CN104857072B - A method of walnut polyphenol chromocor in clothing liquid is gone with macroreticular resin recycling walnut kernel - Google Patents
A method of walnut polyphenol chromocor in clothing liquid is gone with macroreticular resin recycling walnut kernel Download PDFInfo
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Abstract
The invention discloses a kind of in the macroreticular resin recycling walnut kernel method of removing walnut flavones in clothing waste liquid, and this method includes the pretreatment that walnut kernel removes clothing liquid, and operating procedures, the concentration such as isolate and purify and regenerate of macroporous absorbent resin are dried.Walnut flavonoid concentration in pretreatment in the past clothing liquid is diluted to 0.34-0.67mg/mL, pH value is adjusted to 7-9 with concentrated hydrochloric acid, solution is poured into and installs the adsorption tanks of macroreticular resin and adsorbs, adsorption time is 4h or more, after absorption, is desorbed with the ethyl alcohol of 60-80%, obtain ethyl alcohol walnut flavonoids solution, by solution vacuum evaporation and drying, ethyl alcohol is recycled, the fine extract of walnut flavones is finally obtained.The rate of recovery of walnut flavones reaches 70% or more, and purity reaches 50% or more.The process flow is simple, at low cost, high efficiency, and macroreticular resin can be used with regeneration cycle, and industrialization recycling walnut kernel is suitble to remove walnut flavone compound in clothing waste liquid.
Description
Technical field
The present invention relates to a kind of methods for removing walnut flavones in clothing waste liquid with macroreticular resin recycling walnut kernel, belong to food pair
The intensive processing field of product, specially comprehensive utilization walnut kernel go clothing liquid resource, the processing method for extracting walnut flavones.
Background technique
There are the polyphenol chromocors chemical combination such as rutin, ellagic acid, rhodioside, jonquil glycosides, Quercetin, catechin in walnut kernel clothing
Object (Shi Dandan waits food industry scientific and technological, 2014,2:375), is a kind of natural for possessing very strong anti-oxidative activity,
Including remove free radical, prevention cardiovascular disease, anti-cancer, it is anti-radiation, delay the functions such as body aging, protected with high nutrition
Strong value.
With the fast development of food industry, walnut product is continued to introduce new, and wherein Walnut Milk and walnut oil are especially prominent
Out, walnut kernel is rich in walnut polyphenols, and is concentrated mainly on walnut kind skin or walnut clothing, but in Walnut Milk process
In, since walnut kernel endotesta content of tannin is higher, often will affect the mouthfeel and color of walnut product, therefore, it is necessary to by its
It removes.Currently, it is lye dipping method that domestic walnut processing enterprise is most widely used, this large effect walnut kernel nutrition function
Energy ingredient, it has also become the bottleneck of Walnut Industryization development.Walnut kernel is soaking and removes clothing, and polyphenol declines respectively with flavones content
81.7% and 72.2%.In addition, the waste water COD that lye dipping generates is 20000mg/L or so, national secondary sewage row is substantially exceeded
Put standard, enterprise's one ton of Walnut Milk of every production, it will several tons of waste water of production, waste water largely discharges, and will cause neighbouring field
The environmental pollutions such as ground, water quality bring immense pressure to the survival and development of enterprise.
Macroreticular resin is organic high molecular polymer, in use can be old because of the Irreversible Adsorption of certain ingredients
Change, after some cycles, adsorption capacity decline needs to regenerate to restore its absorption property.And still lack to resin at present
The research of regeneration and the method for regeneration technology and the whether satisfactory index of correlation of regenerating resin.
Walnut kernel goes clothing liquid mainly to regard direct discharging of waste water at present, this causes a large amount of of the effective components such as walnut flavones
Loss.In addition, the extraction of document report walnut flavones is usually first to be extracted by organic solvent, after macroreticular resin, film filtering or
The methods of ion exchange obtains purified.These processes are cumbersome, complicated for operation, at high cost.To realize that processing step is few, road
The purpose that line is simple, consumption is low, high-efficient, the present invention are foothold from Business Economic Benefit is improved, and are studied a kind of from walnut kernel
The technique for going in clothing liquid to recycle walnut flavones.
Summary of the invention
It is an object of the present invention to provide a kind of method for removing walnut flavones in clothing liquid with macroreticular resin recycling walnut kernel, the party
Method the following steps are included:
(1) it takes walnut kernel that clothing waste liquid is gone to be centrifuged under the conditions of revolving speed is 3000-5000 rpm, removes suspended matter and solid；
(2) it pre-processes macroreticular resin: sufficiently being rinsed macroreticular resin with distilled water, until the not white muddiness of efflux,
12h is impregnated with the ethyl alcohol that mass percent concentration is 95%, is swollen it sufficiently, then wash with distilled water until no alcohol；With
The NaOH solution that mass percent concentration is 5% impregnates 6h, is then washed to pH close to neutrality with distillation；It is dense with mass percent
It spends and impregnates 6h for 5% HCl solution, be then washed to pH close to macroreticular resin obtained from neutrality with distillation；
(3) the walnut flavonoid concentration gone in clothing waste liquid after centrifugation is diluted to 0.34-0.67mg/mL, and adjusts solution
PH is 7-9；
(4) step (3) solution is poured into the adsorption tanks equipped with macroreticular resin to adsorb, adsorption time 4h or more；
(5) it after adsorbing, is desorbed with the ethyl alcohol that mass percent concentration is 60-80%, obtains ethyl alcohol walnut flavones
Solution, solution vacuum evaporation is dry, ethyl alcohol is recycled, walnut chromocor extract is finally obtained；The rate of recovery of walnut flavones
Reach 70% or more, purity is 50% or more；
(6) macroreticular resin after desorption is eluted with water, can reach the purpose of resin simple regeneration；
(7) when 30% or more adsorbance decline, resin column is crossed with HCl solution, and be washed till close to neutrality, then with pure water
Resin column is crossed with NaOH solution, then pure water is washed till close to neutrality, is finally washed column with ethyl alcohol, and wash away ethyl alcohol with pure water, is made resin
Strengthened regeneration.
The model AB-8 or NAK-9 of macroreticular resin in step (2).
The dosage of water is 5-6 column volume (BV) in step (6).
The dosage of HC1 is 3-4BV, mass percent concentration 2-3% in step (7)；The dosage of NaOH is 3-4BV, quality
Percent concentration is 4-5%；Ethanol consumption is 2-3BV, and mass percent concentration 90-95%, the regeneration rate of resin is in 87.45%-
Between 96.51%.
Advantage for present invention:
(1) the walnut polyphenol chromocor that the present invention removes in clothing liquid walnut kernel has carried out recovery process research, the chemistry used
Regulator is harmless object, can be widely applied to food industrialization production；Operating process is simple and convenient, the salvage material used
(macroreticular resin, ethyl alcohol) is recyclable material, economical and environmentally friendly.The rate of recovery of products therefrom walnut flavones reaches 80% or more,
Purity reaches 60% or more；
(2) the walnut flavones content that the present invention obtains is higher, and processing step is few, route is simple, consumption is low, high-efficient, raw
Cost is produced to substantially reduce.Therefore, the walnut polyphenol chromocor of high efficiency, high-content, low cost can be realized using the method for the present invention
Recycling.The recovery method step is simple and reliable, high-efficient, simple process, strong operability, pollution-free, it is easy to accomplish industrialization
Large-scale production.Therefore there is preferable economic benefit, society and ecological significance.
(3) present invention studies the regeneration of macroreticular resin with technique, wants to establish the correlation of regenerating resin
Index is asked to provide theoretical foundation.
(4) present invention goes clothing liquid to carry out a degree of processing walnut, while recycling walnut flavones therein, to money
Source and environment are of great significance.
(5) the obtained walnut flavones of the present invention with it is anti-oxidant, prevent cardiovascular disease, anti-cancer, it is anti-radiation, delay body
The functions such as aging, enhancing and improvement memory function, are a kind of ideal nutrition and health care drugs.
Specific embodiment
Technical solution of the present invention is further elaborated below by specific embodiment, but protection model of the invention
It encloses and is not limited to this.
Embodiment 1: the method for removing walnut flavones in clothing waste liquid with macroreticular resin recycling walnut kernel carries out as follows:
(1) it takes walnut kernel that 500 mL of clothing liquid, 3000 rpm is gone to be centrifuged in batches, takes supernatant, mix, measure flavones content；
(2) AB-8 type macroreticular resin pre-processes
Resin is sufficiently rinsed with distilled water, is 95% with mass percent concentration until the not white muddiness of efflux
Ethyl alcohol impregnates 12h, is swollen it sufficiently, then wash with distilled water until no alcohol taste；6h is impregnated with 5%NaOH solution, then
PH is washed to close to neutrality with distillation；6h is impregnated with 5% Solution H Cl, is then washed to pH close to neutrality with distillation；
(3) the walnut flavonoid concentration gone in clothing waste liquid after centrifugation is diluted to 0.34mg/mL, and adjusting pH value of solution is 7；
(4) upper prop, adsorption time 4h, after absorption, with mass percent concentration be 60% ethyl alcohol to resin column into
Row desorption, collects ethanol eluate, is concentrated and dried, obtains walnut kernel and remove clothing liquid walnut flavones, the rate of recovery of walnut flavones is
80.24%, purity 53.82%；
(5) resin column is crossed with 3% HCl solution of 3BV, and is washed till with pure water close to neutrality, it is then molten with 5% NaOH of 3BV
Liquid crosses resin column, and pure water is washed till close to neutrality, then washes column with 95% ethyl alcohol of 2BV, and wash away ethyl alcohol with pure water, and resin is again
Raw rate is 87.45%.
Embodiment 2: the method for removing walnut flavones in clothing waste liquid with macroreticular resin recycling walnut kernel carries out as follows:
(1) it takes walnut kernel that 500 mL of clothing liquid, 4000 rpm is gone to be centrifuged in batches, takes supernatant, mix, measure flavones content；
(2) AB-8 type macroreticular resin pre-processes
Resin is sufficiently rinsed with distilled water, 12h is impregnated with the ethyl alcohol that mass percent concentration is 95%, keeps it sufficiently molten
It is swollen, then wash with distilled water until no alcohol taste；6h is impregnated with 5%NaOH solution, is then washed to pH in distillation
Property；6h is impregnated with 5% Solution H Cl, is then washed to pH close to neutrality with distillation；
(3) the walnut flavonoid concentration gone in clothing waste liquid after centrifugation is diluted to 0.5mg/mL, and adjusting pH value of solution is 8；
(4) upper prop, adsorption time 5h, after absorption, with mass percent concentration be 70% ethyl alcohol to resin column into
Row desorption, collects ethanol eluate, is concentrated and dried, obtains walnut kernel and remove clothing liquid walnut flavones, the rate of recovery of walnut flavones is
78.53%, purity 56.94%；
(5) resin column is crossed with 2% HCl solution of 4BV, and is washed till with pure water close to neutrality, it is then molten with 4% NaOH of 4BV
Liquid crosses resin column, and pure water is washed till close to neutrality, then washes column with 90% ethyl alcohol of 3BV, and wash away ethyl alcohol with pure water, and resin is again
Raw rate is 90.64%.
Embodiment 3: the method for removing walnut flavones in clothing waste liquid with macroreticular resin recycling walnut kernel carries out as follows:
(1) it takes walnut kernel that 500 mL of clothing liquid, 5000 rpm is gone to be centrifuged in batches, takes supernatant, mix, measure flavones content；
(2) AB-8 type macroreticular resin pre-processes
Resin is sufficiently rinsed with distilled water, 12h is impregnated with the ethyl alcohol that mass percent concentration is 95%, keeps it sufficiently molten
It is swollen, then wash with distilled water until no alcohol taste；6h is impregnated with 5%NaOH solution, is then washed to pH in distillation
Property；6h is impregnated with 5% Solution H Cl, is then washed to pH close to neutrality with distillation；
(3) the walnut flavonoid concentration gone in clothing waste liquid after centrifugation is diluted to 0.67mg/mL, and adjusting pH value of solution is 9；
(4) upper prop, adsorption time 5h, after absorption, with mass percent concentration be 80% ethyl alcohol to resin column into
Row desorption, collects ethanol eluate, is concentrated and dried, obtains walnut kernel and remove clothing liquid walnut flavones, the rate of recovery of walnut flavones is
84.76%, purity 61.68%；
(5) resin column is crossed with 3% HCl solution of 4BV, and is washed till with pure water close to neutrality, it is then molten with 5% NaOH of 4BV
Liquid crosses resin column, and pure water is washed till close to neutrality, then washes column with 95% ethyl alcohol of 3BV, and wash away ethyl alcohol with pure water, and resin is again
Raw rate is 96.51%.
Embodiment 4: the method for removing walnut flavones in clothing waste liquid with macroreticular resin recycling walnut kernel carries out as follows:
(1) it takes walnut kernel that 500 mL of clothing liquid, 3000rpm is gone to be centrifuged in batches, takes supernatant, mix, measure flavones content；
(2) NAK-9 type macroreticular resin pre-processes
Resin is sufficiently rinsed with distilled water, is that 95% ethyl alcohol impregnates 12h with mass percent concentration, is swollen it sufficiently,
Then wash with distilled water until no alcohol taste；It is that 5%NaOH solution impregnates 6h with mass percent concentration, then uses distilled water
PH is washed till close to neutrality；It is that 5% Solution H Cl impregnates 6h with mass percent concentration, is then washed to pH close to neutrality with distillation；
(3) the walnut flavonoid concentration gone in clothing waste liquid after centrifugation is diluted to 0.34mg/mL, and adjusting pH value of solution is 7；
(4) upper prop, adsorption time 4h, after absorption, with mass percent concentration be 60% ethyl alcohol to resin column into
Row desorption, collects ethanol eluate, is concentrated and dried, obtains walnut kernel and remove clothing liquid walnut flavones, the rate of recovery of walnut flavones is
71.15%, purity 50.72%；
(5) resin column is crossed with 3% HCl solution of 3BV, and is washed till with pure water close to neutrality, it is then molten with 5% NaOH of 3BV
Liquid crosses resin column, and pure water is washed till close to neutrality, then washes column with 95% ethyl alcohol of 2BV, and wash away ethyl alcohol with pure water, and resin is again
Raw rate is 89.26%.
Embodiment 5: the method for removing walnut flavones in clothing waste liquid with macroreticular resin recycling walnut kernel carries out as follows:
(1) it takes walnut kernel that 500 mL of clothing liquid, 4000 rpm is gone to be centrifuged in batches, takes supernatant, mix, measure flavones content；
(2) NAK-9 type macroreticular resin pre-processes
Resin is sufficiently rinsed with distilled water, 12h is impregnated with 95% ethyl alcohol, is swollen it sufficiently, then wash with distilled water
Until no alcohol taste；6h is impregnated with 5%NaOH solution, is then washed to pH close to neutrality with distillation；6h is impregnated with 5% Solution H Cl,
Then pH is washed to close to neutrality with distillation；
(3) the walnut flavonoid concentration gone in clothing waste liquid after centrifugation is diluted to 0.50mg/mL, and adjusting pH value of solution is 8；
(4) upper prop, adsorption time 5h, after absorption, with mass percent concentration be 70% ethyl alcohol to resin column into
Row desorption, collects ethanol eluate, is concentrated and dried, obtains walnut kernel and remove clothing liquid walnut flavones, the rate of recovery of walnut flavones is
75.58%, purity 54.61%；
(5) resin column is crossed with 2% HCl solution of 4BV, and is washed till with pure water close to neutrality, it is then molten with 4% NaOH of 4BV
Liquid crosses resin column, and pure water is washed till close to neutrality, then washes column with 90% ethyl alcohol of 3BV, and wash away ethyl alcohol with pure water, and resin is again
Raw rate is 91.74%.
Embodiment 6: the method for removing walnut flavones in clothing waste liquid with macroreticular resin recycling walnut kernel carries out as follows:
(1) it takes walnut kernel that 500 mL of clothing liquid, 5000 rpm is gone to be centrifuged in batches, takes supernatant, mix, measure flavones content；
(2) NAK-9 type macroreticular resin pre-processes
Resin is sufficiently rinsed with distilled water, 12h is impregnated with 95% ethyl alcohol, is swollen it sufficiently, then wash with distilled water
Until no alcohol taste；6h is impregnated with 5%NaOH solution, is then washed to pH close to neutrality with distillation；6h is impregnated with 5% Solution H Cl,
Then pH is washed to close to neutrality with distillation；
(3) the walnut flavonoid concentration gone in clothing waste liquid after centrifugation is diluted to 0.67mg/mL, and adjusting pH value of solution is 9；
(4) upper prop, adsorption time 5h, after absorption, with mass percent concentration be 80% ethyl alcohol to resin column into
Row desorption, collects ethanol eluate, is concentrated and dried, obtains walnut kernel and remove clothing liquid walnut flavones, the rate of recovery of walnut flavones is
79.82%, purity 58.63%；
(5) resin column is crossed with 3% HCl solution of 4BV, and is washed till with pure water close to neutrality, it is then molten with 5% NaOH of 4BV
Liquid crosses resin column, and pure water is washed till close to neutrality, then washes column with 95% ethyl alcohol of 3BV, and wash away ethyl alcohol with pure water, and resin is again
Raw rate is 94.72%.
Claims (1)
1. a kind of in the macroreticular resin recycling walnut kernel method of removing walnut flavones in clothing waste liquid, it is characterised in that as follows into
Row:
(1) it takes walnut kernel that clothing waste liquid is gone to be centrifuged under the conditions of revolving speed is 3000-5000 rpm, removes suspended matter and solid；
(2) the walnut flavonoid concentration gone in clothing waste liquid after centrifugation is diluted to 0.34-0.67mg/mL, and adjusts pH value of solution and is
7-9；
(3) step (2) solution is poured into equipped with adsorbing in pretreated macroporous resin column, adsorption time 4h or more；
(4) after adsorbing, resin column is desorbed with the ethyl alcohol that mass percent concentration is 60-80%, obtains ethyl alcohol walnut
Flavonoids solution, solution vacuum evaporation is dry, ethyl alcohol is recycled, walnut chromocor extract is finally obtained；
Macroreticular resin the model AB-8 or NAK-9；
The pretreatment macroreticular resin, which refers to, is sufficiently rinsed macroreticular resin with distilled water, until the not white muddiness of efflux,
12h is impregnated with the ethyl alcohol that mass percent concentration is 95%, is swollen it sufficiently, then wash with distilled water until no alcohol；With
The NaOH solution that mass percent concentration is 5% impregnates 6h, is then washed to pH close to neutrality with distillation；It is dense with mass percent
It spends and impregnates 6h for 5% HCl solution, be then washed to pH close to macroreticular resin obtained from neutrality with distillation.
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| CN110558560A (en) * | 2019-07-25 | 2019-12-13 | 西乡县巴山荞园茶业有限公司 | Method for recycling bitter buckwheat soaking water and continuously recovering flavone |
| CN114605480A (en) * | 2022-04-12 | 2022-06-10 | 秦怀跃 | Preparation method of walnut flavone and walnut polyphenol |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102579565A (en) * | 2012-01-18 | 2012-07-18 | 河北联合大学 | Method for microwave reflux extraction of general flavone in walnut peel residue |
| CN103864741A (en) * | 2014-03-06 | 2014-06-18 | 陈朝银 | Preparation and application of walnut shell flavone lipid-decreasing active ingredient |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102579565A (en) * | 2012-01-18 | 2012-07-18 | 河北联合大学 | Method for microwave reflux extraction of general flavone in walnut peel residue |
| CN103864741A (en) * | 2014-03-06 | 2014-06-18 | 陈朝银 | Preparation and application of walnut shell flavone lipid-decreasing active ingredient |
Non-Patent Citations (2)
| Title |
|---|
| 《鲜核桃保险及核桃种皮中多酚化合物的测定、纯化及功能研究》;张天财;《中国优秀硕士学位论文全文数据库 工程科技I辑》;中国学术期刊（光盘版）电子杂志社;20150115(第1期);第84页右栏第2段，参见第86页右栏第2段，第87页右栏第4段 |
| 核桃仁碱液去皮过程中营养功能成分动态变化;吴世兰 等;《中国油脂》;20131231;第38卷(第2期);第8页最后1段，第37页表4.1，最后1段，第38页第1-3段，第39页，第45页最后2段 |
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