CN102146101B - Method for extracting humic acid substances from methane fluid - Google Patents
Method for extracting humic acid substances from methane fluid Download PDFInfo
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- CN102146101B CN102146101B CN 201010107933 CN201010107933A CN102146101B CN 102146101 B CN102146101 B CN 102146101B CN 201010107933 CN201010107933 CN 201010107933 CN 201010107933 A CN201010107933 A CN 201010107933A CN 102146101 B CN102146101 B CN 102146101B
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- humic acid
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- natural pond
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- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 239000004021 humic acid Substances 0.000 title claims abstract description 77
- 239000000126 substance Substances 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 22
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title abstract 10
- 239000012530 fluid Substances 0.000 title abstract 5
- 238000003795 desorption Methods 0.000 claims abstract description 45
- 239000011347 resin Substances 0.000 claims abstract description 36
- 229920005989 resin Polymers 0.000 claims abstract description 36
- 239000012528 membrane Substances 0.000 claims abstract description 31
- 239000003814 drug Substances 0.000 claims abstract description 29
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 27
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000003456 ion exchange resin Substances 0.000 claims abstract description 9
- 229920003303 ion-exchange polymer Polymers 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 238000004064 recycling Methods 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims description 69
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 238000010521 absorption reaction Methods 0.000 claims description 8
- 239000003957 anion exchange resin Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 238000009287 sand filtration Methods 0.000 claims description 6
- 239000000284 extract Substances 0.000 claims description 5
- 238000009472 formulation Methods 0.000 claims description 5
- 238000002203 pretreatment Methods 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001179 sorption measurement Methods 0.000 abstract description 6
- 238000011084 recovery Methods 0.000 abstract description 5
- 238000000746 purification Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000000605 extraction Methods 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- -1 alcohol radical Chemical group 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical class OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000003077 lignite Substances 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 239000003895 organic fertilizer Substances 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000003415 peat Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 244000144977 poultry Species 0.000 description 1
- 238000011027 product recovery Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a method for extracting humic acid substances from methane fluid and belongs to the technical field of separation and purification of humic acid substances from methane fluid. In the method, by combining ion exchange resin and an ultrafiltration membrane, the humic acid substances are extracted from the methane fluid; through adsorption of resin, the humic acid substances are effectively separated from other impurities, and the purity of the humic acid substances in the products is improved; and the desorbed resin can be recovered to the initial state and recycled. Mixed solution of the humic acid substances and a desorption medicine, which is desorbed from the resin is separated through the ultrafiltration membrane, so that the purity and concentration of the humic acid substances can be further improved, the recycling level of the humic acid substances is improved, and the desorption medicine can be separated and recycled so as to reduce operating cost. The method solves the treatment problem that organic matters in the methane fluid are difficult to degrade, the humic acid substances are recycled, and the purity, concentration and recovery rate of the humic acid substances are obviously improved.
Description
Technical field
The invention belongs to liquid humic acid substance purification technique field, natural pond, particularly a kind of method of from the liquid of natural pond, extracting humic acid substance.
Background technology
Natural pond liquid is the high concentrated organic wastewater that produces in the organic waste matter anaerobic digestion process.The waste water that feces of livestock and poultry, kitchen Yu rubbish or sewage plant sludge anaerobic digestion produce and consumer waste landfill percolate etc. all belong to natural pond liquid.Natural pond liquid generally has characteristics such as organic pollutant category is many, concentration is high, the mineral ion kind is many, nutritive element is out of proportion, biodegradability is poor, intractability is big.Natural pond liquid COD generally is about more than 20,000～50, the 000mg/L, is difficult to reach emission standard after carrying out a biological disposal upon, and is difficult to more handle through the natural pond liquid after the biological treatment.Have and studies confirm that the organism major part is the humic acid substance of difficult degradation in the liquid of natural pond, their existence is the unmanageable major cause of natural pond liquid.
Humic acid substance is that a class extensively is present in natural natural polymer organism, and vegeto-animal corpse forms through long physical chemistry of the earth effect.They are mixtures that a class contains oxygen-containing functional groups such as phenyl ring, alcohol radical, hydroxyl, carboxyl, and molecular weight does not wait from the hundreds of to the hundreds of thousands of.Have that specific surface area is big, complex structure, have various active functional group, can interactional characteristics take place with many organic and inorganic things, have been widely used in fields such as industrial or agricultural, medicine, environmental protection.Humic acid substance extensively is present in weathered coal, brown coal and the peat, can stimulate plant growth, strengthens crop anti-adversity and improves product quality.
The humic acid substance degree of humification is low in the liquid of natural pond, and the aromatize degree is low than soil rotten phytic acid class material, and than water body humic acid substance height ,-COOH content belongs to the category of activated humic acid than the height of soil; Than natural humic acid class material, its C, H content is on the low side, and O, N, S content are higher; Natural pond liquid humic acid substance contains all structure of functional groups that natural humic acid class material has, and the two has similar structure forms and character, therefore can be used as the liquid fertilizer recycling or is used for aspect such as contaminated soil reparation.We can say that humic acid substance itself is the multi-functional organic fertilizer of a class, the natural pond liquid that contains humic acid substance then is the resource of untapped utilization still.Separation and Extraction humic acid substance from form complicated natural pond liquid not only can reduce the pollution load of natural pond liquid, can also reclaim valuable humic acid substance product, has namely realized the innoxious and resource utilization of natural pond liquid simultaneously.
Make the technology of efficient organic liquid fertilizer based on ultra-filtration membrane separation and Extraction humic acid substance from the liquid of natural pond and successfully researched and developed and realized the engineering application, but owing to be subjected to the restriction of membrane concentration ratio, the purity and the concentration that reclaim product are limited, it is higher to add calcium, magnesium ion and carbanion content, very easily cause film to pollute, increase resistance of membrane filtration, thereby increase film running cost.
Ion exchange resin can selective adsorption natural pond liquid in humic acid substance, the desorption medicament is introduced salinity inevitably, although and ultra-filtration membrane does not have selectivity to holding back organism, but can implement effectively separate to organism and salinity.Ion exchange resin combines with ultra-filtration membrane, both can increase the rate of recovery of humic acid substance, can improve the purity and the concentration that reclaim product again.
Summary of the invention
Problems such as the rate of recovery that exists at natural pond liquid humic acid substance separation purification is low, purity is low the invention provides a kind of method of extracting humic acid substance from the liquid of natural pond.
A kind of method of extracting humic acid substance from the liquid of natural pond is characterized in that: adopt ion exchange resin to combine with ultra-filtration membrane and extract humic acid substance from the liquid of natural pond, comprise the steps: earlier natural pond liquid to be carried out the sand filtration pre-treatment, remove suspended matter wherein; Through strongly basic anion exchange resin absorption, the feature selection absorption of strongly basic anion exchange resin makes humic acid substance separate with impurity with other organism then; The stripping liquid that recycling desorption medicament is made into from the strongly basic anion exchange resin with the humic acid substance desorption; The mixed solution that contains humic acid substance reconciliation adsorpting formulation separates through ultrafiltration membrane system again, and desorption medicament and humic acid substance are separated, and obtains the humic acid substance product, and the desorption medicament of separation is back to resin desorption unit and carries out recycle.
Described natural pond liquid carries out the sand filtration pre-treatment, behind the removal suspended matter wherein, can adjust pH less than 6.5 with hydrochloric acid or sulfuric acid, is conducive to the long-term stability operation of ultrafiltration membrane system, the pH value that also can not regulate natural pond liquid.
Described strongly basic anion exchange resin comprises 7170 resins, 201 * 4 resins, 201 * 7 resins and D201 resin.
Described stripping liquid is formulated according to mass ratio 17: 83 by desorption medicament and water.
Described desorption medicament is by NaCl, NaOH and Na
3PO
4Form, the ratio of its quality is 10: 2: 5.
The retaining molecular weight scope that described ultrafiltration membrane system adopts is 500～3500Da.
Described ultrafiltration membrane system working pressure is 0.5～1.0MPa.
Concrete treatment step of the present invention is as follows:
(1) natural pond liquid pre-treatment: natural pond liquid is filtered through sand filtration, remove suspended matter, can adjust pH less than 6.5 with hydrochloric acid or sulfuric acid, also can not regulate the pH value of natural pond liquid;
(2) liquid adsorption and desorption in natural pond is attached: pretreated natural pond liquid enters resin column, hydraulic detention time is 2 hours, in the adsorption process, macromolecular substance preferentially adsorbeds such as humic acid substance, if overstand, then all the other small-molecule substances also will be adsorbed on the resin, and (the desorption medicament is by NaCl, NaOH and Na for the stripping liquid that is made into the desorption medicament then
3PO
4Form, the ratio of its quality is 10: 2: 5, stripping liquid is formulated according to mass ratio 17: 83 by desorption medicament and water) humic acid substance on the desorption resin, stripping liquid can utilize ultra-filtration membrane to separate to obtain sees through liquid, its composition can suitably be adjusted its moiety concentration as required based on the desorption medicament;
(3) ultra-filtration membrane separates: the mixed solution that the humic acid substance that desorption obtains is conciliate adsorpting formulation utilizes ultra-filtration membrane to separate, working pressure is 0.5～1.0MPa, concentrated solution is the humic acid substance product, see through liquid based on the desorption medicament, can be back to the unit recycle of resin desorption.
Through above-mentioned technology, the humic acid substance in the liquid of natural pond is separable to extract, and has improved the biodegradability of natural pond liquid, has reduced natural pond liquid subsequent disposal difficulty, can realize simultaneously that the resource utilization of natural pond liquid is with innoxious, innoxious with the resource utilization promotion.And resin desorption medicament can recycle, and saves running cost.
Compared with prior art, method of the present invention has following beneficial effect:
1, utilizes resin absorption, humic acid substance is effectively separated with other impurity, improved the purity of humic acid substance in the product; Resin after the desorption can return to original state, reuses.
2, the humic acid substance that gets off for desorption from resin is conciliate the mixed solution of adsorpting formulation, utilize ultra-filtration membrane to separate, can further improve purity and the concentration of humic acid substance on the one hand, promote humic acid substance resource utilization level, separable and recycle the desorption medicament on the other hand, to reduce running cost.
3, the present invention takes full advantage of the stalling characteristic of resin and film, the two mutual supplement with each other's advantages, effectively combination, both solved the processing difficult problem of organism difficult degradation in the liquid of natural pond, realize the recycling of humic acid substance again, and significantly improved purity, concentration and the rate of recovery of humic acid substance product.
Description of drawings
Fig. 1 is combined from the liquid of natural pond the method flow diagram that extracts humic acid substance for ion exchange resin of the present invention with ultra-filtration membrane.
Embodiment
Below in conjunction with accompanying drawing ion exchange resin of the present invention being combined from the liquid of natural pond the method for extracting humic acid substance with ultra-filtration membrane is further described.
The present invention utilizes the adsorption selectivity of resin that natural pond liquid is separated the humic acid substance in the liquid of natural pond through resin isolation technology with impurity such as other organism, mixed solution after the desorption enters the ultra-filtration membrane unit and carries out membrane sepn, wherein humic acid substance and salinity is further separated obtain extracting.Ion exchange resin be combined with ultra-filtration membrane from the liquid of natural pond extract humic acid substance method flow diagram as shown in Figure 1, concrete steps are as follows:
Natural pond liquid is through resin absorption, and Choice of Resin absorption humic acid substance, other impurity organism etc. have obtained separating and removed.Carry out desorption then, from the resin with the humic acid substance desorption, the resin recycling is carried out natural pond liquid adsorption operations, and entering ultrafiltration membrane system with the mixed solution of desorption medicament, separates humic acid substance, concentrated solution is the humic acid substance product, see through liquid and be mainly the desorption medicament, be circulated to the desorption unit and carry out recycling.
Describe in detail with specific embodiment below.
Embodiment 1
Landfill percolate is a kind of typical natural pond liquid.Be example with certain household refuse landfill sites, its percolate generation is 100m
3/ d, after membrane bioreactor (MBR) processing, effluent COD concentration 1700mg/L, humic acid substance concentration is 1000mg/L (HS content is 59%).Present embodiment is the separation and Extraction humic acid substance from above-mentioned processing water outlet.
Choose 717 resins, adopt three grades of series systems to adsorb.Required resin total amount is 6t, and the resin column cross section is Φ 1.6m, highly is 1.6m.Natural pond liquid is filtered through sand filtration, remove suspended matter, pretreated natural pond liquid enters 717 resin columns, and the apparent hydraulic detention time of percolate is 2 hours, and (desorption medicament used herein is by NaCl, NaOH and Na for the stripping liquid that is made into the desorption medicament then
3PO
4Form, each solute and mass percent thereof are as follows in the stripping liquid: NaCl:10%, NaOH:2%, Na
3PO
4: 5%, the Yu Weishui) humic acid substance on the desorption resin, stripping liquid can utilize ultra-filtration membrane to separate to obtain sees through liquid, and its composition can suitably be adjusted its moiety concentration as required based on the desorption medicament; The mixed solution that contains humic acid substance reconciliation adsorpting formulation separates through ultrafiltration membrane system again, ultra-filtration membrane adopts molecular weight cut-off 1000Da, working pressure is 0.6MPa, cycles of concentration is 10 times, desorption medicament and humic acid substance are separated, obtain the humic acid substance product, the desorption medicament of separation is back to resin desorption unit and carries out recycle.The humic acid material rate of recovery reaches more than 80%, and purity is greater than 80%, and desorption medicament cyclic utilization rate is greater than 85%.
After resin absorption and the processing of membrane sepn combination process, organic concentration in the percolate, particularly unmanageable humic acid substance concentration reduces greatly, can reduce subsequent disposal pollution load and intractability, thereby reduces the percolate processing cost.
Present technique is insensitive to factors such as pH, temperature and ionic strengths, and adaptability is better.Resin can reuse through desorption with after recovering.Extract humic acid substance technology with independent use ultra-filtration membrane and compare, although the operation of ion exchange resin absorbing process is comparatively complicated, occupy certain advantage at aspects such as technological adaptability, product purity, product recovery rates.
Claims (5)
1. method of from the liquid of natural pond, extracting humic acid substance, it is characterized in that: adopt ion exchange resin to combine with ultra-filtration membrane and from the liquid of natural pond, extract humic acid substance, comprise the steps: earlier natural pond liquid to be carried out the sand filtration pre-treatment, remove suspended matter wherein; Through strongly basic anion exchange resin absorption, the feature selection absorption of strongly basic anion exchange resin makes humic acid substance separate with impurity with other organism then; The stripping liquid that recycling desorption medicament is made into from the strongly basic anion exchange resin with the humic acid substance desorption; The mixed solution that contains humic acid substance reconciliation adsorpting formulation separates through ultrafiltration membrane system again, and desorption medicament and humic acid substance are separated, and obtains the humic acid substance product, and the desorption medicament of separation is back to resin desorption unit and carries out recycle; Described strongly basic anion exchange resin is 7170 resins, 201 * 4 resins, 201 * 7 resins or D201 resin; Described desorption medicament is by NaCl, NaOH and Na
3PO
4Form, the ratio of its quality is 10: 2: 5.
2. a kind of method of from the liquid of natural pond, extracting humic acid substance according to claim 1, it is characterized in that: described natural pond liquid carries out the sand filtration pre-treatment, remove suspended matter wherein after, adjust pH less than 6.5 with hydrochloric acid or sulfuric acid.
3. a kind of method of extracting humic acid substance from the liquid of natural pond according to claim 1 is characterized in that: described stripping liquid is formulated according to mass ratio 17: 83 by desorption medicament and water.
4. a kind of method of extracting humic acid substance from the liquid of natural pond according to claim 1, it is characterized in that: the retaining molecular weight scope that described ultrafiltration membrane system adopts is 500～3500Da.
5. a kind of method of extracting humic acid substance from the liquid of natural pond according to claim 1, it is characterized in that: described ultrafiltration membrane system working pressure is 0.5～1.0MPa.
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| CN 201010107933 CN102146101B (en) | 2010-02-05 | 2010-02-05 | Method for extracting humic acid substances from methane fluid |
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| CN 201010107933 CN102146101B (en) | 2010-02-05 | 2010-02-05 | Method for extracting humic acid substances from methane fluid |
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| CN102951997A (en) * | 2011-08-18 | 2013-03-06 | 朱天南 | Method for simultaneously preparing bioethanol, humic acid, and fulvic acid with no pollution by using starchy biomass |
| CN102816332B (en) * | 2012-08-25 | 2017-10-20 | 福建超大集团有限公司 | A kind of feces of livestock and poultry prepares the innoxious extraction process of agricultural biochemical fulvic acid |
| WO2018072280A1 (en) * | 2016-10-21 | 2018-04-26 | 中国环境科学研究院 | Extracting device for fulvic acid dissolved in fresh water body and preparation method therefor |
| CN107935238A (en) * | 2017-11-27 | 2018-04-20 | 南京大学盐城环保技术与工程研究院 | The technique that a kind of water body purification byproduct in process humic acid recycling recycles |
| CN110386748A (en) * | 2019-08-21 | 2019-10-29 | 四川锐源能环科技有限公司 | A kind of sewage plant sludge harmless resource processing system and the method for producing humic acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503312A (en) * | 2009-03-16 | 2009-08-12 | 丁发洪 | Environment friendly biological organic biogas manure and production method thereof |
| CN101544522A (en) * | 2009-04-30 | 2009-09-30 | 山东省农业科学院土壤肥料研究所 | Fermented liquid pasty fertilizer and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503312A (en) * | 2009-03-16 | 2009-08-12 | 丁发洪 | Environment friendly biological organic biogas manure and production method thereof |
| CN101544522A (en) * | 2009-04-30 | 2009-09-30 | 山东省农业科学院土壤肥料研究所 | Fermented liquid pasty fertilizer and preparation method thereof |
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