cotton fibers, carrying out ring-opening reaction on amino in diethylamine and epoxy groups in epichlorohydrin to generate tertiary amino, simultaneously introducing alkyl chloride into a product, carrying out substitution reaction on the alkyl chloride and primary alcohol groups in the pretreated cotton fibers under an alkaline condition to introduce the tertiary amino into the pretreated cotton fibers,
fourthly, weighing a certain amount of benzyl chloride, adding the benzyl chloride into the ethanol solution, adding tertiary aminated cotton fiber into the ethanol solution, heating the mixture to 60-65 ℃, carrying out reflux reaction for 4-5 hours, and then filtering, washing and drying the mixture to obtain quaternized fiber; 0.18-0.21g of benzyl chloride is added into each gram of tertiary aminated cotton fiber, and tertiary amino in the tertiary aminated cotton fiber can react with the benzyl chloride to generate quaternary ammonium group;
fifthly, adding the quaternized fibers prepared in the fourth step into water, adding the modified diatomite prepared in the first step into the water, uniformly stirring, adding p-toluenesulfonic acid into the mixture, heating to 250-; wherein 0.49-0.53g of modified diatomite and 0.13g of p-toluenesulfonic acid are added into each gram of quaternized fibers; because the quaternized fibers contain a large amount of alcoholic hydroxyl groups, a large amount of anhydride groups are grafted on the surface of the modified diatomite, and the modified diatomite and the quaternized fibers can further react under the action of p-toluenesulfonic acid, so that the modified diatomite is grafted among the quaternized fibers and filled among the fibers, the prepared adsorbent contains a large amount of amino cations and can be adsorbed with meta-aluminate ions through the combination action of anions and cations, the surface of the modified diatomite contains a large amount of pore structures, the meta-aluminate ions can be adsorbed through the physical adsorption action, and the efficient adsorption of the meta-aluminate ions can be realized through the combined action of the amino cations and the meta-aluminate ions;
the prepared adsorbent is subjected to static adsorption experiment to determine the adsorption capacity, and the specific determination method comprises the following steps:
weighing a certain amount of sodium metaaluminate, adding the sodium metaaluminate into water to prepare a sodium metaaluminate solution with the concentration of 500mg/L, then weighing 200mL of the sodium metaaluminate solution, adding 10mg of prepared adsorbent into the sodium metaaluminate solution, oscillating the solution in an oscillation box at 30 ℃ for 2 hours, filtering the solution, adding 10mL of concentrated hydrochloric acid into the filtered solution, stirring and mixing the solution for 30 to 40min, then measuring the concentration of aluminum ions in the solution to be C1 through an atomic absorption spectrometer, and calculating the concentration of the aluminate ions in the adsorbed solution to be C1 through the measured concentration of the aluminum ionsThen calculating the adsorption amount of the adsorbentThe calculation shows that the adsorption amount of the adsorbent reaches 93.5 mg/g.
The invention has the beneficial effects that:
1. according to the method, the adsorbent is prepared to realize the adsorption of the metaaluminate ions in the wastewater, and after the metaaluminate ions are adsorbed, the residual sodium hydroxide in the wastewater can be reused again without being neutralized by acid, so that the cost is saved, the waste liquid is not discharged after being neutralized, and the environmental pollution is avoided.
2. The quaternized fibers prepared by the method contain a large amount of alcoholic hydroxyl groups, a large amount of anhydride groups are grafted on the surface of the modified diatomite, the modified diatomite and the modified diatomite can further react under the action of p-toluenesulfonic acid, so that the modified diatomite is grafted between the quaternized fibers, the modified diatomite is filled between the fibers, the prepared adsorbent contains a large amount of amino cations, the amino cations can be adsorbed with metaaluminate ions through the combination of anions and cations, the surface of the modified diatomite contains a large amount of pore structures, the metaaluminate ions can be adsorbed through the physical adsorption effect, the metaaluminate ions can be efficiently adsorbed through the combined action of the modified diatomite and the metaaluminate ions, and the adsorption capacity of the metaaluminate ions reaches 93.5 mg/g.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
AlO in aluminum profile processing wastewater2 -The preparation method of the adsorbent for treatment comprises the following specific preparation processes:
firstly, adding 9.8g of maleic anhydride and 50mL of water into a reaction kettle at the same time, then adding 0.12g of azobisisobutyronitrile into the reaction kettle, heating to 80-90 ℃, stirring for reaction for 30-40min, then dropwise adding 23.4g of 3-trimethoxy silane acrylic ester into the reaction kettle, heating to 120-130 ℃ after complete dropwise addition, carrying out reflux reaction for 5-6h, then carrying out reduced pressure distillation to obtain an active coupling agent, then weighing 1g of diatomite and 15mL of water into the reaction kettle at the same time, stirring to form a suspension, then adding 0.13g of the active coupling agent into the suspension, heating to 80-85 ℃, stirring for reaction for 3-4h, and then filtering, washing and drying to obtain modified diatomite;
step two, firstly, boiling cotton fibers in boiling water for 15-30min, then soaking the cotton fibers in a sodium hydroxide solution with the mass concentration of 15-18% for 2h, then washing the cotton fibers to be neutral, and then drying and storing the cotton fibers in the air to obtain pretreated cotton fibers;
step three, adding 7.3g of diethylamine and 9.3g of epichlorohydrin into a reaction vessel at the same time, carrying out reflux reaction for 4-5h at 60-70 ℃, then adding 30.4g of pretreated cotton fiber and 3.6g of sodium hydroxide, heating to 100 ℃ and 110 ℃, carrying out reflux reaction for 9-10h, then washing to neutrality, and drying to obtain tertiary aminated cotton fiber;
fourthly, weighing 1.8g of benzyl chloride, adding the benzyl chloride into 50mL of ethanol solution, then adding 10g of tertiary aminated cotton fiber into the ethanol solution, heating to 60-65 ℃, carrying out reflux reaction for 4-5h, then filtering, washing and drying to obtain quaternized fiber;
and step five, adding 10g of the quaternized fibers prepared in the step four into 100mL of water, then adding 4.9g of the modified diatomite prepared in the step one into the water, uniformly stirring the mixture, then adding 1.3g of p-toluenesulfonic acid into the mixture, heating the mixture to 250-260 ℃, carrying out reflux reaction for 14-15h, filtering, washing and drying the mixture to obtain the adsorbent.
Example 2:
AlO in aluminum profile processing wastewater2 -The preparation method of the adsorbent for treatment comprises the following specific preparation processes:
firstly, adding 9.8g of maleic anhydride and 50mL of water into a reaction kettle at the same time, then adding 0.13g of azobisisobutyronitrile into the reaction kettle, heating to 80-90 ℃, stirring for reaction for 30-40min, then dropwise adding 23.4g of 3-trimethoxy silane acrylic ester into the reaction kettle, heating to 120-130 ℃ after complete dropwise addition, carrying out reflux reaction for 5-6h, then carrying out reduced pressure distillation to obtain an active coupling agent, then weighing 1g of diatomite and 15mL of water into the reaction kettle at the same time, stirring to form a suspension, then adding 0.15g of the active coupling agent into the suspension, heating to 80-85 ℃, stirring for reaction for 3-4h, and then filtering, washing and drying to obtain modified diatomite;
step two, firstly, boiling cotton fibers in boiling water for 15-30min, then soaking the cotton fibers in a sodium hydroxide solution with the mass concentration of 15-18% for 2h, then washing the cotton fibers to be neutral, and then drying and storing the cotton fibers in the air to obtain pretreated cotton fibers;
step three, adding 7.3g of diethylamine and 9.3g of epichlorohydrin into a reaction vessel at the same time, carrying out reflux reaction for 4-5h at 60-70 ℃, then adding 26.1g of pretreated cotton fiber and 3.6g of sodium hydroxide, heating to 100 ℃ and 110 ℃, carrying out reflux reaction for 9-10h, then washing to neutrality, and drying to obtain tertiary aminated cotton fiber;
fourthly, weighing 2.1g of benzyl chloride, adding the benzyl chloride into 50mL of ethanol solution, then adding 10g of tertiary aminated cotton fiber into the ethanol solution, heating to 60-65 ℃, carrying out reflux reaction for 4-5h, then filtering, washing and drying to obtain quaternized fiber;
and step five, adding 10g of the quaternized fibers prepared in the step four into 100mL of water, then adding 5.3g of the modified diatomite prepared in the step one into the water, uniformly stirring the mixture, then adding 1.3g of p-toluenesulfonic acid into the mixture, heating the mixture to 250-260 ℃, carrying out reflux reaction for 14-15h, filtering, washing and drying the mixture to obtain the adsorbent.
Example 3:
AlO in aluminum profile processing wastewater2 -The preparation method of the adsorbent for treatment comprises the following specific preparation processes:
firstly, steaming cotton fibers for 15-30min by using boiling water, then soaking the cotton fibers for 2h by using a sodium hydroxide solution with the mass concentration of 15-18%, washing to be neutral, and then drying and storing to obtain pretreated cotton fibers;
step two, adding 7.3g of diethylamine and 9.3g of epichlorohydrin into a reaction vessel at the same time, carrying out reflux reaction for 4-5h at 60-70 ℃, then adding 30.4g of pretreated cotton fiber and 3.6g of sodium hydroxide, heating to 100 ℃ and 110 ℃, carrying out reflux reaction for 9-10h, then washing to neutrality, and drying to obtain tertiary aminated cotton fiber;
and thirdly, weighing 1.8g of benzyl chloride, adding the benzyl chloride into 50mL of ethanol solution, adding 10g of tertiary aminated cotton fiber into the ethanol solution, heating to 60-65 ℃, carrying out reflux reaction for 4-5h, filtering, washing and drying to obtain the quaternized fiber, namely the adsorbent.
Example 4:
the adsorbents prepared in example 1, example 2 and example 3 and diatomite were subjected to static adsorption experiments to measure the adsorption amount, and the specific measurement method is as follows: weighing a certain amount of sodium metaaluminate, adding the sodium metaaluminate into water to prepare a sodium metaaluminate solution with the concentration of 500mg/L, then weighing 200mL of the sodium metaaluminate solution, adding 10mg of prepared adsorbent into the sodium metaaluminate solution, oscillating the solution in an oscillation box at 30 ℃ for 2 hours, filtering the solution, adding 10mL of concentrated hydrochloric acid into the filtered solution, stirring the solution for 30-40min after shocking is turbid, determining the concentration of aluminum ions in the solution to be C1 through an atomic absorption spectrometer, and calculating the concentration of the aluminate ions in the adsorbed solution to be C1 through the determined concentration of the aluminum ionsThen calculating the adsorption amount of the adsorbentCalculation shows that the adsorption capacity of the adsorbent prepared in the embodiment 1 reaches 93.5mg/g, the adsorption capacity of the adsorbent prepared in the embodiment 2 reaches 93.1mg/g, the adsorption capacity of the adsorbent prepared in the embodiment 3 reaches 72.6mg/g, and the adsorption capacity of the diatomite to the metaaluminate ions reaches 21.8mg/g, so that the efficient adsorption effect on the metaaluminate ions can be realized through the combination of physical adsorption and chemical adsorption.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (7)
1. AlO in aluminum profile processing wastewater2 -The preparation method of the adsorbent for treatment is characterized by comprising the following specific preparation processes:
firstly, weighing a certain amount of diatomite and water, simultaneously adding the diatomite and the water into a reaction kettle, stirring to form a suspension, then adding an active coupling agent into the suspension, heating to 80-85 ℃, stirring to react for 3-4h, and then filtering, washing and drying to obtain modified diatomite;
step two, firstly, boiling cotton fibers in boiling water for 15-30min, then soaking the cotton fibers in a sodium hydroxide solution with the mass concentration of 15-18% for 2h, then washing the cotton fibers to be neutral, and then drying and storing the cotton fibers in the air to obtain pretreated cotton fibers;
step three, simultaneously adding diethylamine and epichlorohydrin into a reaction vessel, carrying out reflux reaction for 4-5h at 60-70 ℃, then adding pretreated cotton fiber and sodium hydroxide, heating to 100 ℃ and 110 ℃, carrying out reflux reaction for 9-10h, then washing to neutrality, and drying to obtain tertiary aminated cotton fiber;
fourthly, weighing a certain amount of benzyl chloride, adding the benzyl chloride into the ethanol solution, adding tertiary aminated cotton fiber into the ethanol solution, heating the mixture to 60-65 ℃, carrying out reflux reaction for 4-5 hours, and then filtering, washing and drying the mixture to obtain quaternized fiber;
and fifthly, adding the quaternized fibers prepared in the fourth step into water, adding the modified diatomite prepared in the first step into the water, uniformly stirring, adding p-toluenesulfonic acid into the mixture, heating to 250-260 ℃, carrying out reflux reaction for 14-15h, filtering, washing and drying to obtain the adsorbent.
2. AlO in aluminum profile processing wastewater according to claim 12 -The preparation method of the adsorbent for treatment is characterized in that 0.13-0.15g of active coupling agent is added into each gram of diatomite in the first step.
3. AlO in aluminum profile processing wastewater according to claim 12 -The preparation method of the adsorbent for treatment is characterized in that in the third step, diethylamine and epichlorohydrin are mixed according to the mass ratio of 1: 1, and simultaneously adding 0.24-0.28g of ethylenediamine into each gram of the pretreated cotton fibers.
4. AlO in aluminum profile processing wastewater according to claim 12 -The preparation method of the treating adsorbent is characterized in that 0.18-0.21g of benzyl chloride is added into each gram of tertiary aminated cotton fiber in the fourth step.
5. AlO in aluminum profile processing wastewater according to claim 12 -The preparation method of the adsorbent for treatment is characterized in that 0.49-0.53g of modified diatomite and 0.13g of p-toluenesulfonic acid are added into each gram of the quaternized fibers in the fifth step.
6. AlO in aluminum profile processing wastewater according to claim 12 -The preparation method of the adsorbent for treatment is characterized in that the preparation process of the active coupling agent in the first step is as follows: adding maleic anhydride and water into a reaction kettle simultaneously, adding azobisisobutyronitrile, heating to 80-90 ℃, stirring for reaction for 30-40min, dropwise adding 3-trimethoxy silane acrylic acid propyl ester, heating to 120-130 ℃ after complete dropwise addition, carrying out reflux reaction for 5-6h, and carrying out reduced pressure distillation to obtain the active coupling agent.
7. AlO in aluminum profile processing wastewater according to claim 62 -For treatmentThe preparation method of the adsorbent is characterized in that the ratio of the maleic anhydride to the 3-trimethoxy silane acrylic ester according to the mass is 1: 1 while adding 1.2 to 1.3g of azobisisobutyronitrile per mole of 3-trimethoxy silane acrylic ester.
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CN117263402A (en) * | 2023-11-21 | 2023-12-22 | 华沃德源环境技术(济南)有限公司 | Sewage treatment agent based on nitrifying bacteria and preparation method thereof |
CN117263402B (en) * | 2023-11-21 | 2024-02-27 | 华沃德源环境技术(济南)有限公司 | Sewage treatment agent based on nitrifying bacteria and preparation method thereof |
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