CN104857072A - Method for recycling walnut polyphenol and flavone in walnut kernel peeling wastewater through macroporous resin - Google Patents
Method for recycling walnut polyphenol and flavone in walnut kernel peeling wastewater through macroporous resin Download PDFInfo
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- CN104857072A CN104857072A CN201510208587.XA CN201510208587A CN104857072A CN 104857072 A CN104857072 A CN 104857072A CN 201510208587 A CN201510208587 A CN 201510208587A CN 104857072 A CN104857072 A CN 104857072A
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- semen juglandis
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- 239000011347 resin Substances 0.000 title claims abstract description 77
- 229920005989 resin Polymers 0.000 title claims abstract description 77
- 229930003944 flavone Natural products 0.000 title claims abstract description 57
- 235000011949 flavones Nutrition 0.000 title claims abstract description 57
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 title claims abstract description 52
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 title claims abstract description 49
- 150000002212 flavone derivatives Chemical class 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 28
- 241000758789 Juglans Species 0.000 title abstract description 16
- 235000009496 Juglans regia Nutrition 0.000 title abstract description 16
- 235000020234 walnut Nutrition 0.000 title abstract description 16
- 239000002351 wastewater Substances 0.000 title abstract description 9
- 235000013824 polyphenols Nutrition 0.000 title abstract description 8
- 150000008442 polyphenolic compounds Chemical class 0.000 title abstract description 7
- 238000004064 recycling Methods 0.000 title abstract 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 98
- 239000000243 solution Substances 0.000 claims abstract description 48
- 238000001179 sorption measurement Methods 0.000 claims abstract description 14
- 238000010790 dilution Methods 0.000 claims abstract description 9
- 239000012895 dilution Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 4
- 210000000582 semen Anatomy 0.000 claims description 87
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 56
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 52
- 239000007788 liquid Substances 0.000 claims description 39
- 239000012153 distilled water Substances 0.000 claims description 32
- 230000007935 neutral effect Effects 0.000 claims description 30
- 239000002699 waste material Substances 0.000 claims description 20
- 238000010521 absorption reaction Methods 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 8
- 230000008961 swelling Effects 0.000 claims description 8
- 238000011084 recovery Methods 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 2
- 229930003935 flavonoid Natural products 0.000 claims description 2
- 150000002215 flavonoids Chemical class 0.000 claims description 2
- 235000017173 flavonoids Nutrition 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 230000008929 regeneration Effects 0.000 abstract description 14
- 238000011069 regeneration method Methods 0.000 abstract description 14
- 230000008901 benefit Effects 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- -1 flavone compounds Chemical class 0.000 abstract description 2
- 235000019441 ethanol Nutrition 0.000 abstract 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract 2
- 238000003795 desorption Methods 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 238000007738 vacuum evaporation Methods 0.000 abstract 1
- 150000002213 flavones Chemical class 0.000 description 8
- 230000004044 response Effects 0.000 description 8
- 238000010828 elution Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 239000006228 supernatant Substances 0.000 description 6
- 235000013305 food Nutrition 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000006870 function Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 235000020261 walnut milk Nutrition 0.000 description 3
- REFJWTPEDVJJIY-UHFFFAOYSA-N Quercetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 description 2
- 230000001093 anti-cancer Effects 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003405 preventing effect Effects 0.000 description 2
- 230000004223 radioprotective effect Effects 0.000 description 2
- 230000001172 regenerating effect Effects 0.000 description 2
- PFTAWBLQPZVEMU-DZGCQCFKSA-N (+)-catechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-DZGCQCFKSA-N 0.000 description 1
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 description 1
- AFSDNFLWKVMVRB-UHFFFAOYSA-N Ellagic acid Chemical compound OC1=C(O)C(OC2=O)=C3C4=C2C=C(O)C(O)=C4OC(=O)C3=C1 AFSDNFLWKVMVRB-UHFFFAOYSA-N 0.000 description 1
- ATJXMQHAMYVHRX-CPCISQLKSA-N Ellagic acid Natural products OC1=C(O)[C@H]2OC(=O)c3cc(O)c(O)c4OC(=O)C(=C1)[C@H]2c34 ATJXMQHAMYVHRX-CPCISQLKSA-N 0.000 description 1
- 229920002079 Ellagic acid Polymers 0.000 description 1
- 241000191398 Kalanchoe blossfeldiana Species 0.000 description 1
- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 description 1
- HWTZYBCRDDUBJY-UHFFFAOYSA-N Rhynchosin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=CC(O)=C(O)C=C2O1 HWTZYBCRDDUBJY-UHFFFAOYSA-N 0.000 description 1
- 235000019498 Walnut oil Nutrition 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 description 1
- 235000005487 catechin Nutrition 0.000 description 1
- 229950001002 cianidanol Drugs 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229960002852 ellagic acid Drugs 0.000 description 1
- 235000004132 ellagic acid Nutrition 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 230000006386 memory function Effects 0.000 description 1
- FAARLWTXUUQFSN-UHFFFAOYSA-N methylellagic acid Natural products O1C(=O)C2=CC(O)=C(O)C3=C2C2=C1C(OC)=C(O)C=C2C(=O)O3 FAARLWTXUUQFSN-UHFFFAOYSA-N 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 235000005875 quercetin Nutrition 0.000 description 1
- 229960001285 quercetin Drugs 0.000 description 1
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 description 1
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 description 1
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 description 1
- 235000005493 rutin Nutrition 0.000 description 1
- 229960004555 rutoside Drugs 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 230000001228 trophic effect Effects 0.000 description 1
- 239000008170 walnut oil Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Water Treatment By Sorption (AREA)
- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a method for recycling walnut polyphenol and flavone in walnut kernel peeling wastewater through macroporous resin. The method comprises the operating steps of pretreatment of the walnut kernel peeling wastewater, separation, purification and regeneration of the macroporous adsorption resin, concentration and drying. The concentration of the walnut flavone in the pretreated walnut kernel peeling wastewater is reduced to 0.34mg/mL-0.67mg/mL through dilution, the pH value is adjusted to be 7-9 through concentrated hydrochloric acid, a solution is poured into an adsorption tank filled with the macroporous resin to be adsorbed, the adsorption time is more than 4 hours, after adsorption is finished, desorption is conducted through 60%-80% ethyl alcohol to obtain an ethyl alcohol walnut flavone solution, the solution is processed through vacuum evaporation, concentration and drying, the ethyl alcohol is recycled, and finally fine walnut flavone extract is obtained. The recycling rate of the walnut flavone is more than 70%, and the purity of the walnut flavone is more than 50%. The technological process is simple, the cost is low, the benefit is high, the macroporous resin can be regenerated and recycled, and the method is suitable for industrial recycling of walnut flavone compounds in the walnut kernel peeling wastewater.
Description
Technical field
The present invention relates to a kind of method of removing Semen Juglandis flavone in clothing waste liquid with macroporous resin recovery Semen Juglandis, belong to the intensive processing field of food byproducts, be specially comprehensive utilization Semen Juglandis and go clothing liquid resource, extract the processing method of Semen Juglandis flavone.
Background technology
Polyphenol chromocor compound (the Shi Dandan such as rutin, ellagic acid, rhodioside, Kalanchoe blossfeldiana glycosides, Quercetin, catechin are had in Semen Juglandis clothing, Deng. food industry science and technology, 2014,2:375), it is the Natural antioxidant that a class has very strong anti-oxidative activity, comprise scavenging free radicals, angiocardiopathy preventing, anti-cancer, radioprotective, delay the functions such as body aging, there is high healthy nutritive value.
Along with the fast development of food industry; walnut product is constantly weeded out the old and bring forth the new; wherein Walnut Milk and walnut oil are particularly outstanding; Semen Juglandis is rich in Semen Juglandis polyphenols, and mainly concentrates on Semen Juglandis seed coat or Semen Juglandis clothing, but in the Walnut Milk course of processing; because Semen Juglandis endotesta content of tannin is higher; often can affect mouthfeel and the color and luster of walnut product, therefore, need to be removed.At present, domestic Semen Juglandis processing enterprise is most widely used is lye dipping method, and what this was larger have impact on Semen Juglandis trophic function composition, has become the bottleneck of Walnut Industryization development.Semen Juglandis is through soaking and removing clothing, and its polyphenol and flavones content decline 81.7% and 72.2% respectively.In addition, the waste water COD that lye dipping produces is about 20000mg/L, substantially exceed national B-grade sewage discharge standard, enterprise often produces one ton of Walnut Milk, several tons of waste water will be produced, the discharge that waste water is a large amount of, can cause the environmental pollutions such as neighbouring field, water quality again, bring immense pressure to the survival and development of enterprise.
Macroporous resin is organic high molecular polymer, in use can be aging because of the Irreversible Adsorption of some composition, and after using some cycles, its absorbability declines, and needs regeneration to recover its absorption property.And still lack at present method and the whether satisfactory index of correlation of regenerating resin of research and the regeneration technology that resin regeneration is utilized.
Current Semen Juglandis removes clothing liquid mainly as direct discharging of waste water, and this causes a large amount of losses of the effective ingredient such as Semen Juglandis flavone.In addition, the extraction of bibliographical information Semen Juglandis flavone is generally that after macroporous resin, the method such as membrane filtration or ion exchange obtains purified first by organic solvent extraction.These processes are loaded down with trivial details, complicated operation, and cost is high.In order to realize, processing step is few, route simple, consume low, that efficiency is high object, and the present invention is foothold from raising Business Economic Benefit, studies a kind of technique removing to reclaim clothing liquid Semen Juglandis flavone from Semen Juglandis.
Summary of the invention
Object of the present invention reclaims with macroporous resin the method that Semen Juglandis removes Semen Juglandis flavone in clothing liquid for providing a kind of, and the method comprises the following steps:
(1) getting Semen Juglandis goes clothing waste liquid centrifugal under rotating speed is 3000-5000 rpm condition, removing float and solid;
(2) pretreatment macroporous resin: macroporous resin is fully rinsed with distilled water, effluent in till white opacity, is not the soak with ethanol 12h of 95% with mass percent concentration, makes it fully swelling, then with distilled water cleaning to without alcohol; Soak 6h by the NaOH solution that mass percent concentration is 5%, be then washed till pH close to neutral with distilled water; With the HCl solution soaking 6h that mass percent concentration is 5%, be then washed till pH close to neutral and macroporous resin that is that obtain with distilled water;
(3) will Semen Juglandis flavone concentration dilution in clothing waste liquid be gone to 0.34-0.67mg/mL after centrifugal, and regulate pH value of solution to be 7-9;
(4) pour step (3) solution into adsorption tanks that macroporous resin is housed to adsorb, more than adsorption time 4h;
(5) after absorption terminates, carry out desorbing with the ethanol that mass percent concentration is 60-80%, obtain ethanol Semen Juglandis flavonoids solution, by solution for vacuum evaporating, concentrating and drying, reclaim ethanol, finally obtain Semen Juglandis flavone extract; The response rate of Semen Juglandis flavone reaches more than 70%, and purity is more than 50%;
(6) with water, drip washing is carried out to the macroporous resin after desorbing, the object of resin simple regeneration can be reached;
(7) when adsorbance decline more than 30%, cross resin column with HCl solution, and be washed till close to neutral with pure water, then cross resin column by NaOH solution, then pure water is washed till close to neutral, finally washes post with ethanol, and wash away ethanol with pure water, resin is strengthened regeneration.
The model of the macroporous resin in step (2) is AB-8 or NAK-9.
In step (6), the consumption of water is 5-6 column volume (BV).
In step (7), the consumption of HC1 is 3-4BV, and mass percent concentration is 2-3%; The consumption of NaOH is 3-4BV, and mass percent concentration is 4-5%; Ethanol consumption is 2-3BV, and mass percent concentration is 90-95%, and the regeneration rate of resin is between 87.45%-96.51%.
The advantage that the present invention has:
(1) the present invention goes the Semen Juglandis polyphenol chromocor in clothing liquid to carry out recovery process research to Semen Juglandis, and the chemical regulator of use is harmless object, can be widely used in food industrialization and produce; Operating process is simple and convenient, and the salvage material (macroporous resin, ethanol) of use is recyclable material, and economy is environmental protection again.The response rate of products therefrom Semen Juglandis flavone reaches more than 80%, and purity reaches more than 60%;
(2) the Semen Juglandis flavones content of the present invention's acquisition is higher, and processing step is few, route is simple, it is low to consume, efficiency is high, and production cost reduces greatly.Therefore, the inventive method is utilized can to realize the recovery of Semen Juglandis polyphenol chromocor of high efficiency, high-load, low cost.This recovery method step is simple and reliable, and efficiency is high, technique is simple, workable, pollution-free, is easy to realize industrialization large-scale production.Therefore there is good economic benefit, society and ecological significance.
(3) the present invention is studied the regeneration of macroporous resin and technique, for the related request index setting up regenerating resin provides theoretical foundation.
(4) the present invention is to Semen Juglandis process to a certain degree of having gone clothing liquid to carry out, and reclaims Semen Juglandis flavone wherein simultaneously, is significant to resources and environment.
(5) the present invention obtains Semen Juglandis flavone to be had antioxidation, angiocardiopathy preventing, anti-cancer, radioprotective, delays the functions such as body aging, enhancing and Improving memory function, is a kind of desirable nourishing healthy medicine.
Detailed description of the invention
Below by specific embodiment, technical solution of the present invention is elaborated further, but protection scope of the present invention is not limited to this.
Embodiment 1: reclaim with macroporous resin the method that Semen Juglandis removes Semen Juglandis flavone in clothing waste liquid, carry out as follows:
(1) get Semen Juglandis and remove clothing liquid 500 mL, 3000 rpm are in batches centrifugal, get supernatant, mixing, measure flavones content;
(2) AB-8 type macroporous resin pretreatment
Fully rinsed by resin with distilled water, effluent in till white opacity, is not the soak with ethanol 12h of 95% with mass percent concentration, makes it fully swelling, then with distilled water cleaning to without alcohol taste; With 5%NaOH solution soaking 6h, be then washed till pH close to neutral with distilled water; Soak 6h with 5% Solution H Cl, be then washed till pH close to neutral with distilled water;
(3) will Semen Juglandis flavone concentration dilution in clothing waste liquid be gone to 0.34mg/mL after centrifugal, and regulate pH value of solution to be 7;
(4) upper prop, adsorption time is 4h, after absorption terminates, with mass percent concentration be 60% ethanol desorbing is carried out to resin column, collect ethanol elution, concentrated and dry, obtain Semen Juglandis and remove clothing liquid Semen Juglandis flavone, the response rate of Semen Juglandis flavone is 80.24%, and purity is 53.82%;
(5) cross resin column with 3BV 3% HCl solution, and be washed till close to neutral with pure water, then cross resin column by 3BV 5% NaOH solution, and pure water is washed till close to neutral, wash post with 2BV 95% ethanol again, and wash away ethanol with pure water, the regeneration rate of resin is 87.45%.
Embodiment 2: reclaim with macroporous resin the method that Semen Juglandis removes Semen Juglandis flavone in clothing waste liquid, carry out as follows:
(1) get Semen Juglandis and remove clothing liquid 500 mL, 4000 rpm are in batches centrifugal, get supernatant, mixing, measure flavones content;
(2) AB-8 type macroporous resin pretreatment
Fully being rinsed by resin with distilled water, is the soak with ethanol 12h of 95% with mass percent concentration, makes it fully swelling, then with distilled water cleaning to without alcohol taste; With 5%NaOH solution soaking 6h, be then washed till pH close to neutral with distilled water; Soak 6h with 5% Solution H Cl, be then washed till pH close to neutral with distilled water;
(3) will Semen Juglandis flavone concentration dilution in clothing waste liquid be gone to 0.5mg/mL after centrifugal, and regulate pH value of solution to be 8;
(4) upper prop, adsorption time is 5h, after absorption terminates, with mass percent concentration be 70% ethanol desorbing is carried out to resin column, collect ethanol elution, concentrated and dry, obtain Semen Juglandis and remove clothing liquid Semen Juglandis flavone, the response rate of Semen Juglandis flavone is 78.53%, and purity is 56.94%;
(5) cross resin column with 4BV 2% HCl solution, and be washed till close to neutral with pure water, then cross resin column by 4BV 4% NaOH solution, and pure water is washed till close to neutral, wash post with 3BV 90% ethanol again, and wash away ethanol with pure water, the regeneration rate of resin is 90.64%.
Embodiment 3: reclaim with macroporous resin the method that Semen Juglandis removes Semen Juglandis flavone in clothing waste liquid, carry out as follows:
(1) get Semen Juglandis and remove clothing liquid 500 mL, 5000 rpm are in batches centrifugal, get supernatant, mixing, measure flavones content;
(2) AB-8 type macroporous resin pretreatment
Fully being rinsed by resin with distilled water, is the soak with ethanol 12h of 95% with mass percent concentration, makes it fully swelling, then with distilled water cleaning to without alcohol taste; With 5%NaOH solution soaking 6h, be then washed till pH close to neutral with distilled water; Soak 6h with 5% Solution H Cl, be then washed till pH close to neutral with distilled water;
(3) will Semen Juglandis flavone concentration dilution in clothing waste liquid be gone to 0.67mg/mL after centrifugal, and regulate pH value of solution to be 9;
(4) upper prop, adsorption time is 5h, after absorption terminates, with mass percent concentration be 80% ethanol desorbing is carried out to resin column, collect ethanol elution, concentrated and dry, obtain Semen Juglandis and remove clothing liquid Semen Juglandis flavone, the response rate of Semen Juglandis flavone is 84.76%, and purity is 61.68%;
(5) cross resin column with 4BV 3% HCl solution, and be washed till close to neutral with pure water, then cross resin column by 4BV 5% NaOH solution, and pure water is washed till close to neutral, wash post with 3BV 95% ethanol again, and wash away ethanol with pure water, the regeneration rate of resin is 96.51%.
Embodiment 4: reclaim with macroporous resin the method that Semen Juglandis removes Semen Juglandis flavone in clothing waste liquid, carry out as follows:
(1) get Semen Juglandis and remove clothing liquid 500 mL, 3000rpm is in batches centrifugal, gets supernatant, mixing, measures flavones content;
(2) NAK-9 type macroporous resin pretreatment
Fully being rinsed by resin with distilled water, is 95% soak with ethanol 12h with mass percent concentration, makes it fully swelling, then with distilled water cleaning to without alcohol taste; Be 5%NaOH solution soaking 6h with mass percent concentration, be then washed till pH close to neutral with distilled water; Be that 5% Solution H Cl soaks 6h with mass percent concentration, be then washed till pH close to neutral with distilled water;
(3) will Semen Juglandis flavone concentration dilution in clothing waste liquid be gone to 0.34mg/mL after centrifugal, and regulate pH value of solution to be 7;
(4) upper prop, adsorption time is 4h, after absorption terminates, with mass percent concentration be 60% ethanol desorbing is carried out to resin column, collect ethanol elution, concentrated and dry, obtain Semen Juglandis and remove clothing liquid Semen Juglandis flavone, the response rate of Semen Juglandis flavone is 71.15%, and purity is 50.72%;
(5) cross resin column with 3BV 3% HCl solution, and be washed till close to neutral with pure water, then cross resin column by 3BV 5% NaOH solution, and pure water is washed till close to neutral, wash post with 2BV 95% ethanol again, and wash away ethanol with pure water, the regeneration rate of resin is 89.26%.
Embodiment 5: reclaim with macroporous resin the method that Semen Juglandis removes Semen Juglandis flavone in clothing waste liquid, carry out as follows:
(1) get Semen Juglandis and remove clothing liquid 500 mL, 4000 rpm are in batches centrifugal, get supernatant, mixing, measure flavones content;
(2) NAK-9 type macroporous resin pretreatment
With distilled water, resin is fully rinsed, with 95% soak with ethanol 12h, makes it fully swelling, then with distilled water cleaning to without alcohol taste; With 5%NaOH solution soaking 6h, be then washed till pH close to neutral with distilled water; Soak 6h with 5% Solution H Cl, be then washed till pH close to neutral with distilled water;
(3) will Semen Juglandis flavone concentration dilution in clothing waste liquid be gone to 0.50mg/mL after centrifugal, and regulate pH value of solution to be 8;
(4) upper prop, adsorption time is 5h, after absorption terminates, with mass percent concentration be 70% ethanol desorbing is carried out to resin column, collect ethanol elution, concentrated and dry, obtain Semen Juglandis and remove clothing liquid Semen Juglandis flavone, the response rate of Semen Juglandis flavone is 75.58%, and purity is 54.61%;
(5) cross resin column with 4BV 2% HCl solution, and be washed till close to neutral with pure water, then cross resin column by 4BV 4% NaOH solution, and pure water is washed till close to neutral, wash post with 3BV 90% ethanol again, and wash away ethanol with pure water, the regeneration rate of resin is 91.74%.
Embodiment 6: reclaim with macroporous resin the method that Semen Juglandis removes Semen Juglandis flavone in clothing waste liquid, carry out as follows:
(1) get Semen Juglandis and remove clothing liquid 500 mL, 5000 rpm are in batches centrifugal, get supernatant, mixing, measure flavones content;
(2) NAK-9 type macroporous resin pretreatment
With distilled water, resin is fully rinsed, with 95% soak with ethanol 12h, makes it fully swelling, then with distilled water cleaning to without alcohol taste; With 5%NaOH solution soaking 6h, be then washed till pH close to neutral with distilled water; Soak 6h with 5% Solution H Cl, be then washed till pH close to neutral with distilled water;
(3) will Semen Juglandis flavone concentration dilution in clothing waste liquid be gone to 0.67mg/mL after centrifugal, and regulate pH value of solution to be 9;
(4) upper prop, adsorption time is 5h, after absorption terminates, with mass percent concentration be 80% ethanol desorbing is carried out to resin column, collect ethanol elution, concentrated and dry, obtain Semen Juglandis and remove clothing liquid Semen Juglandis flavone, the response rate of Semen Juglandis flavone is 79.82%, and purity is 58.63%;
(5) cross resin column with 4BV 3% HCl solution, and be washed till close to neutral with pure water, then cross resin column by 4BV 5% NaOH solution, and pure water is washed till close to neutral, wash post with 3BV 95% ethanol again, and wash away ethanol with pure water, the regeneration rate of resin is 94.72%.
Claims (3)
1. reclaim with macroporous resin the method that Semen Juglandis removes Semen Juglandis flavone in clothing waste liquid, it is characterized in that carrying out as follows:
(1) getting Semen Juglandis goes clothing waste liquid centrifugal under rotating speed is 3000-5000 rpm condition, removing float and solid;
(2) will Semen Juglandis flavone concentration dilution in clothing waste liquid be gone to 0.34-0.67mg/mL after centrifugal, and regulate pH value of solution to be 7-9;
(3) step (2) solution is poured into be equipped with in pretreated macroporous resin column adsorb, more than adsorption time 4h;
(4) after absorption terminates, be that the ethanol of 60-80% carries out desorbing to resin column with mass percent concentration, obtain ethanol Semen Juglandis flavonoids solution, by solution for vacuum evaporating, concentrating and drying, reclaim ethanol, finally obtain Semen Juglandis flavone extract.
2. method of removing Semen Juglandis flavone in clothing waste liquid with macroporous resin recovery Semen Juglandis according to claim 1, is characterized in that: macroporous resin model is AB-8 or NAK-9.
3. method of removing Semen Juglandis flavone in clothing waste liquid with macroporous resin recovery Semen Juglandis according to claim 1 and 2, it is characterized in that: pretreatment macroporous resin refers to and fully to be rinsed by macroporous resin with distilled water, till effluent is not white opacity, be the soak with ethanol 12h of 95% with mass percent concentration, make it fully swelling, then with distilled water cleaning to without alcohol; Soak 6h by the NaOH solution that mass percent concentration is 5%, be then washed till pH close to neutral with distilled water; With the HCl solution soaking 6h that mass percent concentration is 5%, be then washed till pH close to neutral and macroporous resin that is that obtain with distilled water.
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| CN114605480A (en) * | 2022-04-12 | 2022-06-10 | 秦怀跃 | Preparation method of walnut flavone and walnut polyphenol |
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