CN112058320A - Micro-nano fiber ion exchange resin deiodination agent and preparation method thereof - Google Patents
Micro-nano fiber ion exchange resin deiodination agent and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of chemical engineering, and particularly relates to a micro-nano fiber ion exchange resin deiodination agent and a preparation method thereof. The preparation method comprises the following steps: obtaining micro-nano fibers from polylactic acid and polyvinyl alcohol by an electrostatic spinning method, and then carrying out graft modification on the micro-nano fibers by a pre-irradiation method; and then mixing the modified micro-nano fibers with vinylbenzyl chloride and divinylbenzene to prepare resin, and then placing the resin in an ethanol solution of zirconium acetate and manganese nitrate tetrahydrate for standing to obtain the deiodination agent. The micro-nano fiber ion exchange resin deiodination agent has large adsorption capacity and excellent selectivity.
Description
Technical Field
The invention belongs to the technical field of chemical engineering, and particularly relates to a micro-nano fiber ion exchange resin deiodination agent and a preparation method thereof.
Background
Iodine has great effect, and is not only an essential trace element for maintaining the nervous system and guaranteeing normal metabolism and intelligence development of a human body; is also a basic industrial raw material and an important strategic material, and is widely applied to the fields of food medicine, chemical industry, agriculture, national defense, military and the like. With the rapid development of the industry in China, the annual demand of iodine resources is rapidly increased, but the situation of iodine resource shortage is faced.
The industrially extracted iodine is extracted by taking seaweed, chilies niter, underground brine, phosphate rock and the like as raw materials; the specific extraction method is various, but the principle is that iodine in raw materials is transferred to obtain iodine-containing raw material solution, then the iodine-containing raw material solution is subjected to oxidation or reduction treatment to enrich and convert iodine ions into free iodine, and then crude iodine is further separated and refined. The method for extracting iodine ions in the solution includes adsorption of ion exchange resin and chemical reaction with iodine ions. However, the latter has the problems of high cost, poor chemical stability under acidic conditions, difficult desorption and the like; the former has a problem of poor selectivity.
Disclosure of Invention
Aiming at the technical defects of small adsorption capacity and poor selectivity of an adsorbent in the existing iodine ion adsorption process, the invention provides a micro-nano fiber ion exchange resin deiodination agent and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the method comprises the following steps: uniformly mixing a certain amount of polylactic acid and polyvinyl alcohol, dissolving in a proper amount of chloroform-dimethyl sulfoxide mixed solution, performing ultrasonic treatment for 40-50min, transferring the solution into an injector, and spinning fibers on an electrostatic spinning device in a horizontal manner under a certain condition; and after spinning is finished, drying the sample in an oven at 60-70 ℃ for 6-8 h.
Step two: soaking the fiber prepared in the step one in a nitric acid solution for 2-3h, washing the fiber with deionized water until a washing solution is neutral, putting the washed fiber into a polyethylene sealed bag, discharging air, introducing nitrogen, cooling, irradiating with an electron beam, putting a sample into a mixed solution of trioctyl/decyl tertiary amine and a silane coupling agent KH-560, vacuumizing, and standing in a water bath kettle at 45-50 ℃ for 2-3 h; and then, alternately washing the sample for 3 times by using methanol and deionized water, and then drying the sample in a vacuum drying oven at the temperature of 60-70 ℃ for 10-12h to obtain the modified micro-nanofiber.
Step three: mixing a certain amount of micro-nano fibers with a proper amount of vinylbenzyl chloride and divinylbenzene, stirring for 2-3 hours at room temperature, then slowly dripping a proper amount of ethanolamine solution into the mixed solution, stirring for 20-30 minutes, placing the mixture into an oven, standing and swelling for 70-80 minutes at 35-40 ℃, and placing the mixture into a microwave reactor for reaction for 12-15 minutes after swelling is finished; the obtained sample is washed 4-5 times with acetone and deionized water to obtain the composite resin.
Step four: and putting the resin prepared in the third step into a beaker, stirring and washing the resin by HCl, NaOH and deionized water for 15-20min, filtering the resin, putting the resin into a proper amount of absolute ethanol solution, adding a proper amount of zirconium acetate and manganese nitrate tetrahydrate under stirring, carrying out ultrasonic treatment on the mixed solution for 20-25min, stirring the mixed solution for 30-36h at room temperature, filtering the mixed solution, washing the mixed solution by the deionized water, and freeze-drying the mixed solution in a vacuum freeze-drying box to obtain the micro-nano fiber ion exchange resin deiodination agent.
In the first step, the adding amount of the polylactic acid is 2.3-2.7g, the mass ratio of the polylactic acid to the polyvinyl alcohol is 4:1-5:1, the mass fraction of the mixture of the polylactic acid and the polyvinyl alcohol in the chloroform-dimethyl sulfoxide mixed solution is 10-12%, and the volume ratio of the polylactic acid to the polyvinyl alcohol in the chloroform-dimethyl sulfoxide mixed solution is 2:1-3: 1.
In the second step, the ratio of the fiber to the mixed solution of the trioctyl/decyl tertiary amine-silane KH-560 is 1g:25-30ml, and the volume ratio of the trioctyl/decyl tertiary amine-silane KH-560 in the mixed solution is 1:1-1: 1.5.
The mass ratio of the micro-nano fibers to the vinylbenzyl chloride in the third step is 1:14-1:18, the mass ratio of the divinylbenzene to the vinylbenzyl chloride is 1:30-1:40, and the mass ratio of the vinylbenzyl chloride to the ethanolamine is 1:2-1: 2.5.
The ratio of the resin to the absolute ethyl alcohol in the fourth step is 1g:6-8 ml.
Preferably, in the first step, the voltage of the electrostatic spinning device is 20kV, the distance is 25cm, the diameter of the spinning nozzle is 1.2mm, and the advancing speed is 0.2 mm/s.
Preferably, the concentration of the nitric acid in the second step is 1mol/L, the radiation absorption dose of the fiber is 35kGy, and the dose rate is 0.4 kGy/s.
Preferably, the dropping speed of the ethanolamine in the step III is 3 ml/min.
Preferably, the concentrations of HCl and NaOH in the fourth step are both 1mol/L, and the concentration of zirconium acetate in absolute ethyl alcohol is 0.1 mol/L; the ratio of the amounts of the zirconium acetate and the manganese nitrate tetrahydrate is 1:1.5-1: 1.8.
Has the advantages that: the micro-nano fiber prepared by the invention has ion exchange groups after being treated, and has the advantages of large specific surface area, short mass transfer distance, many adsorption points and the like. The mechanical property of the micro-nano fiber can be improved after the micro-nano fiber is added in the process of preparing the resin, the particle size of the prepared ion exchange resin is improved, and the cross-linking degree of an extractor is improved; the specific surface area and the pore diameter in the prepared resin can be increased, so that the subsequent ion exchange efficiency is improved; and the modified micro-nano fiber has excellent selective adsorption performance, and can overcome the defect of poor selectivity of the ion exchange resin. The applied trioctyl/decyl tertiary amine and KH-560 can generate N, O protonation under acidic condition to carry out the pre-radiation modification on the micro-nano fibers, thereby having the electrostatic adsorption on iodine ions.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
The method comprises the following steps: uniformly mixing 2.5g of polylactic acid and 0.5g of polyvinyl alcohol, dissolving the mixture in a mixed solution of 16.7ml of chloroform and 8.3ml of dimethyl sulfoxide, carrying out ultrasonic treatment for 40min, transferring the solution into an injector, and spinning fibers on an electrostatic spinning device in a horizontal mode under certain conditions; after spinning, the sample was dried in an oven at 60 ℃ for 6 h.
Step two: soaking 2.4g of the fiber prepared in the first step in a nitric acid solution for 3 hours, washing the fiber with deionized water until a washing solution is neutral, putting the washed fiber into a polyethylene sealed bag, discharging air, introducing nitrogen, cooling, irradiating with an electron beam, putting a sample into a mixed solution of 36ml of trioctyl/decyl tertiary amine and 36ml of a silane coupling agent KH-560, vacuumizing, and standing in a 50 ℃ water bath kettle for 3 hours; and then, alternately washing the sample for 3 times by using methanol and deionized water, and then drying the sample in a vacuum drying oven at 60 ℃ for 12 hours to obtain the modified micro-nano fiber.
Step three: mixing 2.4g of micro-nanofiber, 40.2ml of vinylbenzyl chloride and 1.6ml of divinylbenzene, stirring for 3 hours at room temperature, slowly dropping 45.2ml of ethanolamine solution into the mixed solution, stirring for 20 minutes, placing the mixed solution into an oven, standing and swelling for 70-80 minutes at 35 ℃, and placing the mixed solution into a microwave reactor for reaction for 15 minutes after swelling; the resulting sample was then washed 5 times with acetone and deionized water to give a composite resin.
Step four: and (3) putting 16.1g of the resin prepared in the third step into a beaker, stirring and washing the resin with a proper amount of HCl, NaOH and deionized water for 15min, filtering, putting the resin into 128.8ml of absolute ethanol solution, adding 4.21g of zirconium acetate and 5.81g of manganese nitrate tetrahydrate under stirring, carrying out ultrasonic treatment on the mixed solution for 25min, stirring the mixed solution at room temperature for 36h, filtering, washing the mixed solution with deionized water, and freeze-drying the washed solution in a vacuum freeze-drying box to obtain the micro-nano fiber ion exchange resin adsorbent.
Example 2
The method comprises the following steps: uniformly mixing 2.7g of polylactic acid and 0.38g of polyvinyl alcohol, dissolving the mixture in a mixed solution of 16.8ml of chloroform and 5.6ml of dimethyl sulfoxide, carrying out ultrasonic treatment for 46min, transferring the solution into an injector, and spinning fibers on an electrostatic spinning device in a horizontal mode under certain conditions; after spinning, the sample was dried in an oven at 70 ℃ for 8 h.
Step two: soaking 2.46g of the fiber prepared in the first step in a nitric acid solution for 2 hours, washing the fiber with deionized water until a washing solution is neutral, putting the washed fiber into a polyethylene sealed bag, discharging air, introducing nitrogen, cooling, irradiating with an electron beam, putting a sample into a mixed solution of 24.6ml of trioctyl/decyl tertiary amine and 36.9ml of silane coupling agent KH-560, vacuumizing, and standing in a 45 ℃ water bath kettle for 2 hours; and then, alternately washing the sample for 3 times by using methanol and deionized water, and then drying the sample in a vacuum drying oven at 70 ℃ for 10 hours to obtain the modified micro-nano fiber.
Step three: mixing 2.46g of micro-nanofiber, 32.1ml of vinylbenzyl chloride and 1ml of divinylbenzene, stirring for 2 hours at room temperature, slowly dropping 27.6ml of ethanolamine solution into the mixed solution, stirring for 28 minutes, placing the mixed solution into an oven, standing and swelling for 70-80 minutes at 40 ℃, and placing the mixed solution into a microwave reactor for reaction for 14 minutes after swelling is finished; the resulting sample was then washed 5 times with acetone and deionized water to give a composite resin.
Step four: and (3) putting 12.84g of the resin prepared in the third step into a beaker, stirring and washing the resin with a proper amount of HCl, NaOH and deionized water for 19min, filtering, putting the resin into 77.1ml of absolute ethanol solution, adding 2.52g of zirconium acetate and 2.98g of manganese nitrate tetrahydrate under stirring, carrying out ultrasonic treatment on the mixed solution for 20min, stirring the mixed solution at room temperature for 34h, filtering, washing the mixed solution with deionized water, and freeze-drying the washed solution in a vacuum freeze-drying box to obtain the micro-nano fiber ion exchange resin adsorbent.
Example 3
The method comprises the following steps: uniformly mixing 2.6g of polylactic acid and 0.51g of polyvinyl alcohol, dissolving the mixture in a mixed solution of 15.5ml of chloroform and 6.2ml of dimethyl sulfoxide, carrying out ultrasonic treatment for 42min, transferring the solution into an injector, and spinning fibers on an electrostatic spinning device in a horizontal mode under certain conditions; after spinning, the sample was dried in an oven at 65 ℃ for 7 h.
Step two: soaking 2.49g of the fiber prepared in the first step in a nitric acid solution for 2 hours, washing the fiber with deionized water until a washing solution is neutral, putting the washed fiber into a polyethylene sealed bag, discharging air, introducing nitrogen, cooling, irradiating with an electron beam, putting a sample into a mixed solution of 30.1ml of trioctyl/decyl tertiary amine and 42.1ml of silane coupling agent KH-560, vacuumizing, and standing in a water bath kettle at 48 ℃ for 2 hours; and then, alternately washing the sample for 3 times by using methanol and deionized water, and then drying the sample in a vacuum drying oven at 65 ℃ for 11 hours to obtain the modified micro-nano fiber.
Step three: mixing 2.49g of micro-nanofiber, 39.8ml of vinylbenzyl chloride and 1.5ml of divinylbenzene, stirring for 3 hours at room temperature, slowly dropping 37.8ml of ethanolamine solution into the mixed solution, stirring for 24 minutes, placing the mixed solution into an oven, standing and swelling for 70-80 minutes at 37 ℃, and placing the mixed solution into a microwave reactor for reaction for 13 minutes after swelling; the resulting sample was then washed 4 times with acetone and deionized water to give a composite resin.
Step four: and (3) putting 15.92g of the resin prepared in the third step into a beaker, stirring and washing the resin with a proper amount of HCl, NaOH and deionized water for 17min, filtering, putting the resin into 111.4ml of absolute ethanol solution, adding 3.64g of zirconium acetate and 4.73g of manganese nitrate tetrahydrate under stirring, carrying out ultrasonic treatment on the mixed solution for 22min, stirring the mixed solution at room temperature for 32h, filtering, washing the mixed solution with deionized water, and freeze-drying the washed solution in a vacuum freeze-drying box to obtain the micro-nano fiber ion exchange resin adsorbent.
Example 4
The method comprises the following steps: uniformly mixing 2.65g of polylactic acid and 0.44g of polyvinyl alcohol, dissolving the mixture in a mixed solution of 16.5ml of chloroform and 7.5ml of dimethyl sulfoxide, carrying out ultrasonic treatment for 50min, transferring the solution into an injector, and spinning fibers on an electrostatic spinning device in a horizontal mode under certain conditions; after spinning, the sample was dried in an oven at 63 ℃ for 7.5 h.
Step two: soaking 2.47g of the fiber prepared in the first step in a nitric acid solution for 2.5 hours, washing the fiber with deionized water until a washing solution is neutral, putting the washed fiber into a polyethylene sealed bag, discharging air, introducing nitrogen, cooling, irradiating with an electron beam, putting a sample into a mixed solution of 27.7ml of trioctyl/decyl tertiary amine and 41.5ml of silane coupling agent KH-560, vacuumizing, and standing in a 47 ℃ water bath kettle for 3 hours; and then, alternately washing the sample for 3 times by using methanol and deionized water, and then drying the sample in a vacuum drying oven at 63 ℃ for 10.5 hours to obtain the modified micro-nano fiber.
Step three: mixing 2.47g of micro-nanofiber, 37.1ml of vinylbenzyl chloride and 1.3ml of divinylbenzene, stirring for 2.5 hours at room temperature, slowly dropping 35.9ml of ethanolamine solution into the mixed solution, stirring for 30 minutes, placing the mixed solution into an oven, standing and swelling for 70-80 minutes at 36 ℃, and placing the mixed solution into a microwave reactor for reaction for 12 minutes after swelling; the resulting sample was then washed 4 times with acetone and deionized water to give a composite resin.
Step four: and (3) putting 14.84g of the resin prepared in the third step into a beaker, stirring and washing the resin with a proper amount of HCl, NaOH and deionized water for 20min, filtering, putting the resin into 96.5ml of absolute ethanol solution, adding 3.15g of zirconium acetate and 3.78g of manganese nitrate tetrahydrate under stirring, carrying out ultrasonic treatment on the mixed solution for 24min, stirring the mixed solution at room temperature for 30h, filtering, washing the mixed solution with deionized water, and freeze-drying the washed solution in a vacuum freeze-drying box to obtain the micro-nano fiber ion exchange resin adsorbent.
Comparative example 1
According to the preparation method, vinylbenzyl chloride and divinylbenzene are used for synthesizing resin under the condition of not adding micro-nano fibers, and the resin is placed in a salt solution for ion exchange to obtain the adsorbent.
Table 1 shows the values according to the low temperature N2The adsorption isotherms were calculated using BET and BJH model equations to give specific surface areas and pore size distributions for examples 1-4 and comparative example 1. By passingComparison shows that the materials prepared in examples 1-4 have increased specific surface area and total pore volume and increased average pore diameter compared with comparative example 1. The increase in specific surface area and total pore volume indicates that the unit adsorption capacity of examples 1-4 is also greatly increased.
TABLE 1
Table 2 shows the results of passing iodine-containing acetic acid and I-containing acetic acid through the deiodinator ion exchange column prepared in examples 1-4 at room temperature-、Cl-And SO4 2-Allowing the acetic acid containing anions to flow through the deiodination column, controlling the opening of the valve to ensure that the iodine-containing acetic acid is retained in the deiodination column for 2 minutes, and detecting substances in the acetic acid after 40 minutes. Wherein the concentration of each anion in the acetic acid is about 1500 ppb. From Table 2, it can be seen that examples 1 to 4 are pairs containing I alone-And the deiodinated I of acetic acid containing other anions-The concentrations are not very different, which indicates Cl-And SO4 2-The adsorption of iodine by the deiodination agent can not be influenced, and the deiodination effect is better than that of the comparative example 1. In the presence of I-、Cl-And SO4 2-After acetic acid treatment of (2) Cl in acetic acid-And SO4 2-The content of (a) was not greatly changed, which indicates that the deiodination agents prepared in examples 1 to 4 had good selectivity.
TABLE 2
While the invention has been described with respect to a preferred embodiment, it will be understood by those skilled in the art that the foregoing and other changes, omissions and deviations in the form and detail thereof may be made without departing from the scope of this invention.
Claims (6)
1. A preparation method of a micro-nano fiber ion exchange resin deiodination agent is characterized by comprising the following steps:
the method comprises the following steps: uniformly mixing a certain amount of polylactic acid and polyvinyl alcohol, dissolving in a proper amount of chloroform-dimethyl sulfoxide mixed solution, performing ultrasonic treatment for 40-50min, transferring the solution into an injector, and spinning fibers on an electrostatic spinning device in a horizontal manner under a certain condition; after spinning is finished, drying the sample in an oven at the temperature of 60-70 ℃ for 6-8 h;
step two: soaking the fiber prepared in the step one in a nitric acid solution for 2-3h, washing the fiber with deionized water until a washing solution is neutral, putting the washed fiber into a polyethylene sealed bag, discharging air, introducing nitrogen, cooling, irradiating with an electron beam, putting a sample into a mixed solution of trioctyl/decyl tertiary amine and a silane coupling agent KH-560, vacuumizing, and standing in a water bath kettle at 45-50 ℃ for 2-3 h; then, alternately washing the sample for 3 times by using methanol and deionized water, and then drying the sample in a vacuum drying oven at the temperature of 60-70 ℃ for 10-12h to obtain modified micro-nano fibers;
step three: mixing a certain amount of micro-nano fibers with a proper amount of vinylbenzyl chloride and divinylbenzene, stirring for 2-3 hours at room temperature, then slowly dripping a proper amount of ethanolamine solution into the mixed solution, stirring for 20-30 minutes, placing the mixture into an oven, standing and swelling for 70-80 minutes at 35-40 ℃, and placing the mixture into a microwave reactor for reaction for 12-15 minutes after swelling is finished; washing the obtained sample with acetone and deionized water for 4-5 times to obtain composite resin;
step four: putting the resin prepared in the third step into a beaker, stirring and washing the resin by HCl, NaOH and deionized water for 15-20min in sequence, putting the resin into a proper amount of absolute ethanol solution after filtering, adding a proper amount of zirconium acetate and manganese nitrate tetrahydrate under stirring, carrying out ultrasonic treatment on the mixed solution for 20-25min, stirring the mixed solution for 30-36h at room temperature, washing the mixed solution by the deionized water after filtering, and freeze-drying the mixed solution in a vacuum freeze-drying oven to obtain the micro-nano fiber ion exchange resin deiodination agent;
in the first step, the adding amount of polylactic acid is 2.3-2.7g, the mass ratio of polylactic acid to polyvinyl alcohol is 4:1-5:1, the mass fraction of the mixture of polylactic acid and polyvinyl alcohol in chloroform-dimethyl sulfoxide mixed solution is 10-12%, and the volume ratio of the polylactic acid to the polyvinyl alcohol in chloroform-dimethyl sulfoxide mixed solution is 2:1-3: 1; the ratio of the fibers to the mixed solution of the trioctyl/decyl tertiary amine-silane KH-560 in the second step is 1g:25-30ml, and the volume ratio of the fibers to the mixed solution of the trioctyl/decyl tertiary amine-silane KH-560 is 1:1-1: 1.5; the mass ratio of the micro-nano fibers to the vinylbenzyl chloride in the third step is 1:14-1:18, the mass ratio of the divinylbenzene to the vinylbenzyl chloride is 1:30-1:40, and the mass ratio of the vinylbenzyl chloride to the ethanolamine is 1:2-1: 2.5; the ratio of the resin to the absolute ethyl alcohol in the fourth step is 1g:6-8 ml.
2. The method for preparing the deiodination agent for the micro-nano fiber ion exchange resin according to claim 1, wherein in the first step, the voltage of an electrostatic spinning device is 20kV, the distance is 25cm, the diameter of a spinning nozzle is 1.2mm, and the advancing speed is 0.2 mm/s.
3. The method for preparing the deiodination agent for the micro-nano fiber ion exchange resin according to claim 1, wherein the concentration of nitric acid in the second step is 1mol/L, the radiation absorption dose of the fiber is 35kGy, and the dose rate is 0.4 kGy/s.
4. The preparation method of the micro-nanofiber ion exchange resin deiodination agent as claimed in claim 1, wherein the dropping speed of ethanolamine in the third step is 3 ml/min.
5. The preparation method of the micro-nano fiber ion exchange resin deiodination agent according to claim 1, wherein in the step four, the concentrations of HCl and NaOH are both 1mol/L, and the concentration of zirconium acetate in absolute ethyl alcohol is 0.1 mol/L; the ratio of the amounts of the zirconium acetate and the manganese nitrate tetrahydrate is 1:1.5-1: 1.8.
6. The catalyst micro-nanofiber ion exchange resin deiodination agent prepared by the preparation method according to any one of claims 1-5.
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| CN112680960A (en) * | 2020-12-23 | 2021-04-20 | 深圳市他她服装有限公司 | Antibacterial and anti-allergy functional fabric and preparation method thereof |
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| CN112680960A (en) * | 2020-12-23 | 2021-04-20 | 深圳市他她服装有限公司 | Antibacterial and anti-allergy functional fabric and preparation method thereof |
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