CN108636371B - Preparation method of silver modified cellulose cadmium adsorbent - Google Patents

Preparation method of silver modified cellulose cadmium adsorbent Download PDF

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CN108636371B
CN108636371B CN201810523351.9A CN201810523351A CN108636371B CN 108636371 B CN108636371 B CN 108636371B CN 201810523351 A CN201810523351 A CN 201810523351A CN 108636371 B CN108636371 B CN 108636371B
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凌云
凌天阳
金可心
夏戊君
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Zhongyou Environmental Protection Suzhou Co ltd
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Abstract

A preparation method of a silver modified cellulose cadmium adsorbent belongs to the technical field of adsorbents. The preparation process comprises the following steps: cleaning and drying corn straws, then crushing, adding n-hexane, stirring for reaction, filtering, cleaning and drying, then soaking in alkali liquor, cleaning and drying after soaking to obtain cellulose; pouring the dried cellulose into absolute ethyl alcohol, and adding AgNO3Stirring the solution, filtering, washing with deionized water, and drying; crushing the steel slag, then placing the crushed steel slag into an ethanol solution, adding FeCl after ultrasonic oscillation3Solution and FeCl2Heating the solution in an oil bath pan; adding montmorillonite, bentonite and titanium dioxide into the treated cellulose and steel slag, crushing, granulating, and roasting at high temperature. The silver modified cellulose cadmium adsorbent prepared by the method can effectively remove separants in water, the prepared adsorbent has strong cadmium ion adsorption capacity and large adsorption capacity, and 0.5g of the adsorbent is used for adsorbing 200mg/L of Cd2+The solution adsorption rate is 96.4-99.5%, and the method has a wide application prospect in the treatment of heavy metal cadmium wastewater.

Description

Preparation method of silver modified cellulose cadmium adsorbent
Technical Field
The invention belongs to the technical field of adsorbents, and particularly relates to a preparation method of a silver modified cellulose cadmium adsorbent.
Background
Heavy metal contamination refers to environmental contamination caused by heavy metals or compounds thereof. Mainly caused by human factors such as mining, waste gas discharge, sewage irrigation, use of products with heavy metals exceeding standards and the like. At present, in China, in the processes of mining, smelting and processing of heavy metals, a lot of heavy metals such as lead, mercury, cadmium, cobalt and the like enter the atmosphere, water and soil to cause serious environmental pollution. Heavy metals discharged from wastewater, even if having a low concentration, can accumulate in algae and sediment, and are adsorbed on the body surface of fish and shellfish to cause food chain concentration, thereby causing public nuisance. Heavy metals are difficult to be degraded by microorganisms and can be enriched through a food chain, thereby bringing great harm to animals and human beings.
Cd2+Is a common heavy metal ion in industrial wastewater and is the cause of pain. Since the beginning of the 20 th century, cadmiumThe yield of (a) increases year by year. Cadmium is widely applied to the fields of electroplating industry, chemical industry, electronic industry, nuclear industry and the like. Cadmium is a by-product of the zinc industry, mainly used in batteries, dyes or plastic stabilizers, and is more easily adsorbed by crops than other heavy metals. A considerable amount of cadmium is discharged into the environment through waste gas, waste water and waste residues, causing pollution. The pollution source is mainly lead zinc ore, non-ferrous metal smelting, electroplating and factories using cadmium compound as raw material or catalyst. When the environment is polluted by cadmium, the cadmium can be enriched in organisms and enter the human body through food chains to cause chronic poisoning. Cadmium is absorbed by human body to form cadmium sulfur protein in vivo, which is selectively accumulated in liver and kidney. Among them, the kidney can absorb cadmium which enters nearly 1/3 in vivo, and is the 'target organ' of cadmium poisoning. Other organs such as spleen, pancreas, thyroid and hair also accumulate in a certain amount. Diabetes, proteinuria and aminouria develop in patients due to cadmium damage to renal tubules. In particular, it can block the metabolism of bone, and cause a series of symptoms such as osteoporosis, atrophy and deformity.
Common methods for treating heavy metal wastewater include a chemical precipitation method, an ion exchange method, a membrane separation technology, activated carbon adsorption and the like, and the methods have good effects to a certain extent, but also have the problems of high operation cost, low removal efficiency and the like.
Disclosure of Invention
The technical problem to be solved is as follows: aiming at the technical problems, the invention provides the preparation method of the silver modified cellulose cadmium adsorbent, which has the advantages of simple preparation process, low raw material cost, environmental friendliness, strong cadmium ion adsorption capacity and large adsorption capacity of the prepared product, and the like.
The technical scheme is as follows: a preparation method of a silver modified cellulose cadmium adsorbent comprises the following steps:
weighing 50-60 parts by mass of corn straw, cleaning, drying, crushing, sieving with a sieve of 80-120 meshes, putting 10-20 parts by mass of sieved powder into 60-80 parts by mass of n-hexane, stirring at 30-40 ℃ for 3-5 h, filtering, cleaning, drying, soaking in 40-50 parts by mass of 3mol/LNaOH solution for 15-18 h, filtering, sequentially washing with ultrapure water and 95wt.% ethanol, and drying to obtain cellulose;
step two, pouring the dried cellulose into 10-15 parts by mass of absolute ethyl alcohol, fully wetting, and adding 30-50 parts by mass of 5mg/mL AgNO3Continuously stirring the solution, fully reacting for 7-9 h, filtering, washing for 3 times by using deionized water, and drying;
step three, weighing 2-5 parts by mass of steel slag, crushing the steel slag in a steel slag crusher to 80-120 meshes, dissolving the steel slag in 20-30 parts by mass of 75wt.% ethanol solution, performing ultrasonic oscillation for 1-2 hours, and then adding 20-40 parts by mass of 5mol/LFeCl under the protection of nitrogen3Solution and 20-40 parts by mass of 2.5mol/L FeCl2Completely mixing the solution, adjusting the pH of the mixed solution to 9-10 by using ammonia water, simultaneously adding 1-3 parts by mass of hydrazine hydrate, and then heating in an oil bath kettle at the temperature of 80-90 ℃ for 4-6 h;
step four, weighing 2-4 parts by mass of montmorillonite, 3-6 parts by mass of bentonite and 1-3 parts by mass of titanium dioxide, adding into the modified cellulose dried in the step two, adding the magnetic steel slag heated in the step three, uniformly mixing, putting into a grinding machine for grinding, and sieving with a 20-40-mesh sieve;
and step five, taking 10-20 parts by mass of the crushed mixture, adding 4-8 parts by mass of starch and 6-9 parts by mass of water into the mixture to prepare particles with the diameter of 2mm, and roasting the particles for 2-3 hours at the temperature of 350-450 ℃ to finally prepare the silver modified cellulose cadmium absorbent.
Preferably, in the first step, 55 parts by mass of corn straw is weighed, washed, dried, crushed, sieved by a 100-mesh sieve, 15 parts by mass of sieved powder is placed in 75 parts by mass of n-hexane, stirred at the temperature of 35 ℃ for 4 hours, filtered, washed and dried, then placed in 45 parts by mass of 3mol/L NaOH solution for soaking for 16 hours, filtered, washed by ultrapure water and 95wt.% ethanol in sequence, and dried to obtain the cellulose.
Preferably, in the second step, the dried cellulose is poured into 12 parts by mass of absolute ethyl alcohol, and 34 parts by mass of AgNO with the concentration of 5mg/mL is added after the cellulose is fully wetted3And continuously stirring the solution, fully reacting for 8 hours, filtering, washing for 3 times by using deionized water, and drying.
Preferably, in the third step, 4 parts by mass of steel slag is weighed and crushed to 100 meshes in a steel slag crusher, the crushed steel slag is dissolved in 25 parts by mass of 75wt.% ethanol solution, ultrasonic oscillation is carried out for 1.5h, and then 30 parts by mass of 5mol/LFeCl is added under the protection of nitrogen3Solution and 30 parts by mass of 2.5mol/LFeCl2And (3) completely mixing the solution, adjusting the pH of the mixed solution to 10 by using ammonia water, simultaneously adding 2 parts by mass of hydrazine hydrate, and heating the solution in an oil bath kettle at the temperature of 85 ℃ for 5 hours.
Preferably, 3 parts by mass of montmorillonite, 5 parts by mass of bentonite and 2 parts by mass of titanium dioxide are weighed in the fourth step and added into the modified cellulose dried in the second step, then the magnetic steel slag heated in the third step is added and mixed uniformly and then is put into a grinding machine for grinding, and the mixture is sieved by a 30-mesh sieve.
Preferably, in the fifth step, 15 parts by mass of the crushed mixture is added with 6 parts by mass of starch and 7 parts by mass of water to prepare granules with the diameter of 2mm, and then the granules are roasted at the temperature of 400 ℃ for 2.5 hours to finally prepare the silver modified cellulose cadmium absorbent.
Has the advantages that: the method adopts the corn straws as the raw material, reduces pollution while secondarily utilizing the corn straws, and is safe, environment-friendly and environment-friendly. The silver modified cellulose cadmium adsorbent prepared by the method can effectively remove the separants in water through Ag+Modifying cellulose, and combining the synergistic effect of magnetic steel slag, montmorillonite, bentonite and titanium dioxide to make the prepared adsorbent have strong adsorption capacity of cadmium ion and large adsorption capacity, and 0.5g of the adsorbent is used for adsorbing 200mg/L Cd2+The solution adsorption rate is 96.4-99.5%, the preparation process is simple, and the method has a wide application prospect in the treatment of heavy metal cadmium wastewater.
Detailed Description
Example 1
A preparation method of a silver modified cellulose cadmium adsorbent comprises the following steps:
weighing 50 parts by mass of corn straw, cleaning, drying, crushing, sieving with a 80-mesh sieve, putting 10 parts by mass of sieved powder into 60 parts by mass of n-hexane, stirring at 30 ℃ for 3 hours, filtering, cleaning, drying, soaking in 40 parts by mass of 3mol/LNaOH solution for 15 hours, filtering, washing with ultrapure water and 95wt.% ethanol in sequence, and drying to obtain cellulose.
Step two, pouring the dried cellulose into 10 parts by mass of absolute ethyl alcohol, fully wetting, and adding 30 parts by mass of AgNO with the concentration of 5mg/mL3And continuously stirring the solution, fully reacting for 7 hours, filtering, washing for 3 times by using deionized water, and drying.
Step three, weighing 2 parts by mass of steel slag, crushing the steel slag into 80 meshes in a steel slag crusher, dissolving the steel slag into 20 parts by mass of 75wt.% ethanol solution, ultrasonically vibrating for 1h, and then adding 20 parts by mass of 5mol/LFeCl under the protection of nitrogen3Solution and 20 parts by mass of 2.5mol/LFeCl2And (3) completely mixing the solution, adjusting the pH of the mixed solution to 9 by using ammonia water, simultaneously adding 1 part by mass of hydrazine hydrate, and heating the solution in an oil bath kettle at the temperature of 80 ℃ for 4 hours.
And step four, weighing 2 parts by mass of montmorillonite, 3 parts by mass of bentonite and 1 part by mass of titanium dioxide, adding into the modified cellulose dried in the step two, adding the magnetic steel slag heated in the step three, uniformly mixing, putting into a grinding machine for grinding, and sieving by a 20-mesh sieve.
And step five, taking 10 parts by mass of the crushed mixture, adding 4 parts by mass of starch and 6 parts by mass of water to prepare particles with the diameter of 2mm, and roasting at the temperature of 350 ℃ for 2 hours to finally prepare the silver modified cellulose cadmium absorbent.
Example 2
A preparation method of a silver modified cellulose cadmium adsorbent comprises the following steps:
step one, weighing 60 parts by mass of corn straws, cleaning, drying, crushing, sieving with a 120-mesh sieve, putting 20 parts by mass of sieved powder into 80 parts by mass of n-hexane, stirring at 40 ℃ for 5 hours, filtering, cleaning, drying, soaking in 50 parts by mass of 3mol/LNaOH solution for 18 hours, filtering, washing with ultrapure water and 95wt.% ethanol in sequence, and drying to obtain cellulose.
Step two, pouring the dried cellulose into 15 parts by mass of absolute ethyl alcohol, fully wetting, and adding 50 parts by mass of AgNO with the concentration of 5mg/mL3Solution, continuously stirringStirring, reacting for 9h, filtering, washing with deionized water for 3 times, and drying.
Step three, weighing 5 parts by mass of steel slag, crushing the steel slag into 120 meshes in a steel slag crusher, dissolving the steel slag into 30 parts by mass of 75wt.% ethanol solution, ultrasonically vibrating for 2 hours, and then adding 40 parts by mass of 5mol/L FeCl under the protection of nitrogen3Solution and 40 parts by mass of 2.5mol/LFeCl2And (3) completely mixing the solution, adjusting the pH of the mixed solution to 10 by using ammonia water, simultaneously adding 3 parts by mass of hydrazine hydrate, and heating the solution in an oil bath kettle at the temperature of 90 ℃ for 6 hours.
And step four, weighing 4 parts by mass of montmorillonite, 6 parts by mass of bentonite and 3 parts by mass of titanium dioxide, adding into the modified cellulose dried in the step two, adding the magnetic steel slag heated in the step three, uniformly mixing, putting into a grinding machine for grinding, and sieving by a 40-mesh sieve.
And step five, taking 20 parts by mass of the crushed mixture, adding 8 parts by mass of starch and 9 parts by mass of water to prepare particles with the diameter of 2mm, and roasting at the temperature of 450 ℃ for 3 hours to finally prepare the silver modified cellulose cadmium absorbent.
Example 3
A preparation method of a silver modified cellulose cadmium adsorbent comprises the following steps:
weighing 55 parts by mass of corn straws, cleaning, drying, crushing, sieving with a 100-mesh sieve, putting 15 parts by mass of sieved powder into 75 parts by mass of n-hexane, stirring at 35 ℃ for 4 hours, filtering, cleaning, drying, soaking in 45 parts by mass of 3mol/L NaOH solution for 16 hours, filtering, washing with ultrapure water and 95wt.% ethanol in sequence, and drying to obtain cellulose.
Step two, pouring the dried cellulose into 12 parts by mass of absolute ethyl alcohol, fully wetting, and adding 34 parts by mass of AgNO of 5mg/mL3And continuously stirring the solution, fully reacting for 8 hours, filtering, washing for 3 times by using deionized water, and drying.
Step three, weighing 4 parts by mass of steel slag, crushing the steel slag into 100 meshes in a steel slag crusher, dissolving the steel slag into 25 parts by mass of 75wt.% ethanol solution, ultrasonically vibrating for 1.5h, and then adding 30 parts by mass of 5mol/L FeCl under the protection of nitrogen3Solution and 30 substances2.5mol/LFeCl portions2And (3) completely mixing the solution, adjusting the pH of the mixed solution to 10 by using ammonia water, simultaneously adding 2 parts by mass of hydrazine hydrate, and heating the solution in an oil bath kettle at the temperature of 85 ℃ for 5 hours.
And step four, weighing 3 parts by mass of montmorillonite, 5 parts by mass of bentonite and 2 parts by mass of titanium dioxide, adding into the modified cellulose dried in the step two, adding the magnetic steel slag heated in the step three, uniformly mixing, putting into a grinding machine for grinding, and sieving by a 30-mesh sieve.
And step five, taking 15 parts by mass of the crushed mixture, adding 6 parts by mass of starch and 7 parts by mass of water to prepare particles with the diameter of 2mm, and then roasting at the temperature of 400 ℃ for 2.5 hours to finally prepare the silver modified cellulose cadmium absorbent.
Comparative example 1
The difference from example 3 is that titanium dioxide is not added, and the specific preparation process is as follows:
weighing 55 parts by mass of corn straws, cleaning, drying, crushing, sieving with a 100-mesh sieve, putting 15 parts by mass of sieved powder into 75 parts by mass of n-hexane, stirring at 35 ℃ for 4 hours, filtering, cleaning, drying, soaking in 45 parts by mass of 3mol/L NaOH solution for 16 hours, filtering, washing with ultrapure water and 95wt.% ethanol in sequence, and drying to obtain cellulose.
Step two, pouring the dried cellulose into 12 parts by mass of absolute ethyl alcohol, fully wetting, and adding 34 parts by mass of AgNO of 5mg/mL3And continuously stirring the solution, fully reacting for 8 hours, filtering, washing for 3 times by using deionized water, and drying.
Step three, weighing 4 parts by mass of steel slag, crushing the steel slag into 100 meshes in a steel slag crusher, dissolving the steel slag into 25 parts by mass of 75wt.% ethanol solution, ultrasonically vibrating for 1.5h, and then adding 30 parts by mass of 5mol/L FeCl under the protection of nitrogen3Solution and 30 parts by mass of 2.5mol/LFeCl2And (3) completely mixing the solution, adjusting the pH of the mixed solution to 10 by using ammonia water, simultaneously adding 2 parts by mass of hydrazine hydrate, and heating the solution in an oil bath kettle at the temperature of 85 ℃ for 5 hours.
And step four, weighing 3 parts by mass of montmorillonite and 5 parts by mass of bentonite, adding into the modified cellulose dried in the step two, adding the magnetic steel slag heated in the step three, uniformly mixing, crushing in a grinding machine, and sieving with a 30-mesh sieve.
And step five, taking 15 parts by mass of the crushed mixture, adding 6 parts by mass of starch and 7 parts by mass of water to prepare particles with the diameter of 2mm, and then roasting at the temperature of 400 ℃ for 2.5 hours to finally prepare the silver modified cellulose cadmium absorbent.
Adding Cd (NO)3)2·4H2O (analytically pure) is prepared into stock solution with the metal ion concentration of 200mg/L, and the stock solution is sealed and stored at low temperature for later use after 1 wt.% nitric acid is added. Taking four groups of 50mL Cd with initial concentration of 200mg/L2+And (3) putting the solution in a conical flask with the volume of 150mL, adjusting the pH value of the metal ion solution to be 4, then respectively adding 0.5g of the silver modified cellulose cadmium absorbent prepared in the examples 1-3 and the comparative example 1, then rotating and oscillating for 1h at room temperature at the rotating speed of 150r/min, sampling, centrifuging and diluting after the reaction is finished, and measuring the concentration of the heavy metal ions by using an atomic absorption spectrometer. The cadmium removal rate (%) was calculated by the following formula.
The amount of adsorption was calculated as follows:
Figure BDA0001675324400000051
in the formula qeIs the equilibrium adsorption capacity, mg/g; c. C0Is the initial concentration of the solution, mg/L; c. CeIs the equilibrium concentration of the solution after adsorption, mg/L; v is the volume of the solution, L; m is the mass of added adsorbent, g.
The cadmium removal rate eta (%) is calculated as follows:
Figure BDA0001675324400000052
see table below for calculation results.
Cadmium removal rate/%)
Example 1 97.1
Example 2 96.4
Example 3 99.5
Comparative example 1 86.7

Claims (6)

1. The preparation method of the silver modified cellulose cadmium adsorbent is characterized by comprising the following steps:
weighing 50-60 parts by mass of corn straw, cleaning, drying, crushing, sieving with a sieve of 80-120 meshes, putting 10-20 parts by mass of sieved powder into 60-80 parts by mass of n-hexane, stirring at 30-40 ℃ for 3-5 h, filtering, cleaning, drying, soaking in 40-50 parts by mass of 3mol/L NaOH solution for 15-18 h, filtering, washing with ultrapure water and 95wt.% ethanol in sequence, and drying to obtain cellulose;
step two, pouring the dried cellulose into 10-15 parts by mass of absolute ethyl alcohol, fully wetting, and adding 30-50 parts by mass of 5mg/mL AgNO3Continuously stirring the solution, fully reacting for 7-9 h, filtering, washing for 3 times by using deionized water, and drying;
step three, weighing 2-5 parts by mass of steel slag, crushing the steel slag in a steel slag crusher to 80-120 meshes, dissolving the steel slag in 20-30 parts by mass of 75wt.% ethanol solution, performing ultrasonic oscillation for 1-2 hours, and then adding 20-40 parts by mass of 5mol/L FeCl under the protection of nitrogen3Solution and 20-40 parts by mass of 2.5mol/L FeCl2Completely mixing the solution, adjusting the pH of the mixed solution to 9-10 by using ammonia water,simultaneously adding 1-3 parts by mass of hydrazine hydrate, and heating in an oil bath kettle at the temperature of 80-90 ℃ for 4-6 hours;
step four, weighing 2-4 parts by mass of montmorillonite, 3-6 parts by mass of bentonite and 1-3 parts by mass of titanium dioxide, adding into the modified cellulose dried in the step two, adding the magnetic steel slag heated in the step three, uniformly mixing, putting into a grinding machine for grinding, and sieving with a 20-40-mesh sieve;
and step five, taking 10-20 parts by mass of the crushed mixture, adding 4-8 parts by mass of starch and 6-9 parts by mass of water to prepare particles with the diameter of 2mm, and roasting at the temperature of 350-450 ℃ for 2-3 hours to finally prepare the silver modified cellulose cadmium adsorbent.
2. The preparation method of the silver-modified cellulose cadmium adsorbent according to claim 1, wherein 55 parts by mass of corn stalks are weighed in the first step, washed, dried, crushed, sieved by a 100-mesh sieve, 15 parts by mass of sieved powder are placed in 75 parts by mass of n-hexane, stirred at 35 ℃ for 4 hours, filtered, washed and dried, then placed in 45 parts by mass of 3mol/L NaOH solution for soaking for 16 hours, filtered, washed by ultrapure water and 95wt.% ethanol in sequence, and dried to obtain cellulose.
3. The method for preparing the silver modified cellulose cadmium adsorbent according to claim 1, wherein in the second step, the dried cellulose is poured into 12 parts by mass of absolute ethyl alcohol, and 34 parts by mass of 5mg/mL AgNO is added after the cellulose is fully wetted3And continuously stirring the solution, fully reacting for 8 hours, filtering, washing for 3 times by using deionized water, and drying.
4. The preparation method of the silver-modified cellulose cadmium adsorbent according to claim 1, wherein in the third step, 4 parts by mass of steel slag are weighed and crushed to 100 meshes in a steel slag crusher, the crushed steel slag is dissolved in 25 parts by mass of 75wt.% ethanol solution, ultrasonic oscillation is performed for 1.5h, and then 30 parts by mass of 5mol/L FeCl is added under the protection of nitrogen3Solution and 30 parts by mass of 2.5mol/L FeCl2Mixing completely, mixing with ammonia waterThe pH of the solution was adjusted to 10 while adding 2 parts by mass of hydrazine hydrate, and then heated in an oil bath pan at 85 ℃ for 5 hours.
5. The preparation method of the silver modified cellulose cadmium adsorbent according to claim 1, wherein 3 parts by mass of montmorillonite, 5 parts by mass of bentonite and 2 parts by mass of titanium dioxide are weighed in the fourth step and added to the modified cellulose dried in the second step, and then the magnetic steel slag heated in the third step is added to be uniformly mixed and then put into a grinding machine to be ground, and the mixture is sieved by a 30-mesh sieve.
6. The preparation method of the silver modified cellulose cadmium adsorbent according to claim 1, wherein 15 parts by mass of the crushed mixture is taken in the fifth step, 6 parts by mass of starch and 7 parts by mass of water are added to prepare particles with the diameter of 2mm, and then the particles are roasted at 400 ℃ for 2.5 hours to finally prepare the silver modified cellulose cadmium adsorbent.
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