CN104289187B - A kind of preparation of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent - Google Patents

A kind of preparation of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent Download PDF

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CN104289187B
CN104289187B CN201410456613.6A CN201410456613A CN104289187B CN 104289187 B CN104289187 B CN 104289187B CN 201410456613 A CN201410456613 A CN 201410456613A CN 104289187 B CN104289187 B CN 104289187B
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retinervus luffae
luffae fructus
ammonium chloride
dimethyl diallyl
diallyl ammonium
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CN104289187A (en
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李慧芝
周英杰
许崇娟
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University of Jinan
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University of Jinan
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
    • 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
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
    • 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
    • C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton

Abstract

The invention discloses the preparation method and application technology of a kind of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent, feature is: by Fructus Luffae mellow fruit, peeling enucleation, wash removal earth and impurity with water, it is dried, pulverize, chemically treated after drying, obtain chloride Retinervus Luffae Fructus, in the reactor, add by following composition mass percent, dimethyl diallyl ammonium chloride: 56 ~ 71%, chloride Retinervus Luffae Fructus: 10 ~ 20%, water: 12 ~ 26%, Ammonium persulfate.: 0.5 ~ 2.0%, each component sum is absolutely, nitrogen is protected, in 45 ~ 55 DEG C of constant temperature, stirring, back flow reaction 4 ~ 5h, after cooling, it is washed with deionized, sucking filtration, being neutrality to filtrate, vacuum drying oven is dried, obtain dimethyl diallyl ammonium chloride modified loofah sponge adsorbent.This adsorbent has a highest adsorption capacity to oils and fats, excellent physical chemistry and mechanical performance, and regeneration capacity is strong, Reusability often, not only low cost but also environmental protection.

Description

A kind of preparation of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent
Technical field
The present invention relates to the preparation method of a kind of biological adsorption agent, belong to water-treatment technology field, the oil removing being suitable to oil-polluted water purifies, particularly to preparation and the application technology of a kind of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent.
Background technology
Oily waste water is mainly derived from the processes such as the oil recovery of petroleum industry, oil refining, store oil, transport and petrochemical industry production, after oil product enters water body, moisture film can be formed on top layer, stop oxygen to dissolve in water body, thus cause water hypoxia, biological death, cause serious environmental pollution.The rules and regulations such as " People's Republic of China's law of marine environmental protection " that China promulgates at present, oily waste water the highest permission concentration of emission is 10 mg/L.So, the multiple field of petrochemical industry and environmental conservation etc. instantly that the is treated as problem demanding prompt solution of oily waste water.Absorption method is the one in numerous process technique, and recent domestic many scholars process the research of oily waste water and focus mostly at the adsorption efficiency improving adsorbent absorption method, probe into the method for modifying etc. of adsorbent.The features such as it is simple that its absorption method has technique, and adsorption rate is high, applied widely, stable in properties are used widely in sewage disposal.For the active charcoal of adsorbent of oily waste water absorption, expanded graphite, modified alta-mud, modified coal ash, serpentine, attapulgite, zeolite etc..Gao Sainan etc. have studied oil extraction waste water biological treatment water outlet charcoal test, (high match man etc. oil extraction waste water biological treatment water outlet charcoal test is studied. Environmental science and technology, 2010-12,33 (12): 56-65)；Wang Shuzhao etc. have studied the expanded graphite absorption property to oily waste water, (Wang Shuzhao etc. the expanded graphite Study on adsorption properties to oily waste water. scientific and technical innovation Leader .2012 (22): 7-8)；Shu Ming is brave etc. have studied modified alta-mud and processes the test of emulsifying liquid waste water, and Shu Ming is brave. and modified alta-mud processes the experimental study of emulsifying liquid waste water. Chemical Engineer, 2012 (8): 34-38)；Deng Hui etc. have studied flyash and remove the application of oily waste water, (China such as Deng Hui utilizes flyash to remove the applied research of oily waste water. flyash, and 2012 (3): 10-14).
Shortage of resources and environmental pollution have become as two big subject matters of the world today, therefore, utilize natural reproducible resource, development environment friendly product and technology will become the inexorable trend of sustainable development.Retinervus Luffae Fructus is the withered old fruit of the vascular bundle Fructus Luffae in other words in the mature fruit of Cucurbitaceae annual herb plant Fructus Luffae.Fructus Luffae is China's summer and autumn Common Vegetables, there is product most provinces and regions, the whole nation, for cultivation product, Retinervus Luffae Fructus is the regenerated resources that the earth enriches very much, have that light weight is inexpensive, the feature such as degradable and environmental friendliness, Retinervus Luffae Fructus is by the net of the thread fiber interweaving of multilamellar, body is light, matter is tough and tensile, can not fracture, simultaneously containing xylan, mannan, galactan etc., and it has hydrophilic, also with abundant dentate, it is easy to carry out chemical modification, the modified application as adsorbent in adsorption of metal ions of domestic Retinervus Luffae Fructus.
Domestic Retinervus Luffae Fructus is as adsorbent application in adsorption of metal ions, disclosing Retinervus Luffae Fructus in the patent of Application No. 200810034734.6 to many kinds of metal ions absorption property and Retinervus Luffae Fructus as adsorbent application in adsorption of metal ions, wherein Retinervus Luffae Fructus is to Cu2+And Zn2+Desorption rate all about 40%, Retinervus Luffae Fructus is to Cu2+Adsorbance be respectively 0.16mmol/g, to Zn2+Adsorbance be about 0.39mmol/g, in the system that pH is 1, desorption rate is respectively 46%, 47%；Disclosing alkalization modifying method and the application thereof of Retinervus Luffae Fructus in the patent of Application No. 200810034735.0, its alkali processes Retinervus Luffae Fructus to Zn2+Adsorbance relatively Cu2+Height, and adsorbance gap is relatively big, through Atomic Absorption quantitative analysis, Retinervus Luffae Fructus is to Cu2+Adsorbance be about 7 ~ 8mg/g, to Zn2+Adsorbance be about 21 ~ 22mg/g；Disclosing the preparation method of etherized luffa and the application in adsorption of metal ions thereof in the patent of Application No. 200810034737.X, its etherized luffa is to Fe3+Maximal absorptive capacity be 27.4mg/g.To Zn2+Maximal absorptive capacity be 36.3mg/g；Disclosing citric acid loofah sponge preparation method agent application in the patent of Application No. 201110276244.9, its citric acid loofah sponge is to Cd2+Adsorption capacity may be up to 189mg/g, high adsorption rate is up to 98.5%, to Pb2+Maximal absorptive capacity be 285mg/g, High adsorption rate is up to 99.2%, and the maximal absorptive capacity to methylene blue is 316mg/g, and high adsorption rate is up to 96.2%, has carboxylic acid characteristic, can be directly to metal ion species each in water body, the absorption of organic dyestuff and eluting, but not used for the absorption of oil in waste water.
Since the nineties in 20th century, people utilize natural fiber cheap and easy to get to obtain more research in the process of waste water as adsorbent.Neha Gupta etc. have studied the methylene blue in Rhizoma Solani tuber osi straw absorption water and malachite green oxalate, its maximum adsorption capacity is: 52.6mg/g, (Neha Gupta, Application of potato (Solanum tuberosum) plant wastes for the removal of methylene blue and malachite green dye from aqueous Solution. Arabian Journal of Chemistry, (2011))；Runping Han etc. have studied the fallen leaves of phoenix tree to the methylene blue adsorption number in water, its maximum adsorption capacity is: 89.7mg/g, (Runping Han, Biosorption of methylene blue from aqueous solution by fallen phoenix tree ' s leaves. Journal of Hazardous Materials, 141 (2007) 156 162)；Li Shan etc., have studied methylene blue in epoxychloropropane modified Pericarppium arachidis hypogaeae absorption water, and the maximum adsorption capacity of methyl blue is by it: 25mg/g, (Li Shan etc., the research of methylene blue, dyestuff and dyeing in epoxychloropropane modified Pericarppium arachidis hypogaeae absorption water, 2008,45(2): 49 ~ 51)；But natural fiber has no report as adsorbent application in absorption oil.Natural macromolecular material is utilized as adsorbent and has the advantages such as renewable, degradable, environmental protection be friendly, cheap, is important living resources.
Summary of the invention
An object of the present invention is to provide the preparation method of a kind of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent, and the dimethyl diallyl ammonium chloride modified loofah sponge adsorbent mainly making acquisition is bigger to the adsorption capacity of oils and fats in waste water.
The purpose of the present invention is achieved through the following technical solutions.
The preparation method of a kind of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent, is characterised by that the method has a following processing step:
(1) Retinervus Luffae Fructus pretreatment: Retinervus Luffae Fructus derives from Fructus Luffae fruit, is obtained by peeling enucleation, pulverizes, by the sieve of 10 ~ 40 mesh, obtain pretreatment Retinervus Luffae Fructus after the clear water cleaning, drying that are cut into small pieces by Retinervus Luffae Fructus；
(2) oxidation Retinervus Luffae Fructus: in the reactor, add by following composition mass percent, pretreatment Retinervus Luffae Fructus: 10 ~ 20%, water: 71 ~ 87%, NaOH:2 ~ 10%, each component sum is absolutely, soaking at room temperature 12 ~ 24 h, then boil 20 ~ 40min, it is washed with deionized after cooling to neutrality, place in concentrated nitric acid, in 85 ~ 95 DEG C of constant temperature, stirring, back flow reaction 90 ~ 120 Min, after cooling, is washed with deionized, sucking filtration, being neutrality to filtrate, is dried in vacuum drying oven, obtains aoxidizing Retinervus Luffae Fructus；
(3) prepared by chloride Retinervus Luffae Fructus: in the reactor, adds by following composition mass percent, dimethylformamide: 25 ~ 45%, thionyl chloride: 40 ~ 60%, oxidation Retinervus Luffae Fructus: 8 ~ 18%, each component sum is absolutely, in 65 ~ 75 DEG C of constant temperature, stirring, back flow reaction 50 ~ 60 H, washs with acetone reflux after completion of the reaction, removes dimethylformamide and the thionyl chloride of surface adhesion, puts in vacuum drying oven and be dried, obtain chloride Retinervus Luffae Fructus after taking-up；
(4) preparation of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent: in the reactor; add by following composition mass percent; dimethyl diallyl ammonium chloride: 56 ~ 71%; chloride Retinervus Luffae Fructus: 10 ~ 20%; water: 12 ~ 26%; Ammonium persulfate.: 0.5 ~ 2.0%; each component sum is absolutely; nitrogen is protected, in 45 ~ 55 DEG C of constant temperature, stirring, back flow reaction 4 ~ 5 h, after cooling; be washed with deionized, sucking filtration; being neutrality to filtrate, vacuum drying oven is dried, obtains dimethyl diallyl ammonium chloride modified loofah sponge adsorbent.
It is a further object of the present invention to provide the absorption to oil in aqueous systems of the dimethyl diallyl ammonium chloride modified loofah sponge adsorbent, feature is: the dimethyl diallyl ammonium chloride modified loofah sponge adsorbent deionized water prepared is soaked 0.5 ~ 1.0h, adsorbs by static method.
The dimethyl diallyl ammonium chloride modified loofah sponge adsorbent deionized water prepared being soaked 0.5 ~ 1.0h, adsorbs by dynamic method, flow velocity is 1.0 mL/min.
Advantages of the present invention and effect be:
(1) the dimethyl diallyl ammonium chloride modified loofah sponge adsorbent that the present invention obtains has good physical and chemical stability and excellent mechanical strength, and adsorption capacity is big, and Reusability number of times is up to more than 10 times;
(2) the dimethyl diallyl ammonium chloride modified loofah sponge adsorbent that the present invention obtains all has preferably absorption and eluting to oils and fatss various in water body (such as crude oil, diesel oil, lubricating oil, machine oil, vegetable oil, gasoline etc.), adsorption efficiency is high, the speed of absorption is fast, desorption performance is good, it is possible to use in the range of wider soda acid；
(3) little due to the density of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent, water surface can be swum in, the chance contacted with oils and fats is many, to oil clearance high, be natural green product, biodegradable, environmental protection；
(4) condition crossing range request synthesized is easily controlled, and energy consumption is low, simple to operate, renewable resource utilization, it is easy to industrialized production.
Detailed description of the invention
Embodiment 1
(1) Retinervus Luffae Fructus pretreatment: Retinervus Luffae Fructus derives from Fructus Luffae fruit, is obtained by peeling enucleation, pulverizes, by the sieve of 10 mesh, obtain pretreatment Retinervus Luffae Fructus after the clear water cleaning, drying that are cut into small pieces by Retinervus Luffae Fructus；
(2) oxidation Retinervus Luffae Fructus: in the reactor, be separately added into pretreatment Retinervus Luffae Fructus: 15g, water: 80mL, NaOH:5g, soaking at room temperature 20 h, then boil 30min, it is washed with deionized after cooling to neutrality, place in 100mL concentrated nitric acid, in 90 DEG C of constant temperature, stirring, back flow reaction 100 min, after cooling, be washed with deionized, sucking filtration, being neutrality to filtrate, vacuum drying oven is dried, obtains aoxidizing Retinervus Luffae Fructus；
(3) prepared by chloride Retinervus Luffae Fructus: in the reactor, it is separately added into dimethylformamide 35mL, thionyl chloride: 35mL, oxidation Retinervus Luffae Fructus: 10g, in 70 DEG C of constant temperature, stirring, back flow reaction 55 h, wash with acetone reflux after completion of the reaction, remove dimethylformamide and the thionyl chloride of surface adhesion, put after taking-up in vacuum drying oven and be dried, obtain chloride Retinervus Luffae Fructus；
(4) preparation of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent: in the reactor; it is separately added into dimethyl diallyl ammonium chloride: 60mL, chloride Retinervus Luffae Fructus: 15g, water: 24mL; Ammonium persulfate.: 1g; nitrogen is protected, in 50 DEG C of constant temperature, stirring, back flow reaction 4.5 h, after cooling; be washed with deionized, sucking filtration; being neutrality to filtrate, vacuum drying oven is dried, obtains dimethyl diallyl ammonium chloride modified loofah sponge adsorbent.
Embodiment 2
(1) Retinervus Luffae Fructus pretreatment: Retinervus Luffae Fructus derives from Fructus Luffae fruit, is obtained by peeling enucleation, pulverizes, by the sieve of 20 mesh, obtain pretreatment Retinervus Luffae Fructus after the clear water cleaning, drying that are cut into small pieces by Retinervus Luffae Fructus；
(2) oxidation Retinervus Luffae Fructus: in the reactor, be separately added into pretreatment Retinervus Luffae Fructus: 10g, water: 82mL, NaOH:8g, soaking at room temperature 24 h, then boil 40min, it is washed with deionized after cooling to neutrality, place in 80mL concentrated nitric acid, in 85 DEG C of constant temperature, stirring, back flow reaction 90 min, after cooling, be washed with deionized, sucking filtration, being neutrality to filtrate, vacuum drying oven is dried, obtains aoxidizing Retinervus Luffae Fructus；
(3) prepared by chloride Retinervus Luffae Fructus: in the reactor, it is separately added into dimethylformamide 40mL, thionyl chloride: 28mL, oxidation Retinervus Luffae Fructus: 15g, in 65 DEG C of constant temperature, stirring, back flow reaction 60 h, wash with acetone reflux after completion of the reaction, remove dimethylformamide and the thionyl chloride of surface adhesion, put after taking-up in vacuum drying oven and be dried, obtain chloride Retinervus Luffae Fructus；
(4) preparation of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent: in the reactor; it is separately added into dimethyl diallyl ammonium chloride: 66mL, chloride Retinervus Luffae Fructus: 20g, water: 12mL; Ammonium persulfate.: 2g; nitrogen is protected, in 45 DEG C of constant temperature, stirring, back flow reaction 4 h, after cooling; be washed with deionized, sucking filtration; being neutrality to filtrate, vacuum drying oven is dried, obtains dimethyl diallyl ammonium chloride modified loofah sponge adsorbent.
Embodiment 3
(1) Retinervus Luffae Fructus pretreatment: Retinervus Luffae Fructus derives from Fructus Luffae fruit, is obtained by peeling enucleation, pulverizes, by the sieve of 40 mesh, obtain pretreatment Retinervus Luffae Fructus after the clear water cleaning, drying that are cut into small pieces by Retinervus Luffae Fructus；
(2) oxidation Retinervus Luffae Fructus: in the reactor, be separately added into pretreatment Retinervus Luffae Fructus: 18g, water: 72mL, NaOH:10g, soaking at room temperature 12 h, then boil 20min, it is washed with deionized after cooling to neutrality, place in 90mL concentrated nitric acid, in 95 DEG C of constant temperature, stirring, back flow reaction 120 min, after cooling, be washed with deionized, sucking filtration, being neutrality to filtrate, vacuum drying oven is dried, obtains aoxidizing Retinervus Luffae Fructus；
(3) prepared by chloride Retinervus Luffae Fructus: in the reactor, it is separately added into dimethylformamide 27mL, thionyl chloride: 37mL, oxidation Retinervus Luffae Fructus: 13g, in 75 DEG C of constant temperature, stirring, back flow reaction 50 h, wash with acetone reflux after completion of the reaction, remove dimethylformamide and the thionyl chloride of surface adhesion, put after taking-up in vacuum drying oven and be dried, obtain chloride Retinervus Luffae Fructus；
(4) preparation of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent: in the reactor; it is separately added into dimethyl diallyl ammonium chloride: 70mL, chloride Retinervus Luffae Fructus: 10g, water: 20mL; Ammonium persulfate.: 0.5g; nitrogen is protected, in 55 DEG C of constant temperature, stirring, back flow reaction 5 h, after cooling; be washed with deionized, sucking filtration; being neutrality to filtrate, vacuum drying oven is dried, obtains dimethyl diallyl ammonium chloride modified loofah sponge adsorbent.
Embodiment 4
(1) Retinervus Luffae Fructus pretreatment: Retinervus Luffae Fructus derives from Fructus Luffae fruit, is obtained by peeling enucleation, pulverizes, by the sieve of 10 mesh, obtain pretreatment Retinervus Luffae Fructus after the clear water cleaning, drying that are cut into small pieces by Retinervus Luffae Fructus；
(2) oxidation Retinervus Luffae Fructus: in the reactor, be separately added into pretreatment Retinervus Luffae Fructus: 10g, water: 85mL, NaOH:5g, soaking at room temperature 18h, then boil 25min, it is washed with deionized after cooling to neutrality, place in 100mL concentrated nitric acid, in 85 DEG C of constant temperature, stirring, back flow reaction 120 min, after cooling, be washed with deionized, sucking filtration, being neutrality to filtrate, vacuum drying oven is dried, obtains aoxidizing Retinervus Luffae Fructus；
(3) prepared by chloride Retinervus Luffae Fructus: in the reactor, it is separately added into dimethylformamide 45mL, thionyl chloride: 26mL, oxidation Retinervus Luffae Fructus: 12g, in 65 DEG C of constant temperature, stirring, back flow reaction 58 h, wash with acetone reflux after completion of the reaction, remove dimethylformamide and the thionyl chloride of surface adhesion, put after taking-up in vacuum drying oven and be dried, obtain chloride Retinervus Luffae Fructus；
(4) preparation of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent: in the reactor; it is separately added into dimethyl diallyl ammonium chloride: 56mL, chloride Retinervus Luffae Fructus: 18g, water: 25mL; Ammonium persulfate.: 1g; nitrogen is protected, in 50 DEG C of constant temperature, stirring, back flow reaction 5 h, after cooling; be washed with deionized, sucking filtration; being neutrality to filtrate, vacuum drying oven is dried, obtains dimethyl diallyl ammonium chloride modified loofah sponge adsorbent.
Embodiment 5
(1) Retinervus Luffae Fructus pretreatment: Retinervus Luffae Fructus derives from Fructus Luffae fruit, is obtained by peeling enucleation, pulverizes, by the sieve of 10 mesh, obtain pretreatment Retinervus Luffae Fructus after the clear water cleaning, drying that are cut into small pieces by Retinervus Luffae Fructus；
(2) oxidation Retinervus Luffae Fructus: in the reactor, be separately added into pretreatment Retinervus Luffae Fructus: 12g, water: 82mL, NaOH:6g, soaking at room temperature 15 h, then boil 30min, it is washed with deionized after cooling to neutrality, place in 120mL concentrated nitric acid, in 85 DEG C of constant temperature, stirring, back flow reaction 100 min, after cooling, be washed with deionized, sucking filtration, being neutrality to filtrate, vacuum drying oven is dried, obtains aoxidizing Retinervus Luffae Fructus；
(3) prepared by chloride Retinervus Luffae Fructus: in the reactor, it is separately added into dimethylformamide 25mL, thionyl chloride: 36mL, oxidation Retinervus Luffae Fructus: 17g, in 70 DEG C of constant temperature, stirring, back flow reaction 60 h, wash with acetone reflux after completion of the reaction, remove dimethylformamide and the thionyl chloride of surface adhesion, put after taking-up in vacuum drying oven and be dried, obtain chloride Retinervus Luffae Fructus；
(4) preparation of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent: in the reactor; it is separately added into dimethyl diallyl ammonium chloride: 65mL, chloride Retinervus Luffae Fructus: 12g, water: 22mL; Ammonium persulfate.: 1.5g; nitrogen is protected, in 55 DEG C of constant temperature, stirring, back flow reaction 4 h, after cooling; be washed with deionized, sucking filtration; being neutrality to filtrate, vacuum drying oven is dried, obtains dimethyl diallyl ammonium chloride modified loofah sponge adsorbent.
Embodiment 6
Weigh 0.50g dimethyl diallyl ammonium chloride modified loofah sponge adsorbent to be placed in 250mL tool plug conical flask, adding 100mL concentration is in 550mg/L lubricant oil solution, in the range of being 4.5 ~ 10.5 with the pH value of acid or alkali regulation system, at room temperature concussion absorption 2 ~ 4 h, take supernatant, the concentration of oil in solution is measured with infrared spectrum oil content analyzer, according to the concentration difference of oil in water before and after absorption, calculating the adsorption capacity of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent, its adsorption capacity can reach 106.28 Mg/g, the absorption of oil is not affected by pH value adsorbent in the range of 4.5 ~ 10.5, at room temperature concussion absorption more than 2h, adsorbent reaches saturated to the absorption of oil.
Embodiment 7
Weigh 1.0g dimethyl diallyl ammonium chloride modified loofah sponge adsorbent to be placed in 250mL tool plug conical flask, adding 100mL concentration is in 100mg/L oil-containing solutions, in the range of being 6.5 with the pH value of acid or alkali regulation system, at room temperature concussion absorption 4 h, take supernatant, measure the concentration of oil in solution with infrared spectrum oil content analyzer, according to the concentration difference of oil in water before and after absorption, calculate the dimethyl diallyl ammonium chloride modified loofah sponge adsorbent clearance to oil, reach as high as 98.5%%.

Claims (5)

1. the preparation method of a dimethyl diallyl ammonium chloride modified loofah sponge adsorbent, it is characterised in that the method have with Lower processing step:
(1) Retinervus Luffae Fructus pretreatment: Retinervus Luffae Fructus derives from Fructus Luffae fruit, is obtained by peeling enucleation, is cut into by Retinervus Luffae Fructus little Pulverize after block clear water cleaning, drying, by the sieve of 10～40 mesh, obtain pretreatment Retinervus Luffae Fructus；
(2) oxidation Retinervus Luffae Fructus: in the reactor, is added by following composition mass percent, pretreatment Retinervus Luffae Fructus: 10～20%, Water: 71～87%, NaOH:2～10%, each component sum is absolutely, soaking at room temperature 12～24h, then boils 20～40min, It is washed with deionized after cooling to neutrality, places in concentrated nitric acid, in 85～95 DEG C of constant temperature, stirring, back flow reaction 90～120min, After cooling, be washed with deionized, sucking filtration, being neutrality to filtrate, in vacuum drying oven be dried, obtain aoxidize Retinervus Luffae Fructus；
(3) prepared by chloride Retinervus Luffae Fructus: in the reactor, adds by following composition mass percent, dimethylformamide: 25～45%, thionyl chloride: 40～60%, aoxidize Retinervus Luffae Fructus: 8～18%, each component sum is absolutely, in 65～75 DEG C of perseverances Temperature, stirring, back flow reaction 50～60h, after completion of the reaction with acetone reflux wash, remove surface adhesion dimethylformamide and Thionyl chloride, puts after taking-up in vacuum drying oven and is dried, obtain chloride Retinervus Luffae Fructus；
(4) preparation of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent: in the reactor, by following composition quality hundred Proportion by subtraction adds, dimethyl diallyl ammonium chloride: 56～71%, chloride Retinervus Luffae Fructus: 10～20%, water: 12～26%, over cure Acid ammonium: 0.5～2.0%, each component sum is absolutely, and nitrogen is protected, in 45～55 DEG C of constant temperature, stirring, back flow reaction 4～5 H, after cooling, is washed with deionized, sucking filtration, being neutrality to filtrate, is dried, obtains dimethyl two in vacuum drying oven Allyl ammonium chloride modified loofah sponge adsorbent.
2. according to the preparation method of a kind of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent described in claim 1, It is characterized in that: Retinervus Luffae Fructus is Fructus Luffae fruit maturation, peel turns yellow, inside is plucked time withered, removes crust and sarcocarp.
3. according to the preparation method of a kind of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent described in claim 1, It is characterized in that: instrument and equipment used in step (3), reagent can not be aqueous.
4. adsorb according to the dimethyl diallyl ammonium chloride modified loofah sponge prepared by the preparation method described in claim 1 Agent, it is characterised in that: the absorption of oils and fats in dimethyl diallyl ammonium chloride modified loofah sponge Adsorbent For Removal of Heavy.
5. according to the suction of oils and fats in the dimethyl diallyl ammonium chloride modified loofah sponge Adsorbent For Removal of Heavy described in claim 4 It is attached, it is characterised in that: in waste water, oils and fats includes: crude oil, diesel oil, machine oil, vegetable oil, gasoline.
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