CN107626118A - Plant base electro-coppering sewage demulsifier - Google Patents

Abstract

Plant base electro-coppering sewage demulsifier, including at least isatis root extract, tuckahoe extracts, fruit of Rangoon creeper's extract, chrysanthemum extract, Shitake Mushroom P.E, perilla leaf extract, water.

Description

Plant base electro-coppering sewage demulsifier

Technical field

The present invention relates to electro-coppering sewage disposal, more particularly to a kind of plant base electro-coppering sewage demulsifier.

Background technology

NPE is a kind of nonionic surfactant, and it has good infiltration, emulsification, disperses, be anti- Acid, alkali resistant, hard water resistance, anti-reduction, oxidation resistant ability.W/o type emulsifying agent or O/W types emulsifying agent, dispersant are widely used as, is Synthetic detergent primary raw material.NPE can be used as acid bright copper plating carrier brightener.It can be in electricity The adsorption layer on pole surface hinders Cu²⁺Diffusion, have enhancing polarization, the effect of crystal grain thinning.However, NPE Once entering in environment, the stronger Environmental Hormone Nonylphenol of toxicity will be resolved into rapidly.Nonyl phenol is that the whole world is generally acknowledged Environmental hormone.Research shows, even if the concentration of this material discharge is very low, also great harmfulness.It is general dirty using continuous activity Mud method degraded NPE.But stronger, the H therein of acidity of plating copper waste water⁺And Cu²⁺Easily make active component Failure, for the NPE in plating copper waste water, not extraordinary processing method.

The content of the invention

In order to solve prior art problem, the present invention provides a kind of plant base electro-coppering sewage demulsifier, including at least plate Blue root extract, tuckahoe extracts, fruit of Rangoon creeper's extract, chrysanthemum extract, Shitake Mushroom P.E, perilla leaf extract, water.

In some embodiments, described plant base electro-coppering sewage demulsifier, it is in parts by weight, blue including at least plate 14 parts of root extract, 8 parts of tuckahoe extracts, 10 parts of fruit of Rangoon creeper's extract, 8 parts of chrysanthemum extract, 8 parts of Shitake Mushroom P.E, purple perilla 10 parts of leaf extract, 100 parts of water.

In some embodiments, the preparation method of the isatis root extract is：400g Radix Isatidis is cleaned, worn into Powder, 1000mL benzene is added, 5h is preserved in 4 DEG C, with filtered on buchner funnel, collect solid, add 500mL 3wt% acetic acid, then add Enter 5g vulcanized sodium, keep 50 DEG C of constant temperature, soak 3h, filtering, collect solid, add 500mL distilled water, keep 50 DEG C of constant temperature, 3h is soaked, filtering, collects filtrate, then is handled by highly acidic cation exchange column, efflux is discarded, to resin column water Efflux is washed till as neutrality, is then eluted using 0.3mol/L ammoniacal liquor, is collected ammoniacal liquor eluent, be concentrated under reduced pressure into 100mL, 800mL absolute ethyl alcohols are added, separate out crystal, crystal is collected by filtration, 12h is dried in vacuo, produces.

In some embodiments, the preparation method of the tuckahoe extracts is：By 300g Poria cocos grinds, distillation is added Water is heated to reflux 3 times, adds distilled water 600mL every time, and each return time is 3h, and filtering, merging filtrate, vacuum distillation will be molten Liquid is concentrated into 300mL, adds 800mL absolute ethyl alcohols, stands 24h, filtering, collects filtrate, and distillation under pressure is to without ethanol, then By the strong acid ion exchange resins of Zerolie 225, efflux is discarded, it is neutrality resin column to be washed with water to efflux, so Eluted afterwards using 0.5mol/L ammoniacal liquor, collect eluent, be concentrated under reduced pressure into 50mL, stood 24h, filtering, collect solid, very Sky dries 12h, produces.

In some embodiments, the preparation method of fruit of Rangoon creeper's extract is：The 200g fruits of Rangoon creeper are taken, cleans, wears into Powder, 800mL absolute ethers are added, be heated to reflux 5h, cooled and filtered, collect filtrate, be evaporated under reduced pressure to 100mL, it is quiet at 4 DEG C 48h is put, solid is then collected by filtration, 12h is dried in vacuo, produces.

In some embodiments, the preparation method of the chrysanthemum extract is：Chrysanthemum 500g is taken, cleans, grinds, adds Enter 3000mL absolute ethyl alcohols, be heated to reflux 12h, filter, filtrate decompression is distilled, volume concentration to 200mL, adds 500mL Distilled water, 500mL n-butanols are added after stirring, liquid separation, collect butanol solution, are evaporated under reduced pressure, by volume concentration extremely 200mL, 2000mL absolute ethers are added, white precipitate occur, filtered, be dried in vacuo 5h, obtain white solid, white is solid Body is dissolved in 700mL absolute ethyl alcohols, adds 50mL 10wt% hydrochloric acid, is heated to reflux 5h, is concentrated into 200mL after cooling, adds 1000mL distilled water, filtering, remove precipitation, collect filtrate, 12g activated carbons are added in filtrate, heating water bath 30min, are filtered, Filtrate is collected, 50mL is concentrated into, adds 500mL absolute methanols, 5h is placed at -18 DEG C, separates out flake-like crystal, filtering is received Collect crystal, be dried in vacuo 12h, produce.

In some embodiments, the preparation method of the Shitake Mushroom P.E is：Take 300g mushrooms, grinds, in ice bath Lower dropwise addition 500mL 0.5mol/L NaOH, after being added dropwise, continue to stir 3h under ice bath, then filter, collect filtrate, add Enter glacial acetic acid to pH=8, precipitate, washed with 30mL acetone, then washed with 30mL ether, add 500mL distilled water, After stirring, 500mL dimethyl sulfoxides are added, are precipitated, precipitation is collected by filtration, washed with 30mL acetone, is dried in vacuo 3h, produce.

In some embodiments, described plant base electro-coppering sewage demulsifier, in addition to 10 parts of mint extract.

In some embodiments, the preparation method of the mint extract is：Take peppermint 500g, grinds, using super Critical CO₂Extraction, extract is collected, then carry out normal pressure fractionation, collected 200-220 DEG C of cut, produce.

In some embodiments, the preparation method of the perilla leaf extract is：Perilla leaf 500g is taken, grinds, is added Enter 2000mL distilled water, be heated to 80 DEG C, stir 3h, be cooled to room temperature, filter, 200mL 3wt% chlorine is added into filtrate Change calcium solution, stand 24h, filtering, concentrate the filtrate to 50mL, then add saturation ammoniacal liquor to pH=7.2, add 50mL tetra- Hydrogen furans, liquid separation, water layer is collected, be dried in vacuo 12h, produce.

In some embodiments, the plant base electro-coppering sewage demulsifier is used to contain NPE Sewage.

Embodiment

Participate in the election of the detailed description of the invention below for being preferable to carry out method and including embodiment this hair can be more easily understood Bright content.Unless otherwise defined, all technologies used herein and scientific terminology have common with art of the present invention The identical implication that technical staff is generally understood that.When contradiction be present, the definition in this specification is defined.

As used herein term " by ... prepare " it is synonymous with "comprising".Term "comprising" used herein, " comprising ", " having ", " containing " or its any other deformation, it is intended that cover including for non-exclusionism.For example, the combination comprising listed elements Thing, step, method, product or device are not necessarily limited to those key elements, but can include not expressly listed other key elements or Such a composition, step, method, product or the intrinsic key element of device.

Conjunction " Consists of " excludes any key element do not pointed out, step or component.If be used in claim, this Phrase will make claim be closed, it is not included the material in addition to the material of those descriptions, but relative normal Except rule impurity.When being rather than immediately following in the clause that phrase " Consists of " appears in claim main body after theme, It is only limited to the key element described in the clause；Other key elements are not excluded outside the claim as entirety.

Equivalent, concentration or other values or parameter are excellent with scope, preferred scope or a series of upper limit preferred values and lower limit During the Range Representation that choosing value limits, this, which is appreciated that, specifically discloses by any range limit or preferred value and any scope All scopes that any pairing of lower limit or preferred value is formed, regardless of whether the scope separately discloses.For example, when open During scope " 1 to 5 ", described scope should be interpreted as including scope " 1 to 4 ", " 1 to 3 ", " 1 to 2 ", " 1 to 2 and 4 to 5 ", " 1 to 3 and 5 " etc..When number range is described herein, unless otherwise indicated, otherwise the scope is intended to include its end Value and all integers and fraction within the range.

Singulative includes plural number and object is discussed, unless the context clearly dictates otherwise." optional " or it is " any It is a kind of " refer to that the item that describes thereafter or event may or may not occur, and the description include situation that event occurs and The situation that event does not occur.

Approximate term in specification and claims is used for modifying quantity, and it is specific to represent that the present invention is not limited to this Quantity, include the part of the amendment of the acceptable change without cause related basic function close to the quantity.Phase Answer, modify a numerical value with " about ", " about " etc., mean that the invention is not restricted to the exact numerical.It is approximate in some examples Term likely corresponds to the precision of the instrument of measured value.In present specification and claims, scope limits can be with Combine and/or exchange, these scopes include all subranges contained therebetween if not stated otherwise.

In addition, indefinite article " one kind " before key element of the present invention or component and "one" to key element or the quantitative requirement of component (i.e. occurrence number) unrestriction.Therefore "one" or " one kind " should be read as including one or at least one, and odd number The key element or component of form also include plural form, unless the obvious purport of the quantity refers to singulative.

Plant base electro-coppering sewage demulsifier, including at least isatis root extract, tuckahoe extracts, fruit of Rangoon creeper's extract, Chrysanthemum extract, Shitake Mushroom P.E, perilla leaf extract, water.

In some embodiments, described plant base electro-coppering sewage demulsifier, it is in parts by weight, blue including at least plate 14 parts of root extract, 8 parts of tuckahoe extracts, 10 parts of fruit of Rangoon creeper's extract, 8 parts of chrysanthemum extract, 8 parts of Shitake Mushroom P.E, purple perilla 10 parts of leaf extract, 100 parts of water.

Radix Isatidis

Radix Isatidis is cruciferae isatis Isatis indigotica Fort. dry root.In cylinder, slightly turn round Song, long 10~20cm, 0.5~1cm of diameter.Surface light lark or light brown yellow, there is vertical wrinkle and supporting root trace, and hole skin is grown crosswise. Root head slightly expands, it is seen that the petiole residue and intensive verruca of dirty-green or the arrangement of burgundy colyliform.Body is real, and matter is slightly soft, Section skin zone yellow-white, woody part yellow.Gas is micro-, bitter after the micro- sweet tea of taste.It is bitter in taste, tremble with fear.The thoughts of returning home, stomach.Major function heat-clearing solution Poison, cool blood relieving sore-throat.For febrile virulent maculae, tongue is dark reddish purple dark, mumps, larynx numbness, scarlet fever, major part pestilence, erysipelas, carbuncle swells.

Mainly contain and contain amino acid, indigo (indigotin, indigo), indigo red (indirubin), cupreol (β- Sitosterol), clionasterol (γ-sitosterol) and several amino acids：Arginine (arginine), glutamic acid (glutamic acid), tyrosine (tyrosine), proline (proline), valine (valine), γ-aminobutyric acid (γ-aminobu-tyric acid).Also (sinigrin) containing potassium myronate, indigo (indoxyl- β-hlucoside), tryptamines Ketone (trptanthrin), 1- thiocyanic acid -2- hydroxyl butyl- 3- alkene (l-thiocyano-2-hydroxy-3-butene), table accuses her Spring (epigoitrin), gland glucoside (adenosine), palmitic acid (palmitic acid), sucrose (sucrose) and proteoglycan.

In some embodiments, the preparation method of the isatis root extract is：400g Radix Isatidis is cleaned, worn into Powder, 1000mL benzene is added, 5h is preserved in 4 DEG C, with filtered on buchner funnel, collect solid, add 500mL 3wt% acetic acid, then add Enter 5g vulcanized sodium, keep 50 DEG C of constant temperature, soak 3h, filtering, collect solid, add 500mL distilled water, keep 50 DEG C of constant temperature, 3h is soaked, filtering, collects filtrate, then is handled by highly acidic cation exchange column, efflux is discarded, to resin column water Efflux is washed till as neutrality, is then eluted using 0.3mol/L ammoniacal liquor, is collected ammoniacal liquor eluent, be concentrated under reduced pressure into 100mL, 800mL absolute ethyl alcohols are added, separate out crystal, crystal is collected by filtration, 12h is dried in vacuo, produces.

Poria cocos

Poria cocos is On Polyporaceae Poria cocos Poria cocos (Schw.) Wolf dry sclerotia.In spherical, oval Shape, oblateness or irregular agglomerate, it is not of uniform size.Outer thin skin and coarse, sepia to dark brown, there is obvious shrinkage texture. Body weight, matter is solid, section graininess, and some tool cracks, outer layer light brown, inner white, a small number of pale reds, some centres are entertained Pine stump.Odorless, lightly seasoned, that chews sticks to one's teeth.Nature and flavor are sweet, light, put down.The thoughts of returning home, lung, spleen, kidney channel.Major function clearing damp and promoting diuresis, invigorating the spleen are peaceful The heart.For oedema oliguria, phlegm retention anti-dazzle nervous, spleen eating less, loose stool diarrhea, confused and worried, insomnia of palpitating with fear.

Containing β-pachyman, Pachymic acid, pachymic acid, 3 beta-hydroxy wool steroid trienic acids.In addition, still gummy, crust Matter, protein, fat, sterol, lecithin, glucose, adenine, histidine, choline, β-pachyman catabolic enzyme, lipase, Protease etc..

In some embodiments, the preparation method of the tuckahoe extracts is：By 300g Poria cocos grinds, distillation is added Water is heated to reflux 3 times, adds distilled water 600mL every time, and each return time is 3h, and filtering, merging filtrate, vacuum distillation will be molten Liquid is concentrated into 300mL, adds 800mL absolute ethyl alcohols, stands 24h, filtering, collects filtrate, and distillation under pressure is to without ethanol, then By the strong acid ion exchange resins of Zerolie 225, efflux is discarded, it is neutrality resin column to be washed with water to efflux, so Eluted afterwards using 0.5mol/L ammoniacal liquor, collect eluent, be concentrated under reduced pressure into 50mL, stood 24h, filtering, collect solid, very Sky dries 12h, produces.

The fruit of Rangoon creeper

The fruit of Rangoon creeper is combretaceae plant fruit of Rangoon creeper Quisqualis indica L. dry mature fruit.

Oval or oval, have 5 vertical ribs, occasionally there is 4~9 ribs, long 2.5~4cm, diameter about 2cm.Surface dark brown To atropurpureus, smoothly, micro- tool gloss.The narrow point in top, base portion blunt circle, there is the carpopodium trace of obvious circle.Matter is hard, and cross section is in more Pentalpha, edges and corners shell is thicker, and centre is in similar round cavity.Seed oblong or spindle, 2cm is about, diameter is about 1cm；Surface sepia or dark brown, there are most vertical wrinkles；Kind thin skin, it is easily peelable；Cotyledon 2, yellow-white have oiliness, and section has Crackle.Gas micro-perfume, the micro- sweet tea of taste.Nature and flavor are sweet, temperature.Returns spleen, stomach.Major function killing insect and eliminating accumulation.For roundworm, enterobiasis, malnutrition due to parasitic infestation Stomachache, infantile malnutrition.

Mainly contain quisqualic acid, proline, quisqualic acid potassium, fat oil, oleic acid, palmitic acid, stearic acid, sub- oil Acid, myristic acid, arachidic acid, sterol, sucrose, glucose, fructose, pentosan, malic acid, citric acid, butanedioic acid, N- methyl cigarettes Sour inner salt, quisqualic acid potassium, cyanidin monoglycoside.

In some embodiments, the preparation method of fruit of Rangoon creeper's extract is：The 200g fruits of Rangoon creeper are taken, cleans, wears into Powder, 800mL absolute ethers are added, be heated to reflux 5h, cooled and filtered, collect filtrate, be evaporated under reduced pressure to 100mL, it is quiet at 4 DEG C 48h is put, solid is then collected by filtration, 12h is dried in vacuo, produces.

Chrysanthemum

Chrysanthemum is feverfew pot marigold Calendula Officinalis L. flower.It is lightly seasoned；It is mild-natured.Major function is cool Blood stops blooding；Clearing heat-fire.Main hematochezia；Red eye, swell pain.Containing stigmasterol (stismasterol), cupreol (β- Silosterol), campesterol (campesterol), cholesterine (cholesterol), 24- methylenecholesterols (24- Methylenecholesterol), different fucose sterol (isofucosterol), 4 Beta-methyls 7,24 (28)-diene beans steroid -3 β -ol [4 β-methylstigmasta-7,24 (28)-diene-3 beta -ols], 4 Beta-methyl ergot steroids-7,24 (28)-β of diene-3- Alcohol [4 β-methyler-gasta-7,24 (28)-diene-3 beta -ols], methylsterol (methyl sterol), avenasterol (avenasterol), α-amyrin (α-amyrin), β-amyrin, taraxasterol (taraxasterol), ψ-Pu are public English sterol (ψ-taraxasterol), lupeol (lupeol), brein (brein), pot marigold glycol (calenduladiol), Arnica (srnidiol), faradiol (faradiol), Usu enediol (ursa- diol).Erythrodiol (erythrodiol), maniladiol (manilladiol), lupene triol (lupenetriol), Ladanum triol (heliantriol) F, C, Usu alkene triol (ursatriol), longispinogenin (longispinogenine), P-hydroxy Benzoic Acid (phydroxybenzoic acid), p-coumaric acid (p-coumaric acid), gentianic acid (gen- Tisic acid), vanillic acid (vanillic acid), syringic acid (syringic acid), caffeic acid (caffeic acid), O- hydroxyl phenylacetic acid (o-hydroxyphenyl acetic acid), salicylic acid (salicylic acid), protocatechuic acid (protocatechuic acid), umbelliferone (umbelliferone), horse chestnut bark glucoside (esculetin), Anisodus luridus Plain (scopoletin), pot marigold florigen (calendin), the double rhamnosides (calendoflaside) of pot marigold flavones, golden small cup Chrysanthemum glycosides displayed (calendoflavoside), demethyl pot marigold glycosides displayed (calendoflavobioside), narcissin (narcissoside, narcissin), Quercetin (quercetin), Isoquercitrin (isoquercetin), rutinoside (rutinoside), Isorhamnetin (isorhamnetin), Isorhamnetin -3-O- glycosides (isorhamnetin-3-O- ), glucoside Isorhamnetin -3-O- new dried orange peels glucoside (isorhamnetin-3-O-neohes-peridoside), different sandlwood Element -2G- rhamnopyranosyls answer fragrant glucoside (isorhamnetin-2G-rhamnosylrutinoside), quercetin glucoside (quercetin glucoside), Quercetin -2G- rhamnopyranosyl rutinosides (quercetin-2G- ), rhamnosylrutlnoside Quercetin -3-O- new dried orange peels glucoside (quercetin-3-O-neohesperidoside), different mouse Li Su -3-O- α-L- rhamnopyranosyls (1 → 2)-O [α-L- rhamnopyranosyls (1 → 6)]-β-D- glucopyanosides.

In some embodiments, the preparation method of the chrysanthemum extract is：Chrysanthemum 500g is taken, cleans, grinds, adds Enter 3000mL absolute ethyl alcohols, be heated to reflux 12h, filter, filtrate decompression is distilled, volume concentration to 200mL, adds 500mL Distilled water, 500mL n-butanols are added after stirring, liquid separation, collect butanol solution, are evaporated under reduced pressure, by volume concentration extremely 200mL, 2000mL absolute ethers are added, white precipitate occur, filtered, be dried in vacuo 5h, obtain white solid, white is solid Body is dissolved in 700mL absolute ethyl alcohols, adds 50mL 10wt% hydrochloric acid, is heated to reflux 5h, is concentrated into 200mL after cooling, adds 1000mL distilled water, filtering, remove precipitation, collect filtrate, 12g activated carbons are added in filtrate, heating water bath 30min, are filtered, Filtrate is collected, 50mL is concentrated into, adds 500mL absolute methanols, 5h is placed at -18 DEG C, separates out flake-like crystal, filtering is received Collect crystal, be dried in vacuo 12h, produce.

Mushroom

Mushroom Basidiomycetes Agaricales Agaricaceae mushroom Lentinus edodes (Berk.) Sing, is used as medicine with fructification. Nature and flavor are sweet, put down.Major function：QI invigorating is not hungry, controls wind blood-breaking, phlegm-eliminiating and qi-regulating, and beneficial taste helps food.

Volatilized containing lentinan, 1-OCOL (1-octen-3-ol), 2- octen-1-ols (2-octen-1-ol) etc. The peptides such as property material, γ-glutamyl nicotiannine (γ-glutamylnicotianine), saccharopin (saccharopine) Class compound and amino acid, eritadenine (eritadenine), atriphos (adenosine triphos-phate), two The nucleosides such as AMP (adenosine diphosphate), 5'- AMPs (5'-adenosine monophosphate) Acid compounds, ergosterol (er-gosterol), the β -ol of 5,7- ergot steroid diene -3 (ergosta-5,7-dien-3 β - Ol), lentinan (lentinan), provitamin D2 (provitamin D2, PD2), taurine (taurine), formaldehyde (formaldehyde), 2,3- dihydroxy -4- (9- adenyls) butyric acid [2,3-dihydroxy-4- (9-adenyl) Butyricacid), 2- hydroxyls -4- (9- adenyls) butyric acid [2-hydroxy-4- (9-adenyl) butyric acid], Portugal Glycan (glucan), water-soluble miscellaneous galactan (heterogalatan).Also (the polyphenol containing polyphenol oxidase Oxidase), glucosaccharase (α-glucosidase), glucoamylase (glucoamylase).

In some embodiments, the preparation method of the Shitake Mushroom P.E is：Take 300g mushrooms, grinds, in ice bath Lower dropwise addition 500mL 0.5mol/L NaOH, after being added dropwise, continue to stir 3h under ice bath, then filter, collect filtrate, add Enter glacial acetic acid to pH=8, precipitate, washed with 30mL acetone, then washed with 30mL ether, add 500mL distilled water, After stirring, 500mL dimethyl sulfoxides are added, are precipitated, precipitation is collected by filtration, washed with 30mL acetone, is dried in vacuo 3h, produce.

The composition extracted in isatis root extract can allow the sewage containing NPE to be demulsified, shape Separated into water phase and an oil phase, particularly add vulcanized sodium in the preparation process of isatis root extract, material therein can be promoted molten Go out, make demulsification more obvious.Inventor is had found in the research process for completing the present invention, and the fruit of Rangoon creeper is added in system and is carried Thing is taken, can be formed and precipitated with copper ion, so as to exclude interference of the copper ion to isatis root extract.Improve to nonyl in waste water The separating degree of phenol polyethenoxy ether.

In some embodiments, described plant base electro-coppering sewage demulsifier, in addition to 10 parts of mint extract.

Peppermint

Peppermint is Labiatae mint peppermint Mentha haplocalyx Briq. dry aerial parts.Stem is in Square column type, have to branch estranged, long 15~40cm, 0.2~0.4cm of diameter；Surface purple brown or light green, edges and corners tool fine hair, 2~5cm of internode length；Matter is crisp, section white, and marrow is hollow.Leaf has short handle to life；Leaf-shrinkage crimps, and is in after complete person's flattening Wide lanceolar, oblong or avette, long 2~7cm, wide 1~3cm；Upper surface bottle green, lower surface celadon is dilute by fine hair, There is concave point shape glandular scale.Take turns umbrella inflorescence axillary, Calyx mitriform, the fissure of tip 5, corolla lavender.There is special refrigerant fragrance after rubbing, Acrid flavour is cool.

Nature and flavor are pungent, cool.Return lung, Liver Channel.Major function dispelling wind-heat.Refresh oneself, promoting eruption.For anemopyretic cold, at the beginning of wind-warm syndrome Rise, headache, hot eyes, larynx numbness, aphtha, rubella, measles, Breast bilges frowsty.

Mainly contain menthol (menthol), menthones (menthone), isomenthone (isomenthone), pennyroyal mint Ketone (pulegone), decyl acetate (decyl acetate), menthyl acetate (menthyl acetate) methyl benzoate (methylbenzoate), α-and nopinene (pinene), β-thujene (β-thu-jene), 3- amylalcohols (3-pentol), 2- Alcohol (2-hexanol), 3- octanol (3-octanol), dextrorotation laurene (myrcene), limonene (limonene) and folium eucalypti Plain (cineole), alpha-terpineol (α-terpineol) etc..Contain flavones ingredient again：Different Rui Fuling (iso-raifolin), wood Rhinoceros grass element -7- glycosides (luteolin-7-glucoside), peppermint daidzin (methoside)；Determination of Organic Acids：Fan It is repeatedly fragrant sour (lusmarinic acid), caffeic acid (caffeic acid)；Chloro acid composition：Aspartic acid (aspartic Acid), glutamic acid (glutamic acid), serine (alanine), asparagine (asparagine), valine (valine), leucine (leuine) and isoleucine (isoleucine), phenylalanine (phenylalanine), methionine (methionine) lysine (lysine).

In some embodiments, the preparation method of the mint extract is：Take peppermint 500g, grinds, using super Critical CO₂Extraction, extract is collected, then carry out normal pressure fractionation, collected 200-220 DEG C of cut, produce.

After adding mint extract in body series, the demulsification of plating copper waste water can be strengthened, improve polyoxyethylene nonyl phenyl The coefficient of dispersion of the vinethene in oil phase, reduce its coefficient of dispersion in aqueous phase, so that NPE is from dirt Separated in water.

Perilla leaf

Perilla leaf is labiate purple perilla Perilla frutescens (L.) Britt dried leaf.This product blade is more Shrinkage crimps, is broken broken, is in oval after complete person's flattening, long 4~11cm, wide 2.5~9cm.Tip length is sharp or anxious sharp, base portion circle Shape or wide wedge shape, edge tool crenature.Two sides purple or upper surface green, lower surface purple, sparsely grow canescence hair, lower surface has The glandular scale of most concave point shapes.Petiole grows 2~7cm, purple or purple green.Matter is crisp.Band spray person, 2~5mm of diameter of branch are purple green There is marrow at color, section middle part.Gas delicate fragrance, taste micro-pungent.

Perilla leaf mainly contains perillaldehyde (perillaldehyde), limonene (limonene), β-cloves alkene (β- Caryophyllene), α-bergmot Shan alkene (α-bergamotene) and linalool (linlaool), perilla alcohol-β-D- pyrans Portugal Grape glucoside (perillyl- β-D-glucopyranoside), shisonin (perilloside) B, C and 1,2- methylene-dioxy- 4- methoxyl group -5- pi-allyl -3- phenyl β-D- glucopyanosides (1,2-methylenedioxy-4-methoxy-5- allyl-3-phenyl-β-D-glucopyranoside).Aerial part (perillaketone) containing perilla ketone, different common perilla alkene Ketone (isoegomaketone), ergomaketon (ego-maketone), perillene (perillene), ethyl linolenate (ethyllinolenater), leukotrienes (linolenic acid) and cupreol (β-sitosterol).

In some embodiments, the preparation method of the perilla leaf extract is：Perilla leaf 500g is taken, grinds, is added Enter 2000mL distilled water, be heated to 80 DEG C, stir 3h, be cooled to room temperature, filter, 200mL 3wt% chlorine is added into filtrate Change calcium solution, stand 24h, filtering, concentrate the filtrate to 50mL, then add saturation ammoniacal liquor to pH=7.2, add 50mL tetra- Hydrogen furans, liquid separation, water layer is collected, be dried in vacuo 12h, produce.

Perilla leaf extract can prevent isatis root extract to be oxidized, particularly the preparation process in perilla leaf extract In, during only with tetrahydrofuran liquid separation, corresponding impurity can be taken away, and active ingredient is remained.In research process, hair A person of good sense find tetrahydrofuran phase be separated with aqueous phase, it may be possible in the aqueous solution dissolved with solute after, improve tetrahydrofuran Dispersibility between water.So as to allow active ingredient to be retained in aqueous phase, corresponding impurity is taken away by organic phase.

In some embodiments, the plant base electro-coppering sewage demulsifier is used to contain NPE Sewage.

The preparation method of plant base electro-coppering sewage demulsifier of the present invention is to mix each composition at room temperature, Stir, produce.

The present invention is expanded on further with reference to specific embodiment.

Embodiment 1

Plant base electro-coppering sewage demulsifier, in parts by weight, including 14 parts of isatis root extract, 8 parts of tuckahoe extracts, 10 parts of fruit of Rangoon creeper's extract, 8 parts of chrysanthemum extract, 8 parts of Shitake Mushroom P.E, 10 parts of perilla leaf extract, 100 parts of water.

The preparation method of the isatis root extract is：400g Radix Isatidis is cleaned, grinds, 1000mL benzene is added, in 4 DEG C 5h is preserved, with filtered on buchner funnel, collect solid, add 500mL 3wt% acetic acid, add 5g vulcanized sodium, keep constant temperature 50 DEG C, 3h is soaked, filtering, collects solid, adds 500mL distilled water, keeps 50 DEG C of constant temperature, soaked 3h, filtering, collect filter Liquid, then handled by highly acidic cation exchange column, efflux is discarded, it is neutrality resin column to be washed with water to efflux, Then eluted using 0.3mol/L ammoniacal liquor, collect ammoniacal liquor eluent, be concentrated under reduced pressure into 100mL, add the anhydrous second of 800mL Alcohol, crystal is separated out, crystal is collected by filtration, be dried in vacuo 12h, produce.

The preparation method of the tuckahoe extracts is：By 300g Poria cocos grinds, add distilled water and be heated to reflux 3 times, often Secondary addition distilled water 600mL, each return time is 3h, filtering, merging filtrate, is evaporated under reduced pressure solution being concentrated into 300mL, then 800mL absolute ethyl alcohols are added, stand 24h, filtrate is collected in filtering, then distillation under pressure passes through Zerolie 225 to without ethanol Strong acid ion exchange resin, efflux is discarded, it is neutrality resin column to be washed with water to efflux, then using 0.5mol/L ammonia Water is eluted, and collects eluent, is concentrated under reduced pressure into 50mL, is stood 24h, filtering, is collected solid, is dried in vacuo 12h, produces.

The preparation method of fruit of Rangoon creeper's extract is：The 200g fruits of Rangoon creeper are taken, are cleaned, grinds, add the anhydrous second of 800mL Ether, 5h is heated to reflux, cooled and filtered, filtrate is collected, is evaporated under reduced pressure to 100mL, 48h is stood at 4 DEG C, is then collected by filtration Solid, 12h is dried in vacuo, is produced.

The preparation method of the chrysanthemum extract is：Chrysanthemum 500g is taken, is cleaned, grinds, adds 3000mL absolute ethyl alcohols, 12h is heated to reflux, filters, filtrate decompression is distilled, volume concentration to 200mL, 500mL distilled water is added, after stirring 500mL n-butanols are added, liquid separation, collect butanol solution, is evaporated under reduced pressure, by volume concentration to 200mL, adds 2000mL Absolute ether, there is white precipitate, filter, be dried in vacuo 5h, obtain white solid, white solid is dissolved in the anhydrous second of 700mL Alcohol, 50mL 10wt% hydrochloric acid is added, be heated to reflux 5h, 200mL is concentrated into after cooling, add 1000mL distilled water, mistake Filter, remove precipitation, collect filtrate, 12g activated carbons are added in filtrate, heating water bath 30min, filtering, filtrate is collected, is concentrated into 50mL, 500mL absolute methanols are added, 5h is placed at -18 DEG C, separated out flake-like crystal, crystal is collected by filtration, be dried in vacuo 12h, produce.

The preparation method of the Shitake Mushroom P.E is：300g mushrooms are taken, grinds, 500mL0.5mol/ are added dropwise under ice bath L NaOH, after being added dropwise, continue to stir 3h under ice bath, then filter, collect filtrate, add glacial acetic acid to pH=8, occur Precipitation, is washed with 30mL acetone, is then washed with 30mL ether, add 500mL distilled water, after stirring, added 500mL dimethyl sulfoxides, are precipitated, and precipitation is collected by filtration, and are washed with 30mL acetone, are dried in vacuo 3h, are produced.

The preparation method of the perilla leaf extract is：Perilla leaf 500g is taken, grinds, 2000mL distilled water is added, adds Heat stirs 3h, is cooled to room temperature to 80 DEG C, filters, and 200mL 3wt% calcium chloride solution is added into filtrate, stands 24h, Filtering, concentrates the filtrate to 50mL, then adds saturation ammoniacal liquor to pH=7.2, adds 50mL tetrahydrofurans, liquid separation, collect Water layer, 12h is dried in vacuo, is produced.

Embodiment 2

Plant base electro-coppering sewage demulsifier, in parts by weight, including 14 parts of isatis root extract, 8 parts of tuckahoe extracts, 10 parts of fruit of Rangoon creeper's extract, 8 parts of chrysanthemum extract, 8 parts of Shitake Mushroom P.E, 10 parts of perilla leaf extract, 10 parts of mint extract, 100 parts of water.

The preparation method of the isatis root extract is：400g Radix Isatidis is cleaned, grinds, 1000mL benzene is added, in 4 DEG C 5h is preserved, with filtered on buchner funnel, collect solid, add 500mL 3wt% acetic acid, add 5g vulcanized sodium, keep constant temperature 50 DEG C, 3h is soaked, filtering, collects solid, adds 500mL distilled water, keeps 50 DEG C of constant temperature, soaked 3h, filtering, collect filter Liquid, then handled by highly acidic cation exchange column, efflux is discarded, it is neutrality resin column to be washed with water to efflux, Then eluted using 0.3mol/L ammoniacal liquor, collect ammoniacal liquor eluent, be concentrated under reduced pressure into 100mL, add the anhydrous second of 800mL Alcohol, crystal is separated out, crystal is collected by filtration, be dried in vacuo 12h, produce.

The preparation method of the tuckahoe extracts is：By 300g Poria cocos grinds, add distilled water and be heated to reflux 3 times, often Secondary addition distilled water 600mL, each return time is 3h, filtering, merging filtrate, is evaporated under reduced pressure solution being concentrated into 300mL, then 800mL absolute ethyl alcohols are added, stand 24h, filtrate is collected in filtering, then distillation under pressure passes through Zerolie 225 to without ethanol Strong acid ion exchange resin, efflux is discarded, it is neutrality resin column to be washed with water to efflux, then using 0.5mol/L ammonia Water is eluted, and collects eluent, is concentrated under reduced pressure into 50mL, is stood 24h, filtering, is collected solid, is dried in vacuo 12h, produces.

The preparation method of fruit of Rangoon creeper's extract is：The 200g fruits of Rangoon creeper are taken, are cleaned, grinds, add the anhydrous second of 800mL Ether, 5h is heated to reflux, cooled and filtered, filtrate is collected, is evaporated under reduced pressure to 100mL, 48h is stood at 4 DEG C, is then collected by filtration Solid, 12h is dried in vacuo, is produced.

The preparation method of the chrysanthemum extract is：Chrysanthemum 500g is taken, is cleaned, grinds, adds 3000mL absolute ethyl alcohols, 12h is heated to reflux, filters, filtrate decompression is distilled, volume concentration to 200mL, 500mL distilled water is added, after stirring 500mL n-butanols are added, liquid separation, collect butanol solution, is evaporated under reduced pressure, by volume concentration to 200mL, adds 2000mL Absolute ether, there is white precipitate, filter, be dried in vacuo 5h, obtain white solid, white solid is dissolved in the anhydrous second of 700mL Alcohol, 50mL 10wt% hydrochloric acid is added, be heated to reflux 5h, 200mL is concentrated into after cooling, add 1000mL distilled water, mistake Filter, remove precipitation, collect filtrate, 12g activated carbons are added in filtrate, heating water bath 30min, filtering, filtrate is collected, is concentrated into 50mL, 500mL absolute methanols are added, 5h is placed at -18 DEG C, separated out flake-like crystal, crystal is collected by filtration, be dried in vacuo 12h, produce.

The preparation method of the Shitake Mushroom P.E is：300g mushrooms are taken, grinds, 500mL0.5mol/ are added dropwise under ice bath L NaOH, after being added dropwise, continue to stir 3h under ice bath, then filter, collect filtrate, add glacial acetic acid to pH=8, occur Precipitation, is washed with 30mL acetone, is then washed with 30mL ether, add 500mL distilled water, after stirring, added 500mL dimethyl sulfoxides, are precipitated, and precipitation is collected by filtration, and are washed with 30mL acetone, are dried in vacuo 3h, are produced.

The preparation method of the perilla leaf extract is：Perilla leaf 500g is taken, grinds, 2000mL distilled water is added, adds Heat stirs 3h, is cooled to room temperature to 80 DEG C, filters, and 200mL 3wt% calcium chloride solution is added into filtrate, stands 24h, Filtering, concentrates the filtrate to 50mL, then adds saturation ammoniacal liquor to pH=7.2, adds 50mL tetrahydrofurans, liquid separation, collect Water layer, 12h is dried in vacuo, is produced.

The preparation method of the mint extract is：Take peppermint 500g, grinds, using supercritical CO₂Extraction, collect extraction Thing is taken, then carries out normal pressure fractionation, 200-220 DEG C of cut is collected, produces.

Embodiment 3

Plant base electro-coppering sewage demulsifier, in parts by weight, including 14 parts of isatis root extract, 8 parts of tuckahoe extracts, 10 parts of fruit of Rangoon creeper's extract, 8 parts of chrysanthemum extract, 8 parts of Shitake Mushroom P.E, 10 parts of perilla leaf extract, 100 parts of water.

The preparation method of the isatis root extract is：400g Radix Isatidis is cleaned, grinds, 1000mL benzene is added, in 4 DEG C 5h is preserved, with filtered on buchner funnel, collect solid, add 500mL 3wt% acetic acid, keep 50 DEG C of constant temperature, soak 3h, mistake Filter, solid is collected, add 500mL distilled water, keep 50 DEG C of constant temperature, soaked 3h, filtering, collect filtrate, then pass through highly acid Cation exchange column is handled, and discards efflux, and it is neutrality resin column to be washed with water to efflux, then using 0.3mol/L Ammoniacal liquor is eluted, and is collected ammoniacal liquor eluent, is concentrated under reduced pressure into 100mL, adds 800mL absolute ethyl alcohols, separates out crystal, filtering Crystal is collected, 12h is dried in vacuo, produces.

The preparation method of the tuckahoe extracts is：By 300g Poria cocos grinds, add distilled water and be heated to reflux 3 times, often Secondary addition distilled water 600mL, each return time is 3h, filtering, merging filtrate, is evaporated under reduced pressure solution being concentrated into 300mL, then 800mL absolute ethyl alcohols are added, stand 24h, filtrate is collected in filtering, then distillation under pressure passes through Zerolie 225 to without ethanol Strong acid ion exchange resin, efflux is discarded, it is neutrality resin column to be washed with water to efflux, then using 0.5mol/L ammonia Water is eluted, and collects eluent, is concentrated under reduced pressure into 50mL, is stood 24h, filtering, is collected solid, is dried in vacuo 12h, produces.

The preparation method of fruit of Rangoon creeper's extract is：The 200g fruits of Rangoon creeper are taken, are cleaned, grinds, add the anhydrous second of 800mL Ether, 5h is heated to reflux, cooled and filtered, filtrate is collected, is evaporated under reduced pressure to 100mL, 48h is stood at 4 DEG C, is then collected by filtration Solid, 12h is dried in vacuo, is produced.

The preparation method of the chrysanthemum extract is：Chrysanthemum 500g is taken, is cleaned, grinds, adds 3000mL absolute ethyl alcohols, 12h is heated to reflux, filters, filtrate decompression is distilled, volume concentration to 200mL, 500mL distilled water is added, after stirring 500mL n-butanols are added, liquid separation, collect butanol solution, is evaporated under reduced pressure, by volume concentration to 200mL, adds 2000mL Absolute ether, there is white precipitate, filter, be dried in vacuo 5h, obtain white solid, white solid is dissolved in the anhydrous second of 700mL Alcohol, 50mL 10wt% hydrochloric acid is added, be heated to reflux 5h, 200mL is concentrated into after cooling, add 1000mL distilled water, mistake Filter, remove precipitation, collect filtrate, 12g activated carbons are added in filtrate, heating water bath 30min, filtering, filtrate is collected, is concentrated into 50mL, 500mL absolute methanols are added, 5h is placed at -18 DEG C, separated out flake-like crystal, crystal is collected by filtration, be dried in vacuo 12h, produce.

The preparation method of the Shitake Mushroom P.E is：300g mushrooms are taken, grinds, 500mL0.5mol/ are added dropwise under ice bath L NaOH, after being added dropwise, continue to stir 3h under ice bath, then filter, collect filtrate, add glacial acetic acid to pH=8, occur Precipitation, is washed with 30mL acetone, is then washed with 30mL ether, add 500mL distilled water, after stirring, added 500mL dimethyl sulfoxides, are precipitated, and precipitation is collected by filtration, and are washed with 30mL acetone, are dried in vacuo 3h, are produced.

The preparation method of the perilla leaf extract is：Perilla leaf 500g is taken, grinds, 2000mL distilled water is added, adds Heat stirs 3h, is cooled to room temperature to 80 DEG C, filters, and 200mL 3wt% calcium chloride solution is added into filtrate, stands 24h, Filtering, concentrates the filtrate to 50mL, then adds saturation ammoniacal liquor to pH=7.2, adds 50mL tetrahydrofurans, liquid separation, collect Water layer, 12h is dried in vacuo, is produced.

Embodiment 4

Plant base electro-coppering sewage demulsifier, in parts by weight, including 14 parts of isatis root extract, 8 parts of tuckahoe extracts, 10 parts of fruit of Rangoon creeper's extract, 8 parts of chrysanthemum extract, 8 parts of Shitake Mushroom P.E, 10 parts of perilla leaf extract, 100 parts of water.

The preparation method of the isatis root extract is：400g Radix Isatidis is cleaned, grinds, 1000mL benzene is added, in 4 DEG C 5h is preserved, with filtered on buchner funnel, collect solid, add 500mL 3wt% acetic acid, add 5g vulcanized sodium, keep constant temperature 50 DEG C, 3h is soaked, filtering, collects solid, adds 500mL distilled water, keeps 50 DEG C of constant temperature, soaked 3h, filtering, collect filter Liquid, then handled by highly acidic cation exchange column, efflux is discarded, it is neutrality resin column to be washed with water to efflux, Then eluted using 0.3mol/L ammoniacal liquor, collect ammoniacal liquor eluent, be concentrated under reduced pressure into 100mL, add the anhydrous second of 800mL Alcohol, crystal is separated out, crystal is collected by filtration, be dried in vacuo 12h, produce.

The preparation method of the tuckahoe extracts is：By 300g Poria cocos grinds, add distilled water and be heated to reflux 3 times, often Secondary addition distilled water 600mL, each return time is 3h, filtering, merging filtrate, is evaporated under reduced pressure solution being concentrated into 300mL, then 800mL absolute ethyl alcohols are added, stand 24h, filtrate is collected in filtering, then distillation under pressure passes through Zerolie 225 to without ethanol Strong acid ion exchange resin, efflux is discarded, it is neutrality resin column to be washed with water to efflux, then using 0.5mol/L ammonia Water is eluted, and collects eluent, is concentrated under reduced pressure into 50mL, is stood 24h, filtering, is collected solid, is dried in vacuo 12h, produces.

The preparation method of fruit of Rangoon creeper's extract is：The 200g fruits of Rangoon creeper are taken, are cleaned, grinds, add the anhydrous second of 800mL Ether, 5h is heated to reflux, cooled and filtered, filtrate is collected, is evaporated under reduced pressure to 100mL, 48h is stood at 4 DEG C, is then collected by filtration Solid, 12h is dried in vacuo, is produced.

The preparation method of the chrysanthemum extract is：Chrysanthemum 500g is taken, is cleaned, grinds, adds 3000mL absolute ethyl alcohols, 12h is heated to reflux, filters, filtrate decompression is distilled, volume concentration to 200mL, 500mL distilled water is added, after stirring 500mL n-butanols are added, liquid separation, collect butanol solution, is evaporated under reduced pressure, by volume concentration to 200mL, adds 2000mL Absolute ether, there is white precipitate, filter, be dried in vacuo 5h, obtain white solid, white solid is dissolved in the anhydrous second of 700mL Alcohol, 50mL 10wt% hydrochloric acid is added, be heated to reflux 5h, 200mL is concentrated into after cooling, add 1000mL distilled water, mistake Filter, remove precipitation, collect filtrate, 12g activated carbons are added in filtrate, heating water bath 30min, filtering, filtrate is collected, is concentrated into 50mL, 500mL absolute methanols are added, 5h is placed at -18 DEG C, separated out flake-like crystal, crystal is collected by filtration, be dried in vacuo 12h, produce.

The preparation method of the Shitake Mushroom P.E is：300g mushrooms are taken, grinds, 500mL0.5mol/ are added dropwise under ice bath L NaOH, after being added dropwise, continue to stir 3h under ice bath, then filter, collect filtrate, add glacial acetic acid to pH=8, occur Precipitation, is washed with 30mL acetone, is then washed with 30mL ether, add 500mL distilled water, after stirring, added 500mL dimethyl sulfoxides, are precipitated, and precipitation is collected by filtration, and are washed with 30mL acetone, are dried in vacuo 3h, are produced.

The preparation method of the perilla leaf extract is：Perilla leaf 500g is taken, grinds, 2000mL distilled water is added, adds Heat stirs 3h, is cooled to room temperature to 80 DEG C, filters, and 200mL 3wt% calcium chloride solution is added into filtrate, stands 24h, Filtering, concentrates the filtrate to 50mL, then addition saturation ammoniacal liquor to pH=7.2, adds 50mL chloroforms, liquid separation, collects water layer, 12h is dried in vacuo, is produced.

Embodiment 5

Plant base electro-coppering sewage demulsifier, in parts by weight, including 14 parts of isatis root extract, 8 parts of tuckahoe extracts, 8 parts of chrysanthemum extract, 8 parts of Shitake Mushroom P.E, 10 parts of perilla leaf extract, 100 parts of water.

The preparation method of the isatis root extract is：400g Radix Isatidis is cleaned, grinds, 1000mL benzene is added, in 4 DEG C 5h is preserved, with filtered on buchner funnel, collect solid, add 500mL 3wt% acetic acid, add 5g vulcanized sodium, keep constant temperature 50 DEG C, 3h is soaked, filtering, collects solid, adds 500mL distilled water, keeps 50 DEG C of constant temperature, soaked 3h, filtering, collect filter Liquid, then handled by highly acidic cation exchange column, efflux is discarded, it is neutrality resin column to be washed with water to efflux, Then eluted using 0.3mol/L ammoniacal liquor, collect ammoniacal liquor eluent, be concentrated under reduced pressure into 100mL, add the anhydrous second of 800mL Alcohol, crystal is separated out, crystal is collected by filtration, be dried in vacuo 12h, produce.

The preparation method of the tuckahoe extracts is：By 300g Poria cocos grinds, add distilled water and be heated to reflux 3 times, often Secondary addition distilled water 600mL, each return time is 3h, filtering, merging filtrate, is evaporated under reduced pressure solution being concentrated into 300mL, then 800mL absolute ethyl alcohols are added, stand 24h, filtrate is collected in filtering, then distillation under pressure passes through Zerolie 225 to without ethanol Strong acid ion exchange resin, efflux is discarded, it is neutrality resin column to be washed with water to efflux, then using 0.5mol/L ammonia Water is eluted, and collects eluent, is concentrated under reduced pressure into 50mL, is stood 24h, filtering, is collected solid, is dried in vacuo 12h, produces.

The preparation method of the chrysanthemum extract is：Chrysanthemum 500g is taken, is cleaned, grinds, adds 3000mL absolute ethyl alcohols, 12h is heated to reflux, filters, filtrate decompression is distilled, volume concentration to 200mL, 500mL distilled water is added, after stirring 500mL n-butanols are added, liquid separation, collect butanol solution, is evaporated under reduced pressure, by volume concentration to 200mL, adds 2000mL Absolute ether, there is white precipitate, filter, be dried in vacuo 5h, obtain white solid, white solid is dissolved in the anhydrous second of 700mL Alcohol, 50mL 10wt% hydrochloric acid is added, be heated to reflux 5h, 200mL is concentrated into after cooling, add 1000mL distilled water, mistake Filter, remove precipitation, collect filtrate, 12g activated carbons are added in filtrate, heating water bath 30min, filtering, filtrate is collected, is concentrated into 50mL, 500mL absolute methanols are added, 5h is placed at -18 DEG C, separated out flake-like crystal, crystal is collected by filtration, be dried in vacuo 12h, produce.

The preparation method of the Shitake Mushroom P.E is：300g mushrooms are taken, grinds, 500mL0.5mol/ are added dropwise under ice bath L NaOH, after being added dropwise, continue to stir 3h under ice bath, then filter, collect filtrate, add glacial acetic acid to pH=8, occur Precipitation, is washed with 30mL acetone, is then washed with 30mL ether, add 500mL distilled water, after stirring, added 500mL dimethyl sulfoxides, are precipitated, and precipitation is collected by filtration, and are washed with 30mL acetone, are dried in vacuo 3h, are produced.

The preparation method of the perilla leaf extract is：Perilla leaf 500g is taken, grinds, 2000mL distilled water is added, adds Heat stirs 3h, is cooled to room temperature to 80 DEG C, filters, and 200mL 3wt% calcium chloride solution is added into filtrate, stands 24h, Filtering, concentrates the filtrate to 50mL, then adds saturation ammoniacal liquor to pH=7.2, adds 50mL tetrahydrofurans, liquid separation, collect Water layer, 12h is dried in vacuo, is produced.

Embodiment 6

Plant base electro-coppering sewage demulsifier, in parts by weight, including 8 parts of tuckahoe extracts, 10 parts of fruit of Rangoon creeper's extract, 8 parts of chrysanthemum extract, 8 parts of Shitake Mushroom P.E, 10 parts of perilla leaf extract, 100 parts of water.

The preparation method of the tuckahoe extracts is：By 300g Poria cocos grinds, add distilled water and be heated to reflux 3 times, often Secondary addition distilled water 600mL, each return time is 3h, filtering, merging filtrate, is evaporated under reduced pressure solution being concentrated into 300mL, then 800mL absolute ethyl alcohols are added, stand 24h, filtrate is collected in filtering, then distillation under pressure passes through Zerolie 225 to without ethanol Strong acid ion exchange resin, efflux is discarded, it is neutrality resin column to be washed with water to efflux, then using 0.5mol/L ammonia Water is eluted, and collects eluent, is concentrated under reduced pressure into 50mL, is stood 24h, filtering, is collected solid, is dried in vacuo 12h, produces.

The preparation method of fruit of Rangoon creeper's extract is：The 200g fruits of Rangoon creeper are taken, are cleaned, grinds, add the anhydrous second of 800mL Ether, 5h is heated to reflux, cooled and filtered, filtrate is collected, is evaporated under reduced pressure to 100mL, 48h is stood at 4 DEG C, is then collected by filtration Solid, 12h is dried in vacuo, is produced.

The preparation method of the chrysanthemum extract is：Chrysanthemum 500g is taken, is cleaned, grinds, adds 3000mL absolute ethyl alcohols, 12h is heated to reflux, filters, filtrate decompression is distilled, volume concentration to 200mL, 500mL distilled water is added, after stirring 500mL n-butanols are added, liquid separation, collect butanol solution, is evaporated under reduced pressure, by volume concentration to 200mL, adds 2000mL Absolute ether, there is white precipitate, filter, be dried in vacuo 5h, obtain white solid, white solid is dissolved in the anhydrous second of 700mL Alcohol, 50mL 10wt% hydrochloric acid is added, be heated to reflux 5h, 200mL is concentrated into after cooling, add 1000mL distilled water, mistake Filter, remove precipitation, collect filtrate, 12g activated carbons are added in filtrate, heating water bath 30min, filtering, filtrate is collected, is concentrated into 50mL, 500mL absolute methanols are added, 5h is placed at -18 DEG C, separated out flake-like crystal, crystal is collected by filtration, be dried in vacuo 12h, produce.

The preparation method of the Shitake Mushroom P.E is：300g mushrooms are taken, grinds, 500mL0.5mol/ are added dropwise under ice bath L NaOH, after being added dropwise, continue to stir 3h under ice bath, then filter, collect filtrate, add glacial acetic acid to pH=8, occur Precipitation, is washed with 30mL acetone, is then washed with 30mL ether, add 500mL distilled water, after stirring, added 500mL dimethyl sulfoxides, are precipitated, and precipitation is collected by filtration, and are washed with 30mL acetone, are dried in vacuo 3h, are produced.

The preparation method of the perilla leaf extract is：Perilla leaf 500g is taken, grinds, 2000mL distilled water is added, adds Heat stirs 3h, is cooled to room temperature to 80 DEG C, filters, and 200mL 3wt% calcium chloride solution is added into filtrate, stands 24h, Filtering, concentrates the filtrate to 50mL, then adds saturation ammoniacal liquor to pH=7.2, adds 50mL tetrahydrofurans, liquid separation, collect Water layer, 12h is dried in vacuo, is produced.

Embodiment 7

Plant base electro-coppering sewage demulsifier, in parts by weight, including 14 parts of isatis root extract, 8 parts of tuckahoe extracts, 10 parts of fruit of Rangoon creeper's extract, 8 parts of chrysanthemum extract, 8 parts of Shitake Mushroom P.E, 100 parts of water.

The preparation method of the isatis root extract is：400g Radix Isatidis is cleaned, grinds, 1000mL benzene is added, in 4 DEG C 5h is preserved, with filtered on buchner funnel, collect solid, add 500mL 3wt% acetic acid, add 5g vulcanized sodium, keep constant temperature 50 DEG C, 3h is soaked, filtering, collects solid, adds 500mL distilled water, keeps 50 DEG C of constant temperature, soaked 3h, filtering, collect filter Liquid, then handled by highly acidic cation exchange column, efflux is discarded, it is neutrality resin column to be washed with water to efflux, Then eluted using 0.3mol/L ammoniacal liquor, collect ammoniacal liquor eluent, be concentrated under reduced pressure into 100mL, add the anhydrous second of 800mL Alcohol, crystal is separated out, crystal is collected by filtration, be dried in vacuo 12h, produce.

The preparation method of the tuckahoe extracts is：By 300g Poria cocos grinds, add distilled water and be heated to reflux 3 times, often Secondary addition distilled water 600mL, each return time is 3h, filtering, merging filtrate, is evaporated under reduced pressure solution being concentrated into 300mL, then 800mL absolute ethyl alcohols are added, stand 24h, filtrate is collected in filtering, then distillation under pressure passes through Zerolie 225 to without ethanol Strong acid ion exchange resin, efflux is discarded, it is neutrality resin column to be washed with water to efflux, then using 0.5mol/L ammonia Water is eluted, and collects eluent, is concentrated under reduced pressure into 50mL, is stood 24h, filtering, is collected solid, is dried in vacuo 12h, produces.

The preparation method of fruit of Rangoon creeper's extract is：The 200g fruits of Rangoon creeper are taken, are cleaned, grinds, add the anhydrous second of 800mL Ether, 5h is heated to reflux, cooled and filtered, filtrate is collected, is evaporated under reduced pressure to 100mL, 48h is stood at 4 DEG C, is then collected by filtration Solid, 12h is dried in vacuo, is produced.

The preparation method of the chrysanthemum extract is：Chrysanthemum 500g is taken, is cleaned, grinds, adds 3000mL absolute ethyl alcohols, 12h is heated to reflux, filters, filtrate decompression is distilled, volume concentration to 200mL, 500mL distilled water is added, after stirring 500mL n-butanols are added, liquid separation, collect butanol solution, is evaporated under reduced pressure, by volume concentration to 200mL, adds 2000mL Absolute ether, there is white precipitate, filter, be dried in vacuo 5h, obtain white solid, white solid is dissolved in the anhydrous second of 700mL Alcohol, 50mL 10wt% hydrochloric acid is added, be heated to reflux 5h, 200mL is concentrated into after cooling, add 1000mL distilled water, mistake Filter, remove precipitation, collect filtrate, 12g activated carbons are added in filtrate, heating water bath 30min, filtering, filtrate is collected, is concentrated into 50mL, 500mL absolute methanols are added, 5h is placed at -18 DEG C, separated out flake-like crystal, crystal is collected by filtration, be dried in vacuo 12h, produce.

The preparation method of the Shitake Mushroom P.E is：300g mushrooms are taken, grinds, 500mL0.5mol/ are added dropwise under ice bath L NaOH, after being added dropwise, continue to stir 3h under ice bath, then filter, collect filtrate, add glacial acetic acid to pH=8, occur Precipitation, is washed with 30mL acetone, is then washed with 30mL ether, add 500mL distilled water, after stirring, added 500mL dimethyl sulfoxides, are precipitated, and precipitation is collected by filtration, and are washed with 30mL acetone, are dried in vacuo 3h, are produced.

Demulsification performance is tested

Configuration 1000mL contains NPE 400ppm, and the copper ion 50ppm aqueous solution is as testing sample. 20mL embodiment 1-7 are separately added into testing sample, 30min is stirred, then stands 5min, take oil reservoir solution, with efficient liquid Phase chromatogram characterizes the content of the NPE in oil reservoir solution, is designated as S1, and elimination efficiency w1=S1/400 × 100%.Embodiment 1-7 is opened wide in 25 DEG C and placed 3 days, then takes 20mL to be added in testing sample respectively, stirs 30min, so After stand 5min, take oil reservoir solution, with high performance liquid chromatography characterize oil reservoir solution in NPE content, note For S2, elimination efficiency w2=S2/400 × 100%.Test result is listed in the table below.

Foregoing example is merely illustrative, for explaining some features of the present invention.Appended claim is intended to The scope as wide as possible being contemplated that is sought, and embodiments as presented herein is only the combination according to all possible embodiment Selection embodiment explanation.Therefore, the purpose of applicant is appended claim not by the feature of the explanation present invention Example selectional restriction.And the progress in science and technology will be formed due to the inaccuracy of language performance it is not current The possible equivalent or son considered is replaced, and these changes should also be interpreted to be wanted by appended right in the conceived case Ask covering.

Claims (10)

1. plant base electro-coppering sewage demulsifier, it is characterised in that including at least isatis root extract, tuckahoe extracts, make monarch Seed extract, chrysanthemum extract, Shitake Mushroom P.E, perilla leaf extract, water.

2. plant base electro-coppering sewage demulsifier as claimed in claim 1, it is characterised in that in parts by weight, comprise at least 14 parts of isatis root extract, 8 parts of tuckahoe extracts, 10 parts of fruit of Rangoon creeper's extract, 8 parts of chrysanthemum extract, 8 parts of Shitake Mushroom P.E, 10 parts of perilla leaf extract, 100 parts of water.

3. plant base electro-coppering sewage demulsifier as claimed in claim 1, it is characterised in that the system of the isatis root extract Preparation Method is：400g Radix Isatidis is cleaned, grinds, add 1000mL benzene, 5h is preserved in 4 DEG C, with filtered on buchner funnel, collected Solid, 500mL 3wt% acetic acid is added, add 5g vulcanized sodium, keep 50 DEG C of constant temperature, soaked 3h, filtering, collect solid, then 500mL distilled water is added, keeps 50 DEG C of constant temperature, 3h is soaked, filtering, collects filtrate, then enter by highly acidic cation exchange column Row processing, discards efflux, and it is neutrality resin column to be washed with water to efflux, is then eluted using 0.3mol/L ammoniacal liquor, Ammoniacal liquor eluent is collected, is concentrated under reduced pressure into 100mL, adds 800mL absolute ethyl alcohols, crystal is separated out, crystal, vacuum is collected by filtration 12h is dried, is produced.

4. plant base electro-coppering sewage demulsifier as claimed in claim 1, it is characterised in that the preparation of the tuckahoe extracts Method is：By 300g Poria cocos grinds, add distilled water and be heated to reflux 3 times, distilled water 600mL is added every time, when flowing back every time Between be 3h, filtering, merging filtrate, be evaporated under reduced pressure and solution be concentrated into 300mL, add 800mL absolute ethyl alcohols, stand 24h, mistake Filter, collects filtrate, and distillation under pressure, then by the strong acid ion exchange resins of Zerolie 225, discards outflow to without ethanol Liquid, it is neutrality resin column to be washed with water to efflux, is then eluted using 0.5mol/L ammoniacal liquor, collects eluent, decompression 50mL is concentrated into, 24h is stood, filtering, collects solid, be dried in vacuo 12h, produce.

5. plant base electro-coppering sewage demulsifier as claimed in claim 1, it is characterised in that the system of fruit of Rangoon creeper's extract Preparation Method is：The 200g fruits of Rangoon creeper are taken, are cleaned, grinds, add 800mL absolute ethers, 5h is heated to reflux, cooled and filtered, receives Collect filtrate, be evaporated under reduced pressure to 100mL, 48h is stood at 4 DEG C, solid is then collected by filtration, be dried in vacuo 12h, produce.

6. plant base electro-coppering sewage demulsifier as claimed in claim 1, it is characterised in that the preparation of the chrysanthemum extract Method is：Chrysanthemum 500g is taken, is cleaned, grinds, 3000mL absolute ethyl alcohols is added, is heated to reflux 12h, is filtered, by filtrate decompression Distillation, volume concentration to 200mL, adds 500mL distilled water, and 500mL n-butanols are added after stirring, liquid separation, are collected Butanol solution, it is evaporated under reduced pressure, by volume concentration to 200mL, adds 2000mL absolute ethers, white precipitate occur, filters, 5h is dried in vacuo, white solid is obtained, white solid is dissolved in 700mL absolute ethyl alcohols, add 50mL 10wt% hydrochloric acid, add Heat backflow 5h, is concentrated into 200mL after cooling, adds 1000mL distilled water, filter, remove precipitation, filtrate is collected, in filtrate 12g activated carbons are added, heating water bath 30min, filtering, filtrate is collected, is concentrated into 50mL, adds 500mL absolute methanols ,- 5h is placed at 18 DEG C, separates out flake-like crystal, crystal is collected by filtration, 12h is dried in vacuo, produces.

7. plant base electro-coppering sewage demulsifier as claimed in claim 1, it is characterised in that the preparation of the Shitake Mushroom P.E Method is：300g mushrooms are taken, grinds, 500mL 0.5mol/L NaOH are added dropwise under ice bath, after being added dropwise, under ice bath Continue to stir 3h, then filter, collect filtrate, add glacial acetic acid to pH=8, precipitate, washed with 30mL acetone, Ran Houyong 30mL ether is washed, and adds 500mL distilled water, after stirring, adds 500mL dimethyl sulfoxides, precipitate, and filtering is received Collection precipitation, is washed with 30mL acetone, is dried in vacuo 3h, is produced.

8. plant base electro-coppering sewage demulsifier as claimed in claim 2, it is characterised in that also including mint extract 10 Part.

9. plant base electro-coppering sewage demulsifier as claimed in claim 8, it is characterised in that the preparation of the mint extract Method is：Take peppermint 500g, grinds, using supercritical CO₂Extraction, extract is collected, then carry out normal pressure fractionation, collected 200-220 DEG C of cut, is produced.

10. the plant base electro-coppering sewage demulsifier as described in any one of claim 1-9 claim, it is characterised in that The plant base electro-coppering sewage demulsifier is used for the sewage containing NPE.