CN102266756B - Preparation method of citric acid modified rape straw adsorbent and application thereof - Google Patents
Preparation method of citric acid modified rape straw adsorbent and application thereof Download PDFInfo
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- CN102266756B CN102266756B CN 201110208310 CN201110208310A CN102266756B CN 102266756 B CN102266756 B CN 102266756B CN 201110208310 CN201110208310 CN 201110208310 CN 201110208310 A CN201110208310 A CN 201110208310A CN 102266756 B CN102266756 B CN 102266756B
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Abstract
The invention belongs to the technical field of industrial waste water treatment and pollution treatment, in particular to a preparation method of a citric acid modified rape straw adsorbent and an application thereof. The method comprises the following steps of: firstly washing natural rape straws, drying, crashing, sieving for standby; and then modifying the surface of the rape straws with citric acid so as to prepare the novel adsorbent citric acid modified rape straws. The prepared adsorbent is used for treating industrial waste water, and removing cationic dye and heavy metal ions form the waste water. The result of a static absorption test shows the adsorbent has excellent adsorption effect for the cationic dye and heavy metal ions. By the invention, the agriculture waste resource is recycled; and cheap and efficient novel adsorbent is obtained to be used for treating the industrial waste water. The preparation process of the adsorbent is simple, and the prepared adsorbent has low cost and excellent adsorption effect.
Description
Technical field
The present invention relates to the technical field of pollutant control in the preparation of biological adsorption agent and the industrial wastewater, be specifically related to a kind of preparation method and application of citric acid modified rape straw adsorbent.
Background technology
Along with the development of dye industry, problem of environmental pollution becomes increasingly conspicuous, and waste water from dyestuff has become at present one of main harmful industrial wastewater of China.Because having complicated aromatic ring structure, stable in properties is difficult to biodegradation in the dye structure.These groups also can cause skin irritatin to the mankind, allergic dermatitis, the injuries such as cancer and gene mutation.Waste water from dyestuff makes river painted, heavy damage the natural, ecological chain of water body, also greatly reduce simultaneously the economic worth of water body.Therefore, how to remove the focus that dyestuff in the industrial wastewater becomes the lot of domestic and foreign scholar's research.The method of traditional removal Wastewater Dyes has: chemical coagulation process, oxidizing process, filtration method, biological treatment, absorption method etc.Wherein to have technique simple for absorption method, and adsorption efficiency is high, and the scope of application is wide, stable performance and be conducive to the characteristics such as comprehensive utilization and be widely used in sewage disposal.Because kind of dyes is various in the dyeing waste water, selecting suitable adsorbent is the key point of using the absorption method dye wastewater treatment using.
In recent years, utilize material cheap and easy to get in the processing of waste water from dyestuff, to obtain more research as adsorbent.Rape is the industrial crops of extensively planting in China.Annual all can have a large amount of rape stalks to produce.The lignin that contains in the natural straw structure, cellulose and hemicellulose itself can be used as active group and are applied to wastewater treatment, but make its application limited because its absorption property is lower.Therefore, in order to improve the absorption property of rape stalk, strengthen its utilization ratio, the present invention uses citric acid its surface is modified.At present, use citric acid modified rape straw and yet there are no report as adsorbent for the treatment of waste water.
Summary of the invention
For the deficiencies in the prior art, preparation method and the application of a kind of operating procedure citric acid modified rape straw adsorbent simple, with low cost have been the object of the present invention is to provide.
To achieve these goals, the preparation method of a kind of citric acid modified rape straw adsorbent that the present invention proposes, concrete steps are as follows:
(1) physical treatment of material:
Further grind with mixer after the rape stalk of drying is cut into segment, then cross 100 order sub-sieves, getting the sub-sieve lower part of screen divides with after distilled water cleaning 3-6 time, until filtrate becomes clarification, the rape stalk powder that obtains gets dry rape stalk powder behind the dry 24h in 55 ℃ of electric drying oven with forced convections with the vavuum pump suction filtration.(2) chemical modification
1. with the rape stalk powder of drying with the just submergence of 20v/v% isopropyl alcohol, after stirring 24h, use the vavuum pump suction filtration, clean 3 times with the 20v/v% isopropyl alcohol again, clean to filtrate change with distilled water at last and clarify, the gained solid is for subsequent use behind the dry 24h in 55 ℃ of electric drying oven with forced convections.This step can effectively be removed pigment and some polar substances in the stalk.
2. 1. add the NaOH solution of 0.1mol/L with its just submergence in the pressed powder of gained to step, stirred 1 hour, add again distilled water behind the suction filtration with just submergence of solid, stir 45min and carry out again suction filtration, then solid water is washed till filtrate pH=7, at last solid is placed behind 55 ℃ of dry 24h of baking oven for subsequent use.This step can further effectively be removed pigment and half fiber in the stalk, is conducive to next step modification.
3. stir 30min after 2. the citric acid solution of solid and the 0.5mol/L of gained mixes with the ratio of 1g: 12mL with step and obtain citric acid-rape stalk slurry, then citric acid-rape stalk slurry is contained in the stainless steel pallet after under 50 ℃ of air blast conditions dry 24 hours, 90min is reacted in thermalization under 120 ℃ of air blast conditions again, after the cooling, the citric acid modified rape straw that obtains splashes into 0.1mol/L Pb (NO with the distilled water that distilled water cleans after extremely cleaning
3)
2In the time of in the solution till the constant muddiness.
4. adding 0.1mol/L NaOH solution to the pH value of mixed liquor in the citric acid modified rape straw after the washing is 9.5-10.5, stirred 1 hour, then suction filtration and to clean to eluate with distilled water be neutral is dried to constant weight with suction filtration gained solid at last and namely gets adsorbent of the present invention under 50 ℃.
Citric acid modified rape straw adsorbent of the present invention can be used for the processing of industrial dye waste water, and treatment effect is good.
Compared with prior art, advantage of the present invention and beneficial effect are:
1, the raw material rape stalk is cheap and easy to get, wide material sources, and utilize agricultural wastes to synthesize the efficient adsorption material, meet the resource recycling theory.
2, synthetic technology is easy to operate, and is simple.
3, propose first to be used for Study on Industrial Wastewater with citric acid modified rape straw, synthesize a kind of new adsorbent, enriched the adsorbent synthetic chemistry, the development industry is polluted the control new technology practical significance.
4, preparation-obtained new adsorbent citric acid modified rape straw has higher treatment effeciency and absorption property preferably for industrial wastewater, and processing cost is cheap, and is easy to operate.For the processing of the industrial wastewaters such as the poisonous difficult degradation pollutant such as heavy metal ion and the dye of positive ion provides scientific basis.
5, the adsorbent that synthesizes of the present invention belongs to the environmental friendliness shaped material, can not produce secondary pollution.
Description of drawings
Fig. 1 is the scanning electron microscope diagram (* 1000) of rape stalk.
Fig. 2 is that the x-ray photoelectron of the prepared citric acid modified rape straw of the present invention can spectrogram.
Wherein, the rape stalk of a-unmodified, the rape stalk after the b-citric acid modification.
The specific embodiment
Below by concrete Preparation Example and Application Example the present invention is done further to elaborate, so that those skilled in the art understand the present invention.
The preparation of adsorbent
Embodiment 1:
A kind of preparation method of citric acid modified rape straw adsorbent, concrete steps are as follows:
(1) physical treatment of material
Further grind with mixer after the rape stalk of drying is cut into segment, then cross 100 order sub-sieves, getting the sub-sieve lower part of screen divides with after the distilled water cleaning 4 times, until filtrate becomes clarification, the rape stalk powder that obtains gets dry rape stalk powder behind the dry 24h in 55 ℃ of electric drying oven with forced convections with the vavuum pump suction filtration.Fig. 1 is the scanning electron microscope diagram sheet of the rape stalk powder of drying, and as can be seen from Figure, rape stalk has fibrous structure.
(2) chemical modification
1. with the rape stalk powder of drying with the just submergence of 20v/v% isopropyl alcohol, after stirring 24h, use the vavuum pump suction filtration, clean 3 times with the 20v/v% isopropyl alcohol again, clean to filtrate change with distilled water at last and clarify, the gained solid is for subsequent use behind the dry 24h in 55 ℃ of electric drying oven with forced convections.
2. 1. add the NaOH solution of 0.1mol/L with its just submergence in the pressed powder of gained to step, stirred 1 hour, add again distilled water behind the suction filtration with just submergence of solid, carry out again suction filtration after stirring 45min, then the gained solid is cleaned to filtrate pH=7 with distilled water, at last solid is placed behind 55 ℃ of dry 24h of baking oven for subsequent use.
3. stir 30min after 2. the citric acid solution of solid and the 0.5mol/L of gained mixes with the ratio of 1g: 12mL with step and obtain citric acid-rape stalk slurry, then citric acid-rape stalk slurry is contained in the stainless steel pallet after under 50 ℃ of air blast conditions dry 24 hours, 90min is reacted in thermalization under 120 ℃ of air blast conditions again, after the cooling, the citric acid modified rape straw that obtains splashes into 0.1mol/L Pb (NO with the distilled water that distilled water cleans after extremely cleaning
3)
2In the time of in the solution till the constant muddiness.
4. adding 0.1mol/L NaOH solution to the pH value of mixed liquor in the citric acid modified rape straw after the washing is 9.5-10.5, stirred 1 hour, then suction filtration and to clean to eluate with distilled water be neutral is dried to constant weight with suction filtration gained solid at last and namely gets adsorbent of the present invention under 50 ℃.The x-ray photoelectron energy spectrogram of rape stalk powder before and after Fig. 2 is respectively and modifies, as can be seen from Figure, behind the citric acid modified rape straw, the Area Ratio of C=O is increased to 8% by original 6% in the surface texture, illustrate that graft effect has changed the element formation on stalk surface, graft reaction is effective.
Embodiment 1 prepared adsorbent is applied to the absorption of Crystal Violet Dye:
Take by weighing the 0.050-0.35g adsorbent, joining concentration is 100-900mg L
-1Crystal Violet Dye solution in, regulate the pH value behind 3.0-10.0 take acid or alkali, placed on 25-45 ℃ the water bath chader concussion 1-24 hour, the concentration of crystal violet in the supernatant is measured in centrifugation, according to the concentration difference of crystal violet in the water before and after the absorption, determine that adsorbent is to the adsorption effect of crystal violet in the water.
Embodiment 2
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 200mg L
-1The Crystal Violet Dye aqueous solution, the pH value of dye solution is 5.0, at the speed concussion 0.5h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (588nm) of crystal violet, detect the wherein concentration of excess dye, thereby the clearance that obtains Crystal Violet is 97.43%.
Embodiment 3
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 300mg L
-1The Crystal Violet Dye aqueous solution, the pH value of dye solution is 5.32, at the speed concussion 0.5h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (588nm) of crystal violet, detect the wherein concentration of excess dye, thereby the clearance that obtains Crystal Violet is 99.09%.
Embodiment 4
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 400mg L
-1The Crystal Violet Dye aqueous solution, the pH value of dye solution is 6.0, at the speed concussion 0.5h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with the maximum absorption wavelength of spectrophotometer in crystal violet
(588nm) lower its absorbance of surveying detect the wherein concentration of excess dye, thereby the clearance that obtains Crystal Violet is 99.11%.
Embodiment 5
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 500mg L
-1The Crystal Violet Dye aqueous solution, the pH value of dye solution is 6.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (588nm) of crystal violet, detect the wherein concentration of excess dye, thereby the clearance that obtains Crystal Violet is 99.51%.
Embodiment 6
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 600mg L
-1The Crystal Violet Dye aqueous solution, the pH value of dye solution is 6.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (588nm) of crystal violet, detect the wherein concentration of excess dye, thereby the clearance that obtains Crystal Violet is 99.57%.
Embodiment 7
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 700mg L
-1The Crystal Violet Dye aqueous solution, the pH value of dye solution is 6.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (588nm) of crystal violet, detect the wherein concentration of excess dye, thereby the clearance that obtains Crystal Violet is 99.62%.
Embodiment 8
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 800mg L
-1The Crystal Violet Dye aqueous solution, the pH value of dye solution is 6.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (588nm) of crystal violet, detect the wherein concentration of excess dye, thereby the clearance that obtains Crystal Violet is 99.40%.
Embodiment 9
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 300mg L
-1The Crystal Violet Dye aqueous solution, the pH value of dye solution is 3.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (588nm) of crystal violet, detect the wherein concentration of excess dye, thereby the clearance that obtains Crystal Violet is 98.30%.
Embodiment 10
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 300mg L
-1The Crystal Violet Dye aqueous solution, the pH value of dye solution is 4.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (588nm) of crystal violet, detect the wherein concentration of excess dye, thereby the clearance that obtains Crystal Violet is 99.40%.
Embodiment 11
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 300mg L
-1The Crystal Violet Dye aqueous solution, the pH value of dye solution is 5.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (588nm) of crystal violet, detect the wherein concentration of excess dye, thereby the clearance that obtains Crystal Violet is 98.70%.
Embodiment 12
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 300mg L
-1The Crystal Violet Dye aqueous solution, the pH value of dye solution is 6.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (588nm) of crystal violet, detect the wherein concentration of excess dye, thereby the clearance that obtains Crystal Violet is 98.10%.
Embodiment 13
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 300mg L
-1The Crystal Violet Dye aqueous solution, the pH value of dye solution is 7.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (588nm) of crystal violet, detect the wherein concentration of excess dye, thereby the clearance that obtains Crystal Violet is 98.30%.
Embodiment 14
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 300mg L
-1The Crystal Violet Dye aqueous solution, the pH value of dye solution is 8.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (588nm) of crystal violet, detect the wherein concentration of excess dye, thereby the clearance that obtains Crystal Violet is 98.50%.
Embodiment 15
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 300mg L
-1The Crystal Violet Dye aqueous solution, the pH value of dye solution is 9.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (588nm) of crystal violet, detect the wherein concentration of excess dye, thereby the clearance that obtains Crystal Violet is 98.40%.
Embodiment 16
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 300mg L
-1The Crystal Violet Dye aqueous solution, the pH value of dye solution is 10.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (588nm) of crystal violet, detect the wherein concentration of excess dye, thereby the clearance that obtains Crystal Violet is 98.60%.
Embodiment 1 prepared adsorbent is applied to the absorption of other common dyestuffs and heavy metal ion:
Embodiment 17
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 200mg L
-1The methylene blue dye aqueous solution, the pH value of dye solution is 6.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (670nm) of methylene blue, detect the wherein concentration of excess dye, thereby the clearance that obtains the dyestuff methylene blue is 99.56%.
Embodiment 18
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 300mg L
-1The methylene blue dye aqueous solution, the pH value of dye solution is 6.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (670nm) of methylene blue, detect the wherein concentration of excess dye, thereby the clearance that obtains the dyestuff methylene blue is 99.64%.
Embodiment 19
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 400mg L
-1The methylene blue dye aqueous solution, the pH value of dye solution is 6.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (670nm) of methylene blue, detect the wherein concentration of excess dye, thereby the clearance that obtains the dyestuff methylene blue is 99.69%.
Embodiment 20
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 200mg L
-1The dimethyl diaminophenazine chloride aqueous dye solutions, the pH value of dye solution is 4.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (530nm) of dimethyl diaminophenazine chloride, detect the wherein concentration of excess dye, thereby the clearance that obtains the dyestuff dimethyl diaminophenazine chloride is 98.94%.
Embodiment 21
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 300mg L
-1The dimethyl diaminophenazine chloride aqueous dye solutions, the pH value of dye solution is 4.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (530nm) of dimethyl diaminophenazine chloride, detect the wherein concentration of excess dye, thereby the clearance that obtains the dyestuff dimethyl diaminophenazine chloride is 98.82%.
Embodiment 22
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 400mg L
-1The dimethyl diaminophenazine chloride aqueous dye solutions, the pH value of dye solution is 4.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (530nm) of dimethyl diaminophenazine chloride, detect the wherein concentration of excess dye, thereby the clearance that obtains the dyestuff dimethyl diaminophenazine chloride is 99.11%.
Embodiment 23
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 200mg L
-1The malachite green aqueous dye solutions, the pH value of dye solution is 7.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (618nm) of malachite green, detect the wherein concentration of excess dye, thereby the clearance that obtains the dyestuff malachite green is 99.43%.
Embodiment 24
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 300mg L
-1The malachite green aqueous dye solutions, the pH value of dye solution is 7.0, at the speed concussion 24h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, with the supernatant that obtains with spectrophotometer in lower its absorbance of surveying of the maximum absorption wavelength (618nm) of malachite green, detect the wherein concentration of excess dye, thereby the clearance that obtains the dyestuff malachite green is 99.04%.
Embodiment 25
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 100mg L
-1Plumbous (the Pb of metal ion
2+) the aqueous solution, the pH value of metal ion solution is 6.0, at the speed concussion 1h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, the supernatant that obtains is detected the wherein concentration of residual metallic ion with atomic absorption spectrophotometer, thereby the clearance that obtains metal ion lead is 99.23%.
Embodiment 26
The 50mg adsorbent is inserted in the 250mL tool plug conical flask, and adding 50mL concentration is 100mg L
-1Metal ion cadmium (Cd
2+) the aqueous solution, the pH value of metal ion solution is 5.0, at the speed concussion 1h of 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining solution rotating speed with 10000rpm on centrifuge solution is separated with solid, and the supernatant that obtains is detected the wherein concentration of residual metallic ion with atomic absorption spectrophotometer, is 99.56% thereby obtain metal ion hydrolysate rate.
Claims (1)
1. the preparation method of a citric acid modified rape straw adsorbent, concrete steps are as follows:
(1) physical treatment of material
Further grind with mixer after the rape stalk of drying is cut into segment, then cross 100 order sub-sieves, getting the sub-sieve lower part of screen divides with after the distilled water cleaning 4 times, until filtrate becomes clarification, the rape stalk powder that obtains gets dry rape stalk powder behind the dry 24h in 55 ℃ of electric drying oven with forced convections with the vavuum pump suction filtration;
(2) chemical modification
1. with the rape stalk powder of drying with the just submergence of 20v/v% isopropyl alcohol, after stirring 24h, use the vavuum pump suction filtration, clean 3 times with the 20v/v% isopropyl alcohol again, clean to filtrate change with distilled water at last and clarify, the gained solid is for subsequent use behind the dry 24h in 55 ℃ of electric drying oven with forced convections;
2. 1. add the NaOH solution of 0.1mol/L with its just submergence in the pressed powder of gained to step, stirred 1 hour, add again distilled water behind the suction filtration with just submergence of solid, carry out again suction filtration after stirring 45min, then the gained solid is cleaned to filtrate pH=7 with distilled water, at last solid is placed behind 55 ℃ of dry 24h of baking oven for subsequent use;
3. stir 30min after 2. the citric acid solution of solid and the 0.5mol/L of gained mixes with the ratio of 1g:12mL with step and obtain citric acid-rape stalk slurry, then citric acid-rape stalk slurry is contained in the stainless steel pallet after under 50 ℃ of air blast conditions dry 24 hours, 90min is reacted in thermalization under 120 ℃ of air blast conditions again, after the cooling, the citric acid modified rape straw that obtains splashes into 0.1mol/L Pb (NO with the distilled water that distilled water cleans after extremely cleaning
3)
2In the time of in the solution till the constant muddiness;
4. adding 0.1mol/L NaOH solution to the pH value of mixed liquor in the citric acid modified rape straw after the washing is 9.5-10.5, stirred 1 hour, then suction filtration and to clean to eluate with distilled water be neutral is dried to constant weight with suction filtration gained solid at last and get final product under 50 ℃.
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| CN104815619A (en) * | 2015-04-29 | 2015-08-05 | 武汉工程大学 | Oilseed rape straw/hydrotalcite composite material and preparation method and application thereof |
| CN104826604A (en) * | 2015-05-25 | 2015-08-12 | 西北大学 | Preparation method of double ionic straw based hydrogel applied for sewage treatment |
| CN105161155A (en) * | 2015-08-10 | 2015-12-16 | 南华大学 | Method absorbing and processing uranium-bearing waste water via sodium hydroxide modified rice straw absorbent |
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| CN105536714A (en) * | 2015-12-19 | 2016-05-04 | 陈长琼 | Heavy metal cellulose adsorbent and preparation method thereof |
| CN105435748A (en) * | 2015-12-19 | 2016-03-30 | 陈长琼 | Plant cellulose adsorbent |
| CN105536715A (en) * | 2015-12-20 | 2016-05-04 | 吴涛 | Method for preparation of adsorption material by using maple leaf |
| CN105561936A (en) * | 2015-12-20 | 2016-05-11 | 吴涛 | Sweet scented osmanthus leaf modified adsorption material |
| CN105561935A (en) * | 2015-12-20 | 2016-05-11 | 陈长琼 | Plant cellulose modified adsorption material and preparation process thereof |
| CN105536716A (en) * | 2015-12-20 | 2016-05-04 | 吴涛 | Orange peel modified adsorbent material and preparation method thereof |
| CN105381787A (en) * | 2015-12-20 | 2016-03-09 | 吴涛 | New environmentally friendly adsorbent material and preparation process thereof |
| CN105413648A (en) * | 2015-12-20 | 2016-03-23 | 吴涛 | Folium ginkgo adsorbing material and preparation method thereof |
| CN105642245B (en) * | 2016-03-14 | 2017-11-24 | 武汉轻工大学 | A kind of preparation method of magnetic egg white/luffa sorbing material |
| CN105561944B (en) * | 2016-03-14 | 2017-11-24 | 武汉轻工大学 | A kind of preparation method of magnetic egg white/water hyacinth Compound Heavy Metals sorbing material |
| CN106732416B (en) * | 2016-12-01 | 2019-04-12 | 桂林理工大学 | A kind of preparation method and applications of rosin modification stalk adsorbent |
| CN107780209A (en) * | 2017-11-01 | 2018-03-09 | 山东国丰君达化工科技股份有限公司 | One kind inhales color fibre cloth production process |
| CN112239259B (en) * | 2020-08-24 | 2021-12-21 | 中南大学 | Chemical remover for heavy metal polluted wastewater treatment and preparation method and application thereof |
-
2011
- 2011-07-25 CN CN 201110208310 patent/CN102266756B/en active Active
Non-Patent Citations (2)
| Title |
|---|
| 李逢雨等.柠檬酸修饰高粱秸杆吸附水中结晶紫的研究.《武汉工程大学学报》.2010,第32卷(第12期),参见摘要、引言以及正文1 材料和方法部分. |
| 柠檬酸修饰高粱秸杆吸附水中结晶紫的研究;李逢雨等;《武汉工程大学学报》;20101231;第32卷(第12期);参见摘要、引言以及正文1 材料和方法部分 * |
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