CN101029452A - Modified absorben cotton, its production and use - Google Patents

Modified absorben cotton, its production and use Download PDF

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Publication number
CN101029452A
CN101029452A CNA200610156067XA CN200610156067A CN101029452A CN 101029452 A CN101029452 A CN 101029452A CN A200610156067X A CNA200610156067X A CN A200610156067XA CN 200610156067 A CN200610156067 A CN 200610156067A CN 101029452 A CN101029452 A CN 101029452A
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Prior art keywords
cotton
modified absorben
modified
absorben cotton
solution
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CNA200610156067XA
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龚仁敏
朱国萍
胡云
钟克定
张德敏
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Anhui Normal University
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Anhui Normal University
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Abstract

Modified absorbent cotton, its production and usage are disclosed. In the general formula, R is sodium ion and potassium ion. The process is carried out by mixing absorbent cotton with citric acid solution, agitating, drying to constant weight, raising temperature to 115-125degree, keeping temperature, cooling to room temperature, washing by distilled water, filtering, adding base-metal solution into filtrate, agitating for 60mins, filtering, washing filtrate to neutral, drying to constant weight, adjusting pH of waste water containing cation to 4-7, adding into modified absorbent cotton 1-20g/l, agitating for 30mins and filtering. It's simple, cheap, has better chelate performance and can be used to treat cation waste water.

Description

A kind of modified absorben cotton and preparation thereof, using method
Technical field:
The invention belongs to modified absorben cotton and preparation thereof, this technical field of using method, especially belong to carboxyl cotton and preparation thereof, this technical field of using method.
Background technology:
Modified absorben cotton commonly used has Sulfhydryl Cotton, and its preparation method be with TGA, acetic anhydride, acetate, the abundant mixing of the concentrated sulfuric acid, be cooled to room temperature after, adding absorbent cotton.After the immersion fully, be incubated after 2~4 days and take out, suction filtration, washing is to neutrality and in 30 ℃ of oven dry down.The prepared product that goes out must lucifuge, and airtight, low temperature is preserved.It is through being usually used in the analyzing and testing of trace materials, and the Sulfhydryl Cotton chelating ability is poor, while complicated process of preparation, cost height.
Summary of the invention:
Technical problem to be solved by this invention provides the modified absorben cotton of chelating ability.
The technical scheme of technical solution problem of the present invention is: a kind of modified absorben cotton is characterized in that: comprise the following units in its structural formula:
Figure A20061015606700031
Described R is sodium ion, potassium ion, and preferred R is a sodium ion.
The preparation method of modified absorben cotton of the present invention is: with absorbent cotton and 0.1-1M citric acid solution with 1: 10-30 (cotton: acid, W/V) mixed, after stirring is not less than 20 minutes, dry to constant weight at 50-80 ℃, be warming up to 115-125 ℃ and the insulation be not less than 90 minutes, be chilled to room temperature, to solution, there is not citric acid with the distilled water cyclic washing, filter, add the capacity alkali metal soln in the filtered object, stirring is filtered after being not less than 60 minutes, and filtered object is washed with distilled water to neutrality, is dried to constant weight under 50-80 ℃.
Preferred distilled water is distilled water.
Described alkali metal soln is the hydrogen sodium hydride solution, potassium hydroxide solution.
Preferred alkali metal soln is the sodium hydroxide solution of 0.1M.
Preparation principle of the present invention is: citric acid dehydration forms the acid anhydrides with reactivity, so with cellulose in the C of sugar unit 6Hydroxyl generation esterification, generate citric acid cellulose monoesters, transferring two no esterification carboxyls of citric acid in the esterification cotton to alkali metal type by Hydrogen with alkali metal soln again, is that sodium hydroxide solution is an example with used alkali metal soln, reacts available following chemical formula and expresses:
Figure A20061015606700041
The prepared carboxy-modified absorbent cotton of the present invention can be used for processing and contain CATION waste water, and described CATION comprises metal ion, as iron ion, copper ion, lead ion, and the CATION basic-dyeable fibre.
Using method of the present invention is regulated pH to 4-7 for containing CATION waste water, adds the stirring of 1-20g/l modified absorben cotton and is not less than 30 minutes, filters to get final product.
Preferred using method is regulated pH to 5-6 for containing copper ion waste water, adds the stirring of 1-5g/l modified absorben cotton and gets final product in 30-90 minute
The waste water that contains copper ion with processing is example, and its reaction equation is:
Figure A20061015606700042
The present invention compared with prior art, the chelating ability of modified absorben cotton obviously improves, and can be used to handle cationic waste water, enlarged the scope of application of modified absorben cotton, preparation method of the present invention is very simple simultaneously, and raw material is easy to get, cost is low, can apply widely.
Description of drawings:
Fig. 1 for the infrared spectrum of absorbent cotton and modified absorben cotton wherein a be absorbent cotton; B: be modified absorben cotton.
Fig. 2 is the influence of pH to modified absorben cotton absorbing copper ion (divalence).
Fig. 3 is the influence of adsorption time to modified absorben cotton absorbing copper ion (divalence).
Fig. 4 is the influence of copper concentration to modified absorben cotton absorbing copper ion (divalence).
Fig. 5 is the langmuir's adsorption isotherm of copper ion (divalence) on modified absorben cotton
The specific embodiment:
One, preparation method:
Embodiment 1: with absorbent cotton and 0.1M citric acid solution with 1: 15 (cotton: acid, W/V) mixed, stir after 30 minutes, dry to constant weight at 50 ℃, be warming up to 115 ℃ and be incubated 90 minutes, be chilled to room temperature, to solution, there is not citric acid with the distilled water cyclic washing, (being to splash into the 0.1M plumbi nitras in the filtrate not have muddy the generation), add the 0.1M sodium hydroxide solution of capacity in the filtered object, stir after 60 minutes and filter, filtered object is washed with distilled water to neutrality, under 50 ℃, be dried to constant weight, obtain the sodium salt of modified absorben cotton.
The infared spectrum of modified absorben cotton is the b among Fig. 1, and the b among Fig. 1 compares with a, and infrared spectrum is at 1753.4cm -1Tangible carbonylic stretching vibration absworption peak appears in the wave number place, and this obviously is the result that Citrin ester produces.
Embodiment 2: with absorbent cotton and 0.5M citric acid solution with 1: 10 (cotton: acid, W/V) mixed, stir after 20 minutes, dry to constant weight at 60 ℃, be warming up to 120 ℃ and be incubated 120 minutes, be chilled to room temperature, to solution, there is not citric acid with the distilled water cyclic washing, (being to splash into the 0.1M plumbi nitras in the filtrate not have muddy the generation), add the 0.1M potassium hydroxide solution of capacity in the filtered object, stir after 90 minutes and filter, filtered object is extremely neutral with the distilled water washing, under 60 ℃, be dried to constant weight, obtain the sylvite of modified absorben cotton.
Two, using method:
Embodiment 3: get 100ml and used the HCl of 0.1M or NaOH adjust pH to 1-7, the cupric solution of 20mg/l places the conical flask of 250ml, the modified absorben cotton that adds 0.1 gram embodiment 1, airtight bottleneck is in case liquor capacity variation in the experimentation, under the room temperature condition on the speed governing oscillator velocity fluctuation with 150 times/minute be adsorbed to 1 hour, filter, gained solution calculates the adsorbance of copper ion with the surplus value of atomic absorption spectrophotometric determination copper ion with following formula:
q=(C 0-C e)V/W
In the formula, q is the amount (mg.g of every gram adsorbents adsorb copper -1), C 0Initial concentration (mg.L for copper solution -1), Ce is the concentration (mg.L of copper solution after the adsorption equilibrium -1), V is the volume (L) of solution, W is the amount (g) of adsorbent.
Its result is Fig. 2, and the adsorption rate of copper ion is minimum during pH=1, and this is because of a large amount of H in the solution under the low ph condition +Functional group-COO with modified absorben cotton -Be combined into-COOH, thereby influence the absorption of modified absorben cotton copper ion.In the pH=1-4 scope, the absorption of copper ion increases with the pH value, pH 〉=4 o'clock, and the absorption of copper ion reaches equilibrium valve.So subsequent embodiment is all carried out for 5 times at pH.
Embodiment 4: get 100mlpH value=5, the cupric solution of 20mg/l places the conical flask of 250ml, the modified absorben cotton that adds 0.1 gram embodiment 1, airtight bottleneck is in case liquor capacity variation in the experimentation, under the room temperature condition on the speed governing oscillator velocity fluctuation with 150 times/minute be adsorbed to appropriate time, filter, the gained solution surplus value of atomic absorption spectrophotometric determination copper ion, the computational methods of the adsorbance of copper ion are identical with embodiment 3.
Its result is Fig. 3, absorption by the visible incipient stage copper ion of result among the figure is very fast, be a diffusion absorption phase that adsorption rate is gradually slow after the quick absorption of copper ion, last being adsorbed on about 30 minutes of copper ion reaches adsorption equilibrium, so subsequent embodiment all stirred 1 hour.
Embodiment 5: the cupric solution of getting 100mlpH value=5 places the conical flask of 250ml, the modified absorben cotton that adds 0.1 gram embodiment 1, airtight bottleneck is in case liquor capacity variation in the experimentation, under the room temperature condition on the speed governing oscillator velocity fluctuation with 150 times/minute be adsorbed to 1 hour, filter, the gained solution surplus value of atomic absorption spectrophotometric determination copper ion, the computational methods of the adsorbance of copper ion are identical with embodiment 3.
Its result is Fig. 4, and Fig. 4 has shown the influence result of copper ion concentration to modified absorben cotton absorbing copper ion.When copper ion concentration increased to 70mg/l by 5mg/l, the copper ion adsorption rate of modified absorben cotton reduced to 42.62% from 99.74; With the langmuir's adsorption isotherm equation adsorpting data of copper ion among Fig. 4 is carried out match, linear langmuir equation has following form:
C e/q e=1/(aQ m)+C e/Q m
C in the formula eThe liquid concentration of copper ion when (mg/l) being adsorption equilibrium, q eThe adsorbance of copper ion when (mg/g) being adsorption equilibrium, Q m(mg/g) be the maximal absorptive capacity of copper ion, can be by C e/ q eTo C eThe slope 1/Q of mapping gained linear equation m.
Approach 1 linearly dependent coefficient (R from Fig. 5 gained 2=0.9714) absorption of the visible copper ion of numerical value on modified absorben cotton meets langmuir equation, by the slope 1/Q of langmuir's adsorption isotherm gained linear equation mThe maximal absorptive capacity of trying to achieve copper ion is 22.68mg/g.
Embodiment 6: get 100mlpH value=5, the ferric ion solution of 20mg/l places the conical flask of 250ml, the modified absorben cotton that adds 0.1 gram embodiment 2, airtight bottleneck is in case liquor capacity variation in the experimentation, under the room temperature condition on the speed governing oscillator velocity fluctuation with 150 times/minute be adsorbed to 1 hour, filter, the gained solution surplus value of atomic absorption spectrophotometric determination iron ion, the computational methods of the adsorbance of iron ion are identical with embodiment 3.Its adsorbance is 19.47mg/g.
Embodiment 7: get 100mlpH value=5, the lead solution of 20mg/l places the conical flask of 250ml, the modified absorben cotton that adds 0.1 gram embodiment 1, airtight bottleneck is in case liquor capacity variation in the experimentation, under the room temperature condition on the speed governing oscillator velocity fluctuation with 150 times/minute be adsorbed to 1 hour, filter, the gained solution surplus value of atomic absorption spectrophotometric determination lead ion, the computational methods of the adsorbance of lead ion are identical with embodiment 3.Its adsorbance is 30.76mg/g.
Embodiment 8: get 100mlpH value=5, the methylene blue solution of 200mg/l places the conical flask of 250ml, the modified absorben cotton that adds 0.1 gram embodiment 1, airtight bottleneck is in case liquor capacity variation in the experimentation, under the room temperature condition on the speed governing oscillator velocity fluctuation with 150 times/minute be adsorbed to 1 hour, filter, the gained solution surplus value of spectrophotometry methylene blue, the computational methods of the adsorbance of methylene blue are identical with embodiment 3.Its adsorbance is 185.23mg/g.
Embodiment 9: get 100mlpH value=5, the malachite green solution of 20mg/l places the conical flask of 250ml, the modified absorben cotton that adds 0.1 gram embodiment 1, airtight bottleneck is in case liquor capacity variation in the experimentation, under the room temperature condition on the speed governing oscillator velocity fluctuation with 150 times/minute be adsorbed to 1 hour, filter, the gained solution surplus value of spectrophotometry peacock green, the computational methods of the adsorbance of peacock green are identical with embodiment 3.Its adsorbance is 174.75mg/g.
Embodiment 6-9 shows that the present invention can fully be adsorbed the CATION in the waste water.

Claims (8)

1, a kind of modified absorben cotton is characterized in that: comprise the following units in its structural formula:
Figure A2006101560670002C1
Described R is sodium ion, potassium ion.
2, a kind of modified absorben cotton according to claim 1 is characterized in that: described R is a sodium ion.
3, the preparation method of the described modified absorben cotton of a kind of claim 1, it is characterized in that: with absorbent cotton and 0.1-1M citric acid solution with 1: 10-30 (cotton: acid, W/V) mixed, after stirring is not less than 20 minutes, dry to constant weight at 50-80 ℃, be warming up to 115-125 ℃ and the insulation be not less than 90 minutes, be chilled to room temperature, to solution, there is not citric acid with the distilled water cyclic washing, filter, add the capacity alkali metal soln in the filtered object, filter after stirring is not less than 60 minutes, filtered object is washed with distilled water to neutrality, under 50-80 ℃, is dried to constant weight.
4, the preparation method of a kind of modified absorben cotton according to claim 3 is characterized in that: described distilled water is distilled water.
5, the preparation method of a kind of modified absorben cotton according to claim 3 is characterized in that: described alkali metal soln is the hydrogen sodium hydride solution, potassium hydroxide solution.
6, the preparation method of a kind of modified absorben cotton according to claim 5 is characterized in that: described alkali metal soln is the sodium hydroxide solution of 0.1M.
7, the using method of the described modified absorben cotton of a kind of claim 1 is characterized in that: will contain CATION waste water and regulate pH to 4-7, and add the stirring of 1-20g/l modified absorben cotton and be not less than 30 minutes, filtration gets final product.
8, the using method of modified absorben cotton according to claim 7 is characterized in that: will contain copper ion waste water and regulate pH to 5-6, and add the stirring of 1-5g/l modified absorben cotton and got final product in 30-90 minute.
CNA200610156067XA 2006-12-31 2006-12-31 Modified absorben cotton, its production and use Pending CN101029452A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102266757A (en) * 2011-09-10 2011-12-07 大连理工大学 Methods for preparing modified biomass absorbent and removing heavy metal from beverage
CN104088157A (en) * 2014-06-27 2014-10-08 白建华 Method for producing absorbent cotton by using biochemical composite treatment technology

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102266757A (en) * 2011-09-10 2011-12-07 大连理工大学 Methods for preparing modified biomass absorbent and removing heavy metal from beverage
CN102266757B (en) * 2011-09-10 2014-04-23 大连理工大学 Methods for preparing modified biomass absorbent and removing heavy metal from beverage
CN104088157A (en) * 2014-06-27 2014-10-08 白建华 Method for producing absorbent cotton by using biochemical composite treatment technology
CN104088157B (en) * 2014-06-27 2016-04-13 白建华 Biochemical composite treatment technology produces the method for absorbent cotton

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