CN104289187A - Preparation of dimethyl diallyl ammonium chloride modified towel gourd vegetable sponge adsorbent - Google Patents
Preparation of dimethyl diallyl ammonium chloride modified towel gourd vegetable sponge adsorbent Download PDFInfo
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- CN104289187A CN104289187A CN201410456613.6A CN201410456613A CN104289187A CN 104289187 A CN104289187 A CN 104289187A CN 201410456613 A CN201410456613 A CN 201410456613A CN 104289187 A CN104289187 A CN 104289187A
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- luffa
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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
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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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
- 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
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Abstract
The invention discloses a preparation method and an application technology of a dimethyl diallyl ammonium chloride modified towel gourd vegetable sponge adsorbent, and is characterized in that the preparation method comprises the steps: peeling and denucleating mature fruits of towel gourd, washing with water to remove soil and impurities, drying, crushing, and carrying out chemical treatment drying to obtain acylating-chlorination towel gourd vegetable sponge; adding, by the mass percentage, 56-71% of dimethyl diallyl ammonium chloride, 10-20% of the acylating-chlorination towel gourd vegetable sponge, 12-26% of water and 0.5-2.0% of ammonium persulfate into a reactor, wherein the sum of the percentages of all the components is 100%; under the nitrogen protection and at a constant temperature of 45-55 DEG C, stirring and carrying out a reflux reaction for 4-5 h; and after cooling, washing with deionized water, carrying out suction filtration until a filtrate is neutral, drying in a vacuum drying oven, and thus obtaining the dimethyl diallyl ammonium chloride modified towel gourd vegetable sponge adsorbent. The adsorbent has the advantages of quite high adsorption capacity on grease, excellent physicochemical and mechanical properties, strong regeneration capacity, capacity of being repeatedly used many times, low cost, greenness and environmental protection.
Description
Technical field
The present invention relates to a kind of preparation method of biological adsorption agent, belong to water-treatment technology field, what be suitable for oil-polluted water removes oil purification, particularly a kind of preparations and applicatio technology of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent.
Background technology
Oily waste water is mainly derived from the oil recovery of petroleum industry, oil refining, store oil, the process such as 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.Rules and regulations such as " People's Republic of China's law of marine environmental protections " that current China promulgates, the highest permission concentration of emission of oily waste water is 10 mg/L.So, the multiple fields of petrochemical industry and environmental protection etc. instantly that the are treated as problem demanding prompt solution of oily waste water.Absorption method is the one in numerous treatment process, and the research of the many scholars of recent domestic to absorption method process oily waste water focuses mostly at the adsorption efficiency improving adsorbent, probes into the method for modifying etc. of adsorbent.It is simple that its absorption method has technique, and adsorption rate is high, applied widely, and the features such as stable in properties are used widely in sewage disposal.Adsorbent for oily waste water absorption has active carbon, 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, (Gao Sainan 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 absorption property of expanded graphite to oily waste water, (Wang Shuzhao etc. expanded graphite is to the Study on adsorption properties of oily waste water. scientific and technical innovation Leader .2012 (22): 7-8); Shu Ming is brave etc. have studied the test of modified alta-mud process emulsifying liquid waste water, Shu Mingyong etc. the experimental study of modified alta-mud process emulsifying liquid waste water. and 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 application study of oily waste water. flyash, 2012 (3): 10-14).
Shortage of resources and environmental pollution have become two large subject matters of the world today, and therefore, utilize natural reproducible resource, development environment friendly product and technology will become the inexorable trend of sustainable development.Luffa is the withered old fruit of vascular bundle in the ripening fruits of Curcurbitaceae annual herb plant sponge gourd sponge gourd in other words.Sponge gourd is China's summer and autumn Common Vegetables, there is product most provinces and regions, the whole nation, for cultivation product, luffa is the regenerated resources that the earth enriches very much, have that light weight is inexpensive, the feature such as degradable and environmental friendliness, luffa is by the net of the thread fiber interweaving of multilayer, body is light, matter is tough and tensile, can not fracture, simultaneously containing xylan, mannosan, galactan etc., and it has hydrophily, also with abundant dentate, be easy to carry out chemical modification, domestic luffa is modified as the application of adsorbent in adsorption of metal ions.
Domestic luffa is as the application of adsorbent in adsorption of metal ions, application number is disclose luffa in the patent of 200810034734.6 to many kinds of metal ions absorption property and luffa as the application of adsorbent in adsorption of metal ions, and wherein luffa is to Cu
2+and Zn
2+desorption rate all about 40%, luffa is to Cu
2+adsorbance be respectively 0.16mmol/g, to Zn
2+adsorbance be about 0.39mmol/g, be that in the system of 1, desorption rate is respectively 46%, 47% at pH; Be the alkalization modifying method and the application thereof that disclose luffa in the patent of 200810034735.0 at application number, its alkali treatment luffa is to Zn
2+adsorbance comparatively Cu
2+height, and adsorbance gap is comparatively large, through Atomic absorption quantitative analysis, luffa is to Cu
2+adsorbance be about 7 ~ 8mg/g, to Zn
2+adsorbance be about 21 ~ 22mg/g; Be disclose the preparation method of etherized luffa and the application in adsorption of metal ions thereof in the patent of 200810034737.X at application number, its etherized luffa is to Fe
3+maximal absorptive capacity be 27.4mg/g.To Zn
2+maximal absorptive capacity be 36.3mg/g; Application number is disclose citric acid loofah sponge preparation method agent application in the patent of 201110276244.9, and its citric acid loofah sponge is to Cd
2+adsorption capacity can up to 189mg/g, most high adsorption rate can reach 98.5%, to Pb
2+maximal absorptive capacity be 285mg/g, most high adsorption rate can reach 99.2%, be 316mg/g to the maximal absorptive capacity of methylene blue, most high adsorption rate can reach 96.2%, there is carboxylic acid characteristic, can directly to absorption and the wash-out of metal ion species each in water body, organic dyestuff, but not used for the absorption of useless oil-in-water.
Since the nineties in 20th century, people utilize natural fiber cheap and easy to get in the process of waste water, to obtain more research as adsorbent.Neha Gupta etc. have studied methylene blue in potato stalk adsorbed water and malachite green, 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 Chinese parasol tree 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 peanut shell adsorbed water, it to the maximum adsorption capacity of methyl blue is: 25mg/g, (Li Shan etc., the research of methylene blue in epoxychloropropane modified peanut shell adsorbed water, dyestuff and dyeing, 2008,45(2): 49 ~ 51); But natural fiber is applied as adsorbent and is had no report in adsorbed 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 a kind of preparation method of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent, mainly makes the dimethyl diallyl ammonium chloride modified loofah sponge adsorbent of acquisition larger to the adsorption capacity of grease in waste water.
Object of the present invention is achieved through the following technical solutions.
A preparation method for dimethyl diallyl ammonium chloride modified loofah sponge adsorbent, is characterised in that the method has following processing step:
(1) luffa pretreatment: luffa derives from sponge gourd fruit, is obtained by peeling stoning, pulverizes, by 10 ~ 40 object sieve, obtain pretreatment luffa after the clear water cleaning, drying that are cut into small pieces by luffa;
(2) luffa is oxidized: in the reactor, add by following composition mass percent, pretreatment luffa: 10 ~ 20%, water: 71 ~ 87%, NaOH:2 ~ 10%, each component sum is absolutely, soaking at room temperature 12 ~ 24 h, then boils 20 ~ 40min, deionized water is spent to neutral after cooling, put into red fuming nitric acid (RFNA) again, in 85 ~ 95 DEG C of constant temperature, stirring, back flow reaction 90 ~ 120 min, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, dry in vacuum drying chamber, obtain being oxidized luffa;
(3) chloride luffa preparation: in the reactor, add by following composition mass percent, dimethyl formamide: 25 ~ 45%, thionyl chloride: 40 ~ 60%, oxidation luffa: 8 ~ 18%, each component sum is absolutely, in 65 ~ 75 DEG C of constant temperature, stirring, back flow reaction 50 ~ 60 h, after completion of the reaction with acetone reflux washing, the dimethyl formamide of removing surface adhesion and thionyl chloride, put in vacuum drying chamber dry after taking-up, obtain chloride luffa;
(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 luffa: 10 ~ 20%; water: 12 ~ 26%; ammonium persulfate: 0.5 ~ 2.0%; each component sum is absolutely; nitrogen protection, in 45 ~ 55 DEG C of constant temperature, stirring, back flow reaction 4 ~ 5 h, after cooling; spend deionized water, suction filtration; to filtrate is neutrality, dry in vacuum drying chamber, obtain dimethyl diallyl ammonium chloride modified loofah sponge adsorbent.
Another object of the present invention is to provide dimethyl diallyl ammonium chloride modified loofah sponge adsorbent in aqueous systems to the absorption of oil, 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 is soaked 0.5 ~ 1.0h, and by dynamic method absorption, flow velocity is 1.0 mL/min.
Advantage of the present invention and effect are:
(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 large, and Reusability number of times can reach more than 10 times;
(2) the dimethyl diallyl ammonium chloride modified loofah sponge adsorbent that the present invention obtains all has better absorption and wash-out to grease various in water body (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, can use within the scope of wider soda acid;
(3) density due to dimethyl diallyl ammonium chloride modified loofah sponge adsorbent is little, can swim in water surface, and the chance contacted with grease is many, to oil clearance high, be natural green product, biodegradable, environmental protection;
(4) condition of the process entails synthesized easily controls, and energy consumption is low, simple to operate, and renewable resource utilization is easy to suitability for industrialized production.
Detailed description of the invention
Embodiment 1
(1) luffa pretreatment: luffa derives from sponge gourd fruit, is obtained by peeling stoning, pulverizes, by 10 object sieve, obtain pretreatment luffa after the clear water cleaning, drying that are cut into small pieces by luffa;
(2) luffa is oxidized: in the reactor, add pretreatment luffa respectively: 15g, water: 80mL, NaOH:5g, soaking at room temperature 20 h, then boil 30min, deionized water is spent to neutral after cooling, put into 100mL red fuming nitric acid (RFNA) again, in 90 DEG C of constant temperature, stirring, back flow reaction 100 min, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, dry in vacuum drying chamber, obtain being oxidized luffa;
(3) chloride luffa preparation: in the reactor, add dimethyl formamide 35mL respectively, thionyl chloride: 35mL, oxidation luffa: 10g, in 70 DEG C of constant temperature, stirring, back flow reaction 55 h, after completion of the reaction with acetone reflux washing, the dimethyl formamide of removing surface adhesion and thionyl chloride, put in vacuum drying chamber dry after taking-up, obtain chloride luffa;
(4) preparation of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent: in the reactor; add dimethyl diallyl ammonium chloride respectively: 60mL, chloride luffa: 15g, water: 24mL; ammonium persulfate: 1g; nitrogen protection, in 50 DEG C of constant temperature, stirring, back flow reaction 4.5 h, after cooling; spend deionized water, suction filtration; to filtrate is neutrality, dry in vacuum drying chamber, obtain dimethyl diallyl ammonium chloride modified loofah sponge adsorbent.
Embodiment 2
(1) luffa pretreatment: luffa derives from sponge gourd fruit, is obtained by peeling stoning, pulverizes, by 20 object sieve, obtain pretreatment luffa after the clear water cleaning, drying that are cut into small pieces by luffa;
(2) luffa is oxidized: in the reactor, add pretreatment luffa respectively: 10g, water: 82mL, NaOH:8g, soaking at room temperature 24 h, then boil 40min, deionized water is spent to neutral after cooling, put into 80mL red fuming nitric acid (RFNA) again, in 85 DEG C of constant temperature, stirring, back flow reaction 90 min, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, dry in vacuum drying chamber, obtain being oxidized luffa;
(3) chloride luffa preparation: in the reactor, add dimethyl formamide 40mL respectively, thionyl chloride: 28mL, oxidation luffa: 15g, in 65 DEG C of constant temperature, stirring, back flow reaction 60 h, after completion of the reaction with acetone reflux washing, the dimethyl formamide of removing surface adhesion and thionyl chloride, put in vacuum drying chamber dry after taking-up, obtain chloride luffa;
(4) preparation of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent: in the reactor; add dimethyl diallyl ammonium chloride respectively: 66mL, chloride luffa: 20g, water: 12mL; ammonium persulfate: 2g; nitrogen protection, in 45 DEG C of constant temperature, stirring, back flow reaction 4 h, after cooling; spend deionized water, suction filtration; to filtrate is neutrality, dry in vacuum drying chamber, obtain dimethyl diallyl ammonium chloride modified loofah sponge adsorbent.
Embodiment 3
(1) luffa pretreatment: luffa derives from sponge gourd fruit, is obtained by peeling stoning, pulverizes, by 40 object sieve, obtain pretreatment luffa after the clear water cleaning, drying that are cut into small pieces by luffa;
(2) luffa is oxidized: in the reactor, add pretreatment luffa respectively: 18g, water: 72mL, NaOH:10g, soaking at room temperature 12 h, then boil 20min, deionized water is spent to neutral after cooling, put into 90mL red fuming nitric acid (RFNA) again, in 95 DEG C of constant temperature, stirring, back flow reaction 120 min, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, dry in vacuum drying chamber, obtain being oxidized luffa;
(3) chloride luffa preparation: in the reactor, add dimethyl formamide 27mL respectively, thionyl chloride: 37mL, oxidation luffa: 13g, in 75 DEG C of constant temperature, stirring, back flow reaction 50 h, after completion of the reaction with acetone reflux washing, the dimethyl formamide of removing surface adhesion and thionyl chloride, put in vacuum drying chamber dry after taking-up, obtain chloride luffa;
(4) preparation of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent: in the reactor; add dimethyl diallyl ammonium chloride respectively: 70mL, chloride luffa: 10g, water: 20mL; ammonium persulfate: 0.5g; nitrogen protection, in 55 DEG C of constant temperature, stirring, back flow reaction 5 h, after cooling; spend deionized water, suction filtration; to filtrate is neutrality, dry in vacuum drying chamber, obtain dimethyl diallyl ammonium chloride modified loofah sponge adsorbent.
Embodiment 4
(1) luffa pretreatment: luffa derives from sponge gourd fruit, is obtained by peeling stoning, pulverizes, by 10 object sieve, obtain pretreatment luffa after the clear water cleaning, drying that are cut into small pieces by luffa;
(2) luffa is oxidized: in the reactor, add pretreatment luffa respectively: 10g, water: 85mL, NaOH:5g, soaking at room temperature 18h, then boil 25min, deionized water is spent to neutral after cooling, put into 100mL red fuming nitric acid (RFNA) again, in 85 DEG C of constant temperature, stirring, back flow reaction 120 min, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, dry in vacuum drying chamber, obtain being oxidized luffa;
(3) chloride luffa preparation: in the reactor, add dimethyl formamide 45mL respectively, thionyl chloride: 26mL, oxidation luffa: 12g, in 65 DEG C of constant temperature, stirring, back flow reaction 58 h, after completion of the reaction with acetone reflux washing, the dimethyl formamide of removing surface adhesion and thionyl chloride, put in vacuum drying chamber dry after taking-up, obtain chloride luffa;
(4) preparation of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent: in the reactor; add dimethyl diallyl ammonium chloride respectively: 56mL, chloride luffa: 18g, water: 25mL; ammonium persulfate: 1g; nitrogen protection, in 50 DEG C of constant temperature, stirring, back flow reaction 5 h, after cooling; spend deionized water, suction filtration; to filtrate is neutrality, dry in vacuum drying chamber, obtain dimethyl diallyl ammonium chloride modified loofah sponge adsorbent.
Embodiment 5
(1) luffa pretreatment: luffa derives from sponge gourd fruit, is obtained by peeling stoning, pulverizes, by 10 object sieve, obtain pretreatment luffa after the clear water cleaning, drying that are cut into small pieces by luffa;
(2) luffa is oxidized: in the reactor, add pretreatment luffa respectively: 12g, water: 82mL, NaOH:6g, soaking at room temperature 15 h, then boil 30min, deionized water is spent to neutral after cooling, put into 120mL red fuming nitric acid (RFNA) again, in 85 DEG C of constant temperature, stirring, back flow reaction 100 min, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, dry in vacuum drying chamber, obtain being oxidized luffa;
(3) chloride luffa preparation: in the reactor, add dimethyl formamide 25mL respectively, thionyl chloride: 36mL, oxidation luffa: 17g, in 70 DEG C of constant temperature, stirring, back flow reaction 60 h, after completion of the reaction with acetone reflux washing, the dimethyl formamide of removing surface adhesion and thionyl chloride, put in vacuum drying chamber dry after taking-up, obtain chloride luffa;
(4) preparation of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent: in the reactor; add dimethyl diallyl ammonium chloride respectively: 65mL, chloride luffa: 12g, water: 22mL; ammonium persulfate: 1.5g; nitrogen protection, in 55 DEG C of constant temperature, stirring, back flow reaction 4 h, after cooling; spend deionized water, suction filtration; to filtrate is neutrality, dry in vacuum drying chamber, obtain dimethyl diallyl ammonium chloride modified loofah sponge adsorbent.
Embodiment 6
Take 0.50g dimethyl diallyl ammonium chloride modified loofah sponge adsorbent and be placed in 250mL tool plug conical flask, adding 100mL concentration is in 550mg/L lubricant oil solution, be in 4.5 ~ 10.5 scopes with acid or the pH value of alkali regulation system, at room temperature shake absorption 2 ~ 4 h, get 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, calculate the adsorption capacity of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent, its adsorption capacity can reach 106.28 mg/g, pH value adsorbent absorption on oil in 4.5 ~ 10.5 scopes does not affect, , at room temperature concussion absorption more than 2h, the absorption of adsorbent to oil reaches capacity.
Embodiment 7
Take 1.0g dimethyl diallyl ammonium chloride modified loofah sponge adsorbent and be placed in 250mL tool plug conical flask, adding 100mL concentration is in 100mg/L oil-containing solutions, be in 6.5 scopes with acid or the pH value of alkali regulation system, at room temperature shake absorption 4 h, get 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 dimethyl diallyl ammonium chloride modified loofah sponge adsorbent to the clearance of oil, reach as high as 98.5%%.
Claims (5)
1. a preparation method for dimethyl diallyl ammonium chloride modified loofah sponge adsorbent, is characterised in that the method has following processing step:
(1) luffa pretreatment: luffa derives from sponge gourd fruit, is obtained by peeling stoning, pulverizes, by 10 ~ 40 object sieve, obtain pretreatment luffa after the clear water cleaning, drying that are cut into small pieces by luffa;
(2) luffa is oxidized: in the reactor, add by following composition mass percent, pretreatment luffa: 10 ~ 20%, water: 71 ~ 87%, NaOH:2 ~ 10%, each component sum is absolutely, soaking at room temperature 12 ~ 24 h, then boils 20 ~ 40min, deionized water is spent to neutral after cooling, put into red fuming nitric acid (RFNA) again, in 85 ~ 95 DEG C of constant temperature, stirring, back flow reaction 90 ~ 120 min, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, dry in vacuum drying chamber, obtain being oxidized luffa;
(3) chloride luffa preparation: in the reactor, add by following composition mass percent, dimethyl formamide: 25 ~ 45%, thionyl chloride: 40 ~ 60%, oxidation luffa: 8 ~ 18%, each component sum is absolutely, in 65 ~ 75 DEG C of constant temperature, stirring, back flow reaction 50 ~ 60 h, after completion of the reaction with acetone reflux washing, the dimethyl formamide of removing surface adhesion and thionyl chloride, put in vacuum drying chamber dry after taking-up, obtain chloride luffa;
(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 luffa: 10 ~ 20%; water: 12 ~ 26%; ammonium persulfate: 0.5 ~ 2.0%; each component sum is absolutely; nitrogen protection, in 45 ~ 55 DEG C of constant temperature, stirring, back flow reaction 4 ~ 5 h, after cooling; spend deionized water, suction filtration; to filtrate is neutrality, dry in vacuum drying chamber, obtain dimethyl diallyl 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, be characterised in that: pluck when luffa is sponge gourd fruit maturation, pericarp turns yellow, inside is withered, removing crust and pulp.
3., according to the preparation method of a kind of dimethyl diallyl ammonium chloride modified loofah sponge adsorbent described in claim 1, be characterised in that: instrument and equipment used in step (3), reagent can not be moisture.
4. dimethyl diallyl ammonium chloride modified loofah sponge adsorbent prepared by the preparation method described in claim 1, is characterised in that: the absorption of grease in dimethyl diallyl ammonium chloride modified loofah sponge Adsorbent For Removal of Heavy.
5. comprise according to grease in the waste water described in claim 4: crude oil, diesel oil, lubricating oil, machine oil, vegetable oil, gasoline.
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| CN105709700A (en) * | 2016-05-05 | 2016-06-29 | 济南大学 | Preparation method of dimethyl-diallyl ammonium chloride modified reed stem adsorbent |
| CN105749868A (en) * | 2016-05-05 | 2016-07-13 | 济南大学 | Preparation of vinyl benzyl trimethyl ammonium chloride-modified carbon fibre adsorbent |
| CN105854826A (en) * | 2016-05-05 | 2016-08-17 | 济南大学 | Preparation of vinylbenzyltrimethylammonium chloride modified reed straw adsorbent |
| CN107456953A (en) * | 2017-09-11 | 2017-12-12 | 济南大学 | A kind of preparation method of the porous cotton complex microsphere of mercapto-propionyl-glycin modified magnetic |
| CN109107544A (en) * | 2018-08-31 | 2019-01-01 | 曲阜师范大学 | The luffa of hydrophobicity positive charge modification and its application in Solid Phase Extraction |
| CN115403136A (en) * | 2022-09-07 | 2022-11-29 | 岭南生态文旅股份有限公司 | Immobilized microorganism particles for domestic sewage decontamination and preparation method thereof |
| CN118059822A (en) * | 2024-04-19 | 2024-05-24 | 长春市东之星汽车配件有限公司 | Corncob filter element material for engine oil purification and preparation method |
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| JP2006346541A (en) * | 2005-06-14 | 2006-12-28 | Electric Power Dev Co Ltd | Method of manufacturing carboneous adsorbent, and method and apparatus of removing environmental pollutant by using the same |
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| CN105217781B (en) * | 2015-10-10 | 2017-11-24 | 浙江省环境保护科学设计研究院 | A kind of natural polymer subbase material for water treatment and preparation method thereof |
| CN105709700A (en) * | 2016-05-05 | 2016-06-29 | 济南大学 | Preparation method of dimethyl-diallyl ammonium chloride modified reed stem adsorbent |
| CN105749868A (en) * | 2016-05-05 | 2016-07-13 | 济南大学 | Preparation of vinyl benzyl trimethyl ammonium chloride-modified carbon fibre adsorbent |
| CN105854826A (en) * | 2016-05-05 | 2016-08-17 | 济南大学 | Preparation of vinylbenzyltrimethylammonium chloride modified reed straw adsorbent |
| CN105709700B (en) * | 2016-05-05 | 2017-11-14 | 济南大学 | A kind of dimethyl diallyl ammonium chloride is modified the preparation of reed rod adsorbent |
| CN107456953A (en) * | 2017-09-11 | 2017-12-12 | 济南大学 | A kind of preparation method of the porous cotton complex microsphere of mercapto-propionyl-glycin modified magnetic |
| CN109107544A (en) * | 2018-08-31 | 2019-01-01 | 曲阜师范大学 | The luffa of hydrophobicity positive charge modification and its application in Solid Phase Extraction |
| CN115403136A (en) * | 2022-09-07 | 2022-11-29 | 岭南生态文旅股份有限公司 | Immobilized microorganism particles for domestic sewage decontamination and preparation method thereof |
| CN115403136B (en) * | 2022-09-07 | 2023-08-04 | 岭南生态文旅股份有限公司 | Immobilized microorganism particles for decontamination of domestic sewage and preparation method thereof |
| CN118059822A (en) * | 2024-04-19 | 2024-05-24 | 长春市东之星汽车配件有限公司 | Corncob filter element material for engine oil purification and preparation method |
| CN118059822B (en) * | 2024-04-19 | 2024-06-25 | 长春市东之星汽车配件有限公司 | Corncob filter element material for engine oil purification and preparation method |
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