CN107840431A - A kind of preparation method and application for removing solution Nitrite ionic material - Google Patents
A kind of preparation method and application for removing solution Nitrite ionic material Download PDFInfo
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- CN107840431A CN107840431A CN201711054385.XA CN201711054385A CN107840431A CN 107840431 A CN107840431 A CN 107840431A CN 201711054385 A CN201711054385 A CN 201711054385A CN 107840431 A CN107840431 A CN 107840431A
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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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
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Abstract
The invention discloses a kind of preparation method for removing solution Nitrite ionic material, it is comprised the following steps that：Bark of dahurian larch is chosen, it is standby to be ground into bark of dahurian larch powder；Weigh bark of dahurian larch powder dress to immerse in deionized water, stir, obtain mixed liquor：After above-mentioned 40 60 DEG C of hot-water extractions of mixed liquor, filtrate and filter residue are obtained；Deionized water is added in filter residue, repeats aforesaid operations, when filtrate is colourless, obtained filter residue is the bark of dahurian larch powder A for removing solution Nitrite ion.Bark of dahurian larch powder A specific surface areas produced by the present invention are big, and the nitrite ion effect adsorbed in waste water is good, and bark of dahurian larch wide material sources and cheap, green.
Description
Technical field
It is more particularly to a kind of to remove solution Nitrite ion the present invention relates to environmental protection technical field
The preparation method and application of material.
Background technology
With widely using for human being's production life nitrite, rainwash water resource is asked by nitrite pollution
Topic can not be ignored.At present, the method for removing solution Nitrite ion is broadly divided into three major types, is to include UF membrane respectively
The physical method of method, ion-exchange etc., chemical oxidation-reduction method and biological denitrificaion method.Wherein, ion-exchange purification
As a result it is good, but cost is too high is not suitable for the processing of large-scale industrialization water pollution, and can produce the regenerated liquid of high concentration, still need to
Further processing.Oxidation-reduction method is that nitrite ion is converted into N by adding oxidant or reducing agent2、NH3、NH4 +
Deng, but oxidant, the reducing agent added easily causes the secondary pollution of water.Biological denitrificaion method is in anoxic bar by denitrifying bacteria
Nitrite nitrogen is reduced to N under part2, its shortcoming is that the cycle is long, clean-up effect is poor, but also can produce substantial amounts of sludge and discard
Thing, three of the above method are each defective.
" river of three ditch one " (class forming, Ma Jiagou, good faith ditch, the Ash river) in Harbin was once black and odorous water, from 2010
After establishing 5 sewage treatment plants on " river of three ditch one ", partial sector realizes clear water trickling, main contamination index's chemical oxygen demand
Amount, ammonia nitrogen concentration substantially reduce.But the exceeded feelings of black and odorous water Nitrite, nitrate anion, chlorion, phosphate radical plasma
Condition is still more serious.
China's wood processing industry produces substantial amounts of larch (Larix gmelini) bark every year, from larch
The poly- flavanol compound plant polyphenol stock number of bark is relatively abundant.The industrialization product master of the polyphenol water extract of conventional bark of dahurian larch
If larch extract, but because of the defects of its tannin extract is of poor quality, profit is low, rouge and powder problem is serious larch bark tannin extract industry
Increasingly withered, corresponding product is gradually substituted by the tannin extract of red bayberry and Black Wattle source.In bark of dahurian larch water extraction residue, still
Containing many macromolecules or with hydrophobic structure polyphenol be referred to as inextractable polyphenol (NEPs) important phenols (for example,
Rouge and powder).These polyphenols are not utilized effectively, and other conventional products application added values are relatively low, and which results in fall
The serious waste of leaf pine bark residue resource.
Therefore, the nitrite ion for how solving the problems, such as to remove in stream is those skilled in the art's urgent need to resolve.
The content of the invention
In view of this, the invention provides a kind of cost is low, the removing solution Central Asia of clean-up effect more preferably, applied widely
The preparation method and application of nitrate ion material.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of preparation method for removing solution Nitrite ionic material, it is comprised the following steps that：
(1) larch is gathered, and uses its bark, it is standby to be ground into bark of dahurian larch powder；
(2) bark of dahurian larch powder is added in deionized water, stirs, obtain mixed liquor：
(3) above-mentioned mixed liquor is heated in a water bath, after heating water bath, mixed liquor filtered, obtain filtrate and filter residue；
(4) deionized water is added in filter residue, repeat the above steps the operation of (3), until filtrate for it is colourless when, it is obtained
Filter residue is the bark of dahurian larch powder A for removing solution Nitrite ion.
Beneficial effect of the present invention：Using bark of dahurian larch as raw material in the present invention, using can not in bark of dahurian larch
Polyphenol is extracted, inextractable polyphenol is the flavanols condensate that relative molecular mass is more than 3000 in bark of dahurian larch powder, its
The characteristics of with loose structure and being easy to infiltration removes nitrite ion, and will be fallen leaves pine tree by immersion and heating water bath
The condensed tannin filtered out in skin has high added value, improves the utilization rate of bark of dahurian larch.
Preferably, bark of dahurian larch described in step (1) be larch in Xinanlin area, Larix principis-rupprechtii, larix sibirica,
Larch-tree or one or more kinds of mixtures of European larch bark.Inextractable polyphenol in bark of dahurian larch
There is suction-operated to nitrite ion.
Preferably, bark of dahurian larch described in step (1) is to freeze fallen leaves pine tree, the mesh number of described bark of dahurian larch powder
For 20-200 mesh.
Preferably, the bark of dahurian larch powder described in step (2) and the quality solid-liquid ratio of deionized water are 1:20-1:100,
More preferably the quality solid-liquid ratio of bark of dahurian larch powder and deionized water is 1:40-1:60.
Preferably, water bath heating temperature described in step (3) is 50-70 DEG C, and the heating water bath time is 5-7h.More preferably
Water bath heating temperature is 60 DEG C, and the heating water bath time is 6h.
Preferably, mixing time described in step (4) is 15-30min, and more preferably mixing time is 20min.
The present invention also provides a kind of method for being used to remove and nitrite ion material being removed in stream, and its specific steps is such as
Under：
(1) it is water sample to be measured to take the exceeded water sample of nitrous radical ion；
(2) bark of dahurian larch powder A is weighed, is fitted into chromatographic column, chromatographic column is placed on iron stand；
(3) water sample and Al (OH) to be measured are measured3Suspension mixes, and stirs, is mixed liquid and pours into mistake in chromatographic column
Filter, filtrate is obtained, collect filtrate, detect the content of filtrate Nitrite ion.
Preferably, water sample to be measured and Al (OH) in step (3)3Suspension volume ratio is 1:50.Using Al (OH)3Suspension
Measure is influenceed when being in order to avoid having muddy or coloured in water sample to be measured.
Preferably, bark of dahurian larch A quality described in step (3) and the volume ratio of mixed liquor are 4:5.
Using the beneficial effect of above-mentioned technical proposal：Bark of dahurian larch is used as primary raw material in the present invention first, and it is former
Expect wide material sources and cheap；Material preparation process is simple to operate, and clear without using additional chemical reagent, preparation process green
Clean, energy-conservation, low consumption, are easy to industrialize；The condensed tannin filtrate that preparation process obtains, it is the tannin product with high added value,
Add productivity effect.
Embodiment
The embodiment of the invention discloses a kind of preparation method and application for removing solution Nitrite ionic material.
Embodiment 1
A kind of preparation method for removing solution Nitrite ionic material, it is comprised the following steps that：
(1) larch in Xinanlin area is chosen, and uses its bark, it is standby to be ground into bark of dahurian larch powder；
(2) weigh 50g bark of dahurian larch powder to be fitted into 1000mL conical flasks, 1000mL deionizations will be added in conical flask
Water, stir, obtain mixed liquor；
(3) conical flask is heated to 60 DEG C, after heating water bath in a water bath, mixed liquor in conical flask is filtered, obtains filtrate
And filter residue；
(4) after filter residue being reinstalled into conical flask, then 1000mL deionized waters are added in conical flask, repeated the above steps
(3) operation, when filtrate is colourless, obtained filter residue is the bark of dahurian larch powder A for removing solution Nitrite ion.
Embodiment 2
A kind of preparation method for removing solution Nitrite ionic material, it is comprised the following steps that：
(1) larch in Xinanlin area is chosen, and uses its bark, it is standby to be ground into bark of dahurian larch powder；
(2) weigh 40g bark of dahurian larch powder to be fitted into 2000mL conical flasks, 1600mL deionizations will be added in conical flask
Water, stir, obtain mixed liquor；
(3) conical flask is heated to 60 DEG C, after heating water bath in a water bath, mixed liquor in conical flask is filtered, obtains filtrate
And filter residue；
(4) after filter residue being reinstalled into conical flask, then 1600mL deionized waters are added in conical flask, repeated the above steps
(3) operation, when filtrate is colourless, obtained filter residue is the bark of dahurian larch powder A for removing solution Nitrite ion.
Embodiment 3
A kind of preparation method for removing solution Nitrite ionic material, it is comprised the following steps that：
(1) larch in Xinanlin area is chosen, and uses its bark, it is standby to be ground into bark of dahurian larch powder；
(2) 20g bark of dahurian larch powder is weighed to be fitted into 1000mL conical flasks, will be separately added into conical flask 1000mL go from
Sub- water, stirs, and obtains mixed liquor；
(3) conical flask is heated to 60 DEG C, after heating water bath in a water bath, mixed liquor in conical flask is filtered, obtains filtrate
And filter residue；
(4) after filter residue being reinstalled into conical flask, then 1000mL deionized waters are added in conical flask, repeated the above steps
(3) operation, when filtrate is colourless, obtained filter residue is the bark of dahurian larch powder A for removing solution Nitrite ion.
Embodiment 4
A kind of preparation method for removing solution Nitrite ionic material, it is comprised the following steps that：
(1) larch in Xinanlin area is chosen, and uses its bark, it is standby to be ground into bark of dahurian larch powder；
(2) 20g bark of dahurian larch powder is weighed to be fitted into 2000mL conical flasks, will be separately added into conical flask 1200mL go from
Sub- water, stirs, and obtains mixed liquor；
(3) conical flask is heated to 60 DEG C, after heating water bath in a water bath, mixed liquor in conical flask is filtered, obtains filtrate
And filter residue；
(4) after filter residue being reinstalled into conical flask, then 2000mL deionized waters are added in conical flask, repeated the above steps
(3) operation, when filtrate is colourless, obtained filter residue is the bark of dahurian larch powder A for removing solution Nitrite ion.
Embodiment 5
A kind of preparation method for removing solution Nitrite ionic material, it is comprised the following steps that：
(1) larch in Xinanlin area is chosen, and uses its bark, it is standby to be ground into bark of dahurian larch powder；
(2) 20g bark of dahurian larch powder is weighed to be fitted into 2000mL conical flasks, will be separately added into conical flask 1600mL go from
Sub- water, stirs, and obtains mixed liquor；
(3) conical flask is heated to 60 DEG C, after heating water bath in a water bath, mixed liquor in conical flask is filtered, obtains filtrate
And filter residue；
(4) after filter residue being reinstalled into conical flask, then 2000mL deionized waters are added in conical flask, repeated the above steps
(3) operation, when filtrate is colourless, obtained filter residue is the bark of dahurian larch powder A for removing solution Nitrite ion.
Performance test
1st, specific surface area is tested
Gained fallen leaves bark powder A in embodiment 1~5 is respectively placed in ASAP2020 than Surface Tester, is 25 in temperature
DEG C, pressure be 10~5Pa under deaerate 12h after measure specific surface area.It the results are shown in Table 1.
2nd, the test of nitrite ion is adsorbed
The lyophilized sample 0.1g of above-described embodiment 1~5 is put in after adsorbing 24h in 150ug/L nitrous radical ion solution,
Filtering measure filter liquor concentration C, calculates equilibrium adsorption capacities Qs of the bark of dahurian larch A to nitrous radical ion.
Computational methods：
The clearance of nitrite ion is calculated by formula (1)：
R=(C0~Ce)/C0100% wherein：
C0、CeThe respectively preceding heavy metal mass concentration with solution after balance of balance, ug/L；
C0For 150mg/L；It the results are shown in Table 1
The function and performance of the present invention are made and be expanded on further below by way of experiment.
Table 1
By above-mentioned table 1, it is known that specific surface area is smaller, and the suction-operated to nitrite ion is stronger, reaches as high as
93.3%.It is adapted to the removal of the nitrite ions such as trade effluent, sanitary wastewater in the present invention.
Embodiment 6
It is a kind of to be used to remove the method that nitrite ion material is removed in stream, it is characterised in that its specific steps is such as
Under：
(1) it is water sample to be measured to take the class forming water sample that nitrous ion concentration is 3.19mg/L；
(2) obtained bark of dahurian larch powder A in above-described embodiment 1 to 5 is chosen, the high work of about 3cm is inserted into chromatographic column
Change cotton, be further filled with the high fallen leaves bark powder A160g of about 30cm, finally insert the high activation cottons of about 3cm, chromatographic column is placed in brandreth
It is filter on platform.
(3) 125g KAl (SO are taken4)2In 1000mL beakers, 1000mL distilled water is added thereto, is heated to 60 DEG C, so
55mL concentrated ammonia liquors are added afterwards, stirring, is stood to precipitating, is washed repeatedly with decantation and be precipitated to nothing, are eventually adding 300mL steamings
Distilled water can be configured to Al (OH)3Suspension.
Water sample 10ml to be measured is measured, 500ml Al (OH) is added in water sample to be measured3Suspension, 10min is placed after stirring
Suspension is fully precipitated, filter, discard 25ml filtrate, then measure 200ml solution and pour into chromatographic column, filter,
Filtrate is collected, constant volume 200ml, takes 50ml to use the content of spectrophotometry nitrite ion therein.It is shown in Table 2.
Embodiment 7
It is a kind of to be used to remove the method that nitrite ion material is removed in stream, it is characterised in that its specific steps is such as
Under：
(1) it is water sample to be measured to take the horse man ditch water sample that nitrous ion concentration is 4.48mg/L；
(2) obtained bark of dahurian larch powder A in above-described embodiment 1 to 5 is chosen, the high work of about 3cm is inserted into chromatographic column
Change cotton, be further filled with the high fallen leaves bark powder A160g of about 30cm, finally insert the high activation cottons of about 3cm, chromatographic column is placed in brandreth
It is filter on platform.
(3) 125g KAl (SO are taken4)2In 1000mL beakers, 1000mL distilled water is added thereto, is heated to 60 DEG C, so
55mL concentrated ammonia liquors are added afterwards, stirring, is stood to precipitating, is washed repeatedly with decantation and be precipitated to nothing, are eventually adding 300mL steamings
Distilled water can be configured to Al (OH)3Suspension.
Water sample 10ml to be measured is measured, 500ml Al (OH) is added in water sample to be measured3Suspension, 10min is placed after stirring
Suspension is fully precipitated, filter, discard 25ml filtrate, then measure 200ml solution and pour into chromatographic column, filter,
Filtrate is collected, constant volume 200ml, takes 50ml to use the content of spectrophotometry nitrite ion therein.It is shown in Table 2.
Embodiment 8
It is a kind of to be used to remove the method that nitrite ion material is removed in stream, it is characterised in that its specific steps is such as
Under：
(1) it is water sample to be measured to take the good faith ditch water sample that nitrous ion concentration is 4.11mg/L；
(2) obtained bark of dahurian larch powder A in above-described embodiment 1 to 5 is chosen, the high work of about 3cm is inserted into chromatographic column
Change cotton, be further filled with the high fallen leaves bark powder A160g of about 30cm, finally insert the high activation cottons of about 3cm, chromatographic column is placed in brandreth
Filter is formed on platform.
(3) 125g KAl (SO are taken4)2In 1000mL beakers, 1000mL distilled water is added thereto, is heated to 60 DEG C, so
55mL concentrated ammonia liquors are added afterwards, stirring, is stood to precipitating, is washed repeatedly with decantation and be precipitated to nothing, are eventually adding 300mL steamings
Distilled water can be configured to Al (OH)3Suspension.
Water sample 10ml to be measured is measured, 500ml Al (OH) is added in water sample to be measured3Suspension, 10min is placed after stirring
Suspension is fully precipitated, filter, discard 25ml filtrate, then measure 200ml solution and pour into chromatographic column, filter,
Filtrate is collected, constant volume 200ml, takes 50ml to use the content of spectrophotometry nitrite ion therein.It is shown in Table 2.
Table 2
As shown in Table 2, the bark of dahurian larch powder A that prepared by the present invention can effectively remove nitrite ion.
Bark of dahurian larch is used in the present invention, and for primary raw material, its raw material sources is extensive and cheap；It is prepared by material
Journey is simple to operate, and without using additional chemical reagent, the cleaning of preparation process green, energy-conservation, low consumption, is easy to industrialize；Prepared
The condensed tannin filtrate that journey obtains, it is the tannin product with high added value, adds productivity effect.
Each embodiment is described by the way of progressive in this specification, what each embodiment stressed be and other
The difference of embodiment, between each embodiment identical similar portion mutually referring to.For device disclosed in embodiment
For, because it is corresponded to the method disclosed in Example, so description is fairly simple, related part is said referring to method part
It is bright.
The foregoing description of the disclosed embodiments, professional and technical personnel in the field are enable to realize or using the present invention.
A variety of modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The most wide scope caused.
Claims (9)
1. a kind of preparation method for removing solution Nitrite ionic material, it is characterised in that it is comprised the following steps that：
(1) bark of dahurian larch is gathered, is ground into bark of dahurian larch powder, it is standby；
(2) bark of dahurian larch powder is added in deionized water, stirs, obtain mixed liquor：
(3) mixed liquor that step (2) obtains is heated in a water bath, after heating water bath, mixed liquor is filtered, obtains filtrate and filter
Slag；
(4) deionized water is added in filter residue, repeat the above steps the operation of (3), until filtrate for it is colourless when, obtained filter residue
To remove the bark of dahurian larch powder A of solution Nitrite ion.
A kind of 2. preparation method for removing solution Nitrite ionic material according to claim 1, it is characterised in that
Bark of dahurian larch described in step (1) is olga bay larch, Larix principis-rupprechtii, larix sibirica, larch-tree or Europe
One or more kinds of mixtures of continent bark of dahurian larch.
A kind of 3. preparation method for removing solution Nitrite ionic material according to claim 2, it is characterised in that
Bark of dahurian larch powder particle size range described in step (1) is 20-200 mesh.
4. a kind of preparation method of removing solution Nitrite ionic material according to claim any one of 1-3, its
It is characterised by, the feed liquid mass ratio of bark of dahurian larch powder and deionized water described in step (2) is 1:20-1:100.
5. a kind of preparation method of removing solution Nitrite ionic material according to claim any one of 1-3, its
It is characterised by, bath temperature described in step (3) is 50-70 DEG C, water bath time 5-7h.
6. a kind of preparation method of removing solution Nitrite ionic material according to claim any one of 1-3, its
It is characterised by, mixing time described in step (4) is 15-30min.
7. a kind of be used to remove the method that nitrite ion is removed in stream, it is characterised in that it is comprised the following steps that：
(1) it is water sample to be measured to take the exceeded water sample of nitrous radical ion；
(2) the bark of dahurian larch powder A described in any one of claim 1 to 6 is weighed, is fitted into chromatographic column, chromatographic column is placed in iron
On pallet；
(3) water sample and Al (OH) to be measured are measured3Suspension mixes, and stirs, and obtains mixed liquor and be mixed liquid pouring into chromatographic column
Middle filtering, obtains filtrate；Filtrate is collected, detects the content of filtrate Nitrite ion.
8. a kind of method for being used to remove removing nitrite ion material in stream according to claim 7, its feature
It is, water sample to be measured described in step (3) and Al (OH)3Suspension volume ratio is 1:50.
9. a kind of method for being used to remove removing nitrite ion material in stream according to claim 7, its feature
It is, bark of dahurian larch A quality described in step (3) and the volume ratio of mixed liquor are 4:5.
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| CN201711054385.XA CN107840431A (en) | 2017-10-31 | 2017-10-31 | A kind of preparation method and application for removing solution Nitrite ionic material |
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| CA2622814A1 (en) * | 2005-09-19 | 2007-03-29 | Terrenew, Llc | Removal of oils from solid surfaces and water with a substance having a high humate level |
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Application publication date: 20180327 |
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