CN113522254B - Preparation method and application of nylon 65 material with porous structure - Google Patents

Preparation method and application of nylon 65 material with porous structure Download PDF

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CN113522254B
CN113522254B CN202110842975.9A CN202110842975A CN113522254B CN 113522254 B CN113522254 B CN 113522254B CN 202110842975 A CN202110842975 A CN 202110842975A CN 113522254 B CN113522254 B CN 113522254B
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王训遒
高智城
张雷
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Zhengzhou University
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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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    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28042—Shaped bodies; Monolithic structures
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    • 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
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    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract

The invention discloses a preparation method and application of a nylon 65 material with a porous structure, wherein a nylon 65 salt is synthesized by a patent CN108285532B, a nylon 65 raw material is prepared by a patent CN112920401A through melt polymerization, anhydrous formic acid and the nylon 65 material are mixed and dissolved, the nylon 65 formic acid solution which is fully dissolved is placed in a container with a proper size, and a sodium carbonate solution is added for liquid foaming to prepare the nylon 65 material with the porous structure with excellent adsorption performance. The nylon 65 material with the porous structure prepared by the process has strong adsorption property by virtue of the special structure, and has the characteristics of high temperature resistance, strong acid resistance, high efficiency in removing waste water dye, reusability and the like. The nylon 65 adsorbing material can be used for adsorbing dye wastewater, and has the advantages of environmental protection, economy and high efficiency.

Description

Preparation method and application of nylon 65 material with porous structure
Technical Field
The invention belongs to the field of chemical materials, and particularly relates to a preparation method and application of a nylon 65 material with a porous structure and excellent performance for treating dye wastewater.
Background
With the progress of society, people's lives are more colorful, the dye industry is also developed, china has become the first big country of the printing and dyeing industry, the dye yield is 20-25 ten thousand t each year, but along with the generation of dye wastewater, the dye wastewater has various hazards of complex components, deep color, high toxicity, strong acidity (alkalinity), a large amount of negative ions and the like. The main pollutants in the waste water dye comprise high suspended matters, chlorides, sulfates and other soluble substances. Although there is a large amount of water in the wastewater, residual dyes in the wastewater are accumulated, and thus, the concentration and color of the dyes are gradually increased, and since the dyes absorb sunlight and the color has a great influence on the absorption of the sunlight, plants beside the river are killed and the ecosystem is seriously affected.
In view of this, with the development and update of the dye industry, the pollution components in the waste water dye are more and more, the purification technology and method for the waste water dye also need to be continuously updated and developed, and it is also necessary to adopt a proper and low-cost treatment method for different kinds of dye waste water.
The various colors imparted by the dyes are affected by chromophores and auxochromes, and can be classified into acid dyes, basic dyes, disperse dyes, etc. according to the chromophore structure of the dyes, and can also be classified into cationic dyes, anionic dyes, and nonionic dyes by the difference in structure. At present, the dye wastewater treatment methods commonly used in China are a physical method, a chemical method and a biological method. Although the biological method is economical, the treatment time is long, the microbial culture is slow, and the process flow is complex. The chemical method has small equipment and simple equipment management, but has complicated electrode materials, high cost and high operating cost. The adsorption method in the physical method has obvious decolorization, simple operation and high purification speed, and is a more suitable treatment method.
The mode of treating the waste water dye by the adsorption method is to carry out adsorption purification by the complexation, electrostatic interaction, hydrophobic interaction, hydrogen bond interaction and the like of the material and the dye. Eloisa Navarro et al found that nylon 65 has hydrogen bonds in two directions, and Naoya Ogata et al studied the adhesion of affinity groups (hydrogen bonds) of various polyamides to human platelets medically using the microsphere method, and the study showed that nylon 65 has better adhesion than other types of polyamides, indicating that nylon 65 has a special structure. In view of this, the nylon 65 material with the porous structure prepared by the invention has high efficiency and pertinence, the material has the advantages of special molecular structure, porosity and the like, and can adsorb a large amount of dye, the dye removal rate can reach more than 90%, and at present, research on adsorption of dye wastewater by the nylon 65 material with the porous structure is not reported.
Disclosure of Invention
In order to overcome the problems, the invention provides a preparation method and application of a nylon 65 material which has a porous structure and can absorb dye wastewater, wherein the nylon 65 material has a high cost performance, can obtain a material which has a mesoporous structure, is high temperature resistant, has low density and excellent absorption performance, and has a removal rate of dye wastewater of more than 90%.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a nylon 65 material with a porous structure comprises the following steps:
(1) Adding the nylon 65 raw material into anhydrous formic acid, and stirring to fully dissolve;
(2) And (2) adding a sodium carbonate solution into the step (1) and carrying out liquid foaming to obtain the nylon 65 material with high adsorption performance and a porous structure.
Further, the nylon 65 raw material in the step (1) is firstly synthesized into nylon 65 salt by a patent CN108285532B, and then is prepared into the nylon 65 raw material by the melt polymerization of a published patent CN 112920401A.
Further, the mass ratio of the nylon 65 raw material to the anhydrous formic acid in the step (2) is 1:2-1, preferably 1:3-1. If the raw material content in the solution is too low, foaming may be unsuccessful; the solution has too high raw material content, large solution viscosity and poor fluidity, which is not beneficial to foaming.
Further, the mass fraction of the sodium carbonate solution in the step (3) is 1% -40%, preferably 1% -10%, and the addition amount of the sodium carbonate solution is based on foaming.
The specific surface area of the nylon 65 material with the porous structure prepared by the method is 2-40m 2 The mesoporous carbon material has a mesoporous structure, the aperture of mesopores is 1nm-7nm, the removal rate of anionic wastewater dye reaches more than 90%, and the mesoporous carbon material is high-temperature resistant and strong-acid resistant.
The nylon 65 material with the porous structure prepared by the method is used for adsorbing dye wastewater, namely the nylon 65 material adsorbs simulated dye wastewater under the conditions of certain temperature, pH and mechanical oscillation.
Further, the dye is one or more of anionic dye, cationic dye or nonionic dye. The dye wastewater is preferably anionic dye wastewater. According to the molecular structure of nylon 65, the adsorption of the anionic dye wastewater is larger than that of the cationic dye wastewater and the nonionic dye wastewater.
Further, the temperature for adsorbing the dye wastewater is 5-60 ℃, and preferably 20-50 ℃; the pH of the dye-adsorbing wastewater is 2-13, preferably 2-9.
Further, the speed of mechanical oscillation at the time of adsorbing the dye wastewater is 10 to 500rmp, preferably 50 to 200rmp.
Further, the nylon 65 material with the porous structure can be made to have reusability by formulating a desorbent, wherein the desorbent is one or more of sodium hydroxide solution, potassium hydroxide solution, ethanol solution, sodium carbonate solution and sodium bicarbonate solution.
The invention has the beneficial effects that:
(1) The invention provides a preparation method and application conditions of a nylon 65 material with a porous structure and capable of efficiently adsorbing a large amount of dye wastewater.
(2) The adsorbent is economic and environment-friendly, has simple device and convenient operation, can be produced in large quantities, and can be repeatedly used and keep the adsorption performance unchanged under the condition of specific desorbent, thereby greatly improving the economic benefit.
(3) The adsorbent has a porous structure, can greatly improve the effect of adsorbing dye wastewater, has a removal rate of more than 90% on anionic wastewater dye, and is high-temperature resistant and strong-acid resistant.
Drawings
FIG. 1 is a thermogravimetric plot of a nylon 65 material having a cellular structure;
FIG. 2 is a Scanning Electron Microscope (SEM) image of a nylon 65 material having a cellular structure;
fig. 3 is a diagram showing the distribution of pore diameters of a nylon 65 material having a porous structure.
Detailed Description
In order to make the present invention more clear, the present invention is explained in more detail below with reference to some examples. All embodiments of the invention obtained by the person skilled in the art without going into any more creative work are within the scope of protection of the present invention.
In a specific example, after a series of dyes with different concentration gradients are prepared, the absorbance versus concentration is determined by a UV-Vis spectrophotometer. The relationship between absorbance and concentration can be calculated according to the following standard curve equations (1) (2) (3) (4).
(1) Standard curve equation for methyl orange:
Figure BDA0003179724410000041
(2) Standard curve equation for methyl red:
Figure BDA0003179724410000042
(3) Standard curve equation for acid fuchsin:
Figure BDA0003179724410000043
(4) Standard curve equation for orange G:
Figure BDA0003179724410000044
wherein x represents the dye concentration (mg/L) and y represents the absorbance (Abs).
In a specific example, the dye removal rate is calculated using equation (5). The pH was adjusted using 0.1mol/L NaOH and 0.1mol/L HCl solution.
Figure BDA0003179724410000045
Wherein C is i And C f The initial concentration (mg/L) and the final concentration (mg/L) of the dye wastewater are shown.
Example 1
The preparation method of the nylon 65 material with the porous structure and capable of adsorbing the dye wastewater comprises the following steps:
2g of nylon 65 sample prepared by melt polycondensation was added to 8g of formic acid solution to prepare a 20wt% nylon 65 formic acid solution, which was shaken at room temperatureStirring or stirring to dissolve nylon 65 sample, transferring the sample solution into a clean 30ml container, and continuously injecting Na with pinhole syringe 2 CO 3 Aqueous solution (5 wt% Na) 2 CO 3 Aqueous solution) with formic acid to foam to prepare the nylon 65 material with a porous structure.
The prepared porous PA65 is ground and screened and collected by an 80-mesh screen for subsequent experiments.
The application of the nylon 65 material with the porous structure capable of adsorbing the dye wastewater in the embodiment is as follows:
the prepared nylon 65 adsorbent was added to a 100mg/L methyl orange solution using a 50ml glass container, and further, the pH of the solution in the system was adjusted to 5, and the mixture was shaken at 30 ℃ for 1 hour at 100rmp using a mechanical shaker. After the reaction was completed, the adsorbent was filtered, and the filtrate absorbance was measured at 462nm at the maximum absorption wavelength of the dye using a UV-Vis spectrophotometer.
The nylon 65 adsorbent with the porous structure is repeatedly washed for 3-5 times by using a sodium hydroxide/ethanol solution (more than or equal to 2 mol/L), then an adsorption experiment is repeatedly carried out for 10 times under the same condition, and the repeated effect of the nylon 65 adsorbent with the porous structure is measured.
Example 2
The preparation method of the nylon 65 material with the porous structure and capable of adsorbing the dye wastewater comprises the following steps:
adding 4g of nylon 65 sample prepared by a melt polycondensation method into 8g of formic acid solution to prepare 33wt% of nylon 65 formic acid solution, shaking or stirring at room temperature to fully dissolve the nylon 65 sample, transferring the sample solution into a prepared clean container with the size of 30ml, and continuously injecting Na into the container by using a pinhole syringe 2 CO 3 Aqueous solution (5 wt% Na) 2 CO 3 Aqueous solution) was reacted with formic acid to foam to prepare a nylon 65 material having a porous structure.
The prepared porous PA65 is ground and screened and collected by an 80-mesh screen for subsequent experiments.
The application of the nylon 65 material with the porous structure capable of adsorbing the dye wastewater in the embodiment is as follows:
the prepared nylon 65 adsorbent was added to a 50mg/L methyl red solution using a 50ml glass container, and further, the pH of the solution in the system was adjusted to 4, and the mixture was shaken at 35 ℃ for 1 hour at 150rmp using a mechanical shaker. After the reaction was completed, the adsorbent was filtered, and the filtrate absorbance was measured at 410nm at the maximum absorption wavelength of the dye using a UV-Vis spectrophotometer.
The nylon 65 adsorbent with the porous structure is repeatedly washed for 3-5 times by using a sodium hydroxide solution (more than or equal to 2 mol/L), and then an adsorption experiment is carried out for 10 times under the same condition, so that the repeated effect of the nylon 65 adsorbent with the porous structure is measured.
Example 3
The preparation method of the nylon 65 material with the porous structure and capable of adsorbing the dye wastewater comprises the following steps:
adding 2g of nylon 65 sample prepared by a melt polycondensation method into 8g of formic acid solution to prepare 20wt% of nylon 65 formic acid solution, shaking or stirring at room temperature to fully dissolve the nylon 65 sample, transferring the sample solution into a prepared clean container with the size of 30ml, and continuously injecting Na into the container by using a pinhole syringe 2 CO 3 Aqueous solution (3 wt% Na) 2 CO 3 Aqueous solution) with formic acid to foam to prepare the nylon 65 material with a porous structure.
The prepared porous PA65 is ground and screened and collected by an 80-mesh screen for subsequent experiments.
The application of the nylon 65 material with the porous structure capable of adsorbing the dye wastewater in the embodiment is as follows:
the prepared nylon 65 adsorbent was added to a 100mg/L orange G solution using a 50ml glass container, further, the pH of the solution in the system was adjusted to 8, and the mixture was shaken at 30 ℃ for 1 hour at 150rmp using a mechanical shaker. After the reaction was completed, the adsorbent was filtered, and the filtrate absorbance was measured at 476nm at the dye maximum absorption wavelength using a UV-Vis spectrophotometer.
The nylon 65 adsorbent with the porous structure is repeatedly washed for 3-5 times by using potassium hydroxide solution (more than or equal to 2 mol/L), and then 10 repeated adsorption experiments are carried out under the same conditions, and the repeated effect of the nylon 65 adsorbent with the porous structure is measured.
Example 4
The preparation method of the nylon 65 material with the porous structure and capable of adsorbing the dye wastewater comprises the following steps:
adding 1g of nylon 65 sample prepared by a melt polycondensation method into 8g of formic acid solution to prepare 11wt% of nylon 65 formic acid solution, shaking or stirring at room temperature to fully dissolve the nylon 65 sample, transferring the sample solution into a prepared clean container with the size of 30ml, and continuously injecting Na into the container by using a pinhole syringe 2 CO 3 Aqueous solution (5 wt% Na) 2 CO 3 Aqueous solution) was reacted with formic acid to foam to prepare a nylon 65 material having a porous structure.
The prepared porous PA65 is ground and screened and collected by an 80-mesh screen for subsequent experiments.
The application of the nylon 65 material with the porous structure capable of adsorbing the dye wastewater in the embodiment is as follows:
the prepared nylon 65 adsorbent was added to a 100mg/L acid fuchsin solution using a 50ml glass container, further, the pH of the solution in the system was adjusted to 6, and the mixture was shaken at 200rmp for 1 hour at 40 ℃ using a mechanical shaker. After the reaction was completed, the adsorbent was filtered, and the filtrate absorbance was measured at 546nm at the dye maximum absorption wavelength using a UV-Vis spectrophotometer.
The nylon 65 adsorbent with the porous structure is repeatedly washed for 3-5 times by using a potassium hydroxide/ethanol solution (more than or equal to 2 mol/L), then an adsorption experiment is repeatedly carried out for 10 times under the same condition, and the repeated effect of the nylon 65 adsorbent with the porous structure is measured.
Example 5
The preparation method of the nylon 65 material with the porous structure capable of adsorbing the dye wastewater of the embodiment comprises the following steps:
adding 2g of nylon 65 sample prepared by a melt polycondensation method into 8g of formic acid solution to prepare 20wt% of nylon 65 formic acid solution, shaking or stirring at room temperature to fully dissolve the nylon 65 sample, transferring the sample solution into a prepared clean container with the size of 30ml, and continuously injecting Na into the container by using a pinhole syringe 2 CO 3 Aqueous solution (5 wt% Na) 2 CO 3 Aqueous solution) was reacted with formic acid to foam to prepare a nylon 65 material having a porous structure.
The prepared porous PA65 is ground and screened and collected by an 80-mesh sieve for subsequent experiments.
The application of the nylon 65 material with the porous structure capable of adsorbing the dye wastewater in the embodiment is as follows:
the prepared nylon 65 adsorbent was added to a 300mg/L methyl orange solution using a 50ml glass container, and further, the pH of the solution in the system was adjusted to 5, and the mixture was shaken at 50 ℃ for 1 hour at 100rmp using a mechanical shaker. After the reaction was completed, the adsorbent was filtered, and the filtrate absorbance was measured at 462nm at the maximum absorption wavelength of the dye using a UV-Vis spectrophotometer.
The nylon 65 adsorbent with the porous structure is repeatedly washed for 3-5 times by using a sodium hydroxide/ethanol solution (more than or equal to 2 mol/L), then an adsorption experiment is repeatedly carried out for 10 times under the same condition, and the repeated effect of the nylon 65 adsorbent with the porous structure is measured.
Example 6
The preparation method of the nylon 65 material with the porous structure and capable of adsorbing the dye wastewater comprises the following steps:
adding 4g of nylon 65 sample prepared by a melt polycondensation method into 8g of formic acid solution to prepare 33wt% of nylon 65 formic acid solution, shaking or stirring at room temperature to fully dissolve the nylon 65 sample, transferring the sample solution into a prepared clean container with the size of 30ml, and continuously injecting Na into the container by using a pinhole syringe 2 CO 3 Aqueous solution (5 wt% Na) 2 CO 3 Aqueous solution) was reacted with formic acid to foam to prepare a nylon 65 material having a porous structure.
The prepared porous PA65 is ground and screened and collected by an 80-mesh screen for subsequent experiments.
The application of the nylon 65 material with the porous structure capable of adsorbing the dye wastewater in the embodiment is as follows:
the prepared nylon 65 adsorbent was added to a 100mg/L methyl red solution using a 50ml glass container, and further, the pH of the solution in the system was adjusted to 4, and the mixture was shaken at 35 ℃ for 1 hour at 200rmp using a mechanical shaker. After the reaction was completed, the adsorbent was filtered, and the filtrate absorbance was measured at 410nm at the maximum absorption wavelength of the dye using a UV-Vis spectrophotometer.
The nylon 65 adsorbent with the porous structure is repeatedly washed for 3-5 times by using a sodium hydroxide/potassium hydroxide solution (more than or equal to 2 mol/L), then an adsorption experiment is repeatedly carried out for 10 times under the same condition, and the repeated effect of the nylon 65 adsorbent with the porous structure is measured.
Example 7
The preparation method of the nylon 65 material with the porous structure capable of adsorbing the dye wastewater of the embodiment comprises the following steps:
adding 2g of nylon 65 sample prepared by a melt polycondensation method into 8g of formic acid solution to prepare 20wt% of nylon 65 formic acid solution, shaking or stirring at room temperature to fully dissolve the nylon 65 sample, transferring the sample solution into a prepared clean container with the size of 30ml, and continuously injecting Na into the container by using a pinhole syringe 2 CO 3 Aqueous solution (3 wt% Na) 2 CO 3 Aqueous solution) with formic acid to foam to prepare the nylon 65 material with a porous structure.
The prepared porous PA65 is ground and screened and collected by an 80-mesh screen for subsequent experiments.
The application of the nylon 65 material with the porous structure capable of adsorbing the dye wastewater in the embodiment is as follows:
the prepared nylon 65 adsorbent was added to a 100mg/L orange G solution using a 50ml glass container, and further, the pH of the solution in the system was adjusted to 2, and the mixture was shaken at 150rmp for 1 hour at 30 ℃ using a mechanical shaker. After the reaction was completed, the adsorbent was filtered, and the filtrate absorbance was measured at 476nm at the dye maximum absorption wavelength using a UV-Vis spectrophotometer.
The nylon 65 adsorbent with the porous structure is repeatedly washed for 3-5 times by using a sodium hydroxide solution (more than or equal to 2 mol/L), and then an adsorption experiment is carried out for 10 times under the same condition, so that the repeated effect of the nylon 65 adsorbent with the porous structure is measured.
Comparison of Properties in the examples of Table 1
Figure BDA0003179724410000091
Figure BDA0003179724410000101
In conclusion, the nylon 65 adsorbing material with the porous structure is simple to prepare, easy to perform in adsorption conditions, economical and environment-friendly, and can effectively remove anionic dyes under acidic or neutral conditions.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The embodiments described above are some examples of the present invention, and are intended to be illustrative and not limiting. To those skilled in the art, the present invention is susceptible to a certain degree of modification and substitution without departing from the spirit and scope of the technical solution of the embodiments of the present invention. The invention is therefore limited only by the claims and not by the embodiments described above.

Claims (2)

1. Is provided withThe application of the nylon 65 material with the porous structure in dye adsorption wastewater is characterized in that: the specific surface area of the nylon 65 material is 2-40m 2 The material has a mesoporous structure, the aperture of the mesopores is 1-7 nm, and the nylon 65 material adsorbs the simulated dye wastewater under the conditions of certain temperature, pH and mechanical oscillation;
the dye is one or more of anionic dye, cationic dye or nonionic dye; the temperature of the dye adsorption wastewater is 5-60 ℃, and the pH of the dye adsorption wastewater is 2-13;
the speed of mechanical oscillation when adsorbing the dye wastewater is 10-500rmp;
the preparation method of the nylon 65 material with the porous structure comprises the following steps:
(1) Adding the nylon 65 raw material into anhydrous formic acid, and stirring to fully dissolve;
(2) Adding a sodium carbonate solution into the step (1), and performing liquid foaming to obtain a nylon 65 material with high adsorption performance and a porous structure;
the nylon 65 raw material in the step (1) is prepared by firstly synthesizing nylon 65 salt by a patent CN108285532B, and then carrying out melt polymerization by a published patent CN 112920401A;
the mass ratio of the nylon 65 raw material to the anhydrous formic acid in the step (2) is 1:2-1;
the mass fraction of the sodium carbonate solution in the step (2) is 1-40%, and the addition amount of the sodium carbonate solution is based on reaching foaming.
2. Use according to claim 1, characterized in that: the nylon 65 material with a porous structure can be made to have reusability by formulating a desorbent, wherein the desorbent is one or more of sodium hydroxide solution, potassium hydroxide solution, ethanol solution, sodium carbonate solution and sodium bicarbonate solution.
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