CN103274509A - Preparation method of composite flocculant capable of adsorbing heavy metal ions and composite flocculant product through - Google Patents
Preparation method of composite flocculant capable of adsorbing heavy metal ions and composite flocculant product through Download PDFInfo
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Abstract
The invention relates to a preparation method of a chitosan compound flocculant which can effectively remove organic pollutants in water, can adsorb heavy metal ions such as nickel, chromium and lead in water and has high heavy metal ion adsorption capacity and high adsorption efficiency and a chitosan compound flocculant product thereof. The chitosan compound flocculant product is prepared by adopting chitosan as a raw material, glutaraldehyde as a crosslinking agent and washed and acid pickled attapulgite as a modifier. The preparation method of the compound flocculant capable of adsorbing heavy metal ions has the characteristics of simple technology, low cost, no special equipment and easy industrial implementation, the compound flocculant reduces dosage of chiston, and cost is reduced.
Description
Technical field
The present invention relates to polymeric material field, be specifically related to a kind of heavy metal ion such as nickel, chromium, lead to be had composite flocculation agent of favourable absorption function and preparation method thereof.This flocculation agent both can remove organic pollutant in the water effectively, heavy metal ion such as the nickel in again can planar water, chromium, lead, and to heavy metal ion adsorbed amount is big in the water, adsorption efficiency is high, can be applicable to the process field of sewage such as electroplating industry, chemical industry.
Background technology
In recent years, along with the unrest row of the geometric growth of the size of population, modern industry waste water leaves about, municipal wastes, rural area pesticide spraying etc., causing has been few Freshwater resources aggravation shortage originally.Pollute in order to administer water, the mankind explore numerous physics, chemical process, and flocculation agent is exactly a class of consumption maximum in the chemical process water treatment agent.Usually will be referred to as flocculation agent for the water conditioner of Treatment of Industrial Water coagulant precipitation process, its effect is can produce absorption, " bridge formation " to suspended particulates in the water, thereby makes it be agglomerated into thick particle or floc sedimentation, reaches the purpose of accelerating sedimentation.
But at present industrial flocculation agent is not ideal enough to the treatment effect of heavy metal ions in wastewater.Fast development along with China's chemical industry and metallurgical industry, contain lead, copper, pollute every heavy metal wastewater therebies such as, chromium, mercury and just be on the rise from what produce in electrolytic solution, electroplate liquid and mining, the Metal smelting process, heavy metal wastewater thereby pollutes and to have become China's serious social concern, is a crucial difficult problem that presses for the Economic development of solution and Environmental Health, safe drinking water aspect at present.At present, the method that removes heavy metal ions in wastewater mainly contains: chemical precipitation and reduction, biology and plant absorption, solvent extraction and membrane separation technique etc.
In recent years, inorganic materials counterweight Adsorption Properties for Metal Ions more and more receives researcher's concern, most inorganic mineral material costs are low and the counterweight Adsorption Properties for Metal Ions is obvious, particularly noticeable aspect heavy metal ion adsorbed, wherein attapulgite is that tool is typically a kind of.
Attapulgite (claiming polygorskite again) is a kind of natural non-metallic minerals material, be a kind of have a chain laminate structure contain Shuifu County's magnesium silicate clay mineral, typical chemical formula is Si
8Mg
6O
20(OH)
2(OH
2)
44H
2O, structure belongs to 2: 1 type clay minerals, and in each 2: 1 unit structure layer, tetrahedron wafer angle is pushed up at a certain distance direction and is put upside down the form layers chain.Form the passage parallel with chain, filling zeolite water and crystal water in the passage at tetrahedron bar interband.The attapulgite fibrous texture generally comprises three levels: 1. basic structural unit is little bar-shaped or fibrous single crystal, and it is brilliant to be called for short rod.2. the monocrystalline bundle that is formed by the parallel gathering of monocrystalline.3. pile up the aggregate that forms mutually by crystalline substance bundle (comprising that rod is brilliant).The special construction of attapulgite makes it have very big specific surface area, and physical adsorption is very capable.On the other hand, attapulgite has the aspect negative charge, has adsorbed positively charged ion with interchangeability so that charge balance at interlayer, and attapulgite has just had stronger ionic adsorption exchange capacity like this.
The inventor discloses the PVDF hydridization flat sheet membrane [ZL201110254106.0] of Adsorption of Heavy Metal Ions in inventing early stage, utilize dull and stereotyped membrane as carrier, immobilized attapulgite, thus bring into play attapulgite well to the adsorption of heavy metal ion.But, how attapulgite is applied in the sewage disposal, both can remove organic pollutant in the water effectively, the heavy metal ion in again can planar water is a great problem.
Summary of the invention
How not ideal enough and attapulgite is applied to the deficiency that aspect such as sewage disposal exists to the treatment effect of heavy metal ions in wastewater at existing industrial flocculation agent, the technical problem that quasi-solution of the present invention is determined provides and a kind ofly both can remove organic pollutant in the water effectively, heavy metal ion such as the nickel in again can planar water, chromium, lead, and to preparation method of the composite flocculation agent that heavy metal ion adsorbed amount is big in the water, adsorption efficiency is high and products thereof.It is raw material that product of the present invention adopts chitosan, and with glutaraldehyde as cross linker, attapulgite is that properties-correcting agent prepares.
The composite flocculation agent of Adsorption of Heavy Metal Ions of the present invention is made by following method:
(1) pre-treatment of attapulgite.Take by weighing 10g～20g particle diameter 300 orders～1000 purpose attapulgites, use the 1L distilled water wash, treat that post precipitation gets its supernatant liquid, get its supernatant liquid behind the centrifugal 1min of 500rpm, add a small amount of distilled water in the supernatant liquid and mix the centrifugal 1min of back continuation 500rpm, get its supernatant liquid then, behind the repetitive scrubbing supernatant liquid like this 3～5 times, carry out centrifugation with 4000rpm at last, get its precipitation, 90 ℃ of following vacuum-drying 24h grind the sieve of afterwards selecting corresponding order number by size, get the purifying attapulgite.
Configuration concentration is the hydrochloric acid soln of 0.5mol/L～3mol/L, getting 10g～20g purifying attapulgite and 150mL～200mL hydrochloric acid soln joins in the small beaker and mixes, behind the 5min, with mixture heating up to 70 ℃～80 ℃, stir 1h～2h, sonic oscillation 30min～40min then, suction filtration is washed with distilled water to pH and is about about 6,90 ℃ of following vacuum-drying 24h, select the sieve of corresponding order number after grinding by size, get sour attapulgite modified.
(2) preparation of chitin composite flocculant.Take by weighing the 4g chitosan and mix (mass ratio 4: 1～5: 1) with attapulgite after a certain amount of sour modification, adding 100ml concentration is 1%～2% acetum stirring, after treating that it fully dissolves, use the NaOH solution of 1mol/L to regulate pH to 10, add 20ml～30ml glutaraldehyde cross-linking 3h～5h (60 ℃ of water-bath vigorous stirring).With the flocculation agent suction filtration after crosslinked, distilled water is washed till neutrality, namely gets composite flocculation agent of the present invention after 50 ℃～70 ℃ vacuum-dryings.
Beneficial effect of the present invention:
The composite flocculation agent that the present invention solves described Adsorption of Heavy Metal Ions utilizes chitosan and attapulgite modified compound the preparing of acid.Chitosan is the chitin deacetylase based products, uses as flocculation agent, can remove organic pollutant in the water effectively, and have good flocculating property in acidic solution.Attapulgite is a kind of good inorganic mineral of abundant, inexpensive, heavy metal ion adsorbed property of originating, with the flocculation agent of its preparation heavy metal ion in the planar water simultaneously.Therefore, the composite flocculation agent of this project preparation can be brought into play chitosan and attapulgite advantage separately, collaborative its throwing out, the scope of application and the flocculation efficiency of raising composite flocculation agent.In addition, chitosan-attapulgite clay compounded flocculation agent has reduced the consumption of chitosan, has reduced cost.
The prepared composite flocculation agent preparation method of the present invention simply, do not need specific installation, production cost low, be suitable for industrial applications.
Embodiment:
The following examples can make those skilled in the art more fully understand the present invention, but do not limit the present invention in any way
Embodiment 1:
(1) pre-treatment of attapulgite.Take by weighing 10g particle diameter 300 purpose attapulgites, use the 1L distilled water wash, treat that post precipitation gets its supernatant liquid, get its supernatant liquid behind the centrifugal 1min of 500rpm, add a small amount of distilled water in the supernatant liquid and mix the centrifugal 1min of back continuation 500rpm, get its supernatant liquid then, so behind the repetitive scrubbing supernatant liquid 3 times, carry out centrifugation with 4000rpm at last, get its precipitation, 90 ℃ of following vacuum-drying 24h grind the sieve of afterwards selecting corresponding order number by size, get the purifying attapulgite.
Configuration concentration is the hydrochloric acid soln of 0.5mol/L, getting 10g purifying attapulgite and 150mL hydrochloric acid soln joins in the small beaker and mixes, behind the 5min, with mixture heating up to 70 ℃, stir 1h, sonic oscillation 30min then, suction filtration is washed with distilled water to pH and is about about 6,90 ℃ of following vacuum-drying 24h, select the sieve of corresponding order number after grinding by size, get sour attapulgite modified.
(2) preparation of chitin composite flocculant.The attapulgite that takes by weighing after 4g chitosan and a certain amount of sour modification mixes (mass ratio 4: 1), adding 100ml concentration is 1% acetum stirring, after treating that it fully dissolves, use the NaOH solution of 1mol/L to regulate pH to 10, add 20ml glutaraldehyde cross-linking 3h (60 ℃ of water-bath vigorous stirring).With the flocculation agent suction filtration after crosslinked, distilled water is washed till neutrality, namely gets composite flocculation agent of the present invention after 50 ℃ of vacuum-dryings.
Embodiment 2:
(1) pre-treatment of attapulgite.Take by weighing 10g particle diameter 1000 purpose attapulgites, use the 1L distilled water wash, precipitation is got its supernatant liquid, gets its supernatant liquid behind the centrifugal 1min of 500rpm, add a small amount of distilled water in the supernatant liquid and mix the centrifugal 1min of back continuation 500rpm, get its supernatant liquid then, so behind the repetitive scrubbing supernatant liquid 3 times, carry out centrifugation with 4000rpm at last, get its precipitation, 90 ℃ of following vacuum-drying 24h grind the sieve of afterwards selecting corresponding order number by size, get the purifying attapulgite.
Configuration concentration is the hydrochloric acid soln of 0.5mol/L, getting 20g purifying attapulgite and 150mL hydrochloric acid soln joins in the small beaker and mixes, behind the 5min, with mixture heating up to 70 ℃, stir 1h, sonic oscillation 30min then, suction filtration is washed with distilled water to pH and is about about 6,90 ℃ of following vacuum-drying 24h, select the sieve of corresponding order number after grinding by size, get sour attapulgite modified.
(2) preparation of chitin composite flocculant.The attapulgite that takes by weighing after 4g chitosan and a certain amount of sour modification mixes (mass ratio 4: 1), adding 100ml concentration is 2% acetum stirring, after treating that it fully dissolves, use the NaOH solution of 1mol/L to regulate pH to 10, add 20ml glutaraldehyde cross-linking 3h (60 ℃ of water-bath vigorous stirring).With the flocculation agent suction filtration after crosslinked, distilled water is washed till neutrality, namely gets composite flocculation agent of the present invention after 50 ℃ of vacuum-dryings.
Embodiment 3:
(1) pre-treatment of attapulgite.Take by weighing 20g particle diameter 300 purpose attapulgites, use the 1L distilled water wash, precipitation is got its supernatant liquid, gets its supernatant liquid behind the centrifugal 1min of 500rpm, add a small amount of distilled water in the supernatant liquid and mix the centrifugal 1min of back continuation 500rpm, get its supernatant liquid then, so behind the repetitive scrubbing supernatant liquid 5 times, carry out centrifugation with 4000rpm at last, get its precipitation, 90 ℃ of following vacuum-drying 24h grind the sieve of afterwards selecting corresponding order number by size, get the purifying attapulgite.
Configuration concentration is the hydrochloric acid soln of 3mol/L, getting 10g purifying attapulgite and 150mL hydrochloric acid soln joins in the small beaker and mixes, behind the 5min, with mixture heating up to 80 ℃, stir 2h, sonic oscillation 30min then, suction filtration is washed with distilled water to pH and is about about 6,90 ℃ of following vacuum-drying 24h, select the sieve of corresponding order number after grinding by size, get sour attapulgite modified.
(2) preparation of chitin composite flocculant.The attapulgite that takes by weighing after 4g chitosan and a certain amount of sour modification mixes (mass ratio 5: 1), adding 100ml concentration is 2% acetum stirring, after treating that it fully dissolves, use the NaOH solution of 1mol/L to regulate pH to 10, add 20ml glutaraldehyde cross-linking 5h (60 ℃ of water-bath vigorous stirring).With the flocculation agent suction filtration after crosslinked, distilled water is washed till neutrality, namely gets composite flocculation agent of the present invention after 70 ℃ of vacuum-dryings.
Embodiment 4:
(1) pre-treatment of attapulgite.Take by weighing 15g particle diameter 500 purpose attapulgites, use the 1L distilled water wash, precipitation is got its supernatant liquid, gets its supernatant liquid behind the centrifugal 1min of 500rpm, add a small amount of distilled water in the supernatant liquid and mix the centrifugal 1min of back continuation 500rpm, get its supernatant liquid then, so behind the repetitive scrubbing supernatant liquid 5 times, carry out centrifugation with 4000rpm at last, get its precipitation, 90 ℃ of following vacuum-drying 24h grind the sieve of afterwards selecting corresponding order number by size, get the purifying attapulgite.
Configuration concentration is the hydrochloric acid soln of 1mol/L, getting 12g purifying attapulgite and 180mL hydrochloric acid soln joins in the small beaker and mixes, behind the 5min, with mixture heating up to 70 ℃, stir 1h, sonic oscillation 30min then, suction filtration is washed with distilled water to pH and is about about 6,90 ℃ of following vacuum-drying 24h, select the sieve of corresponding order number after grinding by size, get sour attapulgite modified.
(2) preparation of chitin composite flocculant.The attapulgite that takes by weighing after 4g chitosan and a certain amount of sour modification mixes (mass ratio 5: 1), adding 100ml concentration is 1.5% acetum stirring, after treating that it fully dissolves, use the NaOH solution of 1mol/L to regulate pH to 10, add 30ml glutaraldehyde cross-linking 4h (60 ℃ of water-bath vigorous stirring).With the flocculation agent suction filtration after crosslinked, distilled water is washed till neutrality, namely gets composite flocculation agent of the present invention after 60 ℃ of vacuum-dryings.
Embodiment 5:
(1) pre-treatment of attapulgite.Take by weighing 16g particle diameter 800 purpose attapulgites, use the 1L distilled water wash, precipitation is got its supernatant liquid, gets its supernatant liquid behind the centrifugal 1min of 500rpm, add a small amount of distilled water in the supernatant liquid and mix the centrifugal 1min of back continuation 500rpm, get its supernatant liquid then, so behind the repetitive scrubbing supernatant liquid 5 times, carry out centrifugation with 4000rpm at last, get its precipitation, 90 ℃ of following vacuum-drying 24h grind the sieve of afterwards selecting corresponding order number by size, get the purifying attapulgite.
Configuration concentration is the hydrochloric acid soln of 2.5mol/L, getting 18g purifying attapulgite and 160mL hydrochloric acid soln joins in the small beaker and mixes, behind the 5min, with mixture heating up to 70 ℃, stir 2h, sonic oscillation 40min then, suction filtration is washed with distilled water to pH and is about about 6,90 ℃ of following vacuum-drying 24h, select the sieve of corresponding order number after grinding by size, get sour attapulgite modified.
(2) preparation of chitin composite flocculant.The attapulgite that takes by weighing after 4g chitosan and a certain amount of sour modification mixes (mass ratio 5: 1), adding 100ml concentration is 1.8% acetum stirring, after treating that it fully dissolves, use the NaOH solution of 1mol/L to regulate pH to 10, add 25ml glutaraldehyde cross-linking 5h (60 ℃ of water-bath vigorous stirring).With the flocculation agent suction filtration after crosslinked, distilled water is washed till neutrality, namely gets composite flocculation agent of the present invention after 70 ℃ of vacuum-dryings.
Embodiment 6:
(1) pre-treatment of attapulgite.Take by weighing 18g particle diameter 1000 purpose attapulgites, use the 1L distilled water wash, precipitation is got its supernatant liquid, gets its supernatant liquid behind the centrifugal 1min of 500rpm, add a small amount of distilled water in the supernatant liquid and mix the centrifugal 1min of back continuation 500rpm, get its supernatant liquid then, so behind the repetitive scrubbing supernatant liquid 5 times, carry out centrifugation with 4000rpm at last, get its precipitation, 90 ℃ of following vacuum-drying 24h grind the sieve of afterwards selecting corresponding order number by size, get the purifying attapulgite.
Configuration concentration is the hydrochloric acid soln of 3mol/L, getting 20g purifying attapulgite and 180mL hydrochloric acid soln joins in the small beaker and mixes, behind the 5min, with mixture heating up to 75 ℃, stir 1.5h, sonic oscillation 35min then, suction filtration is washed with distilled water to pH and is about about 6,90 ℃ of following vacuum-drying 24h, select the sieve of corresponding order number after grinding by size, get sour attapulgite modified.
(2) preparation of chitin composite flocculant.The attapulgite that takes by weighing after 4g chitosan and a certain amount of sour modification mixes (mass ratio 4: 1), adding 100ml concentration is 1.6% acetum stirring, after treating that it fully dissolves, use the NaOH solution of 1mol/L to regulate pH to 10, add 25ml glutaraldehyde cross-linking 4h (60 ℃ of water-bath vigorous stirring).With the flocculation agent suction filtration after crosslinked, distilled water is washed till neutrality, namely gets composite flocculation agent of the present invention after 60 ℃ of vacuum-dryings.
Claims (5)
1. the composite flocculation agent of a described Adsorption of Heavy Metal Ions is made by following method;
(1) pre-treatment of attapulgite: configuration concentration is the hydrochloric acid soln of 0.5mol/L～3mol/L, getting 10g～20g purifying attapulgite and 150mL～200mL hydrochloric acid soln joins in the small beaker and mixes, behind the 5min, with mixture heating up to 70 ℃～80 ℃, stir 1h～2h, sonic oscillation 30min～40min then, suction filtration is washed with distilled water to pH and is about about 6,90 ℃ of following vacuum-drying 24h, select the sieve of corresponding order number after grinding by size, get sour attapulgite modified;
(2) preparation of chitin composite flocculant.Take by weighing the 4g chitosan and mix (mass ratio 4: 1～5: 1) with attapulgite after a certain amount of sour modification, adding 100ml concentration is 1%～2% acetum stirring, after treating that it fully dissolves, use the NaOH solution of 1mol/L to regulate pH to 10, add 20ml～30ml glutaraldehyde cross-linking 3h～5h (60 ℃ of water-bath vigorous stirring).With the flocculation agent suction filtration after crosslinked, distilled water is washed till neutrality, namely gets composite flocculation agent of the present invention after 50 ℃～70 ℃ vacuum-dryings.
2. the composite flocculation agent of Adsorption of Heavy Metal Ions according to claim 1, it is characterized in that described purifying preparation method of attapulgite is as follows: take by weighing 10g～20g particle diameter 300 orders～1000 order attapulgites, use the 1L distilled water wash, treat that post precipitation gets its supernatant liquid, get its supernatant liquid behind the centrifugal 1min of 500rpm, add a small amount of distilled water in the supernatant liquid and mix the centrifugal 1min of back continuation 500rpm, get its supernatant liquid then, behind the repetitive scrubbing supernatant liquid like this 3～5 times, carry out centrifugation with 4000rpm at last, get its precipitation, 90 ℃ of following vacuum-drying 24h, select the sieve of corresponding order number after grinding by size, get the purifying attapulgite.
3. as the preparation method of the composite flocculation agent of Adsorption of Heavy Metal Ions as described in the right 1-2, comprise the steps:
(1) pre-treatment of attapulgite: configuration concentration is the hydrochloric acid soln of 0.5mol/L～3mol/L, getting 10g～20g purifying attapulgite and 150mL～200mL hydrochloric acid soln joins in the small beaker and mixes, behind the 5min, with mixture heating up to 70 ℃～80 ℃, stir 1h～2h, sonic oscillation 30min～40min then, suction filtration is washed with distilled water to pH and is about about 6,90 ℃ of following vacuum-drying 24h, select the sieve of corresponding order number after grinding by size, get sour attapulgite modified;
(2) preparation of chitin composite flocculant.Take by weighing the 4g chitosan and mix (mass ratio 4: 1～5: 1) with attapulgite after a certain amount of sour modification, adding 100ml concentration is 1%～2% acetum stirring, after treating that it fully dissolves, use the NaOH solution of 1mol/L to regulate pH to 10, add 20ml～30ml glutaraldehyde cross-linking 3h～5h (60 ℃ of water-bath vigorous stirring).With the flocculation agent suction filtration after crosslinked, distilled water is washed till neutrality, namely gets composite flocculation agent of the present invention after 50 ℃～70 ℃ vacuum-dryings.
4. as the preparation method of the composite flocculation agent of Adsorption of Heavy Metal Ions as described in the right 3, step is as follows:
(1) pre-treatment of attapulgite: take by weighing 10g particle diameter 300 purpose attapulgites, use the 1L distilled water wash, treat that post precipitation gets its supernatant liquid, get its supernatant liquid behind the centrifugal 1min of 500rpm, add a small amount of distilled water in the supernatant liquid and mix the centrifugal 1min of back continuation 500rpm, get its supernatant liquid then, behind the repetitive scrubbing supernatant liquid like this 3 times, carry out centrifugation with 4000rpm at last, get its precipitation, 90 ℃ of following vacuum-drying 24h grind the sieve of afterwards selecting corresponding order number by size, get the purifying attapulgite;
Configuration concentration is the hydrochloric acid soln of 0.5mol/L, getting 10g purifying attapulgite and 150mL hydrochloric acid soln joins in the small beaker and mixes, behind the 5min, with mixture heating up to 70 ℃, stir 1h, sonic oscillation 30min then, suction filtration is washed with distilled water to pH and is about about 6,90 ℃ of following vacuum-drying 24h, select the sieve of corresponding order number after grinding by size, get sour attapulgite modified;
(2) preparation of chitin composite flocculant.The attapulgite that takes by weighing after 4g chitosan and a certain amount of sour modification mixes (mass ratio 4: 1), adding 100ml concentration is 1% acetum stirring, after treating that it fully dissolves, use the NaOH solution of 1mol/L to regulate pH to 10, add 20ml glutaraldehyde cross-linking 3h (60 ℃ of water-bath vigorous stirring).With the flocculation agent suction filtration after crosslinked, distilled water is washed till neutrality, namely gets composite flocculation agent of the present invention after 50 ℃ of vacuum-dryings.
5. as the preparation method of the composite flocculation agent of Adsorption of Heavy Metal Ions as described in the right 3, step is as follows:
(1) pre-treatment of attapulgite.Take by weighing 10g particle diameter 1000 purpose attapulgites, use the 1L distilled water wash, treat that post precipitation gets its supernatant liquid, get its supernatant liquid behind the centrifugal 1min of 500rpm, add a small amount of distilled water in the supernatant liquid and mix the centrifugal 1min of back continuation 500rpm, get its supernatant liquid then, so behind the repetitive scrubbing supernatant liquid 3 times, carry out centrifugation with 4000rpm at last, get its precipitation, 90 ℃ of following vacuum-drying 24h grind the sieve of afterwards selecting corresponding order number by size, get the purifying attapulgite;
Configuration concentration is the hydrochloric acid soln of 0.5mol/L, getting 20g purifying attapulgite and 150mL hydrochloric acid soln joins in the small beaker and mixes, behind the 5min, with mixture heating up to 70 ℃, stir 1h, sonic oscillation 30min then, suction filtration is washed with distilled water to pH and is about about 6,90 ℃ of following vacuum-drying 24h, select the sieve of corresponding order number after grinding by size, get sour attapulgite modified;
(2) preparation of chitin composite flocculant.The attapulgite that takes by weighing after 4g chitosan and a certain amount of sour modification mixes (mass ratio 4: 1), adding 100ml concentration is 2% acetum stirring, after treating that it fully dissolves, use the NaOH solution of 1mol/L to regulate pH to 10, add 20ml glutaraldehyde cross-linking 3h (60 ℃ of water-bath vigorous stirring).With the flocculation agent suction filtration after crosslinked, distilled water is washed till neutrality, namely gets composite flocculation agent of the present invention after 50 ℃ of vacuum-dryings.
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