CN106111084A - A kind of preparation method removing chromium ion adsorbent - Google Patents

A kind of preparation method removing chromium ion adsorbent Download PDF

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Publication number
CN106111084A
CN106111084A CN201610618407.XA CN201610618407A CN106111084A CN 106111084 A CN106111084 A CN 106111084A CN 201610618407 A CN201610618407 A CN 201610618407A CN 106111084 A CN106111084 A CN 106111084A
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water
powder
banana stalk
preparation
chromium ion
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CN201610618407.XA
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Chinese (zh)
Inventor
凌雪木
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Guangxi Province Nanning City Guierchuang Environmental Protection Technology Co Ltd
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Guangxi Province Nanning City Guierchuang Environmental Protection Technology Co Ltd
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Priority to CN201610618407.XA priority Critical patent/CN106111084A/en
Publication of CN106111084A publication Critical patent/CN106111084A/en
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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
    • 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
    • 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
    • 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
    • B01J2220/485—Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
    • 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
    • B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C02F2101/22—Chromium or chromium compounds, e.g. chromates

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Water Treatment By Sorption (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a kind of preparation method removing chromium ion adsorbent, it is that treat banana stalk is pulverized, add sodium hydroxide solution to soak, it is washed with water and washs treat banana stalk powder to neutral, maleic acid is added in treat banana stalk powder cellulose, add water at temperature is 80 100 DEG C, is dried 1 2h, obtain modified treat banana stalk powder；Water intaking calabash powder and thiourea add ultrasonic stirrer, add suitable quantity of water and carry out ultrasonic reaction, reacted pastel is placed in heat drying 2 3h in the baking oven of 60 80 DEG C, obtain modified water calabash powder；Above-mentioned modified treat banana stalk granulated slag, modified water calabash powder are added agitator, adds ammonium ceric nitrate and chitosan, add water furnishing pasty state, putting into microwave heating equipment, at temperature is 120 140 DEG C, microwave 30 60min, is cooled to room temperature, grind, obtain chromium ion adsorbent.The adsorbent of the present invention has that raw material sources are extensive, with low cost, specific surface area is big, adsorption capacity is big, adsorption efficiency is high, preparation technology is simple, etc. advantage, hexavalent chromium is had good absorption property.

Description

A kind of preparation method removing chromium ion adsorbent
Technical field
The present invention relates to adsorbing material technical field, a kind of preparation method removing chromium ion adsorbent.
Background technology
In recent years, along with development, the heavy metal wastewater thereby of heavy industries do not add any of process and discharge, result in heavy metal Ion content in natural water increases day by day, and the water contamination accident thus caused occurs again and again.Heavy metal is to cause ring One of major reason of environment pollution problem, in heavy metal enters into environment, can not be biodegradable as innocuous substance, with The particle of Shi Shuizhong passes through absorption and the precipitation of heavy metal ion so that heavy metal in water long-term pollution is produced with regard to this Raw.What is more, and the heavy metal being present in organism, through accumulation, enrichment, also participates in biosphere circulation, and harmful to human is good for Health, is the first kinds of pollution matter very harmful to ecological environment.Heavy metal pollution of water body has had become as that the whole society pays close attention to Global environmental problem.
Chromium is a kind of important environmental contaminants, is mainly derived from the waste water of the industry discharges such as chemical industry, metallurgy and printing and dyeing. In nature, the form of chromium has multiple, but mainly exists with hexavalent chromium form in water body, by pH value, oxygen in water body Changing reducing substances, temperature and the impact of other factors, chromium can occur the mutual conversion between valence state.Trivalent chromium toxicity is the least, but Cr VI is carcinogen.Hexavalent chromium can enter human body by approach such as drinking-water and diet, and then at people's body accumulation, right Human body causes a certain degree of harm, the serious health having threatened the mankind.Therefore, processing waste water containing chrome the most cost-effectively Become as one of important research direction of China.
The processing method of industrial wastewater containing chromium includes chemical precipitation method, coagulant sedimentation, ion exchange, absorption method etc.. Due to absorption method have that technological process is simple, high treating effect, the advantage such as workable, therefore processing an industrial wastewater huge sum of money Belong in chromium and being widely used.Wherein activated carbon can be used for a most of huge sum of money as the effective Wastewater processing absorbent of one Genus, the removing of organic molecule and high adsorption capacity, simply activated carbon resource-constrained, high-volume improvement waste water cost is high, and the life-span is short, Regenerative operation is costly, it is more difficult to be widely used in the most underdeveloped area of economy.Existing polymeric sorbent, utilization Adsorbent prepared by garbage and compound adsorbent etc. there is also that cost is high, adsorption efficiency is low, be easily generated secondary pollution problems. Therefore, how improving the secondary pollution problem that causes during the adsorption efficiency of adsorbent and reducing uses is current research heat Point.
Summary of the invention
The present invention is directed to the problem that existing adsorbent exists, it is provided that a kind of specific surface area is big, adsorption capacity big, adsorption efficiency Height, low cost, preparation technology are simple, the adsorbent for removing chromium ion of safety and environmental protection.
In order to realize object above, the present invention is to be achieved through the following technical solutions:
A kind of preparation method removing chromium ion adsorbent, with mass ratio as 100:5-10:60-70:8-12:5-8:5-10 Treat banana stalk, maleic acid, Herba Eichhorniae powder, thiourea, ammonium ceric nitrate and chitosan, as raw material, make suction by microwave heating method Attached dose, concrete operation step is as follows:
(1) 100 parts of treat banana stalk are pulverized, add sodium hydroxide solution and soak 3-5h, be washed with water and wash treat banana stalk powder extremely neutrality, Treat banana stalk powder cellulose；Adding 5-10 part maleic acid in treat banana stalk powder cellulose, add 80-120 part water, mixing is all Even, at temperature is 80-100 DEG C, it is dried 1-2h, obtains modified treat banana stalk powder；
(2) water intaking calabash powder 60-70 part and thiourea 8-12 part add ultrasonic stirrer, add suitable quantity of water carry out ultrasonic instead Should, reacted pastel is placed in heat drying 2-3h in the baking oven of 60-80 DEG C, obtains modified water calabash powder；
(3) above-mentioned modified treat banana stalk granulated slag, modified water calabash powder are added agitator, add ceric ammonium nitrate solution 5-10 part and shell Polysaccharide 5-10 part, adds water furnishing pasty state, pastel is put into microwave heating equipment, microwave at temperature is 120-140 DEG C 30-60min, is cooled to room temperature, grinds, obtains chromium ion adsorbent.
Preferably, the water content of the above treat banana stalk is 12%.
Preferably, above step (1) is that treat banana stalk is crushed to 40-60 mesh.
Preferably, the concentration of the above sodium hydroxide is 3-5mol/L.
Preferably, the above Herba Eichhorniae powder is that to be dried by Herba Eichhorniae to water content be 10%, is then crushed to 60 mesh, i.e. Obtain Herba Eichhorniae powder.
Preferably, the ultrasonic reaction described in above step (2) is ultrasonic reaction 30-under supersonic frequency is 40-60kHz 60min。
Preferably, the power of above step (3) described microwave is 200-300W.
Preferably, the concentration of the above ceric ammonium nitrate solution is 5mol/L.
Preferably, above step (3) described grinding is that to grind the material to particle diameter be 0.5-1.0mm.
Compared with prior art, advantages of the present invention and having the beneficial effect that
1, adsorbent prepared by the present invention have that raw material sources are extensive, with low cost, specific surface area is big, adsorption capacity is big, absorption Efficiency is high, the simple and environmentally-friendly advantage such as degradable of preparation technology, has good absorption property to hexavalent chromium, at Industry Waste Water has wide market prospect in processing.
2, the present invention is using agricultural waste material treat banana stalk as primary raw material, and not only raw material sources are extensive, cheap, also The resource that can realize garbage recycles, and expands the using value of treat banana stalk.
3, this method utilizes sodium hydroxide and maleic acid to be modified sisal dregs, can remove the color of sisal dregs The materials such as element, lignin and hemicellulose, owing to having substantial amounts of carboxyl isoreactivity group on maleic acid strand, have The effect of Adsorption of Chromium ion, improves the absorption property of adsorbent.
4, the present invention is using Herba Eichhorniae widely distributed, that reproduction speed is fast, growth cycle is short as raw material, is not only Herba Eichhorniae Disaster provides effective process approach, and many hollow structures of Herba Eichhorniae can be that heavy metal is provided with effect ground adsorption site, simultaneously water calabash The multiple macromolecular substances such as reed rich in proteins, polysaccharide and crude fibre, containing functional groups such as substantial amounts of hydroxyl, carboxyl and amino, With heavy metal hexavalent chromium, complex reaction the most completely can occur, thus reach more preferable adsorption effect.
5, this method uses ultrasonic Treatment Herba Eichhorniae powder, it is possible to the cell wall of quick crashing plant, makes more inside Functional group comes out and is combined with metal ion, significantly improves the adsorption effect of waste water hexavalent chromium.
6, the present invention uses thiourea to be modified Herba Eichhorniae powder, and adsorbent can be made to give bigger specific surface area and suction Attached capacity, improves the adsorbent absorption property to chromium ion.
7, this method adds ammonium ceric nitrate in the preparation process of adsorbent, and the adsorption capacity that can improve adsorbent greatly and is inhaled Attached efficiency.
8, the present invention uses microwave method to heat, and has that firing rate is fast, system of being heated homogeneous temperature, consume energy the advantage such as low.
9, the adsorbent that the inventive method prepares has good absorption property, and wherein the specific surface area of adsorbent is 250- 350m2/ g, reaches more than 97% to the adsorption rate of hexavalent chromium.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further described, but is not limited to protection scope of the present invention.
Embodiment 1
A kind of preparation method removing chromium ion adsorbent, concrete operation step is as follows:
(1) treat banana stalk that 100kg water content is 12% being crushed to 40 mesh, adding concentration is that 3mol/L sodium hydroxide solution soaks 5h, is washed with water and washs treat banana stalk powder extremely neutrality, obtain treat banana stalk powder cellulose；8kg maleic is added in treat banana stalk powder cellulose Diacid, adds 100kg water, mix homogeneously, is dried 2h, obtains modified treat banana stalk powder at temperature is 80 DEG C；
(2) water intaking calabash powder 60kg and thiourea 10kg adds ultrasonic stirrer, adds 120kg water, in supersonic frequency is React 60min under 40kHz, reacted pastel is placed in heat drying 3h in the baking oven of 60 DEG C, obtains modified water calabash powder；
(3) above-mentioned modified treat banana stalk granulated slag, modified water calabash powder are added agitator, add ceric ammonium nitrate solution 5kg and shell gathers Sugar 8kg, add water furnishing pasty state, pastel put into microwave heating equipment, power be 200W, temperature be at 120 DEG C micro- Ripple 60min, is cooled to room temperature, and grinding the material to particle diameter is 0.5mm, obtains chromium ion adsorbent.
Embodiment 2
A kind of preparation method removing chromium ion adsorbent, concrete operation step is as follows:
(1) treat banana stalk that 100kg water content is 12% being crushed to 40 mesh, adding concentration is that 5mol/L sodium hydroxide solution soaks 4h, is washed with water and washs treat banana stalk powder extremely neutrality, obtain treat banana stalk powder cellulose；5kg maleic is added in treat banana stalk powder cellulose Diacid, adds 80kg water, mix homogeneously, is dried 1h, obtains modified treat banana stalk powder at temperature is 100 DEG C；
(2) water intaking calabash powder 65kg and thiourea 12kg adds ultrasonic stirrer, adds 150kg water, in supersonic frequency is React 30min under 60kHz, reacted pastel is placed in heat drying 2h in the baking oven of 80 DEG C, obtains modified water calabash powder；
(3) above-mentioned modified treat banana stalk granulated slag, modified water calabash powder are added agitator, add ceric ammonium nitrate solution 6kg and shell gathers Sugar 5kg, add water furnishing pasty state, pastel put into microwave heating equipment, power be 250W, temperature be at 140 DEG C micro- Ripple 30min, is cooled to room temperature, and grinding the material to particle diameter is 0.5mm, obtains chromium ion adsorbent.
Embodiment 3
A kind of preparation method removing chromium ion adsorbent, concrete operation step is as follows:
(1) treat banana stalk that 100kg water content is 12% being crushed to 60 mesh, adding concentration is that 5mol/L sodium hydroxide solution soaks 6h, is washed with water and washs treat banana stalk powder extremely neutrality, obtain treat banana stalk powder cellulose；10kg maleic is added in treat banana stalk powder cellulose Diacid, adds 100kg water, mix homogeneously, is dried 1.5h, obtains modified treat banana stalk powder at temperature is 90 DEG C；
(2) water intaking calabash powder 70kg and thiourea 12kg adds ultrasonic stirrer, adds 150kg water, in supersonic frequency is React 45min under 50kHz, reacted pastel is placed in heat drying 2.5h in the baking oven of 70 DEG C, obtains modified water calabash powder；
(3) above-mentioned modified treat banana stalk granulated slag, modified water calabash powder are added agitator, add ceric ammonium nitrate solution 8kg and shell gathers Sugar 10kg, add water furnishing pasty state, pastel put into microwave heating equipment, power be 300W, temperature be at 120 DEG C micro- Ripple 60min, is cooled to room temperature, and grinding the material to particle diameter is 1.0mm, obtains chromium ion adsorbent.
Embodiment 4
A kind of preparation method removing chromium ion adsorbent, concrete operation step is as follows:
(1) treat banana stalk that 100kg water content is 12% being crushed to 60 mesh, adding concentration is that 5mol/L sodium hydroxide solution soaks 5h, is washed with water and washs treat banana stalk powder extremely neutrality, obtain treat banana stalk powder cellulose；9kg maleic is added in treat banana stalk powder cellulose Diacid, adds 100kg water, mix homogeneously, is dried 2h, obtains modified treat banana stalk powder at temperature is 90 DEG C；
(2) water intaking calabash powder 60kg and thiourea 10kg adds ultrasonic stirrer, adds 120kg water, in supersonic frequency is React 60min under 40kHz, reacted pastel is placed in heat drying 2.5h in the baking oven of 80 DEG C, obtains modified water calabash powder；
(3) above-mentioned modified treat banana stalk granulated slag, modified water calabash powder are added agitator, add ceric ammonium nitrate solution 7kg and shell gathers Sugar 8kg, add water furnishing pasty state, pastel put into microwave heating equipment, power be 250W, temperature be at 130 DEG C micro- Ripple 45min, is cooled to room temperature, and grinding the material to particle diameter is 1.0mm, obtains chromium ion adsorbent.
The using method of adsorbent is: at ambient temperature, the adsorbent of 1g puts into 1L and contains the useless of hexavalent chromium In water, controlling pH is 5, stirs 60min, isolate adsorbent, Cr VI in the most removable waste water under rotating speed is 300r/min Ion.
The adsorbent prepared embodiment 1-4 below carries out the mensuration of absorption property.Specific area measuring is wherein used to inhale The specific surface area of attached dose.Use the concentration of atomic absorption spectroscopy determination hexavalent chromium, calculate further according to below equation Going out adsorption rate, measurement result is as shown in the table.
ŋ=(C0-Ci)×100% /C0
Wherein C0、CiContent (mg/L) before and after adsorbing for hexavalent chromium in waste water, for adsorption rate.
From measurement result it can be seen that adsorbent prepared by the present invention has bigger specific surface area, to hexavalent chromium Adsorption rate reach more than 97%, chromium ion waste water process in have broad application prospects.
Above content is it cannot be assumed that the present invention is embodied as being confined to these explanations, for the technical field of the invention Those of ordinary skill for, without departing under present inventive concept premise, it is also possible to make some simple deduction or replace, all answer When being considered as belonging to the scope of patent protection that the present invention is determined by the claims submitted to.

Claims (9)

1. the preparation method removing chromium ion adsorbent, it is characterised in that: it is with mass ratio as 100:5-10:60-70:8- The treat banana stalk of 12:5-8:5-10, maleic acid, Herba Eichhorniae powder, thiourea, ammonium ceric nitrate and chitosan are as raw material, by micro- Wave heating method makes adsorbent, and concrete operation step is as follows:
100 parts of treat banana stalk are pulverized, adds sodium hydroxide solution and soak 3-5h, be washed with water and wash treat banana stalk powder extremely neutrality, obtain fragrant Any of several broadleaf plants bar powder cellulose；Adding 5-10 part maleic acid in treat banana stalk powder cellulose, add 80-120 part water, mixing is all Even, at temperature is 80-100 DEG C, it is dried 1-2h, obtains modified treat banana stalk powder；
Water intaking calabash powder 60-70 part and thiourea 8-12 part add ultrasonic stirrer, add suitable quantity of water and carry out ultrasonic reaction, will Reacted pastel is placed in heat drying 2-3h in the baking oven of 60-80 DEG C, obtains modified water calabash powder；
Above-mentioned modified treat banana stalk granulated slag, modified water calabash powder are added agitator, adds ceric ammonium nitrate solution 5-10 part and shell gathers Sugar 5-10 part, adds water furnishing pasty state, pastel is put into microwave heating equipment, microwave 30-at temperature is 120-140 DEG C 60min, is cooled to room temperature, grinds, obtains chromium ion adsorbent.
Remove the preparation method of chromium ion adsorbent the most according to claim 1, it is characterised in that: described treat banana stalk aqueous Amount is 12%.
Remove the preparation method of chromium ion adsorbent the most according to claim 2, it is characterised in that: step (1) is by Fructus Musae Bar is crushed to 40-60 mesh.
Remove the preparation method of chromium ion adsorbent the most according to claim 1, it is characterised in that: described sodium hydroxide dense Degree is 3-5mol/L.
The most according to claim 1 remove chromium ion adsorbent preparation method, it is characterised in that: described Herba Eichhorniae powder be by It is 10% that Herba Eichhorniae dries to water content, is then crushed to 60 mesh, obtains Herba Eichhorniae powder.
Remove the preparation method of chromium ion adsorbent the most according to claim 1, it is characterised in that: surpassing described in step (2) Phonoresponse is ultrasonic reaction 30-60min under supersonic frequency is 40-60kHz.
Remove the preparation method of chromium ion adsorbent the most according to claim 1, it is characterised in that: step (3) described microwave Power be 200-300W.
Remove the preparation method of chromium ion adsorbent the most according to claim 1, it is characterised in that: described ceric ammonium nitrate solution Concentration be 5mol/L.
Remove the preparation method of chromium ion adsorbent the most according to claim 1, it is characterised in that: step (3) described grinding It is that to grind the material to particle diameter be 0.5-1.0mm.
CN201610618407.XA 2016-08-01 2016-08-01 A kind of preparation method removing chromium ion adsorbent Pending CN106111084A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107473270A (en) * 2017-09-25 2017-12-15 杭州金丰环保科技有限公司 A kind of method that iron oxide black and calcium chloride are prepared using steel plant's spent acid
CN109198168A (en) * 2018-10-12 2019-01-15 浙江海洋大学 A kind of method that shellfish feeds bait and its removes heavy metal in body of shellfish
CN110586045A (en) * 2019-09-21 2019-12-20 天津大学 Preparation method and application of amphoteric magnetic chitosan adsorbent

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107473270A (en) * 2017-09-25 2017-12-15 杭州金丰环保科技有限公司 A kind of method that iron oxide black and calcium chloride are prepared using steel plant's spent acid
CN107473270B (en) * 2017-09-25 2019-10-18 杭州金丰环保科技有限公司 A method of iron oxide black and calcium chloride are prepared using steel plant's spent acid
CN109198168A (en) * 2018-10-12 2019-01-15 浙江海洋大学 A kind of method that shellfish feeds bait and its removes heavy metal in body of shellfish
CN110586045A (en) * 2019-09-21 2019-12-20 天津大学 Preparation method and application of amphoteric magnetic chitosan adsorbent

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Application publication date: 20161116