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.