CN104525148A - Method for preparing ammonium sulfamate bacterial celluloses for absorbing Pb2+ in waste water - Google Patents

Method for preparing ammonium sulfamate bacterial celluloses for absorbing Pb2+ in waste water Download PDF

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Publication number
CN104525148A
CN104525148A CN201510012471.9A CN201510012471A CN104525148A CN 104525148 A CN104525148 A CN 104525148A CN 201510012471 A CN201510012471 A CN 201510012471A CN 104525148 A CN104525148 A CN 104525148A
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China
Prior art keywords
bacteria cellulose
preparation
seed
bacterial celluloses
waste water
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Pending
Application number
CN201510012471.9A
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Chinese (zh)
Inventor
赵鹏
郭军科
卢立秋
邵林
于金山
郝春艳
苏展
刘鸿芳
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State Grid Corp of China SGCC
State Grid Tianjin Electric Power Co Ltd
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State Grid Corp of China SGCC
State Grid Tianjin Electric Power Co Ltd
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Priority to CN201510012471.9A priority Critical patent/CN104525148A/en
Publication of CN104525148A publication Critical patent/CN104525148A/en
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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
    • 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
    • B01J2220/44—Materials comprising a mixture of organic materials
    • 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
    • B01J2220/4868—Cells, spores, bacteria
    • 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
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds

Abstract

The invention relates to a method for preparing ammonium sulfamate bacterial celluloses for absorbing Pb2+ in waste water. The method includes the steps of (1) preparing bacterial celluloses, wherein the process includes the steps of (a) cultivation of the bacterial celluloses, (b) isolation and purification of the bacterial celluloses and (c) preparation of bacterial cellulose powder; (2) preparing epoxidation bacterial celluloses, wherein the process includes the steps of (a) preparation of alkalization bacterial celluloses and (b) obtaining of epoxy group bacterial celluloses; (3) preparing the ammonium sulfamate bacterial celluloses. By means of the method, the ammonium sulfamate bacterial celluloses serve as absorption materials of the Pb2+, the absorption process is rapid, adsorption equilibrium is achieved at the 90 min in the absorption process, the good linear dependence is achieved, and the theory saturation adsorption amount of the ammonium sulfamate bacterial celluloses is 31.23 mg/g.

Description

The preparation method of the Amcide Ammate bacteria cellulose of Pb2+ in absorption waste water
Technical field
The invention belongs to heavy metals ion processing technical field, Pb in especially a kind of absorption waste water 2+the preparation method of Amcide Ammate bacteria cellulose.
Background technology
Along with the fast development of economy, a large amount of discharges of waste water, heavy metal pollution problem more and more causes the concern of people.Waste water containing heavy metal ion is mainly derived from smelting and the part chemical enterprise of machining, mining, iron and steel and non-ferrous metal.Heavy metal is the first kinds of pollution matter very harmful to ecological environment, mainly comprise mercury, cadmium, chromium, lead, zinc, copper, cobalt, manganese, titanium, molybdenum etc., can not be biodegradable after their entered environments, form can only be changed or be transferred, dilute, participate in food chain circulation and finally accumulate in vivo, destroy organism normal physiological metabolic activity, be detrimental to health.
In order to having a strong impact on of reducing that heavy metal pollution causes the ecosystem to greatest extent, people constantly to make great efforts the new technology of development process heavy metal wastewater thereby always, and achieve certain achievement, but still have many problems to need research.
The method that the treatment research of domestic and international heavy metal waste water is conventional has chemical method, ion-exchange, electrolysis, hyperfiltration, electroosmose process, absorption method and bioanalysis etc.
There is disposal cost and greatly, easily cause the deficiency such as secondary pollution, complicated operation in traditional physico-chemical process process heavy metal wastewater thereby.Therefore, research and develop abundance and cheap adsorbent heavy-metal ion removal, become the development trend in heavy metal containing wastewater treatment field.
At present, mainly concentrate on chitin, starch and derivative thereof the research of adsorbent, but along with the development of economic society, this can not satisfy the demand far away, the new adsorbent of exploitation Cheap highly effective becomes an urgent demand of socio-economic development.Cellulose is the abundantest natural macromolecular material of occurring in nature, and therefore, cellulose and its derivates is widely used in Adsorption of Heavy Metal Ions research.But in cellulose preparation process, a large amount of chemical raw materials need be consumed for highly purified cellulose can be obtained, edify people thus and explore tool and to grow a lot the Microbe synthesis method of potentiality.The bacteria cellulose toxigenic capacity that this method obtains is low, can degrade, and can not produce secondary pollution, specific area is higher, and there is a large amount of hydroxyls in molecule, has good absorption property to metal ion in solution.Progressively be taken seriously in recent years and become study hotspot, particularly as flocculant and chelate sorbent, being widely used in water treatment and environmental protection.Cellulose and its derivates enjoys the concern of people with its wide material sources, lower-price characteristic.But bacteria cellulose is compared with above-mentioned adsorbent, and adsorption effect is not satisfactory, in order to the absorption property of summary bacteria cellulose, study on the modification to be carried out to it.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, Pb in a kind of absorption waste water is provided 2+the preparation method of Amcide Ammate bacteria cellulose.
The present invention solves its technical problem and takes following technical scheme to realize:
Pb in a kind of absorption waste water 2+the preparation method of Amcide Ammate bacteria cellulose, comprise step as follows:
(1) preparation of bacteria cellulose,
1. the cultivation of bacteria cellulose,
I, first order seed shaken cultivation: get the inclined-plane seed access seed culture medium activated, 28 DEG C of shaken cultivation 24h, fully vibrate during inoculation, to discharge thalline;
The extension of II, secondary seed is cultivated: get the seed culture medium after a shaken cultivation with the new seed culture medium of 10% inoculum concentration access same volume, 28 DEG C of shaken cultivation 20h;
III, static fermentation are cultivated: get secondary seed and fill in the culture dish of fermentation medium with 10% inoculum concentration access, 28 DEG C of quiescent culture 7d;
2. the isolation andpurification of bacteria cellulose,
I, from culture dish, take out bacteria cellulose film, repeatedly rinse except striping surface impurity with distilled water, then NaOH solution film being immersed 0.1mol/L boils 30min, remove remaining mycoprotein and culture medium;
II, repeatedly to rinse film by deionized water, then use deionized water rinsing again with after 0.5% acetic acid soaked overnight, survey its surface for neutral to pH test paper, now film is creamy white translucent;
III, 105 DEG C be dried to constant weight after for subsequent use;
3. the preparation of bacteria cellulose powder;
The bacteria cellulose block getting oven dry puts into pulverizer, pulverizes 10min, then is sieved by the bacteria cellulose after pulverizing, and loads in reagent bottle and stores;
(2) preparation of epoxidation bacteria cellulose,
1. take 1g bacteria cellulose powder, add the sodium hydroxide solution 100mL of concentration 29.75%, room temperature lower magnetic force stirs alkalization 1h, filters, is washed to neutrality, 50 DEG C of oven dry, obtained alkalization bacteria cellulose;
2. alkalization bacteria cellulose is put into sealing reaction bulb, add the sodium hydroxide solution of 60.6mL 8%, 3.5mL epoxychloropropane, 4mL ethanol, 20 DEG C of reaction 10 ~ 11h, filter, wash once with 20mL acetone again after being washed to neutrality, be filtered dry rear 50 DEG C of vacuum drying to constant weight, obtain epoxy radicals bacteria cellulose;
(3) preparation of Amcide Ammate bacteria cellulose,
1. the Na of 10g is accurately taken 2cO 3in nitrogen protection container, then add 100mL demineralized water wherein, accurately take 0.1g Amcide Ammate and 1g epoxidation bacteria cellulose after stirring and dissolving, the water bath with thermostatic control oscillator putting into 50 DEG C reacts 2h;
2. reacted cellulose is rinsed to neutral, put into vacuum drying chamber 50 DEG C of vacuum drying, obtain Amcide Ammate bacteria cellulose.
And, abundant vibration when inoculating in I step 1. in described step (1) is: oscillator rotating speed is 120r/min.
And the bacteria cellulose powder 1. walked in described step (2) is the 60 object powder that sieve.
Advantage of the present invention and good effect are:
1, shown by test, Amcide Ammate bacteria cellulose of the present invention can as Pb 2+sorbing material, adsorption process is comparatively quick, and adsorption process reaches adsorption equilibrium at 90min;
2, the absorption of Amcide Ammate bacteria cellulose of the present invention to lead ion meets second-order kinetic equation and Langmuir isothermal adsorpting equation, and has good linear dependence, and its theoretical saturated extent of adsorption is 31.23mg/g.
Detailed description of the invention
Be further described the invention process below, following examples are descriptive, are not determinate, can not limit protection scope of the present invention with this.
Pb in a kind of absorption waste water 2+the preparation method of Amcide Ammate bacteria cellulose, it is as follows that the method comprising the steps of:
(1) preparation of bacteria cellulose;
1. the cultivation of bacteria cellulose,
First order seed shaken cultivation: get the inclined-plane seed access seed culture medium activated, 28 DEG C of shaken cultivation 24h, fully vibrate during inoculation, to discharge thalline;
Wherein, oscillator rotating speed is 120r/min;
Secondary seed extension is cultivated: get the seed culture medium after a shaken cultivation with the new seed culture medium of 10% inoculum concentration access same volume, 28 DEG C of shaken cultivation 20h;
Static fermentation is cultivated: get secondary seed and fill in the culture dish of fermentation medium with 10% inoculum concentration access, 28 DEG C of quiescent culture 7d.
2. the isolation andpurification of bacteria cellulose;
I, from culture dish, take out bacteria cellulose film, repeatedly rinse except striping surface impurity with distilled water, then NaOH solution film being immersed 0.1mol/L boils 30min, remove remaining mycoprotein and culture medium;
II, repeatedly to rinse film by deionized water, then use deionized water rinsing again with after 0.5% acetic acid soaked overnight, survey its surface for neutral to pH test paper, now film is creamy white translucent;
III, 105 DEG C be dried to constant weight after for subsequent use;
3. the preparation of bacteria cellulose powder;
The bacteria cellulose block getting oven dry puts into pulverizer, pulverizes 10min, then is sieved by the bacteria cellulose after pulverizing, and loads in reagent bottle and stores;
(2) preparation of epoxidation bacteria cellulose;
Take 1g bacteria cellulose powder, add the sodium hydroxide solution 100mL of concentration 29.75%, room temperature lower magnetic force stirs alkalization 1h, filters, is washed to neutrality, 50 DEG C of oven dry, obtained alkalization bacteria cellulose;
Wherein, bacteria cellulose powder is the 60 object powder that sieve.
Alkalization bacteria cellulose is put into sealing reaction bulb, add the sodium hydroxide solution of 60.6mL 8%, 3.5mL epoxychloropropane, 4mL ethanol, 20 DEG C of reaction 10.5h, filter, wash once with 20mL acetone again after being washed to neutrality, be filtered dry rear 50 DEG C of vacuum drying to constant weight, obtain epoxy radicals bacteria cellulose, its reaction equation is as follows:
(3) preparation of Amcide Ammate bacteria cellulose
Accurately take the Na of 10g 2cO 3in nitrogen protection container, then add 100mL demineralized water wherein, accurately take 0.1g Amcide Ammate and 1g epoxidation bacteria cellulose after stirring and dissolving, the water bath with thermostatic control oscillator putting into 50 DEG C reacts 2h;
Rinse reacted cellulose to neutral, put into vacuum drying chamber 50 DEG C of vacuum drying, obtain Amcide Ammate bacteria cellulose (ASBC), its reaction equation is as follows:

Claims (3)

1. adsorb a preparation method for the Amcide Ammate bacteria cellulose of Pb2+ in waste water, it is characterized in that comprising step as follows:
(1) preparation of bacteria cellulose,
1. the cultivation of bacteria cellulose,
I, first order seed shaken cultivation: get the inclined-plane seed access seed culture medium activated, 28 DEG C of shaken cultivation 24h, fully vibrate during inoculation, to discharge thalline;
The extension of II, secondary seed is cultivated: get the seed culture medium after a shaken cultivation with the new seed culture medium of 10% inoculum concentration access same volume, 28 DEG C of shaken cultivation 20h;
III, static fermentation are cultivated: get secondary seed and fill in the culture dish of fermentation medium with 10% inoculum concentration access, 28 DEG C of quiescent culture 7d;
2. the isolation andpurification of bacteria cellulose,
I, from culture dish, take out bacteria cellulose film, repeatedly rinse except striping surface impurity with distilled water, then NaOH solution film being immersed 0.1mol/L boils 30min, remove remaining mycoprotein and culture medium;
II, repeatedly to rinse film by deionized water, then use deionized water rinsing again with after 0.5% acetic acid soaked overnight, survey its surface for neutral to pH test paper, now film is creamy white translucent;
III, 105 DEG C be dried to constant weight after for subsequent use;
3. the preparation of bacteria cellulose powder;
The bacteria cellulose block getting oven dry puts into pulverizer, pulverizes 10min, then is sieved by the bacteria cellulose after pulverizing, and loads in reagent bottle and stores;
(2) preparation of epoxidation bacteria cellulose,
1. take 1g bacteria cellulose powder, add the sodium hydroxide solution 100mL of concentration 29.75%, room temperature lower magnetic force stirs alkalization 1h, filters, is washed to neutrality, 50 DEG C of oven dry, obtained alkalization bacteria cellulose;
2. alkalization bacteria cellulose is put into sealing reaction bulb, add the sodium hydroxide solution of 60.6mL 8%, 3.5mL epoxychloropropane, 4mL ethanol, 20 DEG C of reaction 10 ~ 11h, filter, wash once with 20mL acetone again after being washed to neutrality, be filtered dry rear 50 DEG C of vacuum drying to constant weight, obtain epoxy radicals bacteria cellulose;
(3) preparation of Amcide Ammate bacteria cellulose,
1. the Na of 10g is accurately taken 2cO 3in nitrogen protection container, then add 100mL demineralized water wherein, accurately take 0.1g Amcide Ammate and 1g epoxidation bacteria cellulose after stirring and dissolving, the water bath with thermostatic control oscillator putting into 50 DEG C reacts 2h;
2. reacted cellulose is rinsed to neutral, put into vacuum drying chamber 50 DEG C of vacuum drying, obtain Amcide Ammate bacteria cellulose.
2. Pb in absorption waste water according to claim 1 2+the preparation method of Amcide Ammate bacteria cellulose, it is characterized in that: abundant vibration when inoculating in I step 1. in described step (1) is: oscillator rotating speed is 120r/min.
3. Pb in absorption waste water according to claim 1 2+the preparation method of Amcide Ammate bacteria cellulose, it is characterized in that: the bacteria cellulose powder 1. walked in described step (2) is the 60 object powder that sieve.
CN201510012471.9A 2015-01-12 2015-01-12 Method for preparing ammonium sulfamate bacterial celluloses for absorbing Pb2+ in waste water Pending CN104525148A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107033919A (en) * 2017-05-14 2017-08-11 吴刚 A kind of preparation method of sand-consolidating agent
CN107413316A (en) * 2017-08-01 2017-12-01 东华大学 A kind of efficient protein adsorbing separation bacteria cellulose nano-fiber composite film and preparation method thereof
CN108395563A (en) * 2018-05-30 2018-08-14 陕西科技大学 A kind of preparation method of bacteria cellulose powder
CN108395562A (en) * 2018-05-30 2018-08-14 陕西科技大学 A kind of preparation method of high-crystallinity bacteria cellulose powder
CN109701502A (en) * 2018-11-19 2019-05-03 浙江工商大学 Novel chelate fibre and preparation method thereof and in lime-preserved egg Pb (II) detection application
RU2717777C1 (en) * 2019-05-30 2020-03-25 Федеральное государственное бюджетное образовательное учреждение высшего образования "Национальный исследовательский Мордовский государственный университет им. Н.П. Огарёва" Method of extracting heavy metals from aqueous solutions
RU2743012C1 (en) * 2020-08-21 2021-02-12 Федеральное государственное бюджетное образовательное учреждение высшего образования "Национальный исследовательский Мордовский государственный университет им. Н.П. Огарёва" A method of obtaining a microporous sorbent on bacterial cellulose
CN114671485A (en) * 2022-05-30 2022-06-28 杭州师范大学钱江学院 Specific treatment method of wastewater containing heavy metal ions

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107033919A (en) * 2017-05-14 2017-08-11 吴刚 A kind of preparation method of sand-consolidating agent
CN107413316A (en) * 2017-08-01 2017-12-01 东华大学 A kind of efficient protein adsorbing separation bacteria cellulose nano-fiber composite film and preparation method thereof
CN107413316B (en) * 2017-08-01 2020-08-11 东华大学 Bacterial cellulose nanofiber composite membrane for efficient protein adsorption separation and preparation method thereof
CN108395563A (en) * 2018-05-30 2018-08-14 陕西科技大学 A kind of preparation method of bacteria cellulose powder
CN108395562A (en) * 2018-05-30 2018-08-14 陕西科技大学 A kind of preparation method of high-crystallinity bacteria cellulose powder
CN108395562B (en) * 2018-05-30 2020-11-20 陕西科技大学 Preparation method of high-crystallinity bacterial cellulose powder
CN108395563B (en) * 2018-05-30 2021-03-09 陕西科技大学 Preparation method of bacterial cellulose powder
CN109701502A (en) * 2018-11-19 2019-05-03 浙江工商大学 Novel chelate fibre and preparation method thereof and in lime-preserved egg Pb (II) detection application
RU2717777C1 (en) * 2019-05-30 2020-03-25 Федеральное государственное бюджетное образовательное учреждение высшего образования "Национальный исследовательский Мордовский государственный университет им. Н.П. Огарёва" Method of extracting heavy metals from aqueous solutions
RU2743012C1 (en) * 2020-08-21 2021-02-12 Федеральное государственное бюджетное образовательное учреждение высшего образования "Национальный исследовательский Мордовский государственный университет им. Н.П. Огарёва" A method of obtaining a microporous sorbent on bacterial cellulose
CN114671485A (en) * 2022-05-30 2022-06-28 杭州师范大学钱江学院 Specific treatment method of wastewater containing heavy metal ions

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Application publication date: 20150422