CN105854826B - A kind of preparation of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent - Google Patents

A kind of preparation of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent Download PDF

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CN105854826B
CN105854826B CN201610291618.7A CN201610291618A CN105854826B CN 105854826 B CN105854826 B CN 105854826B CN 201610291618 A CN201610291618 A CN 201610291618A CN 105854826 B CN105854826 B CN 105854826B
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reed rod
ammonium chloride
reed
water
adsorbent
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CN105854826A (en
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李慧芝
张腾
潘金营
赵长征
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
    • 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
    • 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
    • B01J2220/4837—Lignin

Abstract

The invention discloses a kind of preparation method of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent, it is characterised in that the reed rod of pretreatment is carried out into sample processing first；The oxidation reed rod after oxidation is carried out using thionyl chloride again to carry out reed rod chloride processing；Then, in the reactor, added by following composition mass percentage concentration, water：60 ~ 68%, vinylbenzyltrimethyl ammonium chloride：14 ~ 22%, chloride reed rod：12 ~ 20%, cerous sulfate：1.0 ~ 3.0%, each component sum is a hundred per cent, in 60 ± 2 DEG C of constant temperature, stirring, the h of back flow reaction 6 ~ 8, after cooling, it is washed with water, untill filtrate is in neutrality, separation of solid and liquid, it is placed in 80 ± 2 DEG C of baking ovens and dries, obtain vinylbenzyltrimethyl ammonium chloride reed rod adsorbent.The adsorbent has very high adsorption capacity, excellent physical chemistry and mechanical performance to grease, and power of regeneration is strong, and often, not only cost was low but also green, and material is easy to get for Reusability.

Description

A kind of preparation of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent
Technical field
The present invention relates to a kind of preparation method of biological adsorption agent, belong to water-treatment technology field, suitable for oil-polluted water Except oil purification, the preparation of more particularly to a kind of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent and application technology.
Background technology
Oil recovery, oil refining, store oil, transport and the petrochemical industry production that oily waste water is mainly derived from petroleum industry waited Journey, after oil product enters water body, moisture film can be formed on top layer, prevent oxygen from dissolving in water body, so as to cause water hypoxia, biology dead Die, cause serious environmental pollution.China promulgates at present《People's Republic of China's law of marine environmental protection》Etc. rules and regulations, Oily waste water highest allows concentration of emission to be 10mg/L.So oily waste water is treated as petrochemical industry instantly and ring The multiple fields urgent problems to be solved such as border protection.Absorption method is one kind in numerous handling process, and recent domestic is many The research that scholar handles absorption method oily waste water focuses mostly in the adsorption efficiency of raising adsorbent, probes into the modification side of adsorbent Method etc..There is its absorption method the features such as technique is simple, and adsorption rate is high, applied widely, and property is stable to be obtained in sewage disposal Extensive use.For the active charcoal of adsorbent of oily waste water absorption, expanded graphite, modified alta-mud, modified coal ash, snake Stone, attapulgite, zeolite etc..Gao Sainan etc. have studied oil extraction waste water biological treatment water outlet charcoal test, (Gao Sainan Environmental science and technologies, 2010-12,33 (12) are studied Deng oil extraction waste water biological treatment water outlets charcoal test:56- 65)；Wang Shuzhao etc. have studied absorption property of the expanded graphite to oily waste water, and (the expanded graphites such as Wang Shuzhao are to oily waste water Study on adsorption properties scientific and technical innovation Leader .2012 (22):7-8)；Shu Ming is brave etc. to be have studied modified alta-mud processing emulsion and gives up The experiment of water, Shu Ming bravely wait the experimental study Chemical Engineers of modified alta-muds processing emulsifying liquid waste water, 2012 (8):34- 38)；Deng Hui etc. have studied the application that flyash removes oily waste water, and (China such as Deng Hui removes oily waste water using flyash Application study flyash, 2012 (3):10-14).
Shortage of resources and environmental pollution have become two big subject matters of the world today, therefore, utilize natural reproducible Resource, development environment friendly product and technology are by as the inexorable trend of sustainable development.Reed, growth is rapid, plant is high Greatly, wide adaptability, strong stress resistance, it is distributed widely in pond, riverbank, the more water areas in He Xi sides, reed pond is commonly formed.It is then wide in China The general Liaohe delta for being distributed in northeast, song-Nen plain, the Three River Plain, the Hulun Buir and Siklingelei grassland in the Inner Mongol, newly Bosten, Ili River Valley and the Tacheng Emin river valley of boundary, the Baiyang Lake Deng Wei areas in the North China Plain.Reed is also often by as feeding Material, rich in non-starch class macromolecular substances such as cellulose, lignin, hemicelluloses, reed is that grass tree section perennial herb is planted for it Thing, in its base shaft containing holocellulos 55.82% (hemicellulose 20.03%, alpha-cellulose 79.97%), lignin 23.52%, Ash content 2.94%.Widely distributed in China, reserves are big, more than 200 ten thousand tons of annual output, account for the 6% of its Gross World Product.And And it has hydrophily, also with abundant dentate, it is easy to carry out chemical modification, domestic reed is modified to be used as adsorbent Application in adsorption of metal ions has been reported.
A kind of method that reed stalk modification prepares sorbing material is disclosed in the patent of Application No. 201410639357.7, And heavy metal is adsorbed；In grain husk etc., it have studied and reed is modified using sodium hydroxide, and to Pb in dyeing waste water2+Absorption, its is right Pb2+Maximal absorptive capacity be 144.1mg/g, (in grain husk etc., modified reed is to Pb in dyeing waste water2+Absorption research, the east area of the Liao River, coextensive with eastern and southern Liaoning Province learn Institute's journal (natural science edition), 2014,21 (2)：81-86)；Li Shanshan etc., it have studied using citric acid-modified reed fiber simultaneously To Cu2+Absorption, its maximal absorptive capacity is 82.902mg/g, and (Li Shanshan etc., modified reed fiber is to simulating industrial wastewater Cu2+ Characterization of adsorption, Jiangsu's agriculture science 2015,43 (11)：455-457)；But reed is modified as natural fiber is used as absorption oil Middle application has no report.Reed, which is used as adsorbent, to be had the advantages that renewable, degradable, environmentally friendly friendly, cheap, is important Living resources, the utilization ratio of reed will be greatly improved.
The content of the invention
An object of the present invention is to provide a kind of system of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent Preparation Method, a kind of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent mainly obtained is in waste water to grease Adsorption capacity is bigger.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent, it is characterised by that this method has There is following processing step：
(1) reed rod pre-processes：After reed rod is cleaned, it is placed in 70 DEG C of baking ovens and dry, pulverize, with the sieve of 30~40 mesh Son sieving, solid-to-liquid ratio 1g is pressed by reed rod after sieving：6~8mL is immersed in the NaOH solution that mass percentage concentration is 16~18% In, in 90 ± 2 DEG C of constant temperature 60~80min of stirring reaction, water washing to neutrality, filtering, it is placed in 80 ± 2 DEG C of baking ovens and dries, i.e., Obtain Reed Pretreated bar；
(2) reed rod is aoxidized：In the reactor, added by following composition mass percentage concentration, water：24~32%, dense sulphur Acid：48~56%, cerous sulfate：5~8%, Reed Pretreated bar：12~18%, each component sum is a hundred per cent, in 80 ± 2 DEG C constant temperature, stirring, 40~60min of back flow reaction, after cooling, separation of solid and liquid, it is placed in 80 ± 2 DEG C of baking ovens and dries, aoxidized Reed rod；
(3) prepared by chloride reed rod：In the reactor, added by following composition mass percentage concentration, dimethyl formyl Amine：48~56%, thionyl chloride：30~38%, aoxidize reed rod：10~18%, azodiisobutyronitrile：1.0~2.0%, respectively Component sum is a hundred per cent, in 60 ± 2 DEG C of constant temperature, stirring, 8~10h of back flow reaction, is washed after completion of the reaction with alcohol reflux Wash, remove the dimethylformamide and thionyl chloride of surface adhesion, water washing, untill filtrate is in neutrality, separation of solid and liquid, be placed in Dried in 80 ± 2 DEG C of baking ovens, obtain chloride reed rod；
(4) preparation of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent：In the reactor, by following composition Mass percentage concentration adds, water：60~68%, vinylbenzyltrimethyl ammonium chloride：14~22%, chloride reed rod：12 ~20%, cerous sulfate：1.0~3.0%, each component sum for absolutely, in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 6~ 8h, after cooling, it is washed with water, untill filtrate is in neutrality, separation of solid and liquid, is placed in 80 ± 2 DEG C of baking ovens and dries, obtain vinyl Benzyltrimethylammonium chloride is modified reed rod adsorbent.
In a kind of preparation method of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent, described water is pure Water.
In a kind of preparation method of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent, described reed rod is Mature native removes root, defoliation, removes reed rod slightly.
It is a further object of the present invention to provide vinylbenzyltrimethyl ammonium chloride reed rod adsorbent in aqueous systems In absorption to oil, feature is：The vinylbenzyltrimethyl ammonium chloride reed rod adsorbent deionization that will be prepared Water soaks 1.5~2.0h, is adsorbed by static method.
By the vinylbenzyltrimethyl ammonium chloride reed rod adsorbent deionized water prepared soak 1.5~ 2.0h, adsorbed by dynamic method, flow velocity 2.0mL/min.
Advantages of the present invention and effect are：
(1) the vinylbenzyltrimethyl ammonium chloride reed rod adsorbent that the present invention obtains has well physico Stability and excellent mechanical strength are learned, adsorption capacity is big, and for maximum adsorption capacity up to 132.20mg/g, Reusability number can Up to more than 10 times；
(2) the vinylbenzyltrimethyl ammonium chloride reed rod adsorbent that the present invention obtains is to various greases in water body (such as crude oil, diesel oil, lubricating oil, machine oil, vegetable oil, gasoline) has preferably absorption and elution, and adsorption efficiency is high, the speed of absorption Degree is fast, and desorption performance is good, can be used in the range of wider soda acid；
(3) because the density of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent is small, water body can be swum in Surface, the chance contacted with grease is more, high to the clearance of oil, is natural green product, biodegradable, environmental protection；
(4) condition for crossing range request of synthesis is easily controlled, and energy consumption is low, simple to operate, renewable resource utilization, is easy to industry Metaplasia is produced.
Embodiment
Embodiment 1
(1) reed rod pre-processes：After reed rod is cleaned, it is placed in 70 DEG C of baking ovens and dry, pulverize, with the sieve of 30~40 mesh Son sieving, reed rod 50g after sieving is immersed in the NaOH solution that 350mL mass percentage concentrations are 17%, in 90 ± 2 DEG C of perseverances Warm stirring reaction 70min, water washing to neutrality, filtering, it is placed in 80 DEG C of baking ovens and dries, that is, obtain Reed Pretreated bar；
(2) reed rod is aoxidized：In the reactor, it is separately added into, water：28mL, the concentrated sulfuric acid：28mL, cerous sulfate：6g, pre- place Manage reed rod：14g, in 80 ± 2 DEG C of constant temperature, stirring, back flow reaction 50min, after cooling, is washed with water, and is in neutrality to filtrate Only, separation of solid and liquid, it is placed in 80 ± 2 DEG C of baking ovens and dries, obtains aoxidizing reed rod；
(3) prepared by chloride reed rod：In the reactor, it is separately added into, dimethylformamide：55mL, thionyl chloride： 21mL, aoxidize reed rod：13g, azodiisobutyronitrile：1.0g, in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 9h, reaction finishes Washed afterwards with alcohol reflux, remove the dimethylformamide and thionyl chloride of surface adhesion, water washing, be in neutrality to filtrate Only, separation of solid and liquid, it is placed in 80 ± 2 DEG C of baking ovens and dries, obtain chloride reed rod；
(4) preparation of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent：In the reactor, it is separately added into, Water：64mL, vinylbenzyltrimethyl ammonium chloride：18g, chloride reed rod：16g, cerous sulfate：2g, in 60 ± 2 DEG C of constant temperature, Stirring, back flow reaction 7h, after cooling, are washed with water, and untill filtrate is in neutrality, separation of solid and liquid, is placed in 80 ± 2 DEG C of baking ovens and does It is dry, obtain vinylbenzyltrimethyl ammonium chloride reed rod adsorbent.
Embodiment 2
(1) reed rod pre-processes：After reed rod is cleaned, it is placed in 70 DEG C of baking ovens and dry, pulverize, with the sieve of 30~40 mesh Son sieving, reed rod 50g after sieving is immersed in the NaOH solution that 300mL mass percentage concentrations are 16%, in 90 ± 2 DEG C of perseverances Warm stirring reaction 80min, water washing to neutrality, filtering, it is placed in 80 DEG C of baking ovens and dries, that is, obtain Reed Pretreated bar；
(2) reed rod is aoxidized：In the reactor, it is separately added into, water：32mL, the concentrated sulfuric acid：26mL, cerous sulfate：8g, pre- place Manage reed rod：12g, in 80 ± 2 DEG C of constant temperature, stirring, back flow reaction 40min, after cooling, is washed with water, and is in neutrality to filtrate Only, separation of solid and liquid, it is placed in 80 ± 2 DEG C of baking ovens and dries, obtains aoxidizing reed rod；
(3) prepared by chloride reed rod：In the reactor, it is separately added into, dimethylformamide：51mL, thionyl chloride： 20mL, aoxidize reed rod：18g, azodiisobutyronitrile：2.0g, in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 10h, reaction finishes Washed afterwards with alcohol reflux, remove the dimethylformamide and thionyl chloride of surface adhesion, water washing, be in neutrality to filtrate Only, separation of solid and liquid, it is placed in 80 ± 2 DEG C of baking ovens and dries, obtain chloride reed rod；
(4) preparation of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent：In the reactor, it is separately added into, Water：68mL, vinylbenzyltrimethyl ammonium chloride：14g, chloride reed rod：17g, cerous sulfate：1g, in 60 ± 2 DEG C of constant temperature, Stirring, back flow reaction 6h, after cooling, are washed with water, and untill filtrate is in neutrality, separation of solid and liquid, is placed in 80 ± 2 DEG C of baking ovens and does It is dry, obtain vinylbenzyltrimethyl ammonium chloride reed rod adsorbent.
Embodiment 3
(1) reed rod pre-processes：After reed rod is cleaned, it is placed in 70 DEG C of baking ovens and dry, pulverize, with the sieve of 30~40 mesh Son sieving, reed rod 50g after sieving is immersed in the NaOH solution that 400mL mass percentage concentrations are 18%, in 90 ± 2 DEG C of perseverances Warm stirring reaction 60min, water washing to neutrality, filtering, it is placed in 80 DEG C of baking ovens and dries, that is, obtain Reed Pretreated bar；
(2) reed rod is aoxidized：In the reactor, it is separately added into, water：24mL, the concentrated sulfuric acid：29mL, cerous sulfate：5g, pre- place Manage reed rod：18g, in 80 ± 2 DEG C of constant temperature, stirring, back flow reaction 60min, after cooling, is washed with water, and is in neutrality to filtrate Only, separation of solid and liquid, it is placed in 80 ± 2 DEG C of baking ovens and dries, obtains aoxidizing reed rod；
(3) prepared by chloride reed rod：In the reactor, it is separately added into, dimethylformamide：59mL, thionyl chloride： 18mL, aoxidize reed rod：12g, azodiisobutyronitrile：1.5g, in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 8h, reaction finishes Washed afterwards with alcohol reflux, remove the dimethylformamide and thionyl chloride of surface adhesion, water washing, be in neutrality to filtrate Only, separation of solid and liquid, it is placed in 80 ± 2 DEG C of baking ovens and dries, obtain chloride reed rod；
(4) preparation of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent：In the reactor, it is separately added into, Water：60mL, vinylbenzyltrimethyl ammonium chloride：22g, chloride reed rod：15g, cerous sulfate：3g, in 60 ± 2 DEG C of constant temperature, Stirring, back flow reaction 8h, after cooling, are washed with water, and untill filtrate is in neutrality, separation of solid and liquid, is placed in 80 ± 2 DEG C of baking ovens and does It is dry, obtain vinylbenzyltrimethyl ammonium chloride reed rod adsorbent.
Embodiment 4
(1) reed rod pre-processes：After reed rod is cleaned, it is placed in 70 DEG C of baking ovens and dry, pulverize, with the sieve of 30~40 mesh Son sieving, reed rod 50g after sieving is immersed in the NaOH solution that 380mL mass percentage concentrations are 17%, in 90 ± 2 DEG C of perseverances Warm stirring reaction 75min, water washing to neutrality, filtering, it is placed in 80 DEG C of baking ovens and dries, that is, obtain Reed Pretreated bar；
(2) reed rod is aoxidized：In the reactor, it is separately added into, water：26mL, the concentrated sulfuric acid：28mL, cerous sulfate：7g, pre- place Manage reed rod：16g, in 80 ± 2 DEG C of constant temperature, stirring, back flow reaction 45min, after cooling, is washed with water, and is in neutrality to filtrate Only, separation of solid and liquid, it is placed in 80 ± 2 DEG C of baking ovens and dries, obtains aoxidizing reed rod；
(3) prepared by chloride reed rod：In the reactor, it is separately added into, dimethylformamide：53mL, thionyl chloride： 23mL, aoxidize reed rod：10g, azodiisobutyronitrile：2.0g, in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 8.5h, react Washed after finishing with alcohol reflux, remove the dimethylformamide and thionyl chloride of surface adhesion, water washing, be in neutrality to filtrate Only, separation of solid and liquid, it is placed in 80 ± 2 DEG C of baking ovens and dries, obtain chloride reed rod；
(4) preparation of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent：In the reactor, it is separately added into, Water：62mL, vinylbenzyltrimethyl ammonium chloride：16g, chloride reed rod：20g, cerous sulfate：2g, in 60 ± 2 DEG C of constant temperature, Stirring, back flow reaction 7.5h, after cooling, are washed with water, and untill filtrate is in neutrality, separation of solid and liquid, are placed in 80 ± 2 DEG C of baking ovens Dry, obtain vinylbenzyltrimethyl ammonium chloride reed rod adsorbent.
Embodiment 5
(1) reed rod pre-processes：After reed rod is cleaned, it is placed in 70 DEG C of baking ovens and dry, pulverize, with the sieve of 30~40 mesh Son sieving, reed rod 100g after sieving is immersed in the NaOH solution that 7000mL mass percentage concentrations are 17%, in 90 ± 2 DEG C Constant temperature stirring reaction 70min, water washing to neutrality, filtering, it is placed in 80 DEG C of baking ovens and dries, that is, obtain Reed Pretreated bar；
(2) reed rod is aoxidized：In the reactor, it is separately added into, water：140mL, the concentrated sulfuric acid：140mL, cerous sulfate：30g, in advance Handle reed rod：70g, in 80 ± 2 DEG C of constant temperature, stirring, back flow reaction 50min, after cooling, it is washed with water, to filtrate in neutrality Untill, separation of solid and liquid, it is placed in 80 ± 2 DEG C of baking ovens and dries, obtains aoxidizing reed rod；
(3) prepared by chloride reed rod：In the reactor, it is separately added into, dimethylformamide：280mL, thionyl chloride： 100mL, aoxidize reed rod：65g, azodiisobutyronitrile：5.0g, in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 9h, reaction finishes Washed afterwards with alcohol reflux, remove the dimethylformamide and thionyl chloride of surface adhesion, water washing, be in neutrality to filtrate Only, separation of solid and liquid, it is placed in 80 ± 2 DEG C of baking ovens and dries, obtain chloride reed rod；
(4) preparation of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent：In the reactor, it is separately added into, Water：320mL, vinylbenzyltrimethyl ammonium chloride：90g, chloride reed rod：80g, cerous sulfate：10g, in 60 ± 2 DEG C of perseverances Temperature, stirring, back flow reaction 7h, after cooling, are washed with water, and untill filtrate is in neutrality, separation of solid and liquid, are placed in 80 ± 2 DEG C of baking ovens Middle drying, obtain vinylbenzyltrimethyl ammonium chloride reed rod adsorbent.
Embodiment 6
0.50g vinylbenzyltrimethyl ammonium chloride reed rod adsorbents are weighed to be placed in 250mL conical flask with cover, Adding 100mL concentration is in 550mg/L lubricant oil solutions, using the pH value of acid or alkali regulation system as in the range of 4.0~10.0, 4~6h of concussion absorption at room temperature, takes supernatant, concentration oily in solution is determined with infrared spectrum oil content analyzer, before and after absorption Oily concentration difference in water, the adsorption capacity of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent is calculated, it is adsorbed Capacity can reach 132.20mg/g, and the pH value absorption of adsorbent on oil in the range of 5.0~9.0 does not influence, in room temperature Lower concussion absorption more than 4h, absorption of the adsorbent to oil reach saturation.
Embodiment 7
1.0g vinylbenzyltrimethyl ammonium chloride reed rod adsorbents are weighed to be placed in 250mL conical flask with cover, Adding 100mL concentration is in 100mg/L oil-containing solutions, using the pH value of acid or alkali regulation system as in the range of 7.0, shakes at room temperature Absorption 4h is swung, takes supernatant, concentration oily in solution is determined with infrared spectrum oil content analyzer, according to concentration oily in water before and after absorption Difference, clearance of the vinylbenzyltrimethyl ammonium chloride reed rod adsorbent to oil is calculated, reaches as high as 97.89%.

Claims (6)

  1. A kind of 1. preparation method of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent, it is characterised in that this method With following processing step：
    (1) reed rod pre-processes：After reed rod is cleaned, it is placed in 70 DEG C of baking ovens and dry, pulverize, with the sieve mistake of 30~40 mesh Sieve, solid-to-liquid ratio 1g is pressed by reed rod after sieving：6~8mL is immersed in the NaOH solution that mass percentage concentration is 16~18%, in 90 ± 2 DEG C of constant temperature 60~80min of stirring reaction, water washing to neutrality, filtering, it is placed in 80 ± 2 DEG C of baking ovens and dries, that is, obtain pre- Handle reed rod；
    (2) reed rod is aoxidized：In the reactor, added by following composition mass percent, water：24~32%, the concentrated sulfuric acid：48~ 56%, cerous sulfate：5~8%, Reed Pretreated bar：12~18%, each component mass percent sum is a hundred per cent, in 80 ± 2 DEG C of constant temperature, stirring, 40~60min of back flow reaction, after cooling, are washed with water, and untill filtrate is in neutrality, separation of solid and liquid, put Dried in 80 ± 2 DEG C of baking ovens, obtain aoxidizing reed rod；
    (3) prepared by chloride reed rod：In the reactor, added by following composition mass percent, dimethylformamide：48~ 56%, thionyl chloride：30~38%, aoxidize reed rod：10~18%, azodiisobutyronitrile：1.0~2.0%, each component quality Percentage sum is a hundred per cent, in 60 ± 2 DEG C of constant temperature, stirring, 8~10h of back flow reaction, is washed after completion of the reaction with alcohol reflux Wash, remove the dimethylformamide and thionyl chloride of surface adhesion, separation of solid and liquid, be placed in 80 ± 2 DEG C of baking ovens and dry, obtain acyl Chlorination reed rod；
    (4) preparation of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent：In the reactor, by following composition quality Percentage adds, water：60~68%, vinylbenzyltrimethyl ammonium chloride：14~22%, chloride reed rod：12~20%, Cerous sulfate：1.0~3.0%, each component mass percent sum is a hundred per cent, in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 6 ~8h, after cooling, it is washed with water, untill filtrate is in neutrality, separation of solid and liquid, is placed in 80 ± 2 DEG C of baking ovens and dries, obtain ethene Base benzyltrimethylammonium chloride is modified reed rod adsorbent.
  2. 2. according to a kind of preparation side of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent described in claim 1 Method, it is characterised in that described water is pure water.
  3. 3. according to a kind of preparation side of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent described in claim 1 Method, it is characterised in that described reed rod removes root, defoliation, removes reed rod slightly for mature native.
  4. 4. according to a kind of preparation side of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent described in claim 1 Method, it is characterised in that instrument and equipment used, reagent can not be aqueous in step (3).
  5. 5. according to a kind of preparation side of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent described in claim 1 Vinylbenzyltrimethyl ammonium chloride reed rod adsorbent prepared by method, it is characterised in that vinylbenzyltrimethyl Application of the ammonium chloride reed rod adsorbent to the absorption of grease in waste water.
  6. 6. according to a kind of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent described in claim 5 in waste water Grease adsorbs, it is characterised in that described grease is：Crude oil, diesel oil, lubricating oil, vegetable oil, gasoline.
CN201610291618.7A 2016-05-05 2016-05-05 A kind of preparation of vinylbenzyltrimethyl ammonium chloride reed rod adsorbent Expired - Fee Related CN105854826B (en)

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