CN106140105A - A kind of preparation method of waste water mercury-removing adsorbent - Google Patents
A kind of preparation method of waste water mercury-removing adsorbent Download PDFInfo
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- CN106140105A CN106140105A CN201610618496.8A CN201610618496A CN106140105A CN 106140105 A CN106140105 A CN 106140105A CN 201610618496 A CN201610618496 A CN 201610618496A CN 106140105 A CN106140105 A CN 106140105A
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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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- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0207—Compounds of Sc, Y or Lanthanides
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0281—Sulfates of compounds other than those provided for in B01J20/045
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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
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
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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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
Abstract
The invention discloses the preparation method of a kind of waste water mercury-removing adsorbent, it is that Pericarpium Musae is pulverized, add sodium hydroxide solution to soak, it is washed with water and washs Fructus Musae corium farinosum to neutral, in Pericarpium Musae cellulose, add ethyl acrylate, add water, mix homogeneously, at temperature is 60 80 DEG C, it is dried 2 3h, obtains modified Fructus Musae corium farinosum;Take Entermorpha powder and thiourea adds ultrasonic stirrer, add suitable quantity of water and carry out ultrasonic reaction, reacted pastel is placed in heat drying 1 2h in the baking oven of 70 80 DEG C, obtains modified Entermorpha powder;Again modification Fructus Musae corium farinosum, modified Entermorpha powder are added agitator, add cerous sulfate solution and sodium alginate, add water furnishing pasty state, pastel is put into microwave heating equipment heat drying, be cooled to room temperature, grind, obtain waste water mercury-removing adsorbent.The adsorbent of the present invention has the advantages such as 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, and waste water mercury ion is had good absorption property.
Description
Technical field
The present invention relates to adsorbing material technical field, the preparation method of a kind of waste water mercury-removing 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.
Mercury-containing waste water is mainly derived from non-ferrous metals smelting works, instrucment and meter plant and some chemical plant etc..Hydrargyrum be a kind of toxicity very
Strong metal.Organomercurial toxicity is more than mercury metal and inorganic mercury compound, thus is easier to be poisoned.Organic mercury and methyl
Hydrargyrum all can pass through respiratory tract, digestive tract, skin intrusion human body.Inorganic mercury is accumulated position in human body and is mainly kidney, next to that
Liver and spleen;Methyl mercury, in addition to being accumulated in the internal organs such as liver, kidney, is accumulated in brain is knitted also by blood brain barrier.In hydrargyrum
Poison energy loss damaging the spleen and stomach pivot nervous system, the lighter show as stomatitis, tremble, irritable, irritability and emotional instability, severe one is the most spiritual disorderly
Disorderly, behavior domination ability reduction, quadriplegia, deaf and blind, even become idiot.Therefore, process the most cost-effectively and contain
Hydrargyrum waste water becomes as one of important research direction of China.
The processing method of mercury-containing waste water is more, and sulphide precipitation, ferrite process, floatation, xanthate are applicable to place
Managing a small amount of mercury-containing waste water, the processing method processing mercurous industrial wastewater of substantial amounts of mercury-containing waste water includes chemical precipitation method, coagulation
The sedimentation method, ion exchange, absorption method etc..Due to absorption method have that technological process is simple, high treating effect, workable etc.
Advantage, is therefore widely used in processing waste water mercury ion.Wherein activated carbon processes as the effective waste water of one and inhales
Attached dose can be used for most of heavy metal, the removing of organic molecule and high adsorption capacity, simply activated carbon resource-constrained, and high-volume is controlled
Reason waste water cost is high, and the life-span is short, and regenerative operation is costly, it is more difficult to be widely used in the most underdeveloped area of economy.Existing
Some polymeric sorbents, utilize adsorbent and compound adsorbent etc. prepared by garbage there is also cost is high, adsorption efficiency is low,
It is easily generated secondary pollution problems.Therefore, cause during how improving the adsorption efficiency of adsorbent, and minimizing adsorbent use
Secondary pollution problem be current study hotspot.
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 the waste water removal of mercury of safety and environmental protection.
In order to realize object above, the present invention is to be achieved through the following technical solutions:
The preparation method of a kind of waste water mercury-removing adsorbent, with mass ratio as 100:10-15:50-70:6-10:4-6:10-15
Pericarpium Musae, ethyl acrylate, Entermorpha powder, thiourea, cerous sulfate and sodium alginate, as raw material, make absorption by microwave heating method
Agent, concrete operation step is as follows:
(1) 100 parts of Pericarpium Musae are pulverized, add sodium hydroxide solution and soak 3-5h, be washed with water and wash Fructus Musae corium farinosum extremely neutrality,
Pericarpium Musae cellulose;Adding 10-15 part ethyl acrylate in Pericarpium Musae cellulose, add 100-120 part water, mixing is all
Even, at temperature is 60-80 DEG C, it is dried 2-3h, obtains modified Fructus Musae corium farinosum;
(2) take Entermorpha powder 50-70 part and thiourea 6-10 part add ultrasonic stirrer, add suitable quantity of water and carry out ultrasonic reaction,
Reacted pastel is placed in heat drying 1-2h in the baking oven of 70-80 DEG C, obtains modified Entermorpha powder;
(3) above-mentioned modified Fructus Musae corium farinosum, modified Entermorpha powder are added agitator, add cerous sulfate solution 4-6 part and sodium alginate
10-15 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 waste water mercury-removing adsorbent.
Preferably, the water content of the above Pericarpium Musae is 12%.
Preferably, above step (1) is that Pericarpium Musae is crushed to 40-60 mesh.
Preferably, the concentration of the above sodium hydroxide is 3-5mol/L.
Preferably, the above waterside platform powder is to be 10% by fresh waterside platform powder cleaning, drying to water content, then is crushed to 80
Mesh, obtains waterside platform powder.
Preferably, the ultrasonic reaction described in above step (2) is ultrasonic reaction 20-under supersonic frequency is 60-80kHz
30min。
Preferably, the power of above step (3) described microwave is 200-300W.
Preferably, the concentration of the above cerous sulfate 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 mercury ion, at industrial wastewater
Reason has wide market prospect.
2, the present invention is using agricultural waste material Pericarpium Musae as primary raw material, and not only raw material sources are extensive, cheap, also
The resource that can realize garbage recycles, and increases the using value of Pericarpium Musae.
3, this method utilizes sodium hydroxide and ethyl acrylate to be modified Pericarpium Musae, can remove the color of Pericarpium Musae
The materials such as element, lignin and hemicellulose, owing to having substantial amounts of carboxyl isoreactivity group on ethyl acrylate strand, can live
Change adsorption site, improve the absorption property of adsorbent.
4, the present invention is using Entermorpha widely distributed, that reproduction speed is fast, growth cycle is short as raw material, is not only waterside platform disaster
Providing effective process approach, many hollow structures of Hu Tai can be that heavy metal is provided with effect ground adsorption site, and Hu Tai is rich in egg simultaneously
The multiple macromolecular substances such as white matter, polysaccharide and crude fibre, containing functional groups such as substantial amounts of hydroxyl, carboxyl and amino, can with hydrargyrum from
There is complex reaction the most completely in son, thus reaches more preferable adsorption effect.
5, this method uses ultrasonic Treatment Entermorpha powder, it is possible to the cell wall of quick crashing plant, makes more internal merit
Can roll into a ball to come out and be combined with metal ion, the adsorption effect of heavy metals mercury ion is significantly improved.
6, the present invention uses thiourea to be modified Entermorpha powder, and adsorbent can be made to give bigger specific surface area and absorption
Capacity, improves the adsorbent absorption property to mercury ion.
7, this method adds cerous sulfate in the preparation process of adsorbent, and the adsorption capacity that can improve adsorbent greatly and is adsorbed
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, adsorbent prepared by the present invention has good absorption property, and wherein the specific surface area of adsorbent is 300-
350m2/ g, reaches more than 98% to the adsorption rate of mercury ion.
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 of waste water mercury-removing adsorbent, concrete operation step is as follows:
(1) Pericarpium Musae that 100kg water content is 12% is crushed to 40 mesh, adds the sodium hydroxide solution leaching that concentration is 5mol/L
Bubble 3h, is washed with water and washs Fructus Musae corium farinosum extremely neutrality, obtain Pericarpium Musae cellulose;12kg acrylic acid second is added in Pericarpium Musae cellulose
Ester, adds 100kg water, mix homogeneously, is dried 3h, obtains modified Fructus Musae corium farinosum at temperature is 60 DEG C;
(2) take Entermorpha powder 50kg and thiourea 6kg and add ultrasonic stirrer, add 100kg water, be 80kHz in supersonic frequency
Lower ultrasonic reaction 20min, is placed in reacted pastel heat drying 2h in the baking oven of 70 DEG C, obtains modified Entermorpha powder;
(3) above-mentioned modified Fructus Musae corium farinosum, modified Entermorpha powder are added agitator, add cerous sulfate solution 5kg and sodium alginate
10kg, adds water furnishing pasty state, pastel is put into microwave heating equipment, power be 250W, temperature be microwave at 120 DEG C
60min, is cooled to room temperature, and grinding the material to particle diameter is 0.5mm, obtains waste water mercury-removing adsorbent.
Embodiment 2
A kind of preparation method of waste water mercury-removing adsorbent, concrete operation step is as follows:
(1) Pericarpium Musae that 100kg water content is 12% being crushed to 40 mesh, adding concentration is that 5mol/L sodium hydroxide solution soaks
3h, is washed with water and washs Fructus Musae corium farinosum extremely neutrality, obtain Pericarpium Musae cellulose;10kg acrylic acid second is added in Pericarpium Musae cellulose
Ester, adds 100kg water, mix homogeneously, is dried 2h, obtains modified Fructus Musae corium farinosum at temperature is 80 DEG C;
(2) take Entermorpha powder 60kg and thiourea 8kg and add ultrasonic stirrer, add 120kg water, be 60kHz in supersonic frequency
Lower ultrasonic reaction 30min, is placed in reacted pastel heat drying 1.5h in the baking oven of 80 DEG C, obtains modified Entermorpha powder;
(3) above-mentioned modified Fructus Musae corium farinosum, modified Entermorpha powder are added agitator, add cerous sulfate solution 4kg and sodium alginate
12kg, adds water furnishing pasty state, pastel is put into microwave heating equipment, power be 200W, temperature be microwave at 130 DEG C
45min, is cooled to room temperature, and grinding the material to particle diameter is 0.5mm, obtains waste water mercury-removing adsorbent.
Embodiment 3
A kind of preparation method of waste water mercury-removing adsorbent, concrete operation step is as follows:
(1) Pericarpium Musae that 100kg water content is 12% being crushed to 60 mesh, adding concentration is that 3mol/L sodium hydroxide solution soaks
5h, is washed with water and washs Fructus Musae corium farinosum extremely neutrality, obtain Pericarpium Musae cellulose;15kg acrylic acid second is added in Pericarpium Musae cellulose
Ester, adds 120kg water, mix homogeneously, is dried 2.5h, obtains modified Fructus Musae corium farinosum at temperature is 80 DEG C;
(2) take Entermorpha powder 70kg and thiourea 10kg and add ultrasonic stirrer, add 150kg water, be 70kHz in supersonic frequency
Lower ultrasonic reaction 30min, is placed in reacted pastel heat drying 2h in the baking oven of 80 DEG C, obtains modified Entermorpha powder;
(3) above-mentioned modified Fructus Musae corium farinosum, modified Entermorpha powder are added agitator, add cerous sulfate solution 6kg and sodium alginate
12kg, adds water furnishing pasty state, pastel is put into microwave heating equipment, power be 300W, temperature be microwave at 140 DEG C
30min, is cooled to room temperature, and grinding the material to particle diameter is 1.0mm, obtains waste water mercury-removing adsorbent.
Embodiment 4
A kind of preparation method of waste water mercury-removing adsorbent, concrete operation step is as follows:
(1) Pericarpium Musae 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 Fructus Musae corium farinosum extremely neutrality, obtain Pericarpium Musae cellulose;12kg acrylic acid second is added in Pericarpium Musae cellulose
Ester, adds 100kg water, mix homogeneously, is dried 2h, obtains modified Fructus Musae corium farinosum at temperature is 80 DEG C;
(2) take Entermorpha powder 60kg and thiourea 10kg and add ultrasonic stirrer, add 120kg water, be 60kHz in supersonic frequency
Lower ultrasonic reaction 60min, is placed in reacted pastel heat drying 1h in the baking oven of 80 DEG C, obtains modified Entermorpha powder;
(3) above-mentioned modified Fructus Musae corium farinosum, modified Entermorpha powder are added agitator, add cerous sulfate solution 5kg and sodium alginate
15kg, adds water furnishing pasty state, pastel is put into microwave heating equipment, power be 250W, temperature be microwave at 120 DEG C
60min, is cooled to room temperature, and grinding the material to particle diameter is 1.0mm, obtains waste water mercury-removing adsorbent.
The using method of adsorbent is: at ambient temperature, is put into by the adsorbent of 3g in the waste water that 1L contains mercury ion,
Controlling pH is 6, stirs 60min, isolate adsorbent, the mercury ion in the most adsorbable waste water under rotating speed is 300r/min.
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 mercury ion, calculate suction further according to below equation
Attached rate, measurement result is as shown in the table.
ŋ=(C0-Ci)×100% /C0
Wherein C0、CiContent (mg/L) before and after adsorbing for mercury ions 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, the suction to mercury ion
Attached rate reaches more than 98%, has broad application prospects in Industrial Wastewater Treatment.
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 of a waste water mercury-removing adsorbent, it is characterised in that: it is with mass ratio as 100:10-15:50-70:6-
The Pericarpium Musae of 10:4-6:10-15, ethyl acrylate, Entermorpha powder, thiourea, cerous sulfate and sodium alginate, as raw material, pass through microwave
Heating makes adsorbent, and concrete operation step is as follows:
(1) 100 parts of Pericarpium Musae are pulverized, add sodium hydroxide solution and soak 3-5h, be washed with water and wash Fructus Musae corium farinosum extremely neutrality,
Pericarpium Musae cellulose;Adding 10-15 part ethyl acrylate in Pericarpium Musae cellulose, add 100-120 part water, mixing is all
Even, at temperature is 60-80 DEG C, it is dried 2-3h, obtains modified Fructus Musae corium farinosum;
(2) take Entermorpha powder 50-70 part and thiourea 6-10 part add ultrasonic stirrer, add suitable quantity of water and carry out ultrasonic reaction,
Reacted pastel is placed in heat drying 1-2h in the baking oven of 70-80 DEG C, obtains modified Entermorpha powder;
(3) above-mentioned modified Fructus Musae corium farinosum, modified Entermorpha powder are added agitator, add cerous sulfate solution 4-6 part and sodium alginate
10-15 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 waste water mercury-removing adsorbent.
The preparation method of waste water mercury-removing adsorbent the most according to claim 1, it is characterised in that: the water content of described Pericarpium Musae
It is 12%.
The preparation method of waste water mercury-removing adsorbent the most according to claim 2, it is characterised in that: step (1) is by Pericarpium Musae
It is crushed to 40-60 mesh.
The preparation method of waste water mercury-removing adsorbent the most according to claim 1, it is characterised in that: the concentration of described sodium hydroxide
For 3-5mol/L.
The preparation method of waste water mercury-removing adsorbent the most according to claim 1, it is characterised in that: described waterside platform powder is by fresh
Waterside platform powder cleaning, drying are 10% to water content, then are crushed to 80 mesh, obtain waterside platform powder.
The preparation method of waste water mercury-removing adsorbent the most according to claim 1, it is characterised in that: ultrasonic described in step (2)
Reaction is ultrasonic reaction 20-30min under supersonic frequency is 60-80kHz.
The preparation method of waste water mercury-removing adsorbent the most according to claim 1, it is characterised in that: step (3) described microwave
Power is 200-300W.
The preparation method of waste water mercury-removing adsorbent the most according to claim 1, it is characterised in that: described cerous sulfate solution dense
Degree is 5mol/L.
The preparation method of waste water mercury-removing adsorbent the most according to claim 1, it is characterised in that: step (3) described grinding is
Grinding the material to particle diameter is 0.5-1.0mm.
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CN107724105B (en) * | 2017-09-29 | 2020-09-04 | 安徽嘉明新材料科技有限公司 | Preparation method of TPU composite material for weather-resistant waterproof tent |
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Application publication date: 20161123 |