CN107364906A - A kind of environment protection sewage inorganic agent - Google Patents

A kind of environment protection sewage inorganic agent Download PDF

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CN107364906A
CN107364906A CN201710683958.9A CN201710683958A CN107364906A CN 107364906 A CN107364906 A CN 107364906A CN 201710683958 A CN201710683958 A CN 201710683958A CN 107364906 A CN107364906 A CN 107364906A
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parts
collected
filtrate
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CN107364906B (en
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王婧宁
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Shanghai Borunke Biotechnology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage

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Abstract

A kind of environment protection sewage inorganic agent, in parts by weight, its preparing raw material includes：8 12 parts of xylotriose, 46 parts of xylobiose, 25 35 parts of Honegsukle flower P.E, 28 32 parts of nutgall extractive, 8 12 parts of Radix Aristolochiae extract, 20 30 parts of licorice, 8 12 parts of Radix Gentianae extract, 300 parts of water.

Description

A kind of environment protection sewage inorganic agent
Technical field
The present invention relates to energy-conserving and environment-protective field, more particularly to a kind of environment protection sewage inorganic agent.
Background technology
NPE is with the nonionic table of nonyl phenol and the oxirane condensation reaction under catalyst action Face activating agent.There are a variety of hydrophilic lipophilic balances.Have been widely used in detergent/printing and dyeing/chemical industry.Polyoxyethylene nonyl phenyl The biodegradability of vinethene is very poor, after sewage effluent, into water body it is difficult to be decomposed by the Institute of Micro-biology of nature, for a long time all It can be present in water body, holding surface activity, foaming, influence dissolved oxygen, it is unfavorable to aquatile.At present for by nonyl phenol The processing method that the water body of APEO uses is mainly that activated carbon, resin adsorption method, and photocatalytic degradation and biology drop Solution.
The content of the invention
In order to solve prior art problem, the first aspect of the present invention provides a kind of environment protection sewage inorganic agent, with parts by weight Meter, its preparing raw material include：Xylotriose 8-12 parts, xylobiose 4-6 parts, Honegsukle flower P.E 25-35 parts, nutgall extractive 28-32 parts, Radix Aristolochiae extract 8-12 parts, licorice 20-30 parts, Radix Gentianae extract 8-12 parts, 300 parts of water.
In some embodiments, its preparing raw material also includes：20 parts of lichen extract.
In some embodiments, the preparation method of the Honegsukle flower P.E is：500g honeysuckles are cleaned, shredded, With 4000mL distilled water refluxing extraction 12h, after cooling, 400mL is concentrated into Rotary Evaporators, then adds saturation NaHCO3Water Solution, to pH=9, then 50mL 10wt% copper chloride solution is added dropwise, precipitates, precipitation is collected by filtration, then by precipitation point It is dispersed in 200mL acetone, adds 50mL 20wt% sulfuric acid under agitation, stirs 30min, filtering, collect filtrate, add Saturation NaHCO3Aqueous solution 50mL, it is evaporated under reduced pressure to without acetone, then add deionized water becomes to clarify to solution, transfers to In separatory funnel, 20mL ethyl acetate is added, 10wt% hydrochloric acid is added dropwise, colourless to lower floor, upper strata is faint yellow, is collected Upper solution, activated carbon 10g is added, stand 12h, filtering, 10mL is concentrated into Rotary Evaporators to filtrate, then adds dichloro Methane 20mL is extracted, and is evaporated extract, is dried in vacuo, is produced.
In some embodiments, the preparation method of the nutgall extractive is：500g Chinese galls are cleaned, dried, Grinds, 3000mL distilled water is added, constant temperature soaks 24h at 45 DEG C, filtering, filtrate then is cooled into 0-4 DEG C, adds 30g activated carbons stir 30min, filtering, and filtrate is collected by gel-type acrylic acid type cation exchange resin and exchanges liquid, with rotation Turn evaporimeter and be concentrated into 300mL, then add 1000mL hexanes, filtering, collect solid, be dried in vacuo 4h, produce.
In some embodiments, the preparation method of the Radix Aristolochiae extract is：300g dutchmanspipe roots are taken, are cleaned, chopping, 3000mL 65vol% ethanol is added, 500g caustic alcohols is added, is soaked at room temperature after stirring 3 days, is filtered, collects filter Liquid, concentrated with Rotary Evaporators, be concentrated into no ethanol, then place 12h at -18 DEG C, solid is collected by filtration, then will The solid being collected into is dissolved in 75 DEG C of distilled water, filters while hot, collects filtrate, naturally cools to room temperature, then in -18 DEG C of decentralizations 3h is put, is filtered, solid is collected, is washed 3 times with acetone, uses acetone 20mL every time, 4h is dried in vacuo, produces.
In some embodiments, the preparation method of the licorice is：500g radix glycyrrhizaes are cleaned, chopping, with steaming Distilled water refluxing extraction 3 times, 5000mL distilled water is used every time, collect extract solution, be concentrated into 1000mL with Rotary Evaporators, stirring The lower dropwise addition concentrated sulfuric acid is mixed, is precipitated, the concentrated sulfuric acid is added dropwise to precipitation is no longer separated out, precipitation is collected by filtration, is washed with acetone, vacuum 4h is dried, is produced.
In some embodiments, the preparation method of the Radix Gentianae extract is：300g rough gentian is cleaned, grinds, used Soaked in absolute ethyl alcohol 12h, filtrate is collected by filtration, then with 2000mL distilled water refluxing extraction 8h, cooled and filtered, into filtrate Addition ammonium sulfate is not redissolved up to ammonium sulfate, and filtrate is then collected by filtration, by dialysing and being freeze-dried, obtains solid, adopts Purified with column chromatography, stationary phase is deae dextran gel A-25 chromatographic columns, and cushioning liquid is dipotassium hydrogen phosphate and biphosphate Potassium, mobile phase are 3.5wt% sodium chloride solution, collect chromatographic solution, are concentrated into 500mL, add 20g cetyl trimethyls Ammonium bromide and 5mL5wt% hydrochloric acid, 20min is stirred, adds 2000mL 86vol% ethanol, obtain sediment, collect precipitation Thing, 12h is dried in vacuo, is produced.
In some embodiments, the preparation method of the lichen extract is：400g lichens are cleaned, grinds, then 2000mL acetone and 5mL triethylamines are added, refluxing extraction 12h, filtering, solid is discarded, filtrate is concentrated into Rotary Evaporators 500mL, 1500mL distilled water is added, stir 10min, precipitate, filtered, collected precipitation, tied again using acetone-ethanol Crystalline substance, solid is collected, be dried in vacuo 12h, produce.
In some embodiments, the environment protection sewage inorganic agent is used to remove NPE.
The second aspect of the present invention provides a kind of preparation method of environment protection sewage inorganic agent, comprises the following steps：With weight Part meter, xylotriose 8-12 parts, xylobiose 4-6 parts, 300 parts of water, nutgall extractive 28-32 parts are added in reactor, stirred 30min is mixed, is then heated to 85 DEG C, Radix Aristolochiae extract 8-12 parts is added, 1h is stirred at 85 DEG C, adds radix glycyrrhizae extraction Thing 20-30 parts, Honegsukle flower P.E 25-35 parts, 20 parts of lichen extract, 30min is stirred, be cooled to room temperature, added rough gentian and carry Thing 8-12 parts are taken, stirs, produces.
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.
The first aspect of the present invention provides a kind of environment protection sewage inorganic agent, and in parts by weight, its preparing raw material includes：Wood three Sugared 8-12 parts, xylobiose 4-6 parts, Honegsukle flower P.E 25-35 parts, nutgall extractive 28-32 parts, Radix Aristolochiae extract 8-12 Part, licorice 20-30 parts, Radix Gentianae extract 8-12 parts, 300 parts of water.
Xylobiose and xylotriose belong to xylo-oligosaccharide, about 155 DEG C of the fusing point of xylobiose, about 110 DEG C of the fusing point of xylotriose. Xylo-oligosaccharide is that to be gradually transformed into intramolecular hydrogen bond be mainly to make to predominant intermolecular forces from intermolecular hydrogen bonding with the increase of the degree of polymerization Firmly.Found during the inventor completion present invention, the weight ratio of xylotriose and xylobiose is 2：When 1, water treatment agent is being made It can possess appropriate viscosity during standby, improve each component, especially improve the Honegsukle flower P.E in the present invention Dispersion stabilization in system, so that the resting period of water treatment agent is longer.
In some embodiments, its preparing raw material also includes：20 parts of lichen extract.
Honeysuckle is caprifoliaceae plant honeysuckle Lonicera japonica Thunb., lonicera hypoglauca miq Lonicera Hypoglauca Miq., Honeysuckle flower (hair calyx honeysuckle) Lonicera confusa DC. or hair style honeysuckle Lonicera Dasystyla Rehd. dry flower or with the flower just opened.Nature and flavor are sweet, tremble with fear.Return lung, the heart, stomach.Major function heat-clearing solution Poison, wind-heat dissipating.For carbuncle swells furunculosis, larynx numbness, erysipelas, toxic-heat and blood stasis, anemopyretic cold, warm disease heating.Mainly contain chlorogenic acid (chlorogenic acid), isochlorogenic acid (isochlorogenic acid), gingko alcohol (ginnol), cupreol (β- Sitosterol), stigmasterol (stigmasterol), cupreol-D-Glucose glucoside (β-sitosteryl-D-gluco- Side), stigmasterol-D-Glucose glucoside (stigmasteryl-D-glucoside)；Also its composition containing volatile oil has linalool (linalool) it is, left-handed-along trimethyl -2- vinyl -5- dihydroxy-tetrahydros pyrans (cis-2,6,6-trimethyl-2- Vinyl-5-hydroxyte-trahydroxyran), ethyl palmitate (ethylpalmitater), 1,1- di- thiacyclohexane (1,1-bicyclohexyl), methyl linoleate (methylinoleate), 3- methyl -2- (2- pentenyls) -2- cyclopentene -1- Ketone [3-methyl-2- (- 2pentenyl)], trans- anti-fanesol (trans-trans-farnesol), ethyl linolenate (ethylli-nolenate), the clear casket oil alkene of β-Bi (β-cubebene), cis- 3- alkene -1- alcohol (cis-3-hex-en-1- Ol), alpha-terpineol (α-terpineol), Geraniol (geraniol), Ergol (benzylbenzoate), 2- first Base-butanol (2-methyl-1-butanol), phenmethylol (benzylalcohol), benzyl carbinol (phenethylalcohol), Cis- linalool oxide (cis-linalool oxide), Eugenol (eugenol) and carvacrol (carvacrol) etc..
In some embodiments, the preparation method of the Honegsukle flower P.E is：500g honeysuckles are cleaned, shredded, With 4000mL distilled water refluxing extraction 12h, after cooling, 400mL is concentrated into Rotary Evaporators, then adds saturation NaHCO3Water Solution, to pH=9, then 50mL 10wt% copper chloride solution is added dropwise, precipitates, precipitation is collected by filtration, then by precipitation point It is dispersed in 200mL acetone, adds 50mL 20wt% sulfuric acid under agitation, stirs 30min, filtering, collect filtrate, add Saturation NaHCO3Aqueous solution 50mL, it is evaporated under reduced pressure to without acetone, then add deionized water becomes to clarify to solution, transfers to In separatory funnel, 20mL ethyl acetate is added, 10wt% hydrochloric acid is added dropwise, colourless to lower floor, upper strata is faint yellow, is collected Upper solution, activated carbon 10g is added, stand 12h, filtering, 10mL is concentrated into Rotary Evaporators to filtrate, then adds dichloro Methane 20mL is extracted, and is evaporated extract, is dried in vacuo, is produced.
Chinese gall, it is Anacardiaceae plant Chinese sumac Rhus chinensis Mill., potanin sumac Rhus potaninii Or the worm on redpunjab sumac root Rhus pun-jabensis Stew.var.sinica (Diels) Rehd.et Wils. leaves Maxim. Goitre, mainly formed by melaphis chinensis Baker Melaphis chinensis (Bell) Baker parasitisms.Nature and flavor are sour, puckery, tremble with fear.It is return lung, big Intestines, kidney channel.Major function is astringed the lung fall fire, relieving diarrhea with astringents, arrest sweating hemostasis, hygroscopic sore.For chronic cough of deficiency lung, lung feverish cough, long Protracted dysentery is rushed down, night sweat, is quenched one's thirst, hemorrhoid blood of having blood in stool, traumatism and bleeding, carbuncle sore tumefacting virus, skin moisture fester.Mainly include：1,2,3,4,6- five-O- Galloyl-beta-D-glucose (1,2,3,4,6-pen-ta-O-galloyl- β-D-glucose), the nutgall acyls of 3-O- bis- Base -1,2, and 4,6- tetra--O- galloyl-beta-D-glucoses (3-O-digalloyl-1,2,4,6-tetra-O-galloyl- β-D-glucose), the galloyls -1,3 of 2-O- bis-, 4,6- tetra--O- galloyl-beta-D-glucoses (2-O- Digalloyl-1,3,4,6-tetra-O-galloyl- β-D-glucose), the galloyls -1,2 of 4-O- bis-, 3,6- tetra--O- Galloyl-beta-D-glucose (4-O-digal-oyl-1,2,3,6-tetra-O-galloyl- β-D-glucose), 2,3- Bis- galloyls of O--the Isosorbide-5-Nitrae ,-O- galloyl-beta-D-glucoses (2,3-bis-O-digalloyl-1,4,6- of 6- tri- Tri-O-galloyl- β-Dglucose), the galloyls -1,2 of 3-O- tri-, 4,6- tetra--O- galloyl-beta-D-glucoses (3-O-trigalloy-1,2,4,6-tetra-O-galloyl- β-D-glucose), 3,4- double galloyl -1 of-O- two, 2,6- tri--O- galloyl-beta-D-glucoses (3,4-bis-O-digalloyl-1,2,6-tri-O-galloyl- β-D- Glucose), the double galloyls -1,3 of-O- two of 2, the 4-,-O- galloyl-beta-D-glucoses (2,4-bis-O- of 6- tri- Digalloyl-1,3,6-O-g alloyl- β-D-glucose).
In some embodiments, the preparation method of the nutgall extractive is：500g Chinese galls are cleaned, dried, Grinds, 3000mL distilled water is added, constant temperature soaks 24h at 45 DEG C, filtering, filtrate then is cooled into 0-4 DEG C, adds 30g activated carbons stir 30min, filtering, and filtrate is collected by gel-type acrylic acid type cation exchange resin and exchanges liquid, with rotation Turn evaporimeter and be concentrated into 300mL, then add 1000mL hexanes, filtering, collect solid, be dried in vacuo 4h, produce.
Gel-type acrylic acid type cation exchange resin is 110 type gel-type acrylic acid series of Liaoyuan new material Co., Ltd Cationic ion-exchange resin.
Dutchmanspipe root, it is aristolochiaceae plant birthwort Aristolochia debilis Sieb.et Zucc. drying Root.Dutchmanspipe root includes aristolone, isoaristolone etc., in addition to luxuriant and rich with fragrance class, monoterpene, sequiterpene, alkaloid etc..Wherein, it is luxuriant and rich with fragrance Class compound such as aristolochic acid, including aristolochic acid A, Aristolochic acid B C, aristolochic acid C, aristolochic acid D, aristolochic acid E, 7- hydroxyl Base aristolochic acid A, 7-methoxy aristolochic acid A, 3,4- dimethoxy -6,8- dimethoxy -1- methyl esters are luxuriant and rich with fragrance, 3,4- diformazan Epoxide -6,8- dimethoxy -10- nitro -1- methyl esters phenanthrene, 6- methoxyl group aristolochic acids C, aristolochic acid A methyl esters, 6,8- dimethoxies Base aristolochic acid C etc..Sesquiterpenoids includes the sesquiterpenoid of four ring fusions, and the sequiterpene of three ring fusions Compound, such as nopinene, p-ymene, limonene, Cineole, methyl eugenol, aristolone, aristoloactone, horse pocket Bell alkene.Alkaloid includes magnoflorine, aporphine water soluble quaternary ammonium alkali, ring wheel rattan phenol alkali, allantoin, cupreol, carrot Glycosides, aristolo-lactam-N- hexose glycosides.
In some embodiments, the preparation method of the Radix Aristolochiae extract is：300g dutchmanspipe roots are taken, are cleaned, chopping, 3000mL 65vol% ethanol is added, 500g caustic alcohols is added, is soaked at room temperature after stirring 3 days, is filtered, collects filter Liquid, concentrated with Rotary Evaporators, be concentrated into no ethanol, then place 12h at -18 DEG C, solid is collected by filtration, then will The solid being collected into is dissolved in 75 DEG C of distilled water, filters while hot, collects filtrate, naturally cools to room temperature, then in -18 DEG C of decentralizations 3h is put, is filtered, solid is collected, is washed 3 times with acetone, uses acetone 20mL every time, 4h is dried in vacuo, produces.
After 3000mL 65vol% ethanol and the mixing of 500g caustic alcohols, the viscosity of solution becomes larger, and it is extremely strong to turn into alkalescence Thick liquid.The wall thickness of dutchmanspipe root relatively after, and with the material that dissolves is difficult to, it is in sticky ethanol/alcohol sodium solution It is easily damaged, cause other Related Component dissolutions, be unlikely to deteriorate the water treatment agent based on plant extracts, prevent microorganism Deng to rotten influence, raising resting period.
Radix glycyrrhizae is glycyrrhizic legume Glycyrrhiza uralensis Fisch., swollen fruit Radix Glycyrrhiza Inflata Bat. or glycyrrhiza glabra Glycyrrhiza glabra L. dry root.Spring, the excavation of season in autumn two, remove fibrous root, shine It is dry.Root is in cylinder, long 25~100cm, 0.6~3.5cm of diameter.Crust is elastic to differ.Surface rufous or taupe brown, tool are aobvious Vertical wrinkle, rill, hole skin and the sparse radicula trace.Matter is solid, and section shows slightly fibroid, yellow-white, mealiness, cambium ring Substantially, ray irradiation shape, some have crack.For rhizome in cylinder, there is bud scar on surface, has marrow in the middle part of section.Gas is micro-, sweet and special Very.It is distributed in the ground such as northeast, North China, Shaanxi, Gansu, Qinghai, Xinjiang, Shandong.With invigorating the spleen and benefiting qi, clearing heat and detoxicating, eliminating the phlegm stops Cough, relieving spasm to stop pain, the effect of coordinating the drug actions of a prescription.It is usually used in weakness of the spleen and the stomach, lassitude hypodynamia, palpitation, coughing with a lot of sputum, gastral cavity abdomen, four Limb contraction urgency pain, carbuncle sore tumefacting virus, alleviate drug toxicity, strong.Radix glycyrrhizae contains glycyrrhizin (glycyrrhizin), i.e. glycyrrhizic acid glycyrrhinic acid,C42H62O16) 6~14%, it is a kind of triterpenoid saponin for the sweet ingredient of radix glycyrrhizae.Glycyrrhizic acid hydrolyzes Produce a molecule enoxolone (glycyrrhetic acid i.e. glycyrrhetinic acid, C30H46O4) and two molecule grapes Uronic acid (glycuronic acid, C6H10O7).And (i.e. liquiritin liquiritin, C containing a small amount of liquiritin21H22O9, it is A kind of flavanols flavanone glucoside, its glucoside member name glycyrrhizin liquiritigenin, C15H12O4And glycyramarin Glycyamarin), isoliquiritin (iso-liquiritin, C21H24O9), dihydroxy enoxolone (dihydroxyglycyrrhetic acid are grabric acid, C30H46O5), licoricidin (licoricidin, C25H32O5, i.e. 3 ', 6- diisoamyl alkene -2 ', 4 ', 5- trihydroxies isoflavan), glycyrol (glycyrol, C21H18O6), 5-0- first Base glycyrol (5-0-methyl glycerol, C22H20O6), isoglycyrol (iso-glycyrol, C21H18O6), in addition, still containing Have mannitol (mannite), glucose 3.8%, sucrose 2.4~6.5%, malic acid, betulinic acid (betulicacid, C30H48O3), asparagine, Yan acid, life element (biotin, C10H16O3N2S) 296 micro- gram grams, trace volatile oil are that radix glycyrrhizae is peculiar The source of foul smell and starch etc..
In some embodiments, the preparation method of the licorice is：500g radix glycyrrhizaes are cleaned, chopping, with steaming Distilled water refluxing extraction 3 times, 5000mL distilled water is used every time, collect extract solution, be concentrated into 1000mL with Rotary Evaporators, stirring The lower dropwise addition concentrated sulfuric acid is mixed, is precipitated, the concentrated sulfuric acid is added dropwise to precipitation is no longer separated out, precipitation is collected by filtration, is washed with acetone, vacuum 4h is dried, is produced.
Rough gentian, Gentiana scabra Bunge, it is gentianaceae plant.Perennial herb is high 30-60 centimetres；Root is yellowish-white Color, cord-like are long more than 20 centimetres.Stem is upright, sturdy, and often band puce, coarse.Leaf is long to life, avette or ovum shape lanceolar It is 3-7 centimetres, wide 1-2 centimetres, there is 3-5 bar arteries and veins, anxious sharp or tapering, stockless, edge and following master pulse are coarse.Flowers give birth to stem end or leaf Armpit；Bract lanceolar, it is closely isometric with calyx；Calyx mitriform, long 2.5-3 centimetres, sliver strip lanceolar are closely isometric with calyx tube； Corolla tubular is bell, bluish violet, and long 4-5 centimetres, sliver is avette, point, pleat triangle, dilute two fissure；Stamen 5, filigree base portion have Wide wing；Style is short, and column cap 2 splits.Capsule square is circular, there is handle；There is wing at seed bar shaped, edge.Effect：Purging the liver of pathogenic fire courage excess fire, is removed Damp-heat in lower-JIAO.Liver Channel excess heat is controlled, frightened epilepsy is manic, encephalitis B, headache, hot eyes, pharyngalgia, jaundice, hot dysentery, carbuncle swells sore, scrotum Swelling and pain, private parts is wet to itch.For damp and hot yellow subcutaneous ulcer, swelling of vulva pruritus vulvae, with, eczema itch, deafness, hypochondriac pain, bitter taste, convulsion.It is main Contain secoiridoid glycosides bitter principle：Gentiopicrin (gentiopicroside), swertiamarin (swertiamarin), Sweroside (sweroside), Amarogentin (amarogentin), Amaroswerin (amaroswerin).Alkaloid：Rough gentian Alkali is gentianin (gentianine0.05%, gentioflavine (gentioflavine).
In some embodiments, the preparation method of the Radix Gentianae extract is：300g rough gentian is cleaned, grinds, used Soaked in absolute ethyl alcohol 12h, filtrate is collected by filtration, then with 2000mL distilled water refluxing extraction 8h, cooled and filtered, into filtrate Addition ammonium sulfate is not redissolved up to ammonium sulfate, and filtrate is then collected by filtration, by dialysing and being freeze-dried, obtains solid, adopts Purified with column chromatography, stationary phase is deae dextran gel A-25 chromatographic columns, and cushioning liquid is dipotassium hydrogen phosphate and biphosphate Potassium, mobile phase are 3.5wt% sodium chloride solution, collect chromatographic solution, are concentrated into 500mL, add 20g cetyl trimethyls Ammonium bromide and 5mL5wt% hydrochloric acid, 20min is stirred, adds 2000mL 86vol% ethanol, obtain sediment, collect precipitation Thing, 12h is dried in vacuo, is produced.
Lichen is Umbilicariaceae fungi lichen Umbilicaria esculenta (Miyoshi) Minks thallus.It is sweet, It is cool in nature.Return lung, the heart, stomach.With Yin nourishing and lung moistening, cooling blood and hemostasis, it is clearing heat and detoxicating the effect of.For deficiency syndrome of the lung phthisical cough, spit blood, collapse Leakage, discharging fresh blood stool, anal fistula, prolapse of the anus, stranguria with turbid discharge, band under, venomous snake bite, scald and knife wound.Main component is umbilicaric acid (gyrophoric acid), atranorine (atranorin), methyl orsellinate (methyl orsellinate) and moss Ethyl ester (ethyl orsellinate), moss (orsellinic acid), methyl β-orcinolcarboxylate (methyl β- Orcinolcarboxylate), usnic acid (usnic acid), D- sweet dew-D- volemitols (D-volemitol), polysaccharide etc..
In some embodiments, the preparation method of the lichen extract is：400g lichens are cleaned, grinds, then 2000mL acetone and 5mL triethylamines are added, refluxing extraction 12h, filtering, solid is discarded, filtrate is concentrated into Rotary Evaporators 500mL, 1500mL distilled water is added, stir 10min, precipitate, filtered, collected precipitation, tied again using acetone-ethanol Crystalline substance, solid is collected, be dried in vacuo 12h, produce.
Lichen extract, using the mixed solvent refluxing extraction of triethylamine and acetone, can allow lichen to carry in preparation process Take thing n nonylphenol APEO that there is preferable demulsification, change the surface charge distribution of NPE, Realize the effect of flocculation.
In some embodiments, the environment protection sewage inorganic agent is used to remove NPE.
Sewage-treating agent provided by the invention is mainly obtained using plant extracts, is a kind of environment protection sewage inorganic agent.Wood Disaccharides and xylotriose have adjusted the dissolubility of each material, especially make the dispersiveness of Radix Aristolochiae extract more preferable.It is provided by the invention Nutgall extractive has catharsis to the surfactant in water, and adds after lichen extract, enhances n nonylphenol The clearance of APEO, tannic acid therein, anionic compound etc. achieves larger amount of dissolution.
The second aspect of the present invention provides a kind of preparation method of environment protection sewage inorganic agent, comprises the following steps：With weight Part meter, xylotriose 8-12 parts, xylobiose 4-6 parts, 300 parts of water, nutgall extractive 28-32 parts are added in reactor, stirred 30min is mixed, is then heated to 85 DEG C, Radix Aristolochiae extract 8-12 parts is added, 1h is stirred at 85 DEG C, adds radix glycyrrhizae extraction Thing 20-30 parts, Honegsukle flower P.E 25-35 parts, 20 parts of lichen extract, 30min is stirred, be cooled to room temperature, added rough gentian and carry Thing 8-12 parts are taken, stirs, produces.
The preparation method of the present invention viscosity of regulation system, is first added using the collocation of xylobiose and xylotriose at 85 DEG C Enter Radix Aristolochiae extract, adding licorice, Honegsukle flower P.E, lichen extract afterwards can be effectively uniform by each component It is scattered, prevent phase separation and reduce effect.
The present invention is expanded on further with reference to specific embodiment.
Embodiment 1
A kind of environment protection sewage inorganic agent, in parts by weight, its preparing raw material includes：10 parts of xylotriose, 5 parts of xylobiose, gold 30 parts of honeysuckle flower extract, 30 parts of nutgall extractive, 10 parts of Radix Aristolochiae extract, 25 parts of licorice, Radix Gentianae extract 10 Part, 300 parts of water.
The preparation method of the Honegsukle flower P.E is：500g honeysuckles are cleaned, shredded, are flowed back with 4000mL distilled water 12h is extracted, after cooling, 400mL is concentrated into Rotary Evaporators, then adds saturation NaHCO3The aqueous solution, to pH=9, then drip Add 50mL 10wt% copper chloride solution, precipitate, precipitation is collected by filtration, then precipitation is dispersed in 200mL acetone, 50mL 20wt% sulfuric acid is added under agitation, is stirred 30min, filtering, is collected filtrate, add saturation NaHCO3The aqueous solution 50mL, it is evaporated under reduced pressure to without acetone, then add deionized water becomes to clarify to solution, transfers in separatory funnel, adds 20mL ethyl acetate, 10wt% hydrochloric acid is added dropwise, colourless to lower floor, upper strata is faint yellow, collects upper solution, adds and lives Property charcoal 10g, stand 12h, filtering is concentrated into 10mL to filtrate with Rotary Evaporators, then adds dichloromethane 20mL extraction, steams Dry extract, vacuum drying, is produced.
The preparation method of the nutgall extractive is：500g Chinese galls are cleaned, dried, grinds, add 3000mL Distilled water, constant temperature soaks 24h at 45 DEG C, filtering, filtrate then is cooled into 0-4 DEG C, adds the stirring of 30g activated carbons 30min, filtering, filtrate are collected by gel-type acrylic acid type cation exchange resin and exchange liquid, be concentrated into Rotary Evaporators 300mL, 1000mL hexanes are then added, filtering, collect solid, 4h is dried in vacuo, produces.
The preparation method of the Radix Aristolochiae extract is：300g dutchmanspipe roots are taken, cleans, chopping, adds 3000mL 65vol% ethanol, 500g caustic alcohols are added, soaked at room temperature after stirring 3 days, filtered, collected filtrate, use rotary evaporation Instrument is concentrated, and is concentrated into no ethanol, then places 12h at -18 DEG C, and solid is collected by filtration, the solid that then will be collected into 75 DEG C of distilled water is dissolved in, is filtered while hot, filtrate is collected, naturally cools to room temperature, 3h is then placed at -18 DEG C, is filtered, is received Collect solid, washed 3 times with acetone, use acetone 20mL every time, be dried in vacuo 4h, produce.
The preparation method of the licorice is：500g radix glycyrrhizaes are cleaned, chopping, with distilled water refluxing extraction 3 times, often It is secondary to use 5000mL distilled water, extract solution is collected, 1000mL is concentrated into Rotary Evaporators, the concentrated sulfuric acid is added dropwise under agitation, goes out Now precipitate, the concentrated sulfuric acid is added dropwise to precipitation is no longer separated out, precipitation is collected by filtration, is washed with acetone, is dried in vacuo 4h, produces.
The preparation method of the Radix Gentianae extract is：300g rough gentian is cleaned, grinds, with soaked in absolute ethyl alcohol 12h, mistake Filtrate is collected in filter, then with 2000mL distilled water refluxing extraction 8h, cooled and filtered, ammonium sulfate is added until sulfuric acid into filtrate Ammonium is not redissolved, and filtrate is then collected by filtration, and by dialysing and being freeze-dried, is obtained solid, is purified using column chromatography, stationary phase For deae dextran gel A-25 chromatographic columns, cushioning liquid is dipotassium hydrogen phosphate and potassium dihydrogen phosphate, and mobile phase is 3.5wt%'s Sodium chloride solution, chromatographic solution is collected, 500mL is concentrated into, adds 20g cetyl trimethylammonium bromides and 5mL 5wt% salt Acid, 20min is stirred, adds 2000mL 86vol% ethanol, obtain sediment, collect sediment, be dried in vacuo 12h, produce.
The preparation method of described environment protection sewage inorganic agent, comprises the following steps：In parts by weight, by 10 parts of xylotriose, 5 parts of xylobiose, 300 parts of water, 30 parts of nutgall extractive are added in reactor, are stirred 30min, are then heated to 85 DEG C, then 10 parts of Radix Aristolochiae extract is added, 1h is stirred at 85 DEG C, adds 25 parts of licorice, 30 parts of Honegsukle flower P.E, stir 30min is mixed, is cooled to room temperature, 10 parts of Radix Gentianae extract is added, stirs, produce.
Embodiment 2
A kind of environment protection sewage inorganic agent, in parts by weight, its preparing raw material includes：10 parts of xylotriose, 5 parts of xylobiose, gold 30 parts of honeysuckle flower extract, 30 parts of nutgall extractive, 10 parts of Radix Aristolochiae extract, 25 parts of licorice, Radix Gentianae extract 10 Part, 300 parts of water, 20 parts of lichen extract.
The preparation method of the Honegsukle flower P.E is：500g honeysuckles are cleaned, shredded, are flowed back with 4000mL distilled water 12h is extracted, after cooling, 400mL is concentrated into Rotary Evaporators, then adds saturation NaHCO3The aqueous solution, to pH=9, then drip Add 50mL 10wt% copper chloride solution, precipitate, precipitation is collected by filtration, then precipitation is dispersed in 200mL acetone, 50mL 20wt% sulfuric acid is added under agitation, is stirred 30min, filtering, is collected filtrate, add saturation NaHCO3The aqueous solution 50mL, it is evaporated under reduced pressure to without acetone, then add deionized water becomes to clarify to solution, transfers in separatory funnel, adds 20mL ethyl acetate, 10wt% hydrochloric acid is added dropwise, colourless to lower floor, upper strata is faint yellow, collects upper solution, adds and lives Property charcoal 10g, stand 12h, filtering is concentrated into 10mL to filtrate with Rotary Evaporators, then adds dichloromethane 20mL extraction, steams Dry extract, vacuum drying, is produced.
The preparation method of the nutgall extractive is：500g Chinese galls are cleaned, dried, grinds, add 3000mL Distilled water, constant temperature soaks 24h at 45 DEG C, filtering, filtrate then is cooled into 0-4 DEG C, adds the stirring of 30g activated carbons 30min, filtering, filtrate are collected by gel-type acrylic acid type cation exchange resin and exchange liquid, be concentrated into Rotary Evaporators 300mL, 1000mL hexanes are then added, filtering, collect solid, 4h is dried in vacuo, produces.
The preparation method of the Radix Aristolochiae extract is：300g dutchmanspipe roots are taken, cleans, chopping, adds 3000mL 65vol% ethanol, 500g caustic alcohols are added, soaked at room temperature after stirring 3 days, filtered, collected filtrate, use rotary evaporation Instrument is concentrated, and is concentrated into no ethanol, then places 12h at -18 DEG C, and solid is collected by filtration, the solid that then will be collected into 75 DEG C of distilled water is dissolved in, is filtered while hot, filtrate is collected, naturally cools to room temperature, 3h is then placed at -18 DEG C, is filtered, is received Collect solid, washed 3 times with acetone, use acetone 20mL every time, be dried in vacuo 4h, produce.
The preparation method of the licorice is：500g radix glycyrrhizaes are cleaned, chopping, with distilled water refluxing extraction 3 times, often It is secondary to use 5000mL distilled water, extract solution is collected, 1000mL is concentrated into Rotary Evaporators, the concentrated sulfuric acid is added dropwise under agitation, goes out Now precipitate, the concentrated sulfuric acid is added dropwise to precipitation is no longer separated out, precipitation is collected by filtration, is washed with acetone, is dried in vacuo 4h, produces.
The preparation method of the Radix Gentianae extract is：300g rough gentian is cleaned, grinds, with soaked in absolute ethyl alcohol 12h, mistake Filtrate is collected in filter, then with 2000mL distilled water refluxing extraction 8h, cooled and filtered, ammonium sulfate is added until sulfuric acid into filtrate Ammonium is not redissolved, and filtrate is then collected by filtration, and by dialysing and being freeze-dried, is obtained solid, is purified using column chromatography, stationary phase For deae dextran gel A-25 chromatographic columns, cushioning liquid is dipotassium hydrogen phosphate and potassium dihydrogen phosphate, and mobile phase is 3.5wt%'s Sodium chloride solution, chromatographic solution is collected, 500mL is concentrated into, adds 20g cetyl trimethylammonium bromides and 5mL 5wt% salt Acid, 20min is stirred, adds 2000mL 86vol% ethanol, obtain sediment, collect sediment, be dried in vacuo 12h, produce.
The preparation method of the lichen extract is：By 400g lichens clean, grinds, add 2000mL acetone and 5mL triethylamines, refluxing extraction 12h, filtering, solid is discarded, filtrate is concentrated into 500mL with Rotary Evaporators, added 1500mL distilled water, 10min is stirred, is precipitated, filtered, collected precipitation, recrystallized using acetone-ethanol, collect solid, very Sky dries 12h, produces.
The preparation method of described environment protection sewage inorganic agent, comprises the following steps：In parts by weight, by 10 parts of xylotriose, 5 parts of xylobiose, 300 parts of water, 30 parts of nutgall extractive are added in reactor, are stirred 30min, are then heated to 85 DEG C, then 10 parts of Radix Aristolochiae extract is added, 1h is stirred at 85 DEG C, adds 25 parts of licorice, 30 parts of Honegsukle flower P.E, stone 20 parts of ear extract, 30min is stirred, be cooled to room temperature, added 10 parts of Radix Gentianae extract, stir, produce.
Embodiment 3
A kind of environment protection sewage inorganic agent, in parts by weight, its preparing raw material includes：15 parts of xylotriose, Honegsukle flower P.E 30 parts, 30 parts of nutgall extractive, 10 parts of Radix Aristolochiae extract, 25 parts of licorice, 10 parts of Radix Gentianae extract, 300 parts of water, 20 parts of lichen extract.
The preparation method of the Honegsukle flower P.E is：500g honeysuckles are cleaned, shredded, are flowed back with 4000mL distilled water 12h is extracted, after cooling, 400mL is concentrated into Rotary Evaporators, then adds saturation NaHCO3The aqueous solution, to pH=9, then drip Add 50mL 10wt% copper chloride solution, precipitate, precipitation is collected by filtration, then precipitation is dispersed in 200mL acetone, 50mL 20wt% sulfuric acid is added under agitation, is stirred 30min, filtering, is collected filtrate, add saturation NaHCO3The aqueous solution 50mL, it is evaporated under reduced pressure to without acetone, then add deionized water becomes to clarify to solution, transfers in separatory funnel, adds 20mL ethyl acetate, 10wt% hydrochloric acid is added dropwise, colourless to lower floor, upper strata is faint yellow, collects upper solution, adds and lives Property charcoal 10g, stand 12h, filtering is concentrated into 10mL to filtrate with Rotary Evaporators, then adds dichloromethane 20mL extraction, steams Dry extract, vacuum drying, is produced.
The preparation method of the nutgall extractive is：500g Chinese galls are cleaned, dried, grinds, add 3000mL Distilled water, constant temperature soaks 24h at 45 DEG C, filtering, filtrate then is cooled into 0-4 DEG C, adds the stirring of 30g activated carbons 30min, filtering, filtrate are collected by gel-type acrylic acid type cation exchange resin and exchange liquid, be concentrated into Rotary Evaporators 300mL, 1000mL hexanes are then added, filtering, collect solid, 4h is dried in vacuo, produces.
The preparation method of the Radix Aristolochiae extract is：300g dutchmanspipe roots are taken, cleans, chopping, adds 3000mL 65vol% ethanol, 500g caustic alcohols are added, soaked at room temperature after stirring 3 days, filtered, collected filtrate, use rotary evaporation Instrument is concentrated, and is concentrated into no ethanol, then places 12h at -18 DEG C, and solid is collected by filtration, the solid that then will be collected into 75 DEG C of distilled water is dissolved in, is filtered while hot, filtrate is collected, naturally cools to room temperature, 3h is then placed at -18 DEG C, is filtered, is received Collect solid, washed 3 times with acetone, use acetone 20mL every time, be dried in vacuo 4h, produce.
The preparation method of the licorice is：500g radix glycyrrhizaes are cleaned, chopping, with distilled water refluxing extraction 3 times, often It is secondary to use 5000mL distilled water, extract solution is collected, 1000mL is concentrated into Rotary Evaporators, the concentrated sulfuric acid is added dropwise under agitation, goes out Now precipitate, the concentrated sulfuric acid is added dropwise to precipitation is no longer separated out, precipitation is collected by filtration, is washed with acetone, is dried in vacuo 4h, produces.
The preparation method of the Radix Gentianae extract is：300g rough gentian is cleaned, grinds, with soaked in absolute ethyl alcohol 12h, mistake Filtrate is collected in filter, then with 2000mL distilled water refluxing extraction 8h, cooled and filtered, ammonium sulfate is added until sulfuric acid into filtrate Ammonium is not redissolved, and filtrate is then collected by filtration, and by dialysing and being freeze-dried, is obtained solid, is purified using column chromatography, stationary phase For deae dextran gel A-25 chromatographic columns, cushioning liquid is dipotassium hydrogen phosphate and potassium dihydrogen phosphate, and mobile phase is 3.5wt%'s Sodium chloride solution, chromatographic solution is collected, 500mL is concentrated into, adds 20g cetyl trimethylammonium bromides and 5mL 5wt% salt Acid, 20min is stirred, adds 2000mL 86vol% ethanol, obtain sediment, collect sediment, be dried in vacuo 12h, produce.
The preparation method of the lichen extract is：By 400g lichens clean, grinds, add 2000mL acetone and 5mL triethylamines, refluxing extraction 12h, filtering, solid is discarded, filtrate is concentrated into 500mL with Rotary Evaporators, added 1500mL distilled water, 10min is stirred, is precipitated, filtered, collected precipitation, recrystallized using acetone-ethanol, collect solid, very Sky dries 12h, produces.
The preparation method of described environment protection sewage inorganic agent, comprises the following steps：In parts by weight, by 15 parts of xylotriose, 300 parts of water, 30 parts of nutgall extractive are added in reactor, are stirred 30min, are then heated to 85 DEG C, add dutchmanspipe root 10 parts of extract, 1h is stirred at 85 DEG C, adds 25 parts of licorice, 30 parts of Honegsukle flower P.E, lichen extract 20 Part, 30min is stirred, is cooled to room temperature, 10 parts of Radix Gentianae extract is added, stirs, produce.
Embodiment 4
A kind of environment protection sewage inorganic agent, in parts by weight, its preparing raw material includes：15 parts of xylobiose, Honegsukle flower P.E 30 parts, 30 parts of nutgall extractive, 10 parts of Radix Aristolochiae extract, 25 parts of licorice, 10 parts of Radix Gentianae extract, 300 parts of water, 20 parts of lichen extract.
The preparation method of the Honegsukle flower P.E is：500g honeysuckles are cleaned, shredded, are flowed back with 4000mL distilled water 12h is extracted, after cooling, 400mL is concentrated into Rotary Evaporators, then adds saturation NaHCO3The aqueous solution, to pH=9, then drip Add 50mL 10wt% copper chloride solution, precipitate, precipitation is collected by filtration, then precipitation is dispersed in 200mL acetone, 50mL 20wt% sulfuric acid is added under agitation, is stirred 30min, filtering, is collected filtrate, add saturation NaHCO3The aqueous solution 50mL, it is evaporated under reduced pressure to without acetone, then add deionized water becomes to clarify to solution, transfers in separatory funnel, adds 20mL ethyl acetate, 10wt% hydrochloric acid is added dropwise, colourless to lower floor, upper strata is faint yellow, collects upper solution, adds and lives Property charcoal 10g, stand 12h, filtering is concentrated into 10mL to filtrate with Rotary Evaporators, then adds dichloromethane 20mL extraction, steams Dry extract, vacuum drying, is produced.
The preparation method of the nutgall extractive is：500g Chinese galls are cleaned, dried, grinds, add 3000mL Distilled water, constant temperature soaks 24h at 45 DEG C, filtering, filtrate then is cooled into 0-4 DEG C, adds the stirring of 30g activated carbons 30min, filtering, filtrate are collected by gel-type acrylic acid type cation exchange resin and exchange liquid, be concentrated into Rotary Evaporators 300mL, 1000mL hexanes are then added, filtering, collect solid, 4h is dried in vacuo, produces.
The preparation method of the Radix Aristolochiae extract is：300g dutchmanspipe roots are taken, cleans, chopping, adds 3000mL 65vol% ethanol, 500g caustic alcohols are added, soaked at room temperature after stirring 3 days, filtered, collected filtrate, use rotary evaporation Instrument is concentrated, and is concentrated into no ethanol, then places 12h at -18 DEG C, and solid is collected by filtration, the solid that then will be collected into 75 DEG C of distilled water is dissolved in, is filtered while hot, filtrate is collected, naturally cools to room temperature, 3h is then placed at -18 DEG C, is filtered, is received Collect solid, washed 3 times with acetone, use acetone 20mL every time, be dried in vacuo 4h, produce.
The preparation method of the licorice is：500g radix glycyrrhizaes are cleaned, chopping, with distilled water refluxing extraction 3 times, often It is secondary to use 5000mL distilled water, extract solution is collected, 1000mL is concentrated into Rotary Evaporators, the concentrated sulfuric acid is added dropwise under agitation, goes out Now precipitate, the concentrated sulfuric acid is added dropwise to precipitation is no longer separated out, precipitation is collected by filtration, is washed with acetone, is dried in vacuo 4h, produces.
The preparation method of the Radix Gentianae extract is：300g rough gentian is cleaned, grinds, with soaked in absolute ethyl alcohol 12h, mistake Filtrate is collected in filter, then with 2000mL distilled water refluxing extraction 8h, cooled and filtered, ammonium sulfate is added until sulfuric acid into filtrate Ammonium is not redissolved, and filtrate is then collected by filtration, and by dialysing and being freeze-dried, is obtained solid, is purified using column chromatography, stationary phase For deae dextran gel A-25 chromatographic columns, cushioning liquid is dipotassium hydrogen phosphate and potassium dihydrogen phosphate, and mobile phase is 3.5wt%'s Sodium chloride solution, chromatographic solution is collected, 500mL is concentrated into, adds 20g cetyl trimethylammonium bromides and 5mL 5wt% salt Acid, 20min is stirred, adds 2000mL 86vol% ethanol, obtain sediment, collect sediment, be dried in vacuo 12h, produce.
The preparation method of the lichen extract is：By 400g lichens clean, grinds, add 2000mL acetone and 5mL triethylamines, refluxing extraction 12h, filtering, solid is discarded, filtrate is concentrated into 500mL with Rotary Evaporators, added 1500mL distilled water, 10min is stirred, is precipitated, filtered, collected precipitation, recrystallized using acetone-ethanol, collect solid, very Sky dries 12h, produces.
The preparation method of described environment protection sewage inorganic agent, comprises the following steps：In parts by weight, by 15 parts of xylobiose, 300 parts of water, 30 parts of nutgall extractive are added in reactor, are stirred 30min, are then heated to 85 DEG C, add dutchmanspipe root 10 parts of extract, 1h is stirred at 85 DEG C, adds 25 parts of licorice, 30 parts of Honegsukle flower P.E, lichen extract 20 Part, 30min is stirred, is cooled to room temperature, 10 parts of Radix Gentianae extract is added, stirs, produce.
Embodiment 5
A kind of environment protection sewage inorganic agent, in parts by weight, its preparing raw material includes：10 parts of xylotriose, 5 parts of xylobiose, gold 30 parts of honeysuckle flower extract, 30 parts of nutgall extractive, 10 parts of Radix Aristolochiae extract, 25 parts of licorice, Radix Gentianae extract 10 Part, 300 parts of water, 20 parts of lichen extract.
The preparation method of the Honegsukle flower P.E is：500g honeysuckles are cleaned, shredded, are flowed back with 4000mL distilled water 12h is extracted, after cooling, 400mL is concentrated into Rotary Evaporators, then adds saturation NaHCO3The aqueous solution, to pH=9, then drip Add 50mL 10wt% copper chloride solution, precipitate, precipitation is collected by filtration, then precipitation is dispersed in 200mL acetone, 50mL 20wt% sulfuric acid is added under agitation, is stirred 30min, filtering, is collected filtrate, add saturation NaHCO3The aqueous solution 50mL, it is evaporated under reduced pressure to without acetone, then add deionized water becomes to clarify to solution, transfers in separatory funnel, adds 20mL ethyl acetate, 10wt% hydrochloric acid is added dropwise, colourless to lower floor, upper strata is faint yellow, collects upper solution, adds and lives Property charcoal 10g, stand 12h, filtering is concentrated into 10mL to filtrate with Rotary Evaporators, then adds dichloromethane 20mL extraction, steams Dry extract, vacuum drying, is produced.
The preparation method of the nutgall extractive is：500g Chinese galls are cleaned, dried, grinds, add 3000mL Distilled water, constant temperature soaks 24h at 45 DEG C, filtering, filtrate then is cooled into 0-4 DEG C, adds the stirring of 30g activated carbons 30min, filtering, filtrate are collected by gel-type acrylic acid type cation exchange resin and exchange liquid, be concentrated into Rotary Evaporators 300mL, 1000mL hexanes are then added, filtering, collect solid, 4h is dried in vacuo, produces.
The preparation method of the Radix Aristolochiae extract is：300g dutchmanspipe roots are taken, cleans, chopping, adds 3000mL 65vol% ethanol, soak 3 days, filter at room temperature after stirring, collect filtrate, concentrated, be concentrated into Rotary Evaporators Without ethanol, 12h then is placed at -18 DEG C, solid is collected by filtration, then the solid being collected into is dissolved in 75 DEG C of distilled water, Filter while hot, collect filtrate, naturally cool to room temperature, 3h is then placed at -18 DEG C, filter, collect solid, washed with acetone 3 times, acetone 20mL is used every time, is dried in vacuo 4h, is produced.
The preparation method of the licorice is：500g radix glycyrrhizaes are cleaned, chopping, with distilled water refluxing extraction 3 times, often It is secondary to use 5000mL distilled water, extract solution is collected, 1000mL is concentrated into Rotary Evaporators, the concentrated sulfuric acid is added dropwise under agitation, goes out Now precipitate, the concentrated sulfuric acid is added dropwise to precipitation is no longer separated out, precipitation is collected by filtration, is washed with acetone, is dried in vacuo 4h, produces.
The preparation method of the Radix Gentianae extract is：300g rough gentian is cleaned, grinds, with soaked in absolute ethyl alcohol 12h, mistake Filtrate is collected in filter, then with 2000mL distilled water refluxing extraction 8h, cooled and filtered, ammonium sulfate is added until sulfuric acid into filtrate Ammonium is not redissolved, and filtrate is then collected by filtration, and by dialysing and being freeze-dried, is obtained solid, is purified using column chromatography, stationary phase For deae dextran gel A-25 chromatographic columns, cushioning liquid is dipotassium hydrogen phosphate and potassium dihydrogen phosphate, and mobile phase is 3.5wt%'s Sodium chloride solution, chromatographic solution is collected, 500mL is concentrated into, adds 20g cetyl trimethylammonium bromides and 5mL 5wt% salt Acid, 20min is stirred, adds 2000mL 86vol% ethanol, obtain sediment, collect sediment, be dried in vacuo 12h, produce.
The preparation method of the lichen extract is：By 400g lichens clean, grinds, add 2000mL acetone and 5mL triethylamines, refluxing extraction 12h, filtering, solid is discarded, filtrate is concentrated into 500mL with Rotary Evaporators, added 1500mL distilled water, 10min is stirred, is precipitated, filtered, collected precipitation, recrystallized using acetone-ethanol, collect solid, very Sky dries 12h, produces.
The preparation method of described environment protection sewage inorganic agent, comprises the following steps：In parts by weight, by 10 parts of xylotriose, 5 parts of xylobiose, 300 parts of water, 30 parts of nutgall extractive are added in reactor, are stirred 30min, are then heated to 85 DEG C, then 10 parts of Radix Aristolochiae extract is added, 1h is stirred at 85 DEG C, adds 25 parts of licorice, 30 parts of Honegsukle flower P.E, stone 20 parts of ear extract, 30min is stirred, be cooled to room temperature, added 10 parts of Radix Gentianae extract, stir, produce.
Embodiment 6
A kind of environment protection sewage inorganic agent, in parts by weight, its preparing raw material includes：10 parts of xylotriose, 5 parts of xylobiose, gold 30 parts of honeysuckle flower extract, 30 parts of nutgall extractive, 10 parts of Radix Aristolochiae extract, 25 parts of licorice, Radix Gentianae extract 10 Part, 300 parts of water, 20 parts of lichen extract.
The preparation method of the Honegsukle flower P.E is：500g honeysuckles are cleaned, shredded, are flowed back with 4000mL distilled water 12h is extracted, after cooling, 400mL is concentrated into Rotary Evaporators, then adds saturation NaHCO3The aqueous solution, to pH=9, then drip Add 50mL 10wt% copper chloride solution, precipitate, precipitation is collected by filtration, then precipitation is dispersed in 200mL acetone, 50mL 20wt% sulfuric acid is added under agitation, is stirred 30min, filtering, is collected filtrate, add saturation NaHCO3The aqueous solution 50mL, it is evaporated under reduced pressure to without acetone, then add deionized water becomes to clarify to solution, transfers in separatory funnel, adds 20mL ethyl acetate, 10wt% hydrochloric acid is added dropwise, colourless to lower floor, upper strata is faint yellow, collects upper solution, adds and lives Property charcoal 10g, stand 12h, filtering is concentrated into 10mL to filtrate with Rotary Evaporators, then adds dichloromethane 20mL extraction, steams Dry extract, vacuum drying, is produced.
The preparation method of the nutgall extractive is：500g Chinese galls are cleaned, dried, grinds, add 3000mL Distilled water, constant temperature soaks 24h at 45 DEG C, filtering, filtrate then is cooled into 0-4 DEG C, adds the stirring of 30g activated carbons 30min, filtering, filtrate are collected by gel-type acrylic acid type cation exchange resin and exchange liquid, be concentrated into Rotary Evaporators 300mL, 1000mL hexanes are then added, filtering, collect solid, 4h is dried in vacuo, produces.
The preparation method of the Radix Aristolochiae extract is：300g dutchmanspipe roots are taken, cleans, chopping, adds 3000mL 65vol% ethanol, 500g caustic alcohols are added, soaked at room temperature after stirring 3 days, filtered, collected filtrate, use rotary evaporation Instrument is concentrated, and is concentrated into no ethanol, then places 12h at -18 DEG C, and solid is collected by filtration, the solid that then will be collected into 75 DEG C of distilled water is dissolved in, is filtered while hot, filtrate is collected, naturally cools to room temperature, 3h is then placed at -18 DEG C, is filtered, is received Collect solid, washed 3 times with acetone, use acetone 20mL every time, be dried in vacuo 4h, produce.
The preparation method of the licorice is：500g radix glycyrrhizaes are cleaned, chopping, with distilled water refluxing extraction 3 times, often It is secondary to use 5000mL distilled water, extract solution is collected, 1000mL is concentrated into Rotary Evaporators, the concentrated sulfuric acid is added dropwise under agitation, goes out Now precipitate, the concentrated sulfuric acid is added dropwise to precipitation is no longer separated out, precipitation is collected by filtration, is washed with acetone, is dried in vacuo 4h, produces.
The preparation method of the Radix Gentianae extract is：300g rough gentian is cleaned, grinds, with soaked in absolute ethyl alcohol 12h, mistake Filtrate is collected in filter, then with 2000mL distilled water refluxing extraction 8h, cooled and filtered, ammonium sulfate is added until sulfuric acid into filtrate Ammonium is not redissolved, and filtrate is then collected by filtration, and by dialysing and being freeze-dried, is obtained solid, is purified using column chromatography, stationary phase For deae dextran gel A-25 chromatographic columns, cushioning liquid is dipotassium hydrogen phosphate and potassium dihydrogen phosphate, and mobile phase is 3.5wt%'s Sodium chloride solution, chromatographic solution is collected, 500mL is concentrated into, adds 20g cetyl trimethylammonium bromides and 5mL 5wt% salt Acid, 20min is stirred, adds 2000mL 86vol% ethanol, obtain sediment, collect sediment, be dried in vacuo 12h, produce.
The preparation method of the lichen extract is：400g lichens are cleaned, grinds, add 2000mL acetone, returned Stream extraction 12h, filtering, discards solid, filtrate is concentrated into 500mL with Rotary Evaporators, add 1500mL distilled water, stir 10min, precipitate, filter, collect precipitation, recrystallized using acetone-ethanol, collect solid, be dried in vacuo 12h, produce.
The preparation method of described environment protection sewage inorganic agent, comprises the following steps：In parts by weight, by 10 parts of xylotriose, 5 parts of xylobiose, 300 parts of water, 30 parts of nutgall extractive are added in reactor, are stirred 30min, are then heated to 85 DEG C, then 10 parts of Radix Aristolochiae extract is added, 1h is stirred at 85 DEG C, adds 25 parts of licorice, 30 parts of Honegsukle flower P.E, stone 20 parts of ear extract, 30min is stirred, be cooled to room temperature, added 10 parts of Radix Gentianae extract, stir, produce.
Embodiment 7
A kind of environment protection sewage inorganic agent, in parts by weight, its preparing raw material includes：10 parts of xylotriose, 5 parts of xylobiose, gold 30 parts of honeysuckle flower extract, 30 parts of nutgall extractive, 25 parts of licorice, 10 parts of Radix Gentianae extract, 300 parts of water, lichen carry Take 20 parts of thing.
The preparation method of the Honegsukle flower P.E is：500g honeysuckles are cleaned, shredded, are flowed back with 4000mL distilled water 12h is extracted, after cooling, 400mL is concentrated into Rotary Evaporators, then adds saturation NaHCO3The aqueous solution, to pH=9, then drip Add 50mL 10wt% copper chloride solution, precipitate, precipitation is collected by filtration, then precipitation is dispersed in 200mL acetone, 50mL 20wt% sulfuric acid is added under agitation, is stirred 30min, filtering, is collected filtrate, add saturation NaHCO3The aqueous solution 50mL, it is evaporated under reduced pressure to without acetone, then add deionized water becomes to clarify to solution, transfers in separatory funnel, adds 20mL ethyl acetate, 10wt% hydrochloric acid is added dropwise, colourless to lower floor, upper strata is faint yellow, collects upper solution, adds and lives Property charcoal 10g, stand 12h, filtering is concentrated into 10mL to filtrate with Rotary Evaporators, then adds dichloromethane 20mL extraction, steams Dry extract, vacuum drying, is produced.
The preparation method of the nutgall extractive is：500g Chinese galls are cleaned, dried, grinds, add 3000mL Distilled water, constant temperature soaks 24h at 45 DEG C, filtering, filtrate then is cooled into 0-4 DEG C, adds the stirring of 30g activated carbons 30min, filtering, filtrate are collected by gel-type acrylic acid type cation exchange resin and exchange liquid, be concentrated into Rotary Evaporators 300mL, 1000mL hexanes are then added, filtering, collect solid, 4h is dried in vacuo, produces.
The preparation method of the licorice is：500g radix glycyrrhizaes are cleaned, chopping, with distilled water refluxing extraction 3 times, often It is secondary to use 5000mL distilled water, extract solution is collected, 1000mL is concentrated into Rotary Evaporators, the concentrated sulfuric acid is added dropwise under agitation, goes out Now precipitate, the concentrated sulfuric acid is added dropwise to precipitation is no longer separated out, precipitation is collected by filtration, is washed with acetone, is dried in vacuo 4h, produces.
The preparation method of the Radix Gentianae extract is：300g rough gentian is cleaned, grinds, with soaked in absolute ethyl alcohol 12h, mistake Filtrate is collected in filter, then with 2000mL distilled water refluxing extraction 8h, cooled and filtered, ammonium sulfate is added until sulfuric acid into filtrate Ammonium is not redissolved, and filtrate is then collected by filtration, and by dialysing and being freeze-dried, is obtained solid, is purified using column chromatography, stationary phase For deae dextran gel A-25 chromatographic columns, cushioning liquid is dipotassium hydrogen phosphate and potassium dihydrogen phosphate, and mobile phase is 3.5wt%'s Sodium chloride solution, chromatographic solution is collected, 500mL is concentrated into, adds 20g cetyl trimethylammonium bromides and 5mL 5wt% salt Acid, 20min is stirred, adds 2000mL 86vol% ethanol, obtain sediment, collect sediment, be dried in vacuo 12h, produce.
The preparation method of the lichen extract is：By 400g lichens clean, grinds, add 2000mL acetone and 5mL triethylamines, refluxing extraction 12h, filtering, solid is discarded, filtrate is concentrated into 500mL with Rotary Evaporators, added 1500mL distilled water, 10min is stirred, is precipitated, filtered, collected precipitation, recrystallized using acetone-ethanol, collect solid, very Sky dries 12h, produces.
The preparation method of described environment protection sewage inorganic agent, comprises the following steps：In parts by weight, by 10 parts of xylotriose, 5 parts of xylobiose, 300 parts of water, 30 parts of nutgall extractive are added in reactor, are stirred 30min, are then heated to 85 DEG C, 1h is stirred at 85 DEG C, adds 25 parts of licorice, 30 parts of Honegsukle flower P.E, 20 parts of lichen extract, stirs 30min, Room temperature is cooled to, 10 parts of Radix Gentianae extract is added, stirs, produce.
Method of testing
1. NPE removes test
The aqueous solution 1000mL for containing 2000mg/L NPEs is prepared as sample, respectively by 7g embodiments 1-7 is added in sample, stirs 2min, and the content of NPE is then determined with ultraviolet-uisible spectrophotometer, And keep a record, mg/L.
2. anti-corrosive properties are tested
Embodiment 1-7 is preserved 30 days in 25 DEG C, sees whether to precipitate, is recorded as without precipitation, muddy, less heavy Form sediment, a large amount of precipitations.
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. a kind of environment protection sewage inorganic agent, it is characterised in that in parts by weight, its preparing raw material includes：Xylotriose 8-12 parts, wood Disaccharides 4-6 parts, Honegsukle flower P.E 25-35 parts, nutgall extractive 28-32 parts, Radix Aristolochiae extract 8-12 parts, radix glycyrrhizae extraction Thing 20-30 parts, Radix Gentianae extract 8-12 parts, 300 parts of water.
2. environment protection sewage inorganic agent as claimed in claim 1, it is characterised in that its preparing raw material also includes：Lichen extract 20 parts.
3. environment protection sewage inorganic agent as claimed in claim 1, it is characterised in that the preparation method of the Honegsukle flower P.E For：500g honeysuckles are cleaned, shreds, with 4000mL distilled water refluxing extraction 12h, after cooling, is concentrated into Rotary Evaporators 400mL, then add saturation NaHCO3The aqueous solution, to pH=9, then 50mL 10wt% copper chloride solution is added dropwise, sinks Form sediment, precipitation is collected by filtration, then precipitation is dispersed in 200mL acetone, add 50mL 20wt% sulfuric acid under agitation, stir 30min is mixed, is filtered, filtrate is collected, adds saturation NaHCO3Aqueous solution 50mL, it is evaporated under reduced pressure to without acetone, then adds and go Ionized water becomes to clarify to solution, transfers in separatory funnel, adds 20mL ethyl acetate, and 10wt% salt is added dropwise Acid, colourless to lower floor, upper strata is faint yellow, collects upper solution, adds activated carbon 10g, stands 12h, filtering, filtrate is revolved Turn evaporimeter and be concentrated into 10mL, then add dichloromethane 20mL extractions, be evaporated extract, be dried in vacuo, produce.
4. environment protection sewage inorganic agent as claimed in claim 1, it is characterised in that the preparation method of the nutgall extractive For：500g Chinese galls are cleaned, dried, grinds, add 3000mL distilled water, constant temperature soaks 24h at 45 DEG C, filters, Then filtrate is cooled to 0-4 DEG C, adds 30g activated carbons stirring 30min, filtering, filtrate by gel-type acrylic acid series sun from Sub-exchange resin, collect and exchange liquid, 300mL is concentrated into Rotary Evaporators, then add 1000mL hexanes, filtering, collect solid Body, 4h is dried in vacuo, is produced.
5. environment protection sewage inorganic agent as claimed in claim 1, it is characterised in that the preparation method of the Radix Aristolochiae extract For：300g dutchmanspipe roots are taken, is cleaned, chopping, is added 3000mL 65vol% ethanol, 500g caustic alcohols are added, after stirring Soak 3 days at room temperature, filtering, collect filtrate, concentrated with Rotary Evaporators, be concentrated into no ethanol, then in -18 DEG C of decentralizations 12h is put, solid is collected by filtration, then the solid being collected into is dissolved in 75 DEG C of distilled water, filtered while hot, collects filtrate, it is natural Room temperature is cooled to, 3h is then placed at -18 DEG C, is filtered, solid is collected, is washed 3 times with acetone, use acetone 20mL every time, 4h is dried in vacuo, is produced.
6. environment protection sewage inorganic agent as claimed in claim 1, it is characterised in that the preparation method of the licorice is： 500g radix glycyrrhizaes are cleaned, chopping, with distilled water refluxing extraction 3 times, use 5000mL distilled water, collection extract solution, with rotation every time Turn evaporimeter and be concentrated into 1000mL, the concentrated sulfuric acid is added dropwise under agitation, precipitates, the concentrated sulfuric acid is added dropwise to no longer precipitation precipitation, mistake Precipitation is collected in filter, is washed with acetone, is dried in vacuo 4h, is produced.
7. environment protection sewage inorganic agent as claimed in claim 1, it is characterised in that the preparation method of the Radix Gentianae extract is： 300g rough gentian is cleaned, grinds, with soaked in absolute ethyl alcohol 12h, filtrate is collected by filtration, then carried with the backflow of 2000mL distilled water Take 8h, cooled and filtered, into filtrate add ammonium sulfate until ammonium sulfate is not redissolved, filtrate is then collected by filtration, by saturating Analysis and freeze-drying, are obtained solid, are purified using column chromatography, and stationary phase is deae dextran gel A-25 chromatographic columns, and buffering is molten Liquid is dipotassium hydrogen phosphate and potassium dihydrogen phosphate, and mobile phase is 3.5wt% sodium chloride solution, collects chromatographic solution, is concentrated into 500mL, 20g cetyl trimethylammonium bromides and 5mL 5wt% hydrochloric acid are added, stir 20min, add 2000mL 86vol% ethanol, sediment is obtained, collect sediment, be dried in vacuo 12h, produce.
8. environment protection sewage inorganic agent as claimed in claim 2, it is characterised in that the preparation method of the lichen extract is： 400g lichens are cleaned, grinds, add 2000mL acetone and 5mL triethylamines, refluxing extraction 12h, filtering, discard solid, Filtrate is concentrated into 500mL with Rotary Evaporators, adds 1500mL distilled water, 10min is stirred, precipitates, is filtered, is collected Precipitation, is recrystallized using acetone-ethanol, collects solid, is dried in vacuo 12h, is produced.
9. environment protection sewage inorganic agent as claimed in claim 1, it is characterised in that the environment protection sewage inorganic agent is used to remove nonyl Base phenol polyethenoxy ether.
10. a kind of preparation method of environment protection sewage inorganic agent as described in any one of claim 1-9 claim, its feature It is, comprises the following steps：In parts by weight, by xylotriose 8-12 parts, xylobiose 4-6 parts, 300 parts of water, nutgall extractive 28-32 parts are added in reactor, are stirred 30min, are then heated to 85 DEG C, Radix Aristolochiae extract 8-12 parts are added, 85 1h is stirred at DEG C, adds licorice 20-30 parts, Honegsukle flower P.E 25-35 parts, 20 parts of lichen extract, is stirred 30min, room temperature is cooled to, adds Radix Gentianae extract 8-12 parts, stir, produce.
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Publication number Priority date Publication date Assignee Title
CN110526326A (en) * 2018-05-23 2019-12-03 河南仁华生物科技有限公司 A kind of multipurpose waste water treating agent

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CN106390166A (en) * 2016-09-17 2017-02-15 佛山市顺德区宝铜金属科技有限公司 Air freshener with sterilizing effect and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106390166A (en) * 2016-09-17 2017-02-15 佛山市顺德区宝铜金属科技有限公司 Air freshener with sterilizing effect and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110526326A (en) * 2018-05-23 2019-12-03 河南仁华生物科技有限公司 A kind of multipurpose waste water treating agent

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