CN104289190B - A kind of preparation of dimethyl diallyl ammonium chloride modified fiber crops adsorbent - Google Patents
A kind of preparation of dimethyl diallyl ammonium chloride modified fiber crops adsorbent Download PDFInfo
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- CN104289190B CN104289190B CN201410456878.6A CN201410456878A CN104289190B CN 104289190 B CN104289190 B CN 104289190B CN 201410456878 A CN201410456878 A CN 201410456878A CN 104289190 B CN104289190 B CN 104289190B
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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
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/045—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing sulfur, e.g. sulfates, thiosulfates, gypsum
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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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- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
Abstract
The invention discloses the preparation method of a kind of dimethyl diallyl ammonium chloride modified fiber crops adsorbent and application technology, it is characterized by: by the waste and old rope made of hemp, gunnysack is cleaned, pulverize after drying, chemically treated after drying, obtain chloride fiber crops, in the reactor, add by following composition mass percent, dimethyl diallyl ammonium chloride: 75 ~ 90%, chloride fiber crops: 5 ~ 18%, water: 2 ~ 10%, potassium peroxydisulfate: 0.5 ~ 3.0%, each component sum is absolutely, nitrogen protection, in 45 ± 3 DEG C of constant temperature, stirring, back flow reaction 4 ~ 6h, after cooling, with deionized water wash, sucking filtration, being neutrality to filtrate, vacuum drying oven dries, obtain dimethyl diallyl ammonium chloride modified fiber crops adsorbent.Oils and fats is had significantly high adsorption capacity, excellent physical chemistry and mechanical performance by this adsorbent, and regeneration capacity is strong, and often, not only cost had been low but also environmental protection, and was garbage recycling for Reusability, i.e. the creation of value has minimizing environmental pollution.
Description
Technical field
The present invention relates to the preparation method of a kind of biological adsorption agent and to the application of oils and fats absorption in industrial wastewater, 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 fiber crops adsorbent.
Background technology
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.Fiber crops are annual herbaceous plant, are one of the most valuable ecological resources, are a kind of Renewable resources.The cultivated area of whole nation Caulis et Folium Lini reaches more than 300 ten thousand mu at present, long stapled yield is typically in about 60kg/ mu, the features such as fiber crops have a series of premium properties as textile fabric, as excellent in softness, good luster, well-pressed, nice and cool, moisture pick-up properties and permeability, are very precious textile fiber materials.China is gunny products big producing country, and yield ranks first in the world.Having a large amount of discarded gunny products every year, such as the leftover bits and pieces etc. of gunnysack, the rope made of hemp, fiber crops seat and industrial waste, along with economic fast development, the garbage amount of fiber crops increases considerably, and deals with improperly and can cause the harm to environment.Make full use of the garbage of these fiber crops both to have reduced environmental pollution and also can create considerable economic benefit, the good mechanical property of fiber crops, density is little, utilize fiber crops synthesizing new adsorbent for the absorption of oils and fats in water body, this adsorbent is made to have feature natural, green, biodegradable simultaneously, can also swim in and the water surface has with oils and fats sufficient contact, the superiority being adsorbed with its uniqueness to oils and fats.
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 causing water hypoxia, biological death, causing serious environmental pollution.The rules and regulations such as " People's Republic of China's law of marine environmental protection " that current China promulgates, the highest permission concentration of emission of oily waste water is 10mg/L.So, the multiple fields of petrochemical industry and environmental conservation etc. instantly that the are treated as problem demanding prompt solution of oily waste water.Absorption method is the one in numerous process technique, and absorption method is processed the research of oily waste water and focuses mostly at the adsorption efficiency improving adsorbent by the many scholars of recent domestic, probes 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.Adsorbent for oily waste water absorption has activated 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, (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).
Fiber crops are modified to be had been reported as the relevant research of adsorbent, Chinese patent CN103464115A discloses one and grows flax the preparation of adsorbent and application, it is characterized in that: chopped fiber Caulis et Folium Lini that Flax Textile Enterprises is discarded is washed, pulverizes after drying, process with NaOH and OP aqueous solution dried, obtain degumming Caulis et Folium Lini, in the reactor, add by following composition mass percent, epoxychloropropane: 22~40%, degumming Caulis et Folium Lini: 12~25%, NaOH:4~8%;Isopropanol: 5~10%;Water: 32~55%, each component sum is absolutely, in 55~65 DEG C of constant temperature, stirring, back flow reaction 1.0~4h, after cooling, with deionized water wash, sucking filtration, being neutrality to filtrate, after a small amount of washing with alcohol, dry, obtain epoxychloropropane and modify Caulis et Folium Lini, for the absorption of water neutral and alkali dyestuff.Chinese patent CN103933942A discloses preparation and the application of the modified Caulis et Folium Lini adsorbent of a kind of mercaptopropyl trimethoxysilane, it is characterized in that: Caulis et Folium Lini is cleaned, cut short, pulverize after drying, process, with treatment fluid A and treatment fluid B, the Caulis et Folium Lini pulverized respectively dried, Caulis et Folium Lini must be aoxidized, in the reactor, add by following composition mass percent, N, dinethylformamide: 50~75%, aoxidizes Caulis et Folium Lini: 10~30%;It is heated with stirring to 65~75 DEG C, is slowly added dropwise thionyl chloride: 12~25%, dropwise, temperature rises to 80~90 DEG C, and isothermal reaction 3~5h is cooled to room temperature, add mercaptopropyl trimethoxysilane: 1.0~3.0%, stirring reaction 6~12h under room temperature, filters, with N, after dinethylformamide washing, vacuum drying, obtains the modified Caulis et Folium Lini of mercaptopropyl trimethoxysilane, adsorbs for arsenic in water in water body.Fiber crops are modified has no report for the adsorption removal of oils and fats in water body.
Summary of the invention
The preparation method that an object of the present invention is to provide a kind of dimethyl diallyl ammonium chloride modified fiber crops adsorbent, the dimethyl diallyl ammonium chloride modified fiber crops 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 fiber crops adsorbent, is characterised by that the method has following processing step:
(1) fiber crops pretreatment: the waste and old rope made of hemp, gunnysack are cleaned, pulverized after drying, by the sieve of 10~20 orders, obtains pretreatment fiber crops;
(2) oxidation fiber crops: in the reactor, add by following composition mass percent, pretreatment fiber crops: 8~20%, water: 15~25%, concentrated nitric acid: 56~75%, each component sum is absolutely, in 90 ± 3 DEG C of constant temperature, stirring, back flow reaction 90~120min, after cooling, with deionized water wash, sucking filtration, being neutrality to filtrate, dry in vacuum drying oven, obtain oxidation fiber crops;
(3) prepared by chloride fiber crops: in the reactor, add by following composition mass percent, dimethylformamide: 6~16%, thionyl chloride: 70~85%, oxidation fiber crops: 8~18%, each component sum is absolutely, in 70 ± 3 DEG C of constant temperature, stirring, back flow reaction 18~24h, wash with acetone reflux after completion of the reaction, remove dimethylformamide and the thionyl chloride of surface adhesion, put in vacuum drying oven dry after taking-up, obtain chloride fiber crops;
(4) preparation of dimethyl diallyl ammonium chloride modified fiber crops adsorbent: in the reactor; add by following composition mass percent; dimethyl diallyl ammonium chloride: 75~90%; chloride fiber crops: 5~18%; water: 2~10%; potassium peroxydisulfate: 0.5~3.0%; each component sum is absolutely; nitrogen protection, in 45 ± 3 DEG C of constant temperature, stirring, back flow reaction 4~6h, after cooling; with deionized water wash, sucking filtration; being neutrality to filtrate, dry in vacuum drying oven, obtain dimethyl diallyl ammonium chloride modified fiber crops adsorbent.
Concentrated nitric acid mass percentage concentration described in step (2) is 68%.
Thionyl chloride described in step (3) is optimum with the mass ratio 10:1 of dimethylformamide.
Dimethyl diallyl ammonium chloride purity described in step (4) is mass percentage concentration 60% aqueous solution.
It is a further object of the present invention to provide dimethyl diallyl ammonium chloride modified fiber crops adsorbent in aqueous systems to oily absorption, feature is: the dimethyl diallyl ammonium chloride modified fiber crops adsorbent deionized water prepared is soaked 0.5~1.0h, adsorbs by static method.
The dimethyl diallyl ammonium chloride modified fiber crops adsorbent deionized water prepared being soaked 0.5~1.0h, adsorbs by dynamic method, flow velocity is 1.0mL/min.
Advantages of the present invention and effect be:
(1) dimethyl diallyl ammonium chloride that the present invention obtains modified fiber crops adsorbent has good physical and chemical stability and excellent mechanical strength, and Reusability number of times is up to more than 10 times;
(2) oils and fatss various in water body (such as crude oil, diesel oil, lubricating oil, machine oil, vegetable oil, gasoline etc.) are all had better absorption and eluting by the dimethyl diallyl ammonium chloride that the present invention obtains modified fiber crops adsorbent, adsorption efficiency is high, the speed of absorption is fast, and adsorption capacity is up to 112.61mg/g;
(3) owing to the density of dimethyl diallyl ammonium chloride modified fiber crops adsorbent is little, it is possible to swimming in water surface, chance contact with oils and fats is many, to oil clearance height, 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) fiber crops pretreatment: the waste and old rope made of hemp, gunnysack are cleaned, pulverized after drying, by the sieve of 10 orders, obtains pretreatment fiber crops;
(2) oxidation fiber crops: in the reactor, it is separately added into, pretreatment fiber crops: 14g, water: 20mL, concentrated nitric acid: 66mL, in 90 ± 3 DEG C of constant temperature, stirring, back flow reaction 100min, after cooling, with deionized water wash, sucking filtration, being neutrality to filtrate, vacuum drying oven dries, obtains oxidation fiber crops;
(3) prepared by chloride fiber crops: in the reactor, it is separately added into dimethylformamide: 11mL, thionyl chloride: 47mL, oxidation fiber crops: 13g, in 70 ± 3 DEG C of constant temperature, stirring, back flow reaction 20h, wash with acetone reflux after completion of the reaction, remove dimethylformamide and the thionyl chloride of surface adhesion, put in vacuum drying oven dry after taking-up, obtain chloride fiber crops;
(4) preparation of dimethyl diallyl ammonium chloride modified fiber crops adsorbent: in the reactor; it is separately added into dimethyl diallyl ammonium chloride: 81mL, chloride fiber crops: 12g, water: 6mL; potassium peroxydisulfate: 1.0g; nitrogen protection, in 45 ± 3 DEG C of constant temperature, stirring, back flow reaction 5h, after cooling; with deionized water wash, sucking filtration; being neutrality to filtrate, dry in vacuum drying oven, obtain dimethyl diallyl ammonium chloride modified fiber crops adsorbent.
Embodiment 2
(1) fiber crops pretreatment: the waste and old rope made of hemp, gunnysack are cleaned, pulverized after drying, by the sieve of 20 orders, obtains pretreatment fiber crops;
(2) oxidation fiber crops: in the reactor, be separately added into, pretreatment fiber crops: 8g, water: 17mL, concentrated nitric acid: 75mL, in 90 ± 3 DEG C of constant temperature, stirring, back flow reaction 90min, after cooling, with deionized water wash, sucking filtration, being neutrality to filtrate, dry in vacuum drying oven, obtain oxidation fiber crops;
(3) prepared by chloride fiber crops: in the reactor, it is separately added into dimethylformamide: 6mL, thionyl chloride: 51mL, oxidation fiber crops: 10g, in 70 ± 3 DEG C of constant temperature, stirring, back flow reaction 18h, wash with acetone reflux after completion of the reaction, remove dimethylformamide and the thionyl chloride of surface adhesion, put in vacuum drying oven dry after taking-up, obtain chloride fiber crops;
(4) preparation of dimethyl diallyl ammonium chloride modified fiber crops adsorbent: in the reactor; it is separately added into dimethyl diallyl ammonium chloride: 90mL, chloride fiber crops: 5g, water: 3mL; potassium peroxydisulfate: 2g; nitrogen protection, in 45 ± 3 DEG C of constant temperature, stirring, back flow reaction 4h, after cooling; with deionized water wash, sucking filtration; being neutrality to filtrate, dry in vacuum drying oven, obtain dimethyl diallyl ammonium chloride modified fiber crops adsorbent.
Embodiment 3
(1) fiber crops pretreatment: the waste and old rope made of hemp, gunnysack are cleaned, pulverized after drying, by the sieve of 10 orders, obtains pretreatment fiber crops;
(2) oxidation fiber crops: in the reactor, it is separately added into, pretreatment fiber crops: 18g, water: 24mL, concentrated nitric acid: 56mL, in 90 ± 3 DEG C of constant temperature, stirring, back flow reaction 120min, after cooling, with deionized water wash, sucking filtration, being neutrality to filtrate, vacuum drying oven dries, obtains oxidation fiber crops;
(3) prepared by chloride fiber crops: in the reactor, it is separately added into dimethylformamide: 18mL, thionyl chloride: 45mL, oxidation fiber crops: 8g, in 70 ± 3 DEG C of constant temperature, stirring, back flow reaction 24h, wash with acetone reflux after completion of the reaction, remove dimethylformamide and the thionyl chloride of surface adhesion, put in vacuum drying oven dry after taking-up, obtain chloride fiber crops;
(4) preparation of dimethyl diallyl ammonium chloride modified fiber crops adsorbent: in the reactor; it is separately added into dimethyl diallyl ammonium chloride: 70mL, chloride fiber crops: 18g, water: 10mL; potassium peroxydisulfate: 2g; nitrogen protection, in 45 ± 3 DEG C of constant temperature, stirring, back flow reaction 6h, after cooling; with deionized water wash, sucking filtration; being neutrality to filtrate, dry in vacuum drying oven, obtain dimethyl diallyl ammonium chloride modified fiber crops adsorbent.
Embodiment 4
(1) fiber crops pretreatment: the waste and old rope made of hemp, gunnysack are cleaned, pulverized after drying, by the sieve of 10 orders, obtains pretreatment fiber crops;
(2) oxidation fiber crops: in the reactor, it is separately added into, pretreatment fiber crops: 10g, water: 15mL, concentrated nitric acid: 75mL, in 90 ± 3 DEG C of constant temperature, stirring, back flow reaction 110min, after cooling, with deionized water wash, sucking filtration, being neutrality to filtrate, vacuum drying oven dries, obtains oxidation fiber crops;
(3) prepared by chloride fiber crops: in the reactor, it is separately added into dimethylformamide: 8mL, thionyl chloride: 49mL, oxidation fiber crops: 12g, in 70 ± 3 DEG C of constant temperature, stirring, back flow reaction 22h, wash with acetone reflux after completion of the reaction, remove dimethylformamide and the thionyl chloride of surface adhesion, put in vacuum drying oven dry after taking-up, obtain chloride fiber crops;
(4) preparation of dimethyl diallyl ammonium chloride modified fiber crops adsorbent: in the reactor; it is separately added into dimethyl diallyl ammonium chloride: 75mL, chloride fiber crops: 14g, water: 8mL; potassium peroxydisulfate: 3g; nitrogen protection, in 45 ± 3 DEG C of constant temperature, stirring, back flow reaction 5h, after cooling; with deionized water wash, sucking filtration; being neutrality to filtrate, dry in vacuum drying oven, obtain dimethyl diallyl ammonium chloride modified fiber crops adsorbent.
Embodiment 5
(1) fiber crops pretreatment: the waste and old rope made of hemp, gunnysack are cleaned, pulverized after drying, by the sieve of 10 orders, obtains pretreatment fiber crops;
(2) oxidation fiber crops: in the reactor, it is separately added into, pretreatment fiber crops: 12g, water: 25mL, concentrated nitric acid: 63mL, in 90 ± 3 DEG C of constant temperature, stirring, back flow reaction 100min, after cooling, with deionized water wash, sucking filtration, being neutrality to filtrate, vacuum drying oven dries, obtains oxidation fiber crops;
(3) prepared by chloride fiber crops: in the reactor, it is separately added into dimethylformamide: 13mL, thionyl chloride: 44mL, oxidation fiber crops: 16g, in 70 ± 3 DEG C of constant temperature, stirring, back flow reaction 21h, wash with acetone reflux after completion of the reaction, remove dimethylformamide and the thionyl chloride of surface adhesion, put in vacuum drying oven dry after taking-up, obtain chloride fiber crops;
(4) preparation of dimethyl diallyl ammonium chloride modified fiber crops adsorbent: in the reactor; it is separately added into dimethyl diallyl ammonium chloride: 85mL, chloride fiber crops: 5g, water: 9mL; potassium peroxydisulfate: 1.0g; nitrogen protection, in 45 ± 3 DEG C of constant temperature, stirring, back flow reaction 4.5h, after cooling; with deionized water wash, sucking filtration; being neutrality to filtrate, dry in vacuum drying oven, obtain dimethyl diallyl ammonium chloride modified fiber crops adsorbent.
Embodiment 6
Weigh the modified fiber crops adsorbent agent of 0.50g dimethyl diallyl ammonium chloride and be placed in 250mL tool plug conical flask, adding 100mL concentration is in 550mg/L crude water solution, with the pH value of acid or alkali regulation system for 4.5~10.5 scopes, at room temperature concussion absorption 2~4h, 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, calculate the adsorption capacity of dimethyl diallyl ammonium chloride modified fiber crops adsorbent agent, its adsorption capacity can reach 121.22mg/g, the absorption of oil is not affected by pH value in 4.5~10.5 scope internal adsorption agent, at room temperature concussion absorption more than 2h, the absorption of oil is reached capacity by adsorbent.
Embodiment 7
Weigh the modified fiber crops adsorbent agent of 1.0g dimethyl diallyl ammonium chloride and be placed in 250mL tool plug conical flask, adding 100mL concentration is that 100mg/L is containing in crude water solution, with the pH value of acid or alkali regulation system for 6.5 scopes, at room temperature concussion absorption 4h, 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, calculate the dimethyl diallyl ammonium chloride modified fiber crops adsorbent agent clearance to oil, reach as high as 98.5%.
Claims (5)
1. the preparation method of a dimethyl diallyl ammonium chloride modified fiber crops adsorbent, it is characterised in that the method has following processing step:
(1) fiber crops pretreatment: the waste and old rope made of hemp, gunnysack are cleaned, pulverized after drying, by the sieve of 10~20 orders, obtains pretreatment fiber crops;
(2) oxidation fiber crops: in the reactor, add by following composition mass percent, pretreatment fiber crops: 8~20%, water: 15~25%, concentrated nitric acid: 56~75%, each component sum is absolutely, in 90 ± 3 DEG C of constant temperature, stirring, back flow reaction 90~120min, after cooling, with deionized water wash, sucking filtration, being neutrality to filtrate, dry in vacuum drying oven, obtain oxidation fiber crops;
(3) prepared by chloride fiber crops: in the reactor, add by following composition mass percent, dimethylformamide: 6~16%, thionyl chloride: 70~85%, oxidation fiber crops: 8~18%, each component sum is absolutely, in 70 ± 3 DEG C of constant temperature, stirring, back flow reaction 18~24h, wash with acetone reflux after completion of the reaction, remove dimethylformamide and the thionyl chloride of surface adhesion, put in vacuum drying oven dry after taking-up, obtain chloride fiber crops;
(4) preparation of dimethyl diallyl ammonium chloride modified fiber crops adsorbent: in the reactor; add by following composition mass percent; dimethyl diallyl ammonium chloride: 75~90%; chloride fiber crops: 5~18%; water: 2~10%; potassium peroxydisulfate: 0.5~3.0%; each component sum is absolutely; nitrogen protection, in 45 ± 3 DEG C of constant temperature, stirring, back flow reaction 4~6h, after cooling; with deionized water wash, sucking filtration; being neutrality to filtrate, dry in vacuum drying oven, obtain dimethyl diallyl ammonium chloride modified fiber crops adsorbent.
2. the preparation method of a kind of dimethyl diallyl ammonium chloride modified fiber crops adsorbent according to claim 1, it is characterised in that the concentrated nitric acid mass percentage concentration described in step (2) is 68%.
3. the preparation method of a kind of dimethyl diallyl ammonium chloride according to claim 1 modified fiber crops adsorbent, it is characterised in that instrument and equipment used in step (3), reagent can not be moisture.
4. the preparation method of a kind of dimethyl diallyl ammonium chloride modified fiber crops adsorbent according to claim 1, it is characterised in that the thionyl chloride described in step (3) is optimum with the mass ratio 10:1 of dimethylformamide.
5. the preparation method of a kind of dimethyl diallyl ammonium chloride modified fiber crops adsorbent according to claim 1, it is characterised in that the dimethyl diallyl ammonium chloride mass percentage concentration described in step (4) is 60% aqueous solution.
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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 |
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