CN116022964A - Method for extracting melanoidin from thermal hydrolysis sludge by using macroporous resin - Google Patents
Method for extracting melanoidin from thermal hydrolysis sludge by using macroporous resin Download PDFInfo
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- CN116022964A CN116022964A CN202310020928.5A CN202310020928A CN116022964A CN 116022964 A CN116022964 A CN 116022964A CN 202310020928 A CN202310020928 A CN 202310020928A CN 116022964 A CN116022964 A CN 116022964A
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- melanoidin
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- macroporous resin
- thermal hydrolysis
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- 239000010802 sludge Substances 0.000 title claims abstract description 53
- 239000011347 resin Substances 0.000 title claims abstract description 34
- 229920005989 resin Polymers 0.000 title claims abstract description 34
- 238000009283 thermal hydrolysis Methods 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000006228 supernatant Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000003480 eluent Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000002390 rotary evaporation Methods 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- 238000001179 sorption measurement Methods 0.000 claims description 19
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 8
- 230000002572 peristaltic effect Effects 0.000 claims description 6
- 239000010865 sewage Substances 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 238000004062 sedimentation Methods 0.000 claims description 4
- 230000003213 activating effect Effects 0.000 claims description 3
- 230000004913 activation Effects 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 239000002156 adsorbate Substances 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims 1
- 230000008020 evaporation Effects 0.000 claims 1
- 238000011010 flushing procedure Methods 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 20
- 230000004071 biological effect Effects 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000029087 digestion Effects 0.000 description 4
- 102000004169 proteins and genes Human genes 0.000 description 4
- 108090000623 proteins and genes Proteins 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 150000004676 glycans Chemical class 0.000 description 3
- 229920001282 polysaccharide Polymers 0.000 description 3
- 239000005017 polysaccharide Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 235000013305 food Nutrition 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 241000383638 Allium nigrum Species 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- -1 amino compound Chemical class 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000000502 dialysis Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 235000013379 molasses Nutrition 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 244000052769 pathogen Species 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
Landscapes
- Extraction Or Liquid Replacement (AREA)
- Treatment Of Sludge (AREA)
Abstract
A method for extracting melanoidin from thermal hydrolysis sludge by using macroporous resin belongs to the technical field of melanoidin extraction. The method comprises the following main steps: (1) Centrifuging and filtering the thermal hydrolysis sludge to obtain supernatant; (2) Adsorbing and desorbing the supernatant by XAD16HP macroporous resin to obtain melanoidin eluent; (3) And (3) carrying out water bath rotary evaporation concentration on the melanoidin eluent, and then drying in a freeze dryer to obtain the solid melanoidin. The invention utilizes the XAD16HP resin to extract the melanoidin from the thermal hydrolysis sludge, has the advantages of high extraction rate, strong specificity, low cost and the like, and the extracted melanoidin can be used for deep research on the aspects of basic composition, chemical structure, biological activity and the like and has important significance.
Description
Technical Field
The invention belongs to the technical field of melanoidin extraction, and particularly relates to a method for extracting melanoidin from thermal hydrolysis sludge by using macroporous resin.
Background
With population growth, economic development and rapid urbanization, environmental pollution and resource crisis become global problems. The residual sludge is used as a byproduct in the sewage treatment process, contains pollutants such as pathogens, antibiotics, heavy metals and the like, and can cause serious harm to the environment and human health. Meanwhile, the residual sludge contains a large amount of organic matters, so that the residual sludge becomes a potential renewable resource. The 'reduction, harmless and recycling' of the residual sludge is an environmental problem to be solved urgently in China and even worldwide.
Anaerobic digestion is one of the most mature sludge treatment processes at present, and can convert organic matters in the surplus sludge into methane. In order to obtain higher anaerobic digestion efficiency, the thermal hydrolysis technology is widely used for pretreatment of anaerobic digestion of sludge. However, during thermal hydrolysis of sludge, a dark brown, refractory soluble organic polymer, melanoidin, is formed. Melanoidin not only affects the anaerobic digestion effect of sludge, but also brings serious negative effects such as inhibiting biological denitrification, reducing ultraviolet disinfection efficiency and the like when the melanoidin flows back to a sewage treatment system.
Melanoidin is a high molecular polymer with complex structure generated by Maillard reaction between saccharide and amino compound (amino acid, polypeptide, protein, etc.). Currently, research into melanoidins has focused mainly on the food field and on the model maillard system. The study of the thermal hydrolysis of sludge melanoidins has remained in an early stage due to the lack of a method for extracting melanoidins from the thermal hydrolysis of sludge. The development of a method for extracting melanoidin from the thermal hydrolysis sludge has important significance for deeply researching the structure and the property of the thermal hydrolysis sludge melanoidin and regulating and controlling the adverse effect of the thermal hydrolysis sludge melanoidin.
Research reports on extraction of melanoidin from coffee, black garlic and other foods and complex substrates such as brewing wastewater, molasses wastewater and the like are long, and macroporous resin adsorption, ultrafiltration and dialysis are three methods which are commonly used. Among these methods, the macroporous resin adsorption method exhibits remarkable advantages in terms of specificity, operability, cost, and the like. Therefore, the invention provides a method for extracting melanoidin from thermal hydrolysis sludge by using macroporous resin.
Disclosure of Invention
The invention aims to provide a method for extracting melanoidin from thermal hydrolysis sludge, which adopts a macroporous resin dynamic adsorption mode and has the advantages of high extraction rate, strong specificity, low cost and the like.
The invention provides the following technical scheme:
a method for extracting melanoidin from thermal hydrolysis sludge by using macroporous resin, wherein the macroporous resin is XAD16HP macroporous resin, the thermal hydrolysis sludge is the thermal hydrolysis sludge discharged after the pre-dehydrated sludge of a town sewage treatment plant is preheated to 100 ℃ in a slurrying tank, the temperature is 160-175 ℃ and the pressure is 6-8bar in a main reactor for 30min, the temperature is reduced to 103-110 ℃ in a flash tank, and the effluent of a secondary sedimentation tank is cooled to normal temperature. The method specifically comprises the following steps:
(1) Centrifuging the thermal hydrolyzed sludge, filtering the upper solution to obtain supernatant, and adjusting the pH of the supernatant to 6.5-7.5;
(2) Activating pretreatment is carried out on the XAD16HP macroporous resin, and the macroporous resin is filled into an adsorption column for standby after activation;
(3) Adsorbing a certain amount of the supernatant fluid of the thermal hydrolysis sludge by an adsorption column at a certain flow rate at 25 ℃;
(4) Washing the adsorption column with deionized water of 2 times of column volume at 25 ℃ at a certain flow rate to remove non-adsorbates;
(5) Eluting with 5 times of 75% acidified ethanol solution at 25deg.C at a certain flow rate to obtain melanoidin eluate;
(6) And (3) carrying out water bath rotary evaporation concentration on the melanoidin eluent, and then drying in a freeze dryer to obtain the solid melanoidin.
Preferably, in the above extraction method, the activation pretreatment process is as follows: the XAD16HP macroporous resin was rinsed with deionized water to remove salts, then the resin was placed in an Erlenmeyer flask containing 75% acidified ethanol solution, shaken in a shaker at 150rpm at 25℃for 15-30 minutes, then the ethanol solution was removed using a peristaltic pump, and the macroporous resin was rinsed with deionized water until no ethanol taste was achieved.
Preferably, in the above extraction method, the amount of the supernatant of the thermal hydrolyzed sludge is 20 to 50% of the column volume.
Preferably, in the above extraction method, the flow rate of the supernatant of the thermal hydrolyzed sludge is 1 to 1.5mL/min through the adsorption column.
Preferably, in the extraction method, deionized water passes through the adsorption column at a certain flow rate of 2-4 mL/min.
Preferably, in the above extraction method, the 75% acidified ethanol solution is a 75% ethanol solution with a pH of less than 3 by volume percent acidified with hydrochloric acid.
Preferably, in the above extraction method, the flow rate of the 75% acidified ethanol solution through the adsorption column is 1 to 1.5mL/min.
Preferably, in the above extraction method, the operation of spin-steaming water bath concentration is carried out at a temperature of 70-80 ℃ for 2-3 hours.
The invention has the beneficial effects that: aiming at the blank of the extraction method of the melanoidin from the thermal hydrolysis sludge, the invention adopts XAD16HP macroporous resin as an adsorption material for the first time, and adopts dynamic adsorption to extract the melanoidin from the thermal hydrolysis sludge. Compared with other methods, the method has the advantages of high extraction rate, strong specificity, low cost and the like. The invention provides a high-efficiency and reliable extraction method for the subsequent deep research on the aspects of basic composition, chemical structure, biological activity and the like of the thermal hydrolysis sludge melanoidin.
Detailed Description
For a better understanding of the present invention, the present invention will be further described with reference to the following examples.
In the invention, the thermal hydrolysis sludge is taken from a certain sewage treatment plant in Beijing city, and is the thermal hydrolysis sludge discharged after pre-dehydrated sludge of the urban sewage treatment plant is preheated to 100 ℃ in a slurrying tank, thermally hydrolyzed in a main reactor (the temperature is 160-175 ℃, the pressure is 6-8bar, the time is 30 min), depressurized and cooled to 103-110 ℃ in a flash tank, and effluent of a secondary sedimentation tank is cooled to normal temperature.
And (3) a flash tank of the thermal hydrolysis system, and sampling after cooling and diluting by using effluent of the secondary sedimentation tank.
Example 1: the method for extracting melanoidin from the thermal hydrolysis sludge by using macroporous resin comprises the following specific steps:
(1) Obtaining a thermal hydrolysis sludge supernatant: centrifuging 50mL of the thermal hydrolysis sludge at 12000rpm and at the temperature of 4 ℃ for 5 minutes, filtering the supernatant liquid by using a 0.45 mu m polyethersulfone membrane to obtain supernatant, and regulating the pH to 7.0;
(2) Pretreatment of macroporous resin: washing XAD16HP macroporous resin with deionized water to remove salts, placing the resin in an conical flask containing 75% acidified ethanol solution (ph=2), shaking for 15 minutes at 25 ℃ in a shaker at 150rpm, removing ethanol solution with a peristaltic pump, washing the macroporous resin with deionized water until no ethanol smell is present, and drying overnight at 60 ℃ for later use;
(3) Adsorption process: loading 80g of pretreated XAD16HP macroporous resin into an adsorption column, and adsorbing 30mL of supernatant by a peristaltic pump at 25 ℃ at a flow rate of 1mL/min through the adsorption column;
(4) And (3) a desorption process: 200mL of deionized water was passed through the adsorption column at 25℃at a flow rate of 3mL/min using a peristaltic pump to remove non-adsorbed material. Subsequently, 500mL of 75% acidified ethanol solution (ph=2) was eluted through the adsorption column at 25 ℃ at a flow rate of 1mL/min with a peristaltic pump;
(5) The concentration process comprises the following steps: placing the eluent into a spherical bottle, and removing ethanol solution by rotary evaporation under the water bath condition of 80 ℃ for 3 hours to obtain melanoidin concentrate.
(6) And (3) drying: and (3) placing the melanoidin concentrated solution into a centrifuge tube, and drying in a freeze dryer for 48 hours to obtain the solid melanoidin.
Concentration of melanoidin, soluble protein and soluble polysaccharide in the supernatant of the thermal hydrolyzed sludge and the concentrated melanoidin solution of example 1 were measured, and extraction yield and purity of melanoidin were characterized, and the results are shown in the following table:
TABLE 1 concentration and extraction yield of melanoidin, soluble protein and soluble polysaccharide in the supernatant and concentrated melanoidin solution of the pyrolyzed sludge
The process of the embodiment can lead the extraction rate of the thermal hydrolysis sludge melanoidin to reach 88.0 percent, and simultaneously, the extraction rates of the protein and the polysaccharide are only 3.8 percent and 6.4 percent respectively, which indicates that the invention has high extraction efficiency and strong specificity for the thermal hydrolysis sludge melanoidin.
Claims (4)
1. A method for extracting melanoidin from thermal hydrolysis sludge by using macroporous resin is characterized in that: the thermal hydrolysis sludge is the thermal hydrolysis sludge discharged after the pre-dehydrated sludge of the urban sewage treatment plant is preheated to 100 ℃ in a slurrying tank, is thermally hydrolyzed in a main reactor, is decompressed and cooled to 103-110 ℃ in a flash tank, and is cooled to normal temperature in the effluent of a secondary sedimentation tank; the thermal hydrolysis temperature is 160-175 ℃, the pressure is 6-8bar, and the time is 30min;
the method comprises the following steps:
(1) Centrifuging the thermal hydrolyzed sludge, filtering the upper solution to obtain supernatant, and adjusting the pH of the supernatant to 6.5-7.5;
(2) Activating pretreatment is carried out on the XAD16HP macroporous resin, and the macroporous resin is filled into an adsorption column for standby after activation;
(3) Adsorbing the supernatant of the thermal hydrolyzed sludge by an adsorption column at 25 ℃ at a flow rate of 1-1.5 mL/min;
(4) Flushing the adsorption column with deionized water with 2 times of column volume at 25 ℃ at a flow rate of 2-4 mL/min to remove non-adsorbates;
(5) Eluting with 5 times of 75% acidified ethanol solution with the volume of the column at 25 ℃ at the flow rate of 1-1.5 mL/min to obtain melanoidin eluent; the 75% acidified ethanol solution is ethanol solution with the pH of less than 3 and the volume percent concentration of 75% which is acidified by hydrochloric acid;
(6) And (3) carrying out water bath rotary evaporation concentration on the melanoidin eluent, and then drying in a freeze dryer to obtain the solid melanoidin.
2. The method for extracting melanoidin from hot hydrolyzed sludge by using macroporous resin according to claim 1, wherein the activating pretreatment process in the step (2) is as follows: the XAD16HP macroporous resin is washed with deionized water to remove salts, then the resin is placed in an conical flask containing an acidified ethanol solution with a volume percent concentration of 75% and a pH of less than 3, and is shaken for 15-30 minutes at 25 ℃ in a shaker at 150rpm, then the acidified ethanol solution is removed using a peristaltic pump, and the macroporous resin is washed with deionized water until no ethanol taste.
3. The method for extracting melanoidin from hot hydrolyzed sludge by the macroporous resin according to claim 1 wherein the supernatant of the hot hydrolyzed sludge in step (3) is 20 to 50 percent of the column volume.
4. The method for extracting melanoidin from hot hydrolyzed sludge by macroporous resin according to claim 1, wherein the operation of water bath spin evaporation concentration in step (6) is carried out at 70-80 ℃ for 2-3 hours.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106746467A (en) * | 2017-01-25 | 2017-05-31 | 同济大学 | A kind of sludge resource recovery method based on digested sludge hydro-thermal process |
| CN109744540A (en) * | 2019-03-15 | 2019-05-14 | 上海交通大学云南（大理）研究院 | The extracting method of melanoidin in a kind of black garlic |
| US20210323888A1 (en) * | 2020-04-20 | 2021-10-21 | Tongji University | Method for sludge dewatering using kitchen waste to synergistically enhance anaerobic biological acidification and low-temperature thermal hydrolysis of excess sludge |
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2023
- 2023-01-06 CN CN202310020928.5A patent/CN116022964B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106746467A (en) * | 2017-01-25 | 2017-05-31 | 同济大学 | A kind of sludge resource recovery method based on digested sludge hydro-thermal process |
| CN109744540A (en) * | 2019-03-15 | 2019-05-14 | 上海交通大学云南（大理）研究院 | The extracting method of melanoidin in a kind of black garlic |
| US20210323888A1 (en) * | 2020-04-20 | 2021-10-21 | Tongji University | Method for sludge dewatering using kitchen waste to synergistically enhance anaerobic biological acidification and low-temperature thermal hydrolysis of excess sludge |
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| CN116022964B (en) | 2024-06-18 |
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