CN107583631B - A kind of preparation method of the porous cotton complex microsphere of dimercaprol dimercaptopropanol modified magnetic - Google Patents
A kind of preparation method of the porous cotton complex microsphere of dimercaprol dimercaptopropanol modified magnetic Download PDFInfo
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- CN107583631B CN107583631B CN201710810811.1A CN201710810811A CN107583631B CN 107583631 B CN107583631 B CN 107583631B CN 201710810811 A CN201710810811 A CN 201710810811A CN 107583631 B CN107583631 B CN 107583631B
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Abstract
The invention discloses a kind of preparation methods of the porous cotton complex microsphere of dimercaprol dimercaptopropanol modified magnetic, which is characterized in that firstly, absorbent cotton and glucan are dissolved in 1- ethyl-3-methylimidazole rhodanate, magnetic porous cotton complex microsphere is prepared；Then, magnetic porous cotton complex microsphere surface amination is obtained by the magnetic porous cotton complex microsphere of amination using γ-aminopropyltrimethoxysilane；Finally, in the reactor, being added by following composition mass percentage concentration, ethyl alcohol: 68 ~ 74%, dimercaprol dimercaptopropanol: 10 ~ 16%, stirring and dissolving, the magnetic porous cotton complex microsphere of amination: 12 ~ 18%, the sum of each component is absolutely, in 50 ± 2 DEG C of constant temperature, stirring, back flow reaction 3h, after cooling, with ethanol washing, it is separated by solid-liquid separation, it is dry, obtain the porous cotton complex microsphere of dimercaprol dimercaptopropanol modified magnetic.The adsorbent has very high adsorption capacity to arsenic, mercury, and not only at low cost but also environmentally protective, high mechanical strength can be Reusability 10 times or more, and adsorbent can be easily separated.
Description
Technical field
The present invention relates to a kind of preparation method of biomagnetism adsorbent, in particular to a kind of dimercaprol dimercaptopropanol modified magnetic
The preparation method of porous cotton complex microsphere and application technology to arsenic, mercury adsorbing separation, belong to Material Field.
Background technique
With the rapid development of industry, mercury pollution refers to the environmental pollution as caused by mercury or compound containing mercury.Mercury (Hg)
It is one of strongest heavy metal element of environment Poisoning, the toxicity difference of various mercury compounds is very big.Mercuric chloride in inorganic mercury is
Extremely toxic substance；Phenyl mercury in organic mercury decomposes comparatively fast, and toxicity is little, and methyl mercury enters human body and is easier to be absorbed by, and is not easy
Very slow, especially easy to accumulate in brain, toxicity maximum is drained in degradation.Mankind's activity causes water body mercury pollution, mainly from chlorine
The waste water of the industrial discharges such as alkali, plastics, battery, electronics and waste and old medical instrument.Mercury industrially apply it is very wide, caused by dirt
Contaminate more serious, very big to Human health effects, therefore must carry out purified treatment to mercury-containing waste water, meeting regulation can discharge.
Arsenic pollution refers to the environmental pollution as caused by arsenic or its compound.The exploitation of arsenic and the metal containing arsenic is smelted, and arsenic is used
Or arsenic compound makees the processes such as glass, pigment, raw medicine, the production of paper and the burning of coal of raw material, all can produce useless containing arsenic
Water, exhaust gas and waste residue, pollute the environment.Atmosphere contains arsenic pollution in addition to the natural causes such as rock weathering, volcano eruption, mainly
Use, burning of coal from industrial production and the pesticide containing arsenic.Arsenic-containing waste water, pesticide and flue dust all can contaminated soils.Arsenic is in soil
It accumulates and thus enters in crops tissue in earth.Arsenic and arsenide generally can enter people by approach such as water, atmosphere and foods
Body causes damages.The toxicity of element arsenic is extremely low, and arsenide is toxic, and trivalent arsenic compound is more than other arsenic compound toxicity
By force.Many methods can be with arsenic removal, mercury, such as chemical deposition, ion-exchange, absorption method, film engineering method, electrochemical process, wadding
Solidifying method and lime method, wherein absorption method because adsorbent diversity, it can be achieved that efficiently, low cost and be widely used.It is ideal
Arsenic removal, mercury absorbent should be not only efficiently, but also it is cheap.Cellulose is the most abundant renewable resource in the world, not only inexpensively,
It is also rich in hydroxyl, can be modified by a variety of chemical reactions (such as esterification, etherificate, grafting), if can be in cellulose fiber dimension table
Sulfydryl is modified in face, and sulfydryl arsenic, mercury ion combine, to remove the arsenic in water body, mercury.
Adsorbent passes through the mutual of the various active groups in surface and adsorbate using its structure abundant, specific surface area in addition
Effect, extracts pollutant, to have the function that purification of water quality from liquid phase.Wherein, absorption method is excellent compared with other techniques
Gesture is to be capable of handling the reluctant metal ion of bioanalysis.But at the same time, absorption method is there is also many shortcomings,
The difficult separation of solid and liquid of middle adsorbent is always the big problem for hindering adsorption technology progress, thus many scholars endeavour in recent years
Removal in studying magnetic adsorbent and applied to polluter in water body.Research is magnetic it is found that with the help of externally-applied magnetic field
Adsorbent can fast implement separation of solid and liquid, and possess the mass transfer rate and good contacting efficiency of high speed simultaneously, thus can be
It largely can solve traditional absorption method problem encountered.
Cotton is one of most important crops in the world, and yield is big, production cost is low, keeps cotton products price relatively low
It is honest and clean.The major-minor product of cotton has higher utility value, as described in forefathers " cotton whole body is all precious ".It is both most important
Fibre crops, and be important oil crops, and the cereal crops containing high protein, or weaving, fine chemical material and
Important strategic materials.Therefore, it is necessary to make great efforts to make Yield Increase In Cotton, do well to comprehensively utilize, increase both production and value, with increase cotton grower income and
Meet the various needs of the national economic development.The application production absorption of this natural macromolecular material have it is natural, green, can give birth to
The features such as object is degraded, mechanical strength is big, resistance to corrosion is strong.
After the application dissolves the cotton fiber of natural polymer using 1- ethyl-3-methylimidazole rhodanate, it is added
Glucan increase is porous, and nano-ferrous acid is added and is magnetized, magnetic composite microsphere is obtained, using modified pair of dimercaprol dimercaptopropanol
Arsenic, mercury carry out adsorbing separation, and making it i.e. has the characteristic of magnetic adsorbent, and have natural polymer sub-feature, while also having
The selectivity of sp act group.
Summary of the invention
An object of the present invention is to provide a kind of preparation method of porous cotton complex microsphere of dimercaprol dimercaptopropanol modified magnetic,
Carry out adsorbing separation of the porous cotton complex microsphere of the dimercaprol dimercaptopropanol modified magnetic of acquisition to arsenic, mercury in aqueous systems.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of the porous cotton complex microsphere of dimercaprol dimercaptopropanol modified magnetic, which is characterized in that this method has
Following processing step:
(1) magnetic porous cotton complex microsphere preparation: in the autoclave with polytetrafluoroethyllining lining, by such as the following group
It is added at mass percentage concentration, 1- ethyl-3-methylimidazole rhodanate: 50 ~ 58%, absorbent cotton: 20 ~ 25%, it is sealed, temperature
Rise to 150 DEG C of constant temperature, 4 h of isothermal reaction, taking-up is cooled to room temperature, be added glucan: 6 ~ 12%, temperature rise to 60 ± 2 DEG C of constant temperature,
Stirring, reaction 4h are cooled to room temperature and are added nano-ferrous acid: 4 ~ 8%, N, N methylene-bisacrylamide: 4 ~ 8%, the sum of each component is
Absolutely, temperature rises to 60 ± 2 DEG C of constant temperature, and strong stirring reacts 100min, and gained viscous liquid is sprayed in liquid stone
It in wax, by the partial size of the diameter control complex microsphere of spray head, cleans, is separated by solid-liquid separation, it is multiple to obtain magnetic porous cotton for freeze-drying
Close microballoon；
(2) the magnetic porous cotton complex microsphere preparation of amination: in the reactor, add by following composition mass percentage concentration
Enter, ethyl alcohol: 48 ~ 52%, γ-aminopropyltrimethoxysilane: 30 ~ 36%, it mixes, magnetic porous cotton complex microsphere: 15 ~ 20%,
The sum of each component is absolutely, in 60 ± 2 DEG C of constant temperature, stirring, 3 ~ 4h of back flow reaction, after cooling, with ethanol washing, solid-liquid point
From, it is dry, obtain the magnetic porous cotton complex microsphere of amination；
(3) preparation of the porous cotton complex microsphere of dimercaprol dimercaptopropanol modified magnetic: in the reactor, by following composition quality hundred
Concentration is divided to be added, ethyl alcohol: 68 ~ 74%, dimercaprol dimercaptopropanol: 10 ~ 16%, stirring and dissolving, the magnetic porous cotton complex microsphere of amination: 12
~ 18%, the sum of each component is absolutely, in 50 ± 2 DEG C of constant temperature, stirring, back flow reaction 3h, after cooling, with ethanol washing, admittedly
Liquid separation, it is dry, obtain the porous cotton complex microsphere of dimercaprol dimercaptopropanol modified magnetic.
The diameter of the spray head described in step (1) is between 500 ~ 1000 μm.
1- ethyl-3-methylimidazole rhodanate, which can recycle, described in step (1) recycles.
The partial size of the porous cotton complex microsphere of prepared dimercaprol dimercaptopropanol modified magnetic is between 500 ~ 1200 μm.
It is a further object of the present invention to provide a kind of porous cotton complex microsphere adsorbents of dimercaprol dimercaptopropanol modified magnetic to water
To the absorption of arsenic, mercury, feature in system are as follows: use the porous cotton complex microsphere adsorbent of the dimercaprol dimercaptopropanol modified magnetic prepared
Deionized water impregnates 2 ~ 4h, adsorbs by static method.
The porous cotton complex microsphere adsorbent deionized water of the dimercaprol dimercaptopropanol modified magnetic prepared is impregnated into 2 ~ 4h, is pressed
Dynamic method absorption.
Compared with the prior art, the present invention has the following advantages and beneficial effects:
(1) the porous cotton complex microsphere adsorbent of dimercaprol dimercaptopropanol modified magnetic that the present invention obtains has good physico
Stability and excellent mechanical strength are learned, since its is porous, large specific surface area, the site for connecting active group is more, adsorption capacity
Greatly, to arsenic maximum adsorption capacity up to 181.20 mg/g, to mercury maximum adsorption capacity up to 192.60 mg/g, it is wear-resisting can Reusability
Number is up to 10 times or more, and the speed of absorption is fast, and absorption chooses, and desorption performance is good, can make within the scope of wider soda acid
With.
(2) the porous cotton complex microsphere adsorbent of dimercaprol dimercaptopropanol modified magnetic that the present invention obtains both had had solid phase carrier material
The advantages of material, also solves the losing issue that active group is applied in water environment, externally-applied magnetic field can will be after the completion of absorption
The advantages that adsorbent is separated from the water, and is easy to separate and recover.
(3) stability is good, is natural green product, and regrown material, waste is biodegradable, from a wealth of sources, price
It is cheap, there is realistic meaning to the pollution amelioration etc. of ambient water, mitigates environmental protection pressure；The condition for crossing range request of synthesis is easy
Control, low energy consumption, easy to operate, belongs to process for cleanly preparing, easy to industrialized production.
Specific embodiment
Embodiment 1
(1) magnetic porous cotton complex microsphere preparation: in the autoclave with polytetrafluoroethyllining lining, respectively plus
Enter, 1- ethyl-3-methylimidazole rhodanate: 54g, absorbent cotton: 23g is sealed, and temperature rises to 150 DEG C of constant temperature, isothermal reaction
4 h, taking-up are cooled to room temperature, and glucan: 8g is added, and temperature rises to 60 ± 2 DEG C of constant temperature, stirring, reaction 4h, are cooled to room temperature addition and receive
Rice cobalt ferrite: 7g, N, N methylene-bisacrylamide: 8g, temperature rise to 60 ± 2 DEG C of constant temperature, and strong stirring reacts 100min, will
Gained viscous liquid sprays in atoleine, passes through the partial size of the diameter control complex microsphere of spray head, cleaning, solid-liquid point
From freeze-drying obtains magnetic porous cotton complex microsphere；
(2) it the magnetic porous cotton complex microsphere preparation of amination: in the reactor, is separately added into, ethyl alcohol: 63 mL, γ-ammonia
Propyl trimethoxy silicane: 33g is mixed, magnetic porous cotton complex microsphere: 17g, in 60 ± 2 DEG C of constant temperature, stirring, back flow reactions
3h after cooling, with ethanol washing, is separated by solid-liquid separation, dry, obtains the magnetic porous cotton complex microsphere of amination；
(3) it the preparation of the porous cotton complex microsphere of dimercaprol dimercaptopropanol modified magnetic: in the reactor, is separately added into, ethyl alcohol: 89
ML, dimercaprol dimercaptopropanol: 12g, stirring and dissolving, the magnetic porous cotton complex microsphere of amination: 18g in 50 ± 2 DEG C of constant temperature, stirring, is returned
Stream reaction 3h after cooling, with ethanol washing, is separated by solid-liquid separation, dry, and it is compound micro- to obtain the porous cotton of dimercaprol dimercaptopropanol modified magnetic
Ball.
Embodiment 2
(1) magnetic porous cotton complex microsphere preparation: in the autoclave with polytetrafluoroethyllining lining, respectively plus
Enter, 1- ethyl-3-methylimidazole rhodanate: 50g, absorbent cotton: 25g is sealed, and temperature rises to 150 DEG C of constant temperature, isothermal reaction
4 h, taking-up are cooled to room temperature, and glucan: 10g is added, and temperature rises to 60 ± 2 DEG C of constant temperature, stirring, reaction 4h, is cooled to room temperature addition
Nano-ferrous acid: 8g, N, N methylene-bisacrylamide: 7g, temperature rise to 60 ± 2 DEG C of constant temperature, and strong stirring reacts 100min,
Gained viscous liquid is sprayed in atoleine, the partial size of the diameter control complex microsphere of spray head, cleaning, solid-liquid point are passed through
From freeze-drying obtains magnetic porous cotton complex microsphere；
(2) it the magnetic porous cotton complex microsphere preparation of amination: in the reactor, is separately added into, ethyl alcohol: 66 mL, γ-ammonia
Propyl trimethoxy silicane: 30g is mixed, magnetic porous cotton complex microsphere: 18g, in 60 ± 2 DEG C of constant temperature, stirring, back flow reactions
4h after cooling, with ethanol washing, is separated by solid-liquid separation, dry, obtains the magnetic porous cotton complex microsphere of amination；
(3) it the preparation of the porous cotton complex microsphere of dimercaprol dimercaptopropanol modified magnetic: in the reactor, is separately added into, ethyl alcohol: 94
ML, dimercaprol dimercaptopropanol: 14g, stirring and dissolving, the magnetic porous cotton complex microsphere of amination: 12g in 50 ± 2 DEG C of constant temperature, stirring, is returned
Stream reaction 3h after cooling, with ethanol washing, is separated by solid-liquid separation, dry, and it is compound micro- to obtain the porous cotton of dimercaprol dimercaptopropanol modified magnetic
Ball.
Embodiment 3
(1) magnetic porous cotton complex microsphere preparation: in the autoclave with polytetrafluoroethyllining lining, respectively plus
Enter, 1- ethyl-3-methylimidazole rhodanate: 58g, absorbent cotton: 20g is sealed, and temperature rises to 150 DEG C of constant temperature, isothermal reaction
4 h, taking-up are cooled to room temperature, and glucan: 10g is added, and temperature rises to 60 ± 2 DEG C of constant temperature, stirring, reaction 4h, is cooled to room temperature addition
Nano-ferrous acid: 6g, N, N methylene-bisacrylamide: 6g, temperature rise to 60 ± 2 DEG C of constant temperature, and strong stirring reacts 100min,
Gained viscous liquid is sprayed in atoleine, the partial size of the diameter control complex microsphere of spray head, cleaning, solid-liquid point are passed through
From freeze-drying obtains magnetic porous cotton complex microsphere；
(2) it the magnetic porous cotton complex microsphere preparation of amination: in the reactor, is separately added into, ethyl alcohol: 631mL, γ-ammonia
Propyl trimethoxy silicane: 32g is mixed, magnetic porous cotton complex microsphere: 20g, in 60 ± 2 DEG C of constant temperature, stirring, back flow reactions
3.5h after cooling, with ethanol washing, is separated by solid-liquid separation, dry, obtains the magnetic porous cotton complex microsphere of amination；
(3) it the preparation of the porous cotton complex microsphere of dimercaprol dimercaptopropanol modified magnetic: in the reactor, is separately added into, ethyl alcohol: 86
ML, dimercaprol dimercaptopropanol: 16g, stirring and dissolving, the magnetic porous cotton complex microsphere of amination: 16g in 50 ± 2 DEG C of constant temperature, stirring, is returned
Stream reaction 3h after cooling, with ethanol washing, is separated by solid-liquid separation, dry, and it is compound micro- to obtain the porous cotton of dimercaprol dimercaptopropanol modified magnetic
Ball.
Embodiment 4
(1) magnetic porous cotton complex microsphere preparation: in the autoclave with polytetrafluoroethyllining lining, respectively plus
Enter, 1- ethyl-3-methylimidazole rhodanate: 56g, absorbent cotton: 24g is sealed, and temperature rises to 150 DEG C of constant temperature, isothermal reaction
4 h, taking-up are cooled to room temperature, and glucan: 12g is added, and temperature rises to 60 ± 2 DEG C of constant temperature, stirring, reaction 4h, is cooled to room temperature addition
Nano-ferrous acid: 4g, N, N methylene-bisacrylamide: 4g, temperature rise to 60 ± 2 DEG C of constant temperature, and strong stirring reacts 100min,
Gained viscous liquid is sprayed in atoleine, the partial size of the diameter control complex microsphere of spray head, cleaning, solid-liquid point are passed through
From freeze-drying obtains magnetic porous cotton complex microsphere；
(2) it the magnetic porous cotton complex microsphere preparation of amination: in the reactor, is separately added into, ethyl alcohol: 62 mL, γ-ammonia
Propyl trimethoxy silicane: 36g is mixed, magnetic porous cotton complex microsphere: 15g, in 60 ± 2 DEG C of constant temperature, stirring, back flow reactions
3h after cooling, with ethanol washing, is separated by solid-liquid separation, dry, obtains the magnetic porous cotton complex microsphere of amination；
(3) it the preparation of the porous cotton complex microsphere of dimercaprol dimercaptopropanol modified magnetic: in the reactor, is separately added into, ethyl alcohol: 92
ML, dimercaprol dimercaptopropanol: 10g, stirring and dissolving, the magnetic porous cotton complex microsphere of amination: 17g in 50 ± 2 DEG C of constant temperature, stirring, is returned
Stream reaction 3h after cooling, with ethanol washing, is separated by solid-liquid separation, dry, and it is compound micro- to obtain the porous cotton of dimercaprol dimercaptopropanol modified magnetic
Ball.
Embodiment 5
The porous cotton complex microsphere of 0.10g dimercaprol dimercaptopropanol modified magnetic is weighed as adsorbent and is respectively placed in 250mL tool plug
2 ~ 4h is impregnated in conical flask, after filtration washing, then being separately added into 100mL concentration is 500mg/L arsenic, in mercury standard solution, with dilute
The pH value of acid or alkali regulation system is in 2.0 ~ 11.0 ranges, and 0.2 ~ 2h of concussion absorption, takes supernatant, use electrochemistry at room temperature
Method measures the concentration of arsenic, is counted with the concentration of cold-vapour atomic absorption method measurement mercury according to the concentration difference of arsenic, mercury in the water of absorption front and back
Calculate the adsorption capacity of the porous cotton complex microsphere of dimercaprol dimercaptopropanol modified magnetic, the modified magnetic of dimercaprol dimercaptopropanol obtained by the present invention
The porous cotton complex microsphere of property to the absorption pH value of arsenic in 5.0 ~ 7.0 ranges, to the absorption pH value of mercury in 1.0 ~ 3.5 ranges,
Adsorbent is maximum to the adsorption capacity of arsenic, mercury and stablizes, at room temperature concussion absorption 0.5h, and arsenic, this absorption of mercuri are complete,
Arsenic, mercury maximum adsorption capacity be respectively 181.20 mg/g, 192.60 mg/g.
Embodiment 6
The porous cotton complex microsphere of 1.0g dimercaprol dimercaptopropanol modified magnetic is weighed as adsorbent and is respectively placed in 250mL tool plug
2 ~ 4h is impregnated in conical flask, after filtration washing, additions 100mL concentration is 200mg/L arsenic, in mercury standard solution, with diluted acid or alkali
The pH value of regulation system is 6.0, and concussion absorption 0.5h, takes supernatant at room temperature, measures arsenic, the pH value of system is 2.0, in room
The lower concussion absorption 0.5h of temperature, takes supernatant, and the concentration of mercury calculates dimercapto according to the concentration difference of arsenic, mercury in the water of absorption front and back
The porous cotton complex microsphere of propyl alcohol modified magnetic as adsorbent to the removal rate of arsenic, mercury, dimercaprol dimercaptopropanol obtained by the present invention
The porous cotton complex microsphere of modified magnetic as adsorbent to the removal rate of arsenic, mercury all 96.16% or more, reach as high as 99.4%.
Claims (4)
1. a kind of preparation method of the porous cotton complex microsphere of dimercaprol dimercaptopropanol modified magnetic, which is characterized in that this method have with
Lower processing step:
(1) magnetic porous cotton complex microsphere preparation: in the autoclave with polytetrafluoroethyllining lining, by following composition matter
It measures percentage concentration to be added, 1- ethyl-3-methylimidazole rhodanate: 50~58%, absorbent cotton: 20~25%, it is sealed, temperature
Rise to 150 DEG C of constant temperature, isothermal reaction 4h, taking-up is cooled to room temperature, be added glucan: 6~12%, temperature rise to 60 ± 2 DEG C of constant temperature,
Stirring, reaction 4h are cooled to room temperature and are added nano-ferrous acid: 4~8%, N, N methylene-bisacrylamide: 4~8%, each group point it
With for absolutely, temperature rises to 60 ± 2 DEG C of constant temperature, strong stirring reacts 100min, and gained viscous liquid is sprayed in liquid
It in body paraffin, by the partial size of the diameter control complex microsphere of spray head, cleans, is separated by solid-liquid separation, freeze-drying obtains magnetic porous
Cotton complex microsphere；
(2) it the magnetic porous cotton complex microsphere preparation of amination: in the reactor, is added by following composition mass percentage concentration, second
Alcohol: 48~52%, γ-aminopropyltrimethoxysilane: 30~36%, it mixes, magnetic porous cotton complex microsphere: 15~20%,
The sum of each component is absolutely, in 60 ± 2 DEG C of constant temperature, stirring, 3~4h of back flow reaction, after cooling, with ethanol washing, solid-liquid
Separation, it is dry, obtain the magnetic porous cotton complex microsphere of amination；
(3) preparation of the porous cotton complex microsphere of dimercaprol dimercaptopropanol modified magnetic: in the reactor, dense by following composition quality percentage
Degree is added, ethyl alcohol: 68~74%, dimercaprol dimercaptopropanol: and 10~16%, stirring and dissolving, the magnetic porous cotton complex microsphere of amination: 12
~18%, the sum of each component be absolutely, in 50 ± 2 DEG C of constant temperature, stirring, back flow reaction 3h, after cooling, with ethanol washing,
It is separated by solid-liquid separation, it is dry, obtain the porous cotton complex microsphere of dimercaprol dimercaptopropanol modified magnetic.
2. a kind of preparation method of the porous cotton complex microsphere of dimercaprol dimercaptopropanol modified magnetic according to claim 1,
It is characterized in that, the diameter of spray head described in step (1) is between 500~1000 μm.
3. a kind of preparation method of the porous cotton complex microsphere of dimercaprol dimercaptopropanol modified magnetic according to claim 1,
It is characterized in that, the partial size of the porous cotton complex microsphere of prepared dimercaprol dimercaptopropanol modified magnetic is between 500~1200 μm.
4. a kind of preparation method of the porous cotton complex microsphere of dimercaprol dimercaptopropanol modified magnetic according to claim 1 is made
The porous cotton complex microsphere adsorbent of standby dimercaprol dimercaptopropanol modified magnetic.
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