CN108530648A - A kind of extraction and purification method of sludge composting fulvic acid - Google Patents
A kind of extraction and purification method of sludge composting fulvic acid Download PDFInfo
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Abstract
The present invention relates to a kind of extraction and purification methods of sludge composting fulvic acid；The method extracted from sludge composting fulvic acid and fulvic acid is purified using 8 type macroreticular resins of XAD.Decomposed compost is air-dried into raw material of the grinding as extraction fulvic acid, first acid, alkaline extracting solution is added in sequence according to certain solid-to-liquid ratio into compost, and heating stirring is centrifugally separating to obtain fulvic acid solution.Fulvic acid solution is loaded in 8 type macroporous resin columns of XAD, then salinity remaining in column is eluted with distilled water.Use organic solvent as the fulvic acid of elution macroporous resin adsorption, fulvic acid solid matter is obtained using vacuum drying method, it is respectively 46.83%, 5.39%, 6.35%, 0.94% and 34.74% to purify fulvic acid sample organic element C, H, N, S and O content, remaining impurity is mainly Cl, Fe and Ca, and content is respectively 4.0%, 2.47% and 0.22%.
Description
Technical field
It is carried out the present invention relates to fulvic acid extraction in sludge composting and using XAD-8 types macroreticular resin to extraction fulvic acid pure
The method of change belongs to environmental protection and solid wastes recycling field.
Background technology
Fulvic acid (FA) is not only to be dissolved in acid in humus and be dissolved in the component of alkali, element form it is complex, mainly
Including the elements such as C, H, O, N and a small amount of S, P.Fulvic acid contains more polar structure, and armaticity is stronger, has higher life
Object activity, molecular structure is interior to contain a large amount of acidic functionality, including carboxyl and phenolic hydroxyl group etc..There are various benzene in fulvic acid
Ring, thick phenyl ring and heterocycle are connected to various functional groups on ring and branch, therefore with stronger ion exchange, Absorptive complex wave energy
Power can interact with metal ion, oxide and comprising the organic matter including poisonous and harmful substance, to influence these
The environmental chemical behavio4 of substance.Fulvic acid in work, agriculture, herd, cure etc. and have extensive effect.In industrial aspect, fulvic acid
The processing of harmful metal ion can be carried out to stain disease as metal ion adsorbent；Agriculturally, fulvic acid can be improved
Soil improves drought resisting, the disease resistance of crop, promotes fertilizer efficiency, promotes plant growth and improves plant quality, while to heavy metal
Contaminated land has repair.In terms of animal husbandry, fulvic acid additive can prevent livestock and poultry common disease, promote growth hair
It educates.In terms of medical treatment, fulvic acid sodium is considered to have eliminating inflammation and expelling toxin, analgesic, desensitizes, removes necrosis and promote granulation and adjust immune function,
By the basic research and clinical practice of decades, it has been applied to the treatment of a variety of diseases, and has achieved certain curative effect.
Currently, the extracting method of fulvic acid has hydrochloric acid extraction method and sodium hydroxide alkali soluble acid-precipitation method, sulfuric acid acetone method, ion
Exchanger resin method, chemical oxygen solution, electroosmose process etc..Due to containing a large amount of inorganic salts in sludge composting, such as Ca, Mg, Al, Fe
The equal impurity such as metal ions and chlorion, to obtain pure fulvic acid solid must then purify it.Macroporous absorption tree
Fat is a kind of nonionic large aperture adsorbent of the space network to grow up in 20th century, it is to utilize in fulvic acid not
It is different with adsorption capacity of the component on different resins of chemical property, and a kind of method that fulvic acid is classified, is purified.
Compared with the inorganic adsorbents such as aluminium oxide, calcium carbonate and silica gel, macroporous absorbent resin has the similar organic compound of polarity
Higher absorption and elution efficiency, and the influence to organic compound chemical structure is smaller.Macroporous absorbent resin absorption at present is rich
In sour eluent mainly have HCl, NaOH, Na4P2O7Buffer solution, NH3Water and methanol and alcohol solvent.
The acquisition resource of fulvic acid is concentrated mainly in the mineral such as peat, lignite and weathered coal at present, from these raw materials
There is the vegetation in mineral resources exhaustion and recovery process and environmental disruption in extraction fulvic acid.With wastewater treatment in China factory
Increase, sludge yield is also continuously increased therewith.And at present China Treatment of Sludge mostly use landfill greatly, throw sea and burn etc. it is traditional
Mode, these modes are although simple and convenient, but the problems such as land occupation, marine environmental pollution and atmosphere pollution can be brought.It adopts
It is to utilize municipal sewage plant excess sludge with the present invention, using aerobic compost, after microbiological treatment there is pollution in sludge
Machine object is converted into stable humus.It is found by the early-stage study analysis of this seminar, the fulvic acid content in sludge composting
Much larger than the content of fulvic acid in coal class mineral.The present invention is to be taken using acid, alkali carries for the fulvic acid in sludge composting
Afterwards, the inorganic salt impurities in extracting solution are purified using macroreticular resin, the fulvic acid solution purified obtains after drying
Pure fulvic acid solid.The invention thinking not only can be to avoid the problem of fulvic acid mineral resources exhaustion, moreover it is possible to solve city
Belong to sludge difficulty disposal difficulties, while avoiding the Heavy Metal Ecological pollution risk that sludge composting directly uses, realizes sludge
Turn waste into wealth the purpose of (pure fulvic acid solid).
Invention content
The object of the present invention is to provide a kind of methods of the extraction and purification of sludge composting fulvic acid, can be municipal sludge
High efficient resourcing processing provides the choice of technology.
Technical scheme is as follows：
A kind of extraction and purification method of sludge composting fulvic acid, includes the following steps：
1) decomposed fertile sample, is air-dried into grinding, the aqueous hydrochloric acid solution of 1~4M is added in fertile sample, is heated using electric furnace
To boiling, 1~3h is stirred, is then centrifuged, supernatant contains fulvic acid substance；
2) alkali extract, is added into the solid after centrifugation, with heating water bath to stirring 1h at 80~100 DEG C~
3h is then centrifuged, and supernatant uses 1M HCl/water solution to be acidified to pH as 2, and stands 2h, then centrifuges again,
Contain fulvic acid substance in its supernatant；
3), by step 1) and 2), the supernatant containing fulvic acid mixes, and then is adjusted to be 7 by pH with the molten aqueous of NaOH, quiet
2h is set, is then centrifuged for isolating sediment, the feed liquid that supernatant is purified as XAD-8 type macroreticular resins；
4), the feed liquid that step 3) obtains peristaltic pump is fitted into XAD-8 type macroporous resin columns, 1h is stood after installing column；
Then, the inorganic salinity in column is eluted with distilled water, until inspection does not measure chlorion in efflux；
5), the fulvic acid of macroporous absorbent resin absorption is eluted as eluant, eluent using the mixed solvent of formic acid and ethyl alcohol
Get off, and collects in a reservoir；
6) eluent, is subjected to vacuum evaporation drying, the fulvic acid solid sample purified.
The solid-to-liquid ratio 1 of the aqueous hydrochloric acid solution of 1~4M is added in the step 1) into fertile sample:5~20g/mL.
The solid-to-liquid ratio 1 of alkali extract is added in the step 2) to the solid after centrifugation:10~20g/mL.
Alkali extract is the NaOH and NH of 0.5~2M in the step 2)4HCO3It is 4 according to volume ratio:1 is mixed molten
Liquid.
The mixed solvent volume ratio of the step 5) formic acid and ethyl alcohol is 4：1~1：4.
The side that the present invention is extracted from sludge composting fulvic acid and purified to fulvic acid using XAD-8 types macroreticular resin
Method.Raw material by the air-dried grinding of decomposed compost as extraction fulvic acid, into compost, according to certain solid-to-liquid ratio, first sequence adds
Enter acid, alkaline extracting solution, heating stirring is centrifugally separating to obtain fulvic acid solution.It is big that fulvic acid solution is loaded to XAD-8 types
On the resin column of hole, then salinity remaining in column is eluted with distilled water.Finally use organic solvent as elution
The fulvic acid of macroporous resin adsorption, finally uses vacuum drying method to obtain fulvic acid solid matter, and content of organics is more than
93%.The present invention obtains a kind of sour sludge composting fulvic acid, alkali extracting method and XAD-8 types macroreticular resin to purifying fulvic acid
Method.
Description of the drawings
Fig. 1：Purify fulvic acid solid powder x-ray diffraction pattern；
Fig. 2：Purify fulvic acid solid infrared spectrogram；
Fig. 3：Purify fulvic acid solid thermogravimetric-differential scanning amount thermal map.
Specific implementation mode
The present invention is described in further detail with reference to the accompanying drawings and detailed description：
Using following optimal technical scheme：
1) it is ground after, air-drying decomposed fertile sample, fertile sample is put into container, then according to solid-to-liquid ratio 1:5~20 (g/ml)
The aqueous hydrochloric acid solution of 1~4M is added, then is heated to boiling using electric furnace, boil 1~3h of lower stirring, is then centrifuged
Separation, supernatant contain fulvic acid substance；
2), into the solid after centrifugation according to solid-to-liquid ratio 1:It is 4 that volume ratio, which is added, in 10~20 (g/ml):The 0.5 of 1~
2M NaOH and NH4HCO3Alkali extract is mixed, with heating water bath to 80~100 DEG C, 1h~3h is stirred, then centrifuges, supernatant
Liquid uses 1M HCl/water solution to be acidified to pH as 2, and stands 2h, then centrifuges again, fulvic acid is contained in supernatant
Substance；
3), by step 1) and 2), the supernatant containing fulvic acid mixes, and then is adjusted to be 7 by pH with the molten aqueous of NaOH, quiet
2h is set, is then centrifuged for isolating sediment, the feed liquid that supernatant is purified as XAD-8 type macroreticular resins；
4), the feed liquid that step 3) obtains peristaltic pump is fitted into XAD-8 type macroporous resin columns, 1h is stood after installing column；
Then, the inorganic salinity in column is eluted with distilled water, until inspection does not measure chlorion in efflux；
5), the fulvic acid of macroporous absorbent resin absorption is eluted as eluant, eluent using the mixed solvent of formic acid and ethyl alcohol
Get off, and collects in a reservoir；
6) eluent, is subjected to vacuum evaporation drying, the fulvic acid solid sample purified.
Embodiment 1.
1) it is ground after, air-drying decomposed fertile sample, fertile sample is put into container, then according to solid-to-liquid ratio 1:5 (g/ml) are added
The aqueous hydrochloric acid solution of 1M then is heated to boiling using electric furnace, and boil lower stirring 1h, is then centrifuged, supernatant
Liquid contains fulvic acid substance；
2), into the solid after centrifugation according to solid-to-liquid ratio 1:It is 4 that volume ratio, which is added, in 10 (g/ml):1 0.5M NaOH
Alkali extract is mixed with 0.5M NH4HCO3, with heating water bath to 80 DEG C, 1h is stirred, then centrifuges, supernatant uses 1M
It is 2 that HCl/water solution, which is acidified to pH, and stands 2h, is then centrifuged again, and fulvic acid substance is contained in supernatant；
3), by step 1) and 2), the supernatant containing fulvic acid mixes, and then is adjusted to be 7 by pH with the molten aqueous of NaOH, quiet
2h is set, is then centrifuged for isolating sediment, the feed liquid that supernatant is purified as XAD-8 type macroreticular resins；
4), the feed liquid that step 3) obtains peristaltic pump is fitted into XAD-8 type macroporous resin columns, 1h is stood after installing column；
Then, the inorganic salinity in column is eluted with distilled water, until inspection does not measure chlorion in efflux；
5), use volume ratio for 4:1 formic acid and the mixed solvent of ethyl alcohol adsorb macroporous absorbent resin as eluant, eluent
Fulvic acid elute, and collect in a reservoir；
6) eluent, is subjected to vacuum evaporation drying, the fulvic acid solid sample purified.
It is 2.0% that fulvic acid solid product yield is purified after above-mentioned processing.Purifying fulvic acid sample organic element C,
H, N, S and O content are respectively 46.83%, 5.39%, 6.35%, 0.94% and 34.74%, remaining impurity be mainly Cl, Fe and
Ca, content are respectively 4.0%, 2.47% and 0.22%.X-ray diffractogram (XRD) such as Fig. 1 for purifying fulvic acid solid, only 2
θ is that there are a larger steamed bun peaks, the fulvic acid sample of purifying to belong to unformed solid at 10-30 °.Purify fulvic acid sample
Infrared spectrum (FTIR) as shown in Fig. 2, there are carboxyl, hydroxyl and fat and aromatic structures.Purify thermogravimetric-differential of fulvic acid
Scanning amount thermal map (TG-DSC) has certain thermal stability as shown in figure 3, the initial temperature that sample decomposes is about 260 DEG C.
Embodiment 2.
1) it is ground after, air-drying decomposed fertile sample, fertile sample is put into container, then according to solid-to-liquid ratio 1:10 (g/ml) are added
The aqueous hydrochloric acid solution of 2M then is heated to boiling using electric furnace, and boil lower stirring 2h, is then centrifuged, supernatant
Liquid contains fulvic acid substance；
2), into the solid after centrifugation according to solid-to-liquid ratio 1:It is 4 that volume ratio, which is added, in 15 (g/ml):1 1MNaOH and
1M NH4HCO3 mix alkali extract, with heating water bath to 90 DEG C, stir 2h, then centrifuge, supernatant uses 1M HCl/waters
It is 2 that solution, which is acidified to pH, and stands 2h, is then centrifuged again, and fulvic acid substance is contained in supernatant；
3), by step 1) and 2), the supernatant containing fulvic acid mixes, and then is adjusted to be 7 by pH with the molten aqueous of NaOH, quiet
2h is set, is then centrifuged for isolating sediment, the feed liquid that supernatant is purified as XAD-8 type macroreticular resins；
4), the feed liquid that step 3) obtains peristaltic pump is fitted into XAD-8 type macroporous resin columns, 1h is stood after installing column；
Then, the inorganic salinity in column is eluted with distilled water, until inspection does not measure chlorion in efflux；
5), use volume ratio for 1:1 formic acid and the mixed solvent of ethyl alcohol adsorb macroporous absorbent resin as eluant, eluent
Fulvic acid elute, and collect in a reservoir；
6) eluent, is subjected to vacuum evaporation drying, the fulvic acid solid sample purified.
It is 2.4% that fulvic acid solid product yield is purified after above-mentioned processing.Pass through elemental analysis and x-ray fluorescence point
Analysis is it is found that purifying fulvic acid sample organic element C, H, N, S and O content are respectively 46.83%, 5.39%, 6.35%, 0.94%
With 34.74%, remaining impurity is mainly Cl, Fe and Ca, and content is respectively 4.0%, 2.47% and 0.22%.It is solid to purify fulvic acid
The X-ray diffractogram (XRD) of body such as Fig. 1 is only that there are a larger steamed bun peak, the fulvic acid samples of purifying at 10-30 ° in 2 θ
Product belong to unformed solid.The infrared spectrum (FTIR) of fulvic acid sample is purified as shown in Fig. 2, there are carboxyl, hydroxyl and fat
And aromatic structure.Thermogravimetric-differential scanning amount thermal map (TG-DSC) of fulvic acid is purified as shown in figure 3, the starting temperature that sample decomposes
About 260 DEG C of degree, has certain thermal stability.
Embodiment 3.
1) it is ground after, air-drying decomposed fertile sample, fertile sample is put into container, then according to solid-to-liquid ratio 1:20 (g/ml) are added
The aqueous hydrochloric acid solution of 4M then is heated to boiling using electric furnace, and boil lower stirring 3h, is then centrifuged, supernatant
Liquid contains fulvic acid substance；
2), into the solid after centrifugation according to solid-to-liquid ratio 1:It is 4 that volume ratio, which is added, in 20 (g/ml):1 2M NaOH and
2M NH4HCO3 mix alkali extract, with heating water bath to 100 DEG C, stir 3h, then centrifuge, supernatant uses 1M HCl/waters
It is 2 that solution, which is acidified to pH, and stands 2h, is then centrifuged again, and fulvic acid substance is contained in supernatant；
3), by step 1) and 2), the supernatant containing fulvic acid mixes, and then is adjusted to be 7 by pH with the molten aqueous of NaOH, quiet
2h is set, is then centrifuged for isolating sediment, the feed liquid that supernatant is purified as XAD-8 type macroreticular resins；
4), the feed liquid that step 3) obtains peristaltic pump is fitted into XAD-8 type macroporous resin columns, 1h is stood after installing column；
Then, the inorganic salinity in column is eluted with distilled water, until inspection does not measure chlorion in efflux；
5), use volume ratio for 4:1 formic acid and the mixed solvent of ethyl alcohol adsorb macroporous absorbent resin as eluant, eluent
Fulvic acid elute, and collect in a reservoir；
6) eluent, is subjected to vacuum evaporation drying, the fulvic acid solid sample purified.
It is 2.7% that fulvic acid solid product yield is purified after above-mentioned processing.Pass through elemental analysis and x-ray fluorescence point
Analysis is it is found that purifying fulvic acid sample organic element C, H, N, S and O content are respectively 46.83%, 5.39%, 6.35%, 0.94%
With 34.74%, remaining impurity is mainly Cl, Fe and Ca, and content is respectively 4.0%, 2.47% and 0.22%.It is solid to purify fulvic acid
The X-ray diffractogram (XRD) of body such as Fig. 1 is only that there are a larger steamed bun peak, the fulvic acid samples of purifying at 10-30 ° in 2 θ
Product belong to unformed solid.The infrared spectrum (FTIR) of fulvic acid sample is purified as shown in Fig. 2, there are carboxyl, hydroxyl and fat
And aromatic structure.Thermogravimetric-differential scanning amount thermal map (TG-DSC) of fulvic acid is purified as shown in figure 3, the starting temperature that sample decomposes
About 260 DEG C of degree, has certain thermal stability.
The method that the present invention disclosed and proposed the extraction and purifying resin of the fulvic acid in sludge composting.People in the art
Member can be by using for reference present disclosure, and the appropriate extracting method for changing fulvic acid or the composition for the treatment of conditions and resin eluent are
It can be achieved.In particular, it should be pointed out that all similar replacements and change are apparent for a person skilled in the art
, they are considered as being included in spirit of that invention, range and content.
Claims (5)
1. a kind of extraction and purification method of sludge composting fulvic acid, it is characterized in that including the following steps：
1) decomposed fertile sample, is air-dried into grinding, the aqueous hydrochloric acid solution of 1~4M is added in fertile sample, is heated to boiling using electric furnace
It rises, stirs 1~3h, be then centrifuged, supernatant contains fulvic acid substance；
2) alkali extract, is added into the solid after centrifugation, with heating water bath to stirring 1h~3h at 80~100 DEG C, with
After centrifuge, supernatant uses 1M HCl/water solution to be acidified to pH as 2, and stands 2h, then centrifuges again, supernatant
Contain fulvic acid substance in liquid；
3), by step 1) and 2), the supernatant containing fulvic acid mixes, and then is adjusted to be 7 by pH with the molten aqueous of NaOH, stands 2h,
It is then centrifuged for isolating sediment, the feed liquid that supernatant is purified as XAD-8 type macroreticular resins；
4), the feed liquid that step 3) obtains peristaltic pump is fitted into XAD-8 type macroporous resin columns, 1h is stood after installing column；Then,
The inorganic salinity in column is eluted with distilled water, until inspection does not measure chlorion in efflux；
5), the fulvic acid that macroporous absorbent resin adsorbs is eluted as eluant, eluent using the mixed solvent of formic acid and ethyl alcohol,
And it collects in a reservoir；
6) eluent, is subjected to vacuum evaporation drying, the fulvic acid solid sample purified.
2. the method as described in claim 1, it is characterized in that the aqueous hydrochloric acid solution of 1~4M is added in the step 1) into fertile sample
Solid-to-liquid ratio 1:5~20g/mL.
3. the method as described in claim 1, it is characterized in that alkali density is added to the solid after centrifugation in the step 2)
The solid-to-liquid ratio 1 of liquid:10~20g/mL.
4. the method as described in claim 1, it is characterized in that alkali extract is 0.5~2M in the step 2) NaOH and
NH4HCO3It is 4 according to volume ratio:1 mixed solution.
5. the method as described in claim 1, it is characterized in that the mixed solvent volume ratio of the step 5) formic acid and ethyl alcohol is 4：1
~1：4.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112504746A (en) * | 2020-12-24 | 2021-03-16 | 山东微谱检测技术有限公司 | Water sample extraction method |
| CN113075345A (en) * | 2021-03-31 | 2021-07-06 | 浙江省农业科学院 | Method for analyzing and determining whether aerobic high-temperature compost is decomposed stably by adopting high performance liquid chromatography |
| CN115058022A (en) * | 2022-04-07 | 2022-09-16 | 天津大学 | Method for separating and extracting fulvic acid from surface water and/or soil |
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| CN105203374A (en) * | 2015-09-16 | 2015-12-30 | 中国环境科学研究院 | Method for extracting small-molecule humic acid from soil through XAD resin |
| CN106220863A (en) * | 2016-08-30 | 2016-12-14 | 中国环境科学研究院 | A kind of mud and the grading purification method of humic acid subfraction in straw hybrid composting |
| CN106349486A (en) * | 2016-08-30 | 2017-01-25 | 中国环境科学研究院 | Sequential extraction method of fulvic acid XAD resin in sludge and straw mixing compost |
| CN107177039A (en) * | 2017-06-12 | 2017-09-19 | 贵州民族大学 | Extraction, purifying and the stage division of humus in a kind of deposit |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105203374A (en) * | 2015-09-16 | 2015-12-30 | 中国环境科学研究院 | Method for extracting small-molecule humic acid from soil through XAD resin |
| CN106220863A (en) * | 2016-08-30 | 2016-12-14 | 中国环境科学研究院 | A kind of mud and the grading purification method of humic acid subfraction in straw hybrid composting |
| CN106349486A (en) * | 2016-08-30 | 2017-01-25 | 中国环境科学研究院 | Sequential extraction method of fulvic acid XAD resin in sludge and straw mixing compost |
| CN107177039A (en) * | 2017-06-12 | 2017-09-19 | 贵州民族大学 | Extraction, purifying and the stage division of humus in a kind of deposit |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112504746A (en) * | 2020-12-24 | 2021-03-16 | 山东微谱检测技术有限公司 | Water sample extraction method |
| CN113075345A (en) * | 2021-03-31 | 2021-07-06 | 浙江省农业科学院 | Method for analyzing and determining whether aerobic high-temperature compost is decomposed stably by adopting high performance liquid chromatography |
| CN113075345B (en) * | 2021-03-31 | 2022-06-24 | 浙江省农业科学院 | Method for analyzing and determining whether aerobic high-temperature compost is decomposed stably |
| CN115058022A (en) * | 2022-04-07 | 2022-09-16 | 天津大学 | Method for separating and extracting fulvic acid from surface water and/or soil |
| CN115058022B (en) * | 2022-04-07 | 2023-03-21 | 天津大学 | Method for separating and extracting fulvic acid from surface water and/or soil |
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Application publication date: 20180914 |