CN110665467A - Preparation method of straw-based adsorbent for adsorbing anions/cations - Google Patents
Preparation method of straw-based adsorbent for adsorbing anions/cations Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
Abstract
The invention relates to a preparation method of a straw-based adsorbent for adsorbing anions/cations, belonging to the field of sewage purification treatment. The method comprises the steps of taking straw stalks as raw materials, purifying the straw stalks, carrying out acetylation reaction, preparing a straw stalk base powder material, and grafting carbon disulfide and 2, 3-epoxypropyltrimethylammonium chloride to the straw stalk base powder material respectively to obtain the straw stalk base adsorbent containing anions/cations. The straw stalk-based adsorbent can adsorb anions/cations simultaneously, has obvious adsorption effect, can achieve adsorption balance in 20min, and has adsorption amounts of 79.9mg/g and 93.4mg/g for cationic cadmium ions and anionic acid dye red 1 respectively. The straw stalk based adsorbent for adsorbing anions/cations has the advantages of simple preparation process, obvious adsorption effect, low cost and wide application prospect.
Description
Technical Field
The invention relates to a preparation method of a straw-based adsorbent for adsorbing anions/cations, belonging to the field of sewage purification treatment.
Background
At present, the treatment of water pollution is a main problem facing to people at present. The water pollution treatment method is various, and the adsorbent adsorption method is an important method. Contaminated water bodies contain many various ions, of which anions and cations account for the major part. In many of the current adsorbents, they are mainly directed to adsorption of a single ion, such as a single anion, or a single cation, etc. The invention has great significance if the anions and the cations can be simultaneously adsorbed and removed, and the invention prepares the straw stalk-based adsorbent for adsorbing the anions/the cations based on the purpose, and the adsorbent can simultaneously adsorb the anions and the cations in the water body.
The straw stalk is not suitable for the main recycling way due to the reasons of low lignin content, low nutritional value, low calorific value and the like, is burnt or discarded in large quantity, wastes a large amount of biomass energy and pollutes the environment. Water pollution has seriously affected human health, and the treatment of water pollution is an urgent problem to be solved. If the straw stalk can be effectively applied to the treatment of water pollution, the research is meaningful; in fact, the efficient utilization of biomass resources has become a research hotspot in today's scientific community. The straw stalk contains a large amount of cellulose, hemicellulose and lignin and a small amount of crude protein, inorganic salt and the like, wherein the cellulose, the hemicellulose and the lignin contain a large amount of active hydroxyl groups, so that good conditions are provided for chemical modification of the cellulose, the hemicellulose and the lignin, and in addition, the active hydroxyl groups are good adsorption groups. Application number 201110247024.3 reports preparation and application methods of sulfur dioxide straw stalk adsorbent, the sulfur dioxide straw stalk adsorbent is prepared by swelling, oxidizing and aminating modification of straw stalks, and the straw stalk adsorbent prepared by the method is mainly used for adsorbing sulfur dioxide gas, and harmful ions in water cannot be removed. Due to the uniqueness of the structure and the universality of resources, the straw stalk is interesting for researchers when being used as an adsorbent for adsorbing various water ions. However, the straw-based adsorbent has small density due to the structural characteristics of the straw-based adsorbent, is not easy to sink in water, and is still difficult to change the characteristic of floating in a water body after simple chemical modification; in addition, the specific surface area is small, the number of adsorption sites is small, the adsorption amount needs to be further improved, and the situation that simple chemical modification is difficult to change is also present. Aiming at the adverse factors, the invention aims to prepare the straw stalks into the adsorbent of the powder material, which can simultaneously adsorb anions/cations in the water body.
Disclosure of Invention
The pollution of heavy metal cations and organic dye anions in water bodies to the environment is increasingly intensified, and in order to solve the problem of pollution of the heavy metal cations and the organic dye anions in the water bodies, the invention aims to provide a method for preparing a straw stalk-based adsorbent for adsorbing anions/cations, which comprises the following steps:
(1) and (3) purifying the straw stalks: washing the rice straw for many times by using tap water, and crushing the washed rice straw to 50-100 meshes by using a crusher; sequentially soaking for 1h by using 0.1mol/L hydrochloric acid solution and 0.5mol/L sodium hydroxide solution, and cleaning to be neutral by using clear water; and drying the cleaned straw stalks for later use.
(2) Preparation of acetylated straw stalks: swelling 5-10g of the straw stalks purified in the step (1) in 50mL of glacial acetic acid for 2h, dissolving the straw stalks in a mixed solution of 50-100mL of acetic anhydride and 50-100mL of acetic acid, dropwise adding 2-5mL of 5% dilute sulfuric acid into the system, reacting at 50-70 ℃ for 2h, after the reaction is finished, neutralizing with 1-3g of anhydrous magnesium acetate, pouring the reactant into 800-1000mL of distilled water to separate out acetylated straw stalks, centrifuging and washing the obtained acetylated straw stalks to be neutral, and drying in vacuum.
(3) Preparation of the emulsion: taking 3-5g of acetylated straw stalk material prepared in the step (2) to a round-bottom flask, adding 20-40mL of petroleum ether, and continuously stirring and completely dissolving the acetylated straw stalk material at 38-43 ℃ on a constant temperature electromagnetic stirrer. When the acetylated straw stalks are completely dissolved, adding the mixed solution into a round-bottom flask containing 2-5mL of Ning milk 32, and stirring to uniformly mix the materials. Slowly adding the mixed solution into 50-100mL of saturated stearic acid aqueous solution, and uniformly stirring by using a magnetic rotor to obtain oil-in-water (O/W) type emulsion.
(4) Solidifying the straw-based powder material: adding the emulsion prepared in the step (3) into 300-1000mL of ethyl acetate solvent under the condition of continuous stirring, and continuously stirring to obtain a precipitation solution. And carrying out centrifugal separation, multiple times of washing and low-temperature vacuum drying on the precipitation liquid to obtain the straw stalk-based powder material.
(5) Grafting carbon disulfide on the straw stalk-based powder material: placing 3-5g of the straw stalk-based powder material prepared in the step (4) into a three-neck flask at 45-60 ℃, and placing 5-10mLCS2And 1-2g of potassium carbonate are dissolved in 50-100mL of tetrahydrofuran solution, and the solution is dripped into the straw stalk base powder in 1-2hAnd (3) after the dripping is finished, continuously stirring and reacting for 2-3h, and then filtering, washing and drying to obtain the carbon disulfide grafted straw stalk-based powder material.
(6) Preparation of the straw stalk-based adsorbent: and (2) placing 1-2g of the carbon disulfide grafted straw stalk-based powder material prepared in the step (5) into a three-neck flask at the temperature of 55-65 ℃, regulating and controlling the pH value of the aqueous solution in the three-neck flask to 8-10, dropwise adding 20mL of 10-15% aqueous solution of 2, 3-epoxypropyltrimethylammonium chloride (EPC) into the three-neck flask containing the carbon disulfide grafted straw stalk-based powder material within 0.5-1h, continuously stirring for reaction for 2-3h after dropwise adding, and then filtering, washing and drying to obtain the straw stalk-based adsorbent for adsorbing anions/cations.
The preparation method of the straw stalk-based adsorbent for adsorbing anions/cations of the invention relates to the following chemical reactions:
the chemical reaction involved in the step (5):
the chemical reaction involved in the step (6):
compared with the prior art, the invention has the following beneficial effects:
(1) the adsorbent prepared by the invention takes straw as a main raw material, the straw is a renewable biomass resource, the price is low, and the economic value of the straw can be greatly improved by efficiently utilizing the straw.
(2) The adsorbent prepared by the invention can simultaneously adsorb anions/cations, has obvious adsorption effect, can achieve adsorption balance in 20min, and has the adsorption quantities of 79.9mg/g and 93.4mg/g for cationic cadmium ions and anionic acid dye red 1 respectively.
(3) The straw stalk based adsorbent for adsorbing anions/cations has the advantages of simple preparation process, obvious adsorption effect, low cost and wide application prospect.
Detailed Description
Example 1:
(1) and (3) purifying the straw stalks: washing the rice straw for many times by using tap water, and crushing the washed rice straw to 50 meshes by using a crusher; sequentially soaking for 1h by using 0.1mol/L hydrochloric acid solution and 0.5mol/L sodium hydroxide solution, and cleaning to be neutral by using clear water; and drying the cleaned straw stalks for later use.
(2) Preparation of acetylated straw stalks: swelling 5g of the rice straw purified in the step (1) in 50mL of glacial acetic acid for 2h, dissolving the rice straw in a mixed solution of 50mL of acetic anhydride and 50mL of acetic acid, dropwise adding 2mL of 5% dilute sulfuric acid into the system, reacting at 58 ℃ for 2h, neutralizing with 1g of anhydrous magnesium acetate after the reaction is finished, pouring the reactant into 1000mL of distilled water to separate out acetylated rice straw, centrifuging and washing the obtained acetylated rice straw to be neutral, and drying in vacuum.
(3) Preparation of the emulsion: 3g of the acetylated straw stalk material prepared in step (2) was taken to a round bottom flask, 20mL of petroleum ether was added, and it was continuously stirred and completely dissolved at 39 ℃ on a constant temperature electromagnetic stirrer. When the acetylated straw stalks are completely dissolved, the mixed solution is added into a round-bottom flask containing 2mL of Ningru 32, and the mixture is stirred to be uniformly mixed. Slowly adding the mixed solution into 50mL of saturated stearic acid aqueous solution, and uniformly stirring by using a magnetic rotor to obtain O/W type emulsion.
(4) Solidifying the straw-based powder material: and (3) adding the emulsion prepared in the step (3) into 800mL of ethyl acetate solvent under the condition of continuous stirring, and continuously stirring to obtain a precipitate. And carrying out centrifugal separation, multiple times of washing and low-temperature vacuum drying on the precipitation liquid to obtain the straw stalk-based powder material.
(5) Grafting carbon disulfide on the straw stalk-based powder material: placing 3g of the straw stalk-based powder material prepared in the step (4) into a three-neck flask at 50 ℃, and placing 5ml of solution in the flask2And 1g of potassium carbonate is dissolved in 100mL of tetrahydrofuran solution, the solution is dripped into a three-neck flask filled with straw stalk-based powder material within 1-2h, the stirring reaction is continued for 2-3h after the dripping is finished, and then the mixture is filtered, washed and driedObtaining the carbon disulfide grafted straw stalk base powder material.
(6) Preparation of the straw stalk-based adsorbent: and (2) placing 2g of the carbon disulfide grafted straw stalk-based powder material prepared in the step (5) into a three-neck flask at the temperature of 60 ℃, regulating and controlling the pH value of the aqueous solution in the three-neck flask to 8-10, dropwise adding 20mL of 10% aqueous solution of 2, 3-epoxypropyltrimethylammonium chloride (EPC) into the three-neck flask containing the carbon disulfide grafted straw stalk-based powder material within 0.5-1h, continuously stirring and reacting for 2-3h after dropwise adding is finished, and then filtering, washing and drying to obtain the straw stalk-based adsorbent I for adsorbing anions/cations.
Example 2:
(1) and (3) purifying the straw stalks: washing the rice straw for many times by using tap water, and crushing the washed rice straw to 50 meshes by using a crusher; sequentially soaking for 1h by using 0.1mol/L hydrochloric acid solution and 0.5mol/L sodium hydroxide solution, and cleaning to be neutral by using clear water; and drying the cleaned straw stalks for later use.
(2) Preparation of acetylated straw stalks: swelling 10g of the rice straw purified in the step (1) in 50mL of glacial acetic acid for 2h, dissolving the rice straw in a mixed solution of 100mL of acetic anhydride and 100mL of acetic acid, dropwise adding 5mL of 5% dilute sulfuric acid into the system, reacting at 61 ℃ for 2h, neutralizing with 2g of anhydrous magnesium acetate after the reaction is finished, pouring the reactant into 1000mL of distilled water to separate out acetylated rice straw, centrifuging and washing the obtained acetylated rice straw to be neutral, and drying in vacuum.
(3) Preparation of the emulsion: taking 4g of acetylated straw stalk material prepared in step (2) into a round bottom flask, adding 25mL of petroleum ether, allowing it to continue stirring and dissolve completely at 40 ℃ on a constant temperature electromagnetic stirrer. When the acetylated straw stalks are completely dissolved, the mixed solution is added into a round-bottom flask containing 2.5mL of Ningru 32, and the mixture is stirred to be uniformly mixed. Slowly adding the mixed solution into 80mL of saturated stearic acid aqueous solution, and uniformly stirring by using a magnetic rotor to obtain O/W type emulsion.
(4) Solidifying the straw-based powder material: and (3) adding the emulsion prepared in the step (3) into 1000mL of ethyl acetate solvent under the condition of continuous stirring, and continuously stirring to obtain a precipitate. And carrying out centrifugal separation, multiple times of washing and low-temperature vacuum drying on the precipitation liquid to obtain the straw stalk-based powder material.
(5) Grafting carbon disulfide on the straw stalk-based powder material: placing 3g of the straw stalk-based powder material prepared in the step (4) into a three-neck flask at 52 ℃, and placing 5ml of solution in the flask2And 1.5g of potassium carbonate is dissolved in 80mL of tetrahydrofuran solution, the solution is dripped into a three-neck flask filled with the straw stalk-based powder material within 1-2h, the stirring reaction is continued for 2-3h after the dripping is finished, and then the carbon disulfide grafted straw stalk-based powder material is obtained after filtration, washing and drying.
(6) Preparation of the straw stalk-based adsorbent: and (2) placing 2.5g of the carbon disulfide grafted straw stalk-based powder material prepared in the step (5) into a three-neck flask at the temperature of 61 ℃, regulating and controlling the pH value of an aqueous solution in the three-neck flask to be 8-10, dropwise adding 20mL of 15% aqueous solution of 2, 3-epoxypropyltrimethylammonium chloride (EPC) into the three-neck flask containing the carbon disulfide grafted straw stalk-based powder material within 0.5-1h, continuously stirring and reacting for 2-3h after dropwise adding is finished, and then filtering, washing and drying to obtain the straw stalk-based adsorbent II for adsorbing anions/cations.
Example 3:
(1) and (3) purifying the straw stalks: washing the rice straw for many times by using tap water, and crushing the washed rice straw to 100 meshes by using a crusher; sequentially soaking for 1h by using 0.1mol/L hydrochloric acid solution and 0.5mol/L sodium hydroxide solution, and cleaning to be neutral by using clear water; and drying the cleaned straw stalks for later use.
(2) Preparation of acetylated straw stalks: swelling 8g of the rice straw purified in the step (1) in 50mL of glacial acetic acid for 2h, dissolving the rice straw in a mixed solution of 80mL of acetic anhydride and 80mL of acetic acid, dropwise adding 4mL of 5% dilute sulfuric acid into the system, reacting at 60 ℃ for 2h, neutralizing with 3g of anhydrous magnesium acetate after the reaction is finished, pouring the reactant into 1000mL of distilled water to separate out acetylated rice straw, centrifuging and washing the obtained acetylated rice straw to be neutral, and drying in vacuum.
(3) Preparation of the emulsion: 5g of acetylated straw stalk material prepared in step (2) was taken to a round bottom flask, 40mL of petroleum ether was added, and it was stirred continuously and completely dissolved at 40 ℃ on a constant temperature electromagnetic stirrer. When the acetylated straw stalks are completely dissolved, the mixed solution is added into a round-bottom flask containing 5mL of Ningru 32, and the mixture is stirred to be uniformly mixed. The mixed solution is slowly added into 100mL of saturated stearic acid aqueous solution, and is uniformly stirred by a magnetic rotor to obtain O/W type emulsion.
(4) Solidifying the straw-based powder material: adding the emulsion prepared in the step (3) into 900mL of ethyl acetate solvent under the condition of continuous stirring, and continuously stirring to obtain a precipitate. And carrying out centrifugal separation, multiple times of washing and low-temperature vacuum drying on the precipitation liquid to obtain the straw stalk-based powder material.
(5) Grafting carbon disulfide on the straw stalk-based powder material: putting 4.5g of the straw stalk-based powder material prepared in the step (4) into a three-neck flask at 52 ℃, and putting 10mLCS2And 2g of potassium carbonate is dissolved in 100mL of tetrahydrofuran solution, the solution is dripped into a three-neck flask filled with the straw stalk-based powder material within 1-2h, the stirring reaction is continued for 2-3h after the dripping is finished, and then the carbon disulfide grafted straw stalk-based powder material is obtained after filtration, washing and drying.
(6) Preparation of the straw stalk-based adsorbent: and (2) placing 2g of the carbon disulfide grafted straw stalk base powder material prepared in the step (5) into a three-neck flask at the temperature of 61 ℃, regulating and controlling the pH value of the aqueous solution in the three-neck flask to 8-10, dropwise adding 20mL of 10% aqueous solution of 2, 3-epoxypropyltrimethylammonium chloride (EPC) into the three-neck flask containing the carbon disulfide grafted straw stalk base powder material within 0.5-1h, continuously stirring and reacting for 2-3h after dropwise adding is finished, and then filtering, washing and drying to obtain the straw stalk base adsorbent III for adsorbing anions/cations.
The straw stalk based adsorbents I, II and III prepared by the invention for adsorbing anions/cations are subjected to adsorption performance test:
a. test of Effect of adsorption concentration on adsorption Performance
Preparing activated red 195 solutions with mass concentrations of 20, 40, 100, 200, 300, 400 and 600mg/L respectively, weighing 50mL of each solution with pH of 7, adding 0.1g of straw-based adsorbent I, shaking at a constant temperature of 20 ℃ for 2h, filtering, and measuring the concentration change of the activated red 195 in the solution before and after adsorption by taking the filtrate. The same operation method is adopted, the adsorbents are replaced by straw-based adsorbents II and III, and the activated carbon and the titanium dioxide are respectively measured to obtain the adsorption quantity shown in the table 1.
TABLE 1 adsorption Properties of straw stalk-based adsorbents I, II, III at different adsorption concentrations
As can be seen from Table 1, the adsorption amount of the straw stalk-based adsorbents I, II and III on the active dye activated red 195 is obviously higher than that of the active carbon and titanium dioxide under the same dye concentration.
b. Test of Effect of adsorption temperature on adsorption Performance
Preparing an active red 195 solution with the mass concentration of 300mg/L, weighing 50mL of the solution at each concentration, calibrating the pH value of the solution to be 7, adding 0.1g of straw-based adsorbent I, vibrating at constant temperature of 10 ℃, 20 ℃, 30 ℃, 40 ℃ and 50 ℃ for 2h, filtering, and measuring the concentration change of the active red 195 in the solution before and after adsorption by taking a filtrate. The same operation method was used, and the adsorbents were replaced with straw-based adsorbents II, III, activated carbon and titanium dioxide, and the adsorption amounts were measured, respectively, as shown in Table 2.
TABLE 2 adsorption Properties of straw stalk-based adsorbents I, II, III at different temperatures
As can be seen from Table 2, the adsorption amount of the straw stalk-based adsorbents I, II and III on the active dye activated red 195 is obviously higher than that of the activated carbon and the titanium dioxide at the same temperature. In addition, the adsorption amount of the straw stalk-based adsorbents I, II and III is slightly increased along with the increase of the temperature.
c. Test of the Effect of adsorption time on adsorption Performance
Preparing an active red 195 solution with the mass concentration of 300mg/L, weighing 50mL of the solution at each concentration, calibrating the pH value of the solution to be 7, adding 0.1g of straw-based adsorbent I, shaking for 10min, 20min, 30min, 40min and 50min at a constant temperature of 20 ℃, filtering, and taking the filtrate to measure the concentration change of the active red 195 in the solution before and after adsorption. The same operation method was used, and the adsorbents were replaced with straw-based adsorbents II, III, activated carbon and titanium dioxide, and the adsorption amounts were measured, respectively, as shown in Table 3.
TABLE 3 adsorption performance of the straw stalk-based adsorbents I, II, III after different adsorption times
As can be seen from table 3, the adsorption time of the straw-based adsorbents I, II, and III reaches equilibrium within 20min, and the adsorption equilibrium time of the activated carbon and the titanium dioxide is 30min, which indicates that the straw-based adsorbents I, II, and III can realize the adsorption of the dye within a short time.
d. Adsorption performance test for different kinds of organic dye containing anions
Preparing various dye solutions with the mass concentration of 300mg/L, respectively weighing 50mL of each dye solution with the concentration, calibrating the pH value of the solution to be 7, respectively adding 0.1g of straw-based adsorbent I, oscillating for 2h at the constant temperature of 20 ℃, filtering, and taking the filtrate to measure the concentration change of the dye in the solution before and after adsorption. The same operation method was used to replace the straw-based adsorbent I with the straw-based adsorbents II and III, activated carbon and titanium dioxide, and the adsorption amounts were measured respectively, as shown in table 4.
TABLE 4 adsorption Properties of straw stalk-based adsorbents I, II, III for different kinds of organic dyes containing anions
As can be seen from table 4, for different types of anion containing organic dyes, such as: the reactive dye active red 195, the direct dye lake blue 71, the direct dye red 4BS, the acid dye blue 80, the acid dye red 1 and the straw stalk-based adsorbents I, II and III all have strong adsorption performance.
e. Adsorption performance test for different kinds of metal cations
Preparing various dye solutions with the mass concentration of 300mg/L, respectively weighing 50mL of each dye solution with the concentration, calibrating the pH value of the solution to be 7, respectively adding 0.1g of straw-based adsorbent I, oscillating for 2h at the constant temperature of 20 ℃, filtering, and taking the filtrate to measure the concentration change of the dye in the solution before and after adsorption. The same operation method was used to replace the straw-based adsorbent I with the straw-based adsorbents II and III, activated carbon and titanium dioxide, and the adsorption amounts were measured, respectively, as shown in table 5.
TABLE 5 adsorption Properties of straw-based adsorbents I, II, III for different kinds of metal cations
As can be seen from table 5, for different kinds of metal cations, such as: ca2+、Zn2+、Cu2+、Cd2+、 Hg2+The straw stalk-based adsorbents I, II and III have strong adsorption performance.
f. Testing the adsorption performance of an aqueous solution containing both metal cations and organic dyes containing anions
Preparing a mixed aqueous solution of metal cations with the mass concentration of 300mg/L and organic dye containing anions with the mass concentration of 300mg/L, respectively weighing 50mL of the mixed aqueous solution with the pH value of 7, respectively adding 0.1g of straw-based adsorbent I, oscillating for 2h at the constant temperature of 20 ℃, filtering, and measuring the concentration change of the dye in the solution before and after adsorption by taking the filtrate. The same operation method was used, and the adsorbents were replaced with straw-based adsorbents II and III, activated carbon and titanium dioxide, and were measured, respectively, to obtain the adsorption amounts shown in table 6.
TABLE 6 adsorption performance of straw stalk based adsorbents I, II and III on aqueous solution containing metal cations and organic dye containing anions
As can be seen from Table 6, the straw stalk-based adsorbents I, II and III have strong adsorption performance for the aqueous solution containing both metal cations and organic dyes containing anions.
Finally, it should be noted that the above-mentioned description is only a preferred embodiment of the present invention, and those skilled in the art can make various similar representations without departing from the spirit and scope of the present invention.
Claims (1)
1. A preparation method of a straw stalk-based adsorbent for adsorbing anions/cations is characterized by comprising the following steps:
(1) and (3) purifying the straw stalks: washing the rice straw for many times by using tap water, and crushing the washed rice straw to 50-100 meshes by using a crusher; sequentially soaking for 1h by using 0.1mol/L hydrochloric acid solution and 0.5mol/L sodium hydroxide solution, and cleaning to be neutral by using clear water; and drying the cleaned straw stalks for later use.
(2) And (2) preparing acetylated straw stalks, namely swelling 5-10g of the straw stalks purified in the step (1) in 50mL of glacial acetic acid for 2h, dissolving the swollen straw stalks in a mixed solution of 50-100mL of acetic anhydride and 50-100mL of acetic acid, dropwise adding 2-5mL of 5% dilute sulfuric acid into the system, reacting at 50-70 ℃ for 2h, neutralizing with 1-3g of anhydrous magnesium acetate after the reaction is finished, pouring the reactant into 800-1000mL of distilled water to separate out the acetylated straw stalks, centrifugally washing the obtained acetylated straw stalks to be neutral, and drying in vacuum.
(3) Preparation of the emulsion: taking 3-5g of acetylated straw stalk material prepared in the step (2) to a round-bottom flask, adding 20-40mL of petroleum ether, and continuously stirring and completely dissolving the acetylated straw stalk material at 38-43 ℃ on a constant temperature electromagnetic stirrer. When the acetylated straw stalks are completely dissolved, adding the mixed solution into a round-bottom flask containing 2-5mL of Ning milk 32, and stirring to uniformly mix the materials. Slowly adding the mixed solution into 50-100mL of saturated stearic acid aqueous solution, and uniformly stirring by using a magnetic rotor to obtain O/W type emulsion.
(4) Solidifying the straw-based powder material: adding the emulsion prepared in the step (3) into 300-1000mL of ethyl acetate solvent under the condition of continuous stirring, and continuously stirring to obtain a precipitation solution. And carrying out centrifugal separation, multiple times of washing and low-temperature vacuum drying on the precipitation liquid to obtain the straw stalk-based powder material.
(5) Grafting carbon disulfide on the straw stalk-based powder material: placing 3-5g of the straw stalk-based powder material prepared in the step (4) into a three-neck flask at 45-60 ℃, and placing 5-10mLCS2And dissolving 1-2g of potassium carbonate in 50-100mL of tetrahydrofuran solution, dropwise adding the solution into a three-neck flask filled with the straw stalk-based powder material within 1-2h, continuously stirring for reaction for 2-3h after dropwise adding is finished, and then filtering, washing and drying to obtain the carbon disulfide grafted straw stalk-based powder material.
(6) Preparation of the straw stalk-based adsorbent: and (2) placing 1-2g of the carbon disulfide grafted straw stalk-based powder material prepared in the step (5) into a three-neck flask at the temperature of 55-65 ℃, regulating and controlling the pH value of the aqueous solution in the three-neck flask to 8-10, dropwise adding 20mL of 10-15% aqueous solution of 2, 3-epoxypropyltrimethylammonium chloride (EPC) into the three-neck flask containing the carbon disulfide grafted straw stalk-based powder material within 0.5-1h, continuously stirring for reaction for 2-3h after dropwise adding is finished, and then filtering, washing and drying to obtain the straw stalk-based adsorbent for adsorbing anions/cations.
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| CN111389378A (en) * | 2020-03-27 | 2020-07-10 | 重庆大学 | Amphoteric self-floating adsorbent, preparation method and application |
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