CN115301213A - Polyaniline/montmorillonite/charcoal composite adsorption material and preparation method and application thereof - Google Patents
Polyaniline/montmorillonite/charcoal composite adsorption material and preparation method and application thereof Download PDFInfo
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- CN115301213A CN115301213A CN202210941863.3A CN202210941863A CN115301213A CN 115301213 A CN115301213 A CN 115301213A CN 202210941863 A CN202210941863 A CN 202210941863A CN 115301213 A CN115301213 A CN 115301213A
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- 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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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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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
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Abstract
The invention relates to an adsorbent material for chemical production, in particular to a polyaniline/montmorillonite/charcoal composite adsorption material and a preparation method and application thereof. Polyaniline in the polyaniline/montmorillonite/charcoal composite adsorbing material is obtained by polymerization reaction of aniline, charcoal is aminated charcoal powder, and montmorillonite is montmorillonite modified by a silane coupling agent containing amino; the weight ratio of montmorillonite, charcoal and aniline in the raw materials is 0.5-3. The invention can improve the adsorption performance of the material, and realizes low treatment cost and good treatment effect on the iodine-containing wastewater.
Description
Technical Field
The invention relates to an adsorbent material for chemical production, in particular to a polyaniline/montmorillonite/charcoal composite adsorption material and a preparation method and application thereof.
Background
Acetic acid is a chemical raw material with wide application, the main preparation mode of the acetic acid is the methanol carbonyl method, and the yield of the acetic acid produced by the technology reaches over 99 percent of the total yield of the acetic acid in the world. In the process of preparing acetic acid by using methanol carbonyl, methanol and carbon monoxide are main raw materials for preparing the acetic acid, and rhodium/iridium-iodine is used as a catalyst for producing the acetic acid.
The methanol carbonylation process produces a variety of impurities in addition to acetic acid (e.g., acetaldehyde, acetone, methyl ethyl ketone, butyraldehyde, crotonaldehyde, 2-ethyl crotonaldehyde, and 2-ethyl butyraldehyde, and the like, and their aldol condensation products). The content of the carbonyl impurities is at most acetaldehyde, which can react with an iodide catalyst promoter to generate impurities such as multi-carbon alkyl iodide and the like, and a certain amount of iodine-containing wastewater is generated in the impurity removal process. Most of the traditional iodine-containing wastewater treatment materials have the defects of high material cost, complex preparation process, poor treatment effect and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a polyaniline/montmorillonite/charcoal composite adsorbing material which can adsorb iodine-containing wastewater and has low treatment cost and good treatment effect, and a preparation method and application thereof.
The invention provides a polyaniline/montmorillonite/charcoal composite adsorption material, wherein polyaniline is obtained by polymerization reaction of aniline, charcoal is aminated charcoal powder, and montmorillonite is montmorillonite modified by a silane coupling agent containing amino; the weight ratio of montmorillonite, charcoal and aniline in the raw materials is 0.5-3.
Preferably, in the preparation process of the aminated charcoal powder, the silane coupling agent containing amino, ammonia water and a solvent are mixed uniformly, react for 12-18h at 45-50 ℃, and are subjected to solid-liquid separation to obtain the aminated charcoal powder.
Preferably, in the preparation process of the aminated charcoal powder, the weight ratio of the charcoal powder, the silane coupling agent containing amino and ammonia water is 1.
Preferably, in the preparation process of the aminated charcoal powder, the solvent is 85-95% ethanol water solution by volume fraction.
Preferably, the grain size of the aminated charcoal powder is less than or equal to 0.5 μm; preferably, the particle size of the montmorillonite is less than or equal to 0.5 mu m.
The silane coupling agent containing amino can be gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, etc.; the ammonia water is an aqueous solution containing 25wt% -28wt% of ammonia.
The preparation method of the polyaniline/montmorillonite/charcoal composite adsorbing material comprises the following steps: uniformly dispersing montmorillonite and aminated charcoal powder in aniline, adding protonic acid aqueous solution, uniformly mixing, adjusting temperature, dropwise adding an initiator, carrying out heat preservation reaction, and carrying out solid-liquid separation to obtain the polyaniline/montmorillonite/charcoal composite adsorbing material.
Preferably, montmorillonite and aminated charcoal powder are uniformly dispersed in aniline by ultrasonic treatment for 4-6 h.
Preferably, the temperature is adjusted to be-15 to-5 ℃, and the reaction time is kept for 12 to 18 hours.
Preferably, the protic acid is acetic acid.
Preferably, the concentration of the protonic acid aqueous solution is 0.15 to 0.2mol/L.
Preferably, the weight ratio of aniline, protonic acid and initiator is 1.9-1.1.
The initiator can be ammonium persulfate, sodium persulfate and the like; the initiator is added in the form of an aqueous solution, and the concentration of the aqueous initiator solution can be 2-2.5mol/L.
The invention also discloses application of the polyaniline/montmorillonite/charcoal composite adsorbing material in treating iodine-containing wastewater.
Preferably, the iodine-containing wastewater is iodine-containing wastewater generated in the preparation of acetic acid.
The polyaniline/montmorillonite/charcoal composite adsorbing material can adsorb multi-carbon alkyl iodide, iodide ions, iodine simple substances and other substances in iodine-containing wastewater, and can also adsorb other substances in the wastewater to improve the water quality.
The invention also discloses an iodine-containing wastewater treatment method, which is characterized in that the polyaniline/montmorillonite/charcoal composite adsorption material is used for carrying out column chromatography treatment on iodine-containing wastewater, wherein the number n of times of column chromatography treatment is more than or equal to 3, the flow rate of column chromatography is 1.8-2.2 resin bed volumes, and the time of column chromatography is 8-12min; the chromatography liquid of the nth time is used as the liquid to be treated when the column chromatography of the (n + 1) th time is carried out; preferably, the iodine-containing wastewater is iodine-containing wastewater generated in the preparation of acetic acid.
The advantages of the invention are embodied in that: the charcoal and the montmorillonite are modified, so that the dispersibility of the charcoal and the montmorillonite is improved, amino groups are grafted on the charcoal and the montmorillonite, then the charcoal and the montmorillonite are uniformly dispersed in aniline by ultrasonic, and in-situ polymerization reaction is carried out to obtain the polyaniline/montmorillonite/charcoal composite adsorbing material; the charcoal and the amino groups on the montmorillonite can participate in the polymerization reaction, and the charcoal, the montmorillonite and the polyaniline are mutually matched, so that the adsorption performance of the material can be improved, and the efficient treatment of the iodine-containing wastewater is realized; the iodine content of the iodine-containing wastewater generated in the preparation of acetic acid with the iodine content of 4500ppm can be reduced to be lower than 3ppm by three times of column chromatography treatment; the invention has low sewage treatment cost and good treatment effect.
Drawings
Fig. 1 is an SEM image of the polyaniline/montmorillonite/charcoal composite adsorbing material.
Detailed Description
Hereinafter, the technical solution of the present invention will be described in detail by specific examples, but these examples should be explicitly proposed for illustration, but should not be construed as limiting the scope of the present invention.
Example 1
A preparation method of a polyaniline/montmorillonite/charcoal composite adsorption material comprises the following steps:
adding 90g of gamma-aminopropyltriethoxysilane and 9g of ammonia water into 95% ethanol water solution, adding 300g of charcoal powder, ultrasonically dispersing for 30min, heating to 45 ℃, stirring for reacting for 18h, filtering, washing a filter cake with ethanol, drying, and grinding to obtain aminated charcoal powder with the particle size of less than or equal to 0.5 mu m;
100g of gamma-aminopropyltriethoxysilane modified montmorillonite with the particle size of less than or equal to 0.5 mu m and 300g of aminated charcoal powder with the particle size of less than or equal to 0.5 mu m are added into 200g of aniline and ultrasonically dispersed for 4 hours uniformly, then 17L of acetic acid aqueous solution with the concentration of 0.2mol/L is added and uniformly mixed, the temperature is adjusted to-15 ℃, 500mL of sodium persulfate aqueous solution with the concentration of 2.5mol/L is dripped, the heat preservation reaction is carried out for 18 hours, and the polyaniline/montmorillonite/charcoal composite adsorbing material is obtained through solid-liquid separation.
Example 2
A preparation method of a polyaniline/montmorillonite/charcoal composite adsorption material comprises the following steps:
adding 120g of gamma-aminopropyltriethoxysilane and 21g of ammonia water into 85% ethanol water solution, then adding 300g of charcoal powder, performing ultrasonic dispersion for 30min, heating to 50 ℃, stirring for reaction for 12h, filtering, washing a filter cake with ethanol, drying, and grinding to obtain aminated charcoal powder with the particle size of less than or equal to 0.5 mu m;
200g of gamma-aminopropyltriethoxysilane modified montmorillonite with the particle size of less than or equal to 0.5 mu m and 300g of aminated charcoal powder with the particle size of less than or equal to 0.5 mu m are added into 100g of aniline and ultrasonically dispersed for 6 hours uniformly, 11L of acetic acid aqueous solution with the concentration of 0.15mol/L is added and uniformly mixed, the temperature is adjusted to be minus 5 ℃, 340mL of sodium persulfate aqueous solution with the concentration of 2.5mol/L is dripped, the heat preservation reaction is carried out for 12 hours, and the polyaniline/montmorillonite/charcoal composite adsorbing material is obtained through solid-liquid separation.
Example 3
A preparation method of a polyaniline/montmorillonite/charcoal composite adsorption material comprises the following steps:
adding 105g of gamma-aminopropyltriethoxysilane and 15g of ammonia water into 90% ethanol water solution, then adding 300g of charcoal powder, carrying out ultrasonic dispersion for 30min, heating to 50 ℃, stirring for reaction for 15h, filtering, washing a filter cake with ethanol, drying, and grinding to obtain aminated charcoal powder with the particle size of less than or equal to 0.5 mu m;
300g of gamma-aminopropyltriethoxysilane modified montmorillonite with the particle size of less than or equal to 0.5 mu m and 300g of aminated charcoal powder with the particle size of less than or equal to 0.5 mu m are added into 100g of aniline and ultrasonically dispersed for 5 hours uniformly, then 8.4L of acetic acid aqueous solution with the concentration of 0.2mol/L is added and uniformly mixed, the temperature is adjusted to-10 ℃, 300mL of sodium persulfate aqueous solution with the concentration of 2.5mol/L is dripped, the heat preservation reaction is carried out for 15 hours, and the polyaniline/montmorillonite/charcoal composite adsorbing material is obtained through solid-liquid separation.
The polyaniline/montmorillonite/charcoal composite adsorbing material prepared in example 3 was subjected to electron microscope scanning, and the result is shown in fig. 1. Fig. 1 is an SEM image of the polyaniline/montmorillonite/charcoal composite adsorbing material.
As can be seen from fig. 1: the polyaniline/montmorillonite/charcoal composite adsorbing material is micron-level particles.
Example 4
The first iodine-containing wastewater treatment experiment:
taking the composite material prepared in the embodiment 3, and washing the composite material by water until the pH value of a washing liquid is about 7 and the conductivity is about 20 us/cm; then the composite material is put into a double-layer sand core chromatographic column, pure water is put into a glass liquid storage ball after the double-layer sand core chromatographic column is well put, and the flow rate is adjusted to 2 resin bed volumes (BV for short) by pressing an adjusting valve; then discharging the pure water in the glass liquid storage ball, and blow-drying the double-layer sand core chromatographic column;
taking iodine-containing wastewater (the iodine content in the iodine-containing wastewater is 4500ppm, PH =3.71, TDS =573ppm, COD =17439ppm and conductivity =960 us/cm), removing impurities such as suspended matters and ribbons by nanofiltration treatment, and then filling the wastewater into a glass liquid storage ball; keeping the flow rate at 2 BV, performing iodide ion adsorption treatment for 60min, taking the chromatography liquid with 100ml PE sampling bottle every 5min, detecting COD of the chromatography liquid with visible spectrophotometer, measuring conductivity of the chromatography liquid with conductivity meter, measuring PH of the chromatography liquid with acidity meter, measuring TDS of the chromatography liquid with millet TDS pen, and measuring iodide ion content of the chromatography liquid with ICP instrument. The results of wastewater treatment are shown in Table 1.
TABLE 1 results of first treatment of iodine-containing wastewater
As can be seen from Table 1, the iodine content in the chromatography liquid was the lowest at 10min after the adsorption treatment, and the present invention also can adsorb other substances in the wastewater to improve the water quality.
Example 5
A second iodine-containing wastewater treatment experiment was carried out by replacing the composite material prepared in example 3 with the chromatography liquid for adsorption treatment in example 4 for 10min, according to the method in example 4, and the wastewater treatment results are shown in table 2.
TABLE 2 second treatment results of iodine-containing wastewater
As can be seen from Table 2, the iodine content in the chromatography liquid was the lowest at 10min after the adsorption treatment, and the present invention also can adsorb other substances in the wastewater to improve the water quality.
Example 6
A third iodine-containing wastewater treatment experiment was carried out by replacing the composite material prepared in example 3 with the chromatography liquid for adsorption treatment in example 5 for 10min, according to the method in example 4, and the wastewater treatment results are shown in table 3.
TABLE 3 third treatment result of iodine-containing wastewater
As can be seen from Table 3, after adsorption treatment for 10min, the iodine content was 3ppm; the wastewater with the iodine content of 4500ppm is subjected to continuous column chromatography treatment for three times by the polyaniline/montmorillonite/charcoal composite adsorbing material, and the iodine content can be reduced to 3ppm; after the three times of adsorption treatment, the iodine removal rate reaches 99.93 percent, the treatment effect on the iodine-containing wastewater is good, and the invention can also adsorb other substances in the wastewater and improve the water quality.
Comparative example 1
The procedure of example 3 was repeated except that the gamma-aminopropyltriethoxysilane-modified montmorillonite was not added.
Comparative example 2
The procedure of example 3 was repeated except that no aminated charcoal powder was added.
Comparative example 3
The procedure of example 3 was repeated except that the gamma-aminopropyltriethoxysilane-modified montmorillonite and aminated charcoal powder were not added.
Taking the composite materials prepared in examples 1-3 and comparative examples 1-3, carrying out iodine-containing wastewater treatment experiments according to the method of example 4, and detecting the content of iodide ions in chromatographic solution subjected to adsorption treatment for 10 min. The results are shown in Table 4.
TABLE 4 treatment results of iodine-containing wastewater of examples 1 to 3 and comparative examples 1 to 3
It can be seen from Table 4 that the adsorption treatment performance of the present invention on iodine-containing wastewater is much better than that of the comparative examples 1 to 3.
After the iodine-containing wastewater is adsorbed, the composite material in the double-layer sand core chromatographic column needs to be analyzed, and the method comprises the following specific steps: discharging iodine-containing wastewater in the glass liquid storage ball, cleaning the glass liquid storage ball by using pure water, then adding 30wt% of sodium hydroxide aqueous solution into the glass liquid storage ball, adjusting the flow rate to be 1.5 BV, carrying out analysis for 60min, taking the analysis solution by using a 100ml PE sampling bottle every 10min, detecting until the content of COD, conductivity, PH, TDS and iodide ions of the analysis solution meets the specification, stopping analysis, discharging the 30wt% of sodium hydroxide aqueous solution in the glass liquid storage ball, cleaning the glass liquid storage ball by using the pure water, then placing the pure water into the glass liquid storage ball, adjusting the flow rate to be 3 BV, and leaching until the pH of the leaching solution is about 8.
The iodine-containing wastewater (the iodine content is 4500 ppm) generated in the acetic acid production process is treated at present, the polyaniline/montmorillonite/charcoal composite adsorbing material is used for adsorption treatment for three times through continuous column chromatography, the iodine content can be reduced to 3ppm, and the iodine-containing wastewater treatment cost can be greatly reduced.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (10)
1. A polyaniline/montmorillonite/charcoal composite adsorption material is characterized in that: the polyaniline in the components is obtained by polymerization reaction of aniline, charcoal is aminated charcoal powder, and montmorillonite is montmorillonite modified by silane coupling agent containing amino; the weight ratio of montmorillonite, charcoal and aniline in the raw materials is 0.5-3.
2. The polyaniline/montmorillonite/charcoal composite adsorbing material as claimed in claim 1, wherein: the preparation process of the aminated charcoal powder comprises the steps of uniformly mixing the charcoal powder, a silane coupling agent containing amino, ammonia water and a solvent, reacting for 12-18h at 45-50 ℃, and carrying out solid-liquid separation to obtain the aminated charcoal powder.
3. The polyaniline/montmorillonite/charcoal composite adsorbing material as described in claim 2, wherein: in the preparation process of the aminated charcoal powder, the weight ratio of the charcoal powder, the silane coupling agent containing amino and ammonia water is 1.3-0.4; the solvent is 85-95% ethanol water solution by volume fraction.
4. The polyaniline/montmorillonite/charcoal composite adsorbent material according to any one of claims 1 to 3, wherein: the grain size of the aminated charcoal powder is less than or equal to 0.5 mu m; the grain size of the montmorillonite is less than or equal to 0.5 mu m.
5. A method for preparing the polyaniline/montmorillonite/charcoal composite adsorbing material as described in any one of claims 1 to 4, which is characterized in that: the method comprises the following steps of uniformly dispersing montmorillonite and aminated charcoal powder in aniline, adding protonic acid aqueous solution, uniformly mixing, adjusting the temperature, dropwise adding an initiator, carrying out heat preservation reaction, and carrying out solid-liquid separation to obtain the polyaniline/montmorillonite/charcoal composite adsorbing material.
6. The method for preparing the polyaniline/montmorillonite/charcoal composite adsorbing material as claimed in claim 5, wherein the method comprises the following steps: the montmorillonite and the aminated charcoal powder are evenly dispersed in aniline by ultrasonic for 4-6 h.
7. The method for preparing the polyaniline/montmorillonite/charcoal composite adsorbing material as claimed in claim 5, wherein the method comprises the following steps: regulating the temperature to-15 to-5 ℃, and keeping the temperature for reaction for 12 to 18 hours.
8. The preparation method of the polyaniline/montmorillonite/charcoal composite adsorbing material according to any one of claims 5 to 7, characterized by comprising the following steps: the protonic acid is acetic acid; the concentration of protonic acid aqueous solution is 0.15-0.2mol/L; the weight ratio of aniline, protonic acid and initiator is 1.9-1.1.
9. Use of the polyaniline/montmorillonite/charcoal composite adsorbent material as described in any one of claims 1 to 4 in the treatment of iodine-containing wastewater; the iodine-containing wastewater is iodine-containing wastewater generated in the preparation of acetic acid.
10. The iodine-containing wastewater treatment method is characterized by comprising the following steps: performing column chromatography treatment on the iodine-containing wastewater by using the polyaniline/montmorillonite/charcoal composite adsorbing material as claimed in any one of claims 1 to 4, wherein the number n of the column chromatography treatment is more than or equal to 3, the flow rate of the column chromatography is 1.8 to 2.2 resin bed volumes, and the time of the column chromatography is 8 to 12min; the nth chromatography solution is used as the solution to be treated in the (n + 1) th column chromatography.
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Citations (6)
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| CN102886250A (en) * | 2012-10-23 | 2013-01-23 | 安徽工业大学 | Preparation method of polyaniline/montmorillonite composite adsorbent with sheet structure |
| CN103111272A (en) * | 2013-03-07 | 2013-05-22 | 西北师范大学 | Preparation and application of modified polyaniline-palygorskite composite adsorbent |
| CN104619410A (en) * | 2012-04-23 | 2015-05-13 | 能源及环境研究中心基金会 | Carbon nanocomposite sorbent and methods of using the same for separation of one or more materials from a gas stream |
| US20160122908A1 (en) * | 2013-04-12 | 2016-05-05 | China Petroleum & Chemical Corporation | Polyer/filler/metal composite fiber and preparation method thereof |
| CN105597697A (en) * | 2015-12-30 | 2016-05-25 | 浙江博尼锦纶科技有限公司 | Bamboo charcoal and montmorillonoid composite adsorbent and preparation method thereof |
| CN106334539A (en) * | 2016-10-04 | 2017-01-18 | 青岛大学 | Cationic polymer modified montmorillonoid adsorbent and preparation method thereof |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104619410A (en) * | 2012-04-23 | 2015-05-13 | 能源及环境研究中心基金会 | Carbon nanocomposite sorbent and methods of using the same for separation of one or more materials from a gas stream |
| CN102886250A (en) * | 2012-10-23 | 2013-01-23 | 安徽工业大学 | Preparation method of polyaniline/montmorillonite composite adsorbent with sheet structure |
| CN103111272A (en) * | 2013-03-07 | 2013-05-22 | 西北师范大学 | Preparation and application of modified polyaniline-palygorskite composite adsorbent |
| US20160122908A1 (en) * | 2013-04-12 | 2016-05-05 | China Petroleum & Chemical Corporation | Polyer/filler/metal composite fiber and preparation method thereof |
| CN105597697A (en) * | 2015-12-30 | 2016-05-25 | 浙江博尼锦纶科技有限公司 | Bamboo charcoal and montmorillonoid composite adsorbent and preparation method thereof |
| CN106334539A (en) * | 2016-10-04 | 2017-01-18 | 青岛大学 | Cationic polymer modified montmorillonoid adsorbent and preparation method thereof |
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