CN107583618A - A kind of sodium alginate/mussel shell powder microballoon and application thereof - Google Patents
A kind of sodium alginate/mussel shell powder microballoon and application thereof Download PDFInfo
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- CN107583618A CN107583618A CN201710892043.9A CN201710892043A CN107583618A CN 107583618 A CN107583618 A CN 107583618A CN 201710892043 A CN201710892043 A CN 201710892043A CN 107583618 A CN107583618 A CN 107583618A
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Abstract
The present invention discloses a kind of sodium alginate/mussel shell powder microballoon and application thereof, belongs to heavy metal absorbent technical field, mosanom/mussel shell powder method for preparing microsphere is as follows:1)Take atoleine to be placed in conical flask, emulsifying agent is added under water bath condition, be stirred until homogeneous ensuing crop oil phase;2)The aqueous solution is made into sodium alginate, is aqueous phase, adds in oil phase and stirs, forms w/o type emulsion, adds 2 ~ 4wt% CaCL2The modification mussel shell powder solution of solution and 30 ~ 45wt%, slow-speed of revolution crosslinking curing, add petroleum ether and stirring, centrifuge taking precipitate, washed with isopropanol, dry sodium alginate/mussel shell powder microballoon, the present invention is using the accessory substance of marine products processing as raw material, cost is low, the microballoon good dispersion of preparation, no microballoon adhesion situation, particle diameter distribution are narrower, heavy metal ionic adsorption is good, and adsorption rate is high.
Description
Technical field
The invention belongs to heavy metal absorbent technical field, and in particular to a kind of sodium alginate/mussel shell powder microballoon and its
Purposes.
Background technology
With the development of global economy and society, environmental pollution getting worse, wherein industrial wastewater are as main environment
Pollution sources, it is a great problem for perplexing countries in the world for a long time.Heavy metal ion in industrial wastewater have it is strong it is carcinogenic,
Teratogenesis, mutagenic effect, serious threat is constituted to health and ecological environment, therefore strictly control heavy metal wastewater thereby
Polluting most important, traditional process for treating heavy-metal waste water mainly has chemical precipitation method, ion-exchange, membrane separation process etc.,
These methods are generally in the presence of investment is big, high energy consumption, operating cost are high, is also easy to produce secondary pollution problems, using being restricted.Inhale
Attached method is using the pollutant in adsorbent absorption water, so as to purify the method for waste water, is had simple to operate, fast and effectively special
Point, is widely used, and how to obtain the adsorbent that cheap, adsorption capacity is strong, adsorptive selectivity is high, has become and grind
Study carefully the focus of exploitation.
The content of the invention
An object of the present invention is to provide a kind of accessory substance using marine products processing as raw material, and cost is low, preparation it is micro-
The phenomenon of ball good dispersion, no microballoon adhesion or cluster cohesion, particle diameter distribution is narrower, and a kind of excellent sodium alginate of adsorptivity/
Mussel shell powder microballoon.
It is heavy metal ion adsorbed for being that the second object of the present invention is to provide a kind of sodium alginate/mussel shell powder microballoon
Purposes in agent.
The technical scheme taken to achieve the above object of the present invention is:It is prepared by a kind of sodium alginate/mussel shell powder microballoon
Method is as follows:
1)Take atoleine to be placed in conical flask, emulsifying agent is added under water bath condition, be stirred until homogeneous ensuing crop oil phase;
2)The aqueous solution is made into sodium alginate, is aqueous phase, adds in oil phase and stirs, forms w/o type emulsion, adds 2 ~ 4wt%'s
CaCL2The modification mussel shell powder solution of solution and 30 ~ 45wt%, slow-speed of revolution crosslinking curing add petroleum ether and stirring, and centrifuging and taking is sunk
Starch, washed with isopropanol, dry sodium alginate/mussel shell powder microballoon, sodium alginate have obvious pH sensitiveness and
Absorption property, mussel shell powder have a micro-nano structure, and sodium alginate quick under conditions of extremely gentle can form gel, when having
In the presence of the cations such as Ca2+, Sr2+, with bivalent cation ion-exchange reactions, G units accumulation shape occur for the Na+ on G units
Into cross-linked network structure, so as to form hydrogel, use the microballoon sphere diameter obtained by outside solidification method small in above-mentioned steps 1,2, ball
Body distribution uniform, sharp outline between ball and ball, balling-up in order, no microballoon cluster phenomenon, and the raw material utilized come
From the accessory substance of marine product, make full use of resource, accessory substance is carried out it is high-valued, microballoon prepare cost it is low.
Preferably, the emulsifying agent in step 1 is Arlacel-80, Tween-80, APES, Sorbitan alcohol ester
One or more in fat acid esters, after one or more combinations in mentioned component manufactured emulsifying agent can shape film forming elastomer it is big
Dense composite film, and the composition in emulsifying agent is not easy to dissociate into oil phase, the excellent in stability of composite membrane.
Preferably, the preparation method of modified oyster shell whiting is in step 2:Took 60-100 mesh mussel shell powder to be added to concentration to be
In the mixed solution of 2-4wt% citric acid solution and 1-3wt% polyvinylpyrrolidone and stir, solid-to-liquid ratio 1:2-
Acid activation mussel shell powder liquid is obtained after 4, acid activation 0.5-1.5h, by above-mentioned acid activation mussel shell powder liquid at 500 DEG C -680 DEG C
Thermal activation is carried out, is taken out after 0.5-1h and obtains thermal activation mussel shell powder, after thermal activation mussel shell powder crushed into 180-220 mesh
Obtain being modified mussel shell powder, using citric acid and polyvinylpyrrolidonesolution solution to after the progress acid activation of mussel shell part and after warp
The modification mussel shell powder that continuous thermal activation treatment obtains can effectively avoid calcium chloride solution in solidification process from causing microballoon cluster to coagulate
Poly- phenomenon, and modified mussel shell powder has loose structure, acquirement arrives unexpected nonlinear adsorption effect, can make heavy metal
Ion is easier the sodium alginate/mussel shell powder microballoon absorption being produced.
Preferably, citric acid solution is in 0.1T to stirring 10-15min under 0.3T magnetic fields, and magnetic direction parallel to
Mixing direction;There is electrode in the stirring rod that stirring exchange step uses, and there is electrode in stirring container;Stirring rod is in stirring
It is 0.3 to 0.4V to mix the voltage between container, regulates and controls switched environment using magnetic environment combination weak current, can make citric acid solution pair
Mussel shell powder has more preferable acid activation effect, and to strengthen the adsorption effect of modified mussel shell powder, and process cost is low, effect
Fruit is good.
Preferably, the ratio of step 2 reclaimed water oil phase is 1:0.95-1.03, emulsification is beneficial to using the ratio of above-mentioned water oil phase,
The microballoon of preparation is rounded, and form is complete, and particle diameter distribution is uniform, good dispersion, and no adhesion situation occurs.
Preferably, the mixing speed in step 2 is 480-550r/min, the alginic acid prepared using above-mentioned mixing speed
Sodium/mussel shell powder microballoon is spherical good, rounded shape, and spherical complete, good dispersion, no adhesion phenomenon.
Preferably, sodium alginate soln mass fraction is 2%-5% in step 2, and the sodium alginate soln in aqueous phase uses
Microballoon sphere diameter prepared by above-mentioned mass fraction is small, spheroid distribution uniform, sharp outline between ball and ball, and balling-up situation is good
It is good, no microballoon cluster phenomenon.
APES containing 1%-1.5%wt in petroleum ether, improves the sedimentation of the product in whipping process
Speed and sedimentation rate, be advantageous to the yield and effect of final mosanom/mussel shell powder microballoon.
A kind of purposes of sodium alginate/mussel shell powder microballoon, sodium alginate/mussel shell powder microballoon be used for be heavy metal from
Purposes on sub- adsorbent, sodium alginate have obvious pH sensitiveness and absorption property, and mussel shell powder has micro-nano structure,
There is certain absorption property, the raw material utilized is all from the accessory substance of marine product, makes full use of resource, and accessory substance is carried out into high level
Change, microballoon preparation cost is low, and sodium alginate/mussel shell powder microballoon of preparation easily adsorbs heavy metal ion, and adsorption rate is high.
Compared with prior art, beneficial effects of the present invention:The preparing raw material of the present invention is all from the accessory substance of marine product,
Make full use of resource, accessory substance is carried out it is high-valued, microballoon prepare cost it is low;It can effectively avoid solidifying by modified mussel shell powder
During calcium chloride solution cause the phenomenon that microballoon cluster condenses, and modified mussel shell powder has loose structure, obtains to expecting
Less than nonlinear adsorption effect, heavy metal ion can be made to be easier the sodium alginate that is produced/mussel shell powder microballoon absorption;System
Standby sodium alginate/mussel shell powder microballoon sphere diameter is small, spheroid distribution uniform, sharp outline between ball and ball, and balling-up situation is good
Good, no microballoon cluster phenomenon, microballoon easily adsorbs heavy metal ion, and adsorption rate is high.
Embodiment
The present invention is described in further detail with reference to embodiments:
Embodiment 1:
A kind of sodium alginate/mussel shell powder method for preparing microsphere is as follows:
1)Take the atoleine of 27 parts by weight to be placed in 300ml conical flasks, emulsifying agent, emulsifying agent are added under 38 DEG C of water bath conditions
For two kinds of mixtures of Arlacel-80 and APES, ensuing crop oil phase, mixing speed 480- are stirred until homogeneous
550r/min;
2)The aqueous solution is made into as aqueous phase using sodium alginate, sodium alginate soln mass fraction is 3%, adds in oil phase and stirs, water oil
The ratio of phase is 1:0.98, mixing speed 520r/min, w/o type emulsion is formed, add 3wt% CaCL2Solution and 38wt%
Modification mussel shell powder solution, slow-speed of revolution crosslinking curing 30min, the petroleum ether and stirring 14min of 11 parts by weight is added, in petroleum ether
APES containing 1%wt, 9min taking precipitates are centrifuged under the conditions of 5200r/min, 3 are washed repeatedly with isopropanol
It is secondary, dry sodium alginate/mussel shell powder microballoon at 48 DEG C;
The preparation method of modified oyster shell whiting is:80 mesh mussel shell powder were taken to be added to the citric acid solution and 1wt% that concentration is 3wt%
Polyvinylpyrrolidone mixed solution in and stir, citric acid solution is in 0.1T to stirring under 0.3T magnetic fields
12min, and magnetic direction parallel to mixing direction;There is electrode in the stirring rod that stirring exchange step uses, and stir and hold
There is electrode on device;Voltage of the stirring rod between stirring container is 0.3 to 0.4V, and the solid-to-liquid ratio of mussel shell powder and mixed solution is
1:Acid activation mussel shell powder liquid is obtained after 3, acid activation 1h, above-mentioned acid activation mussel shell powder liquid is subjected to thermal activation at 570 DEG C,
Taken out after 0.6h and obtain thermal activation mussel shell powder, obtain being modified mussel shell powder after thermal activation mussel shell powder crushed into 200 mesh.
A kind of purposes of sodium alginate/mussel shell powder microballoon, sodium alginate/mussel shell powder microballoon be used for be heavy metal from
Purposes on sub- adsorbent, sodium alginate have obvious pH sensitiveness and absorption property, and mussel shell powder has micro-nano structure,
There is certain absorption property, the raw material utilized is all from the accessory substance of marine product, makes full use of resource, and accessory substance is carried out into high level
Change, microballoon preparation cost is low, and sodium alginate/mussel shell powder microballoon of preparation easily adsorbs heavy metal ion, and adsorption rate is high.
Embodiment 2:
A kind of sodium alginate/preferred preparation method of mussel shell powder microballoon is as follows:
1)Take the atoleine of 27 parts by weight to be placed in 300ml conical flasks, emulsifying agent, emulsifying agent are added under 40 DEG C of water bath conditions
For three kinds of mixtures in Tween-80, APES, sorbitan fatty acid ester, ensuing crop is stirred until homogeneous
Oil phase, mixing speed 490r/min;
2)The aqueous solution is made into as aqueous phase using sodium alginate, sodium alginate soln mass fraction is 3%, adds in oil phase and stirs, water oil
The ratio of phase is 1:1, mixing speed 530r/min, w/o type emulsion is formed, add 4wt% CaCL2Solution and 37wt%'s changes
Property mussel shell powder solution, slow-speed of revolution crosslinking curing 30min adds the petroleum ether and stirring 14min of 12 parts by weight, contains in petroleum ether
1.3%wt APESs, 8min taking precipitates are centrifuged under the conditions of 6000r/min, are washed repeatedly with isopropanol 2 times,
Dry sodium alginate/mussel shell powder microballoon at 48 DEG C;
The preparation method of modified oyster shell whiting is:80 mesh mussel shell powder were taken to be added to the citric acid solution and 3wt% that concentration is 3wt%
Polyvinylpyrrolidone mixed solution in and stir, citric acid solution is in 0.1T to stirring under 0.3T magnetic fields
12min, and magnetic direction parallel to mixing direction;There is electrode in the stirring rod that stirring exchange step uses, and stir and hold
There is electrode on device;Voltage of the stirring rod between stirring container is 0.3 to 0.4V, and the solid-to-liquid ratio of mussel shell powder and mixed solution is
1:Acid activation mussel shell powder liquid is obtained after 3, acid activation 1h, above-mentioned acid activation mussel shell powder liquid is subjected to thermal activation at 650 DEG C,
Taken out after 0.5h and obtain thermal activation mussel shell powder, obtain being modified mussel shell powder after thermal activation mussel shell powder crushed into 180 mesh.
300ml conical flasks inwall in above-mentioned preparation process is coated with release coating, and release coating is by following component and again
Measure part composition:Chlorosulfonated polyethylene 65-72 parts, N- sodium hydroxy methyl glycinate 0.7-0.75 parts, graphite 2-17 parts, molybdenum disulfide
0.5-2 parts, potassium antimony tartrate 0.02-0.07 parts, conical flask inwall coat release coating and dry after can be formed one layer it is anti-sticking
Coating, the N- sodium hydroxy methyl glycinates of addition and potassium antimony tartrate combination coating remaining composition can be formed in the coating surface of formation
Crystallizing layer, the dense degree of coating is improved, avoid chemical composition from being adhered to conical flask inwall, while be also beneficial in microballoon preparation process
Each composition can fully react, and the lifting of the operating effect such as stirring, temperature conduction.
A kind of purposes of sodium alginate/mussel shell powder microballoon, sodium alginate/mussel shell powder microballoon be used for be heavy metal from
Purposes on sub- adsorbent, sodium alginate have obvious pH sensitiveness and absorption property, and mussel shell powder has micro-nano structure,
There is certain absorption property, the raw material utilized is all from the accessory substance of marine product, makes full use of resource, and accessory substance is carried out into high level
Change, microballoon preparation cost is low, and sodium alginate/mussel shell powder microballoon of preparation easily adsorbs heavy metal ion, and adsorption rate is high.
Embodiment 3:
A kind of sodium alginate/mussel shell powder method for preparing microsphere is as follows:
1)Take the atoleine of 32 parts by weight to be placed in 300ml conical flasks, emulsifying agent, emulsifying agent are added under 38 DEG C of water bath conditions
For three kinds of Arlacel-80, Tween-80, APES mixtures, ensuing crop oil phase is stirred until homogeneous, mixing speed is
500r/min;
2)The aqueous solution is made into as aqueous phase using sodium alginate, sodium alginate soln mass fraction is 3%, adds in oil phase and stirs, water oil
The ratio of phase is 1:1.02, mixing speed 510r/min, w/o type emulsion is formed, add 3wt% CaCL2Solution and 38wt%
Modification mussel shell powder solution, slow-speed of revolution crosslinking curing 30min, the petroleum ether and stirring 12min of 11 parts by weight is added, in petroleum ether
APES containing 1.1%wt, 9min taking precipitates are centrifuged under the conditions of 5500r/min, are washed repeatedly with isopropanol
3 times, dry sodium alginate/mussel shell powder microballoon at 48 DEG C;
The preparation method of modified oyster shell whiting is:70 mesh mussel shell powder were taken to be added to the citric acid solution and 2wt% that concentration is 3wt%
Polyvinylpyrrolidone mixed solution in and stir, citric acid solution is in 0.1T to stirring under 0.3T magnetic fields
13min, and magnetic direction parallel to mixing direction;There is electrode in the stirring rod that stirring exchange step uses, and stir and hold
There is electrode on device;Voltage of the stirring rod between stirring container is 0.3 to 0.4V, and the solid-to-liquid ratio of mussel shell powder and mixed solution is
1:Acid activation mussel shell powder liquid is obtained after 3, acid activation 1.5h, above-mentioned acid activation mussel shell powder liquid is carried out into heat at 650 DEG C lives
Change, taken out after 0.8h and obtain thermal activation mussel shell powder, obtain being modified mussel shell after thermal activation mussel shell powder crushed into 180 mesh
Powder.
A kind of purposes of sodium alginate/mussel shell powder microballoon, sodium alginate/mussel shell powder microballoon be used for be heavy metal from
Purposes on sub- adsorbent, sodium alginate have obvious pH sensitiveness and absorption property, and mussel shell powder has micro-nano structure,
There is certain absorption property, the raw material utilized is all from the accessory substance of marine product, makes full use of resource, and accessory substance is carried out into high level
Change, microballoon preparation cost is low, and sodium alginate/mussel shell powder microballoon of preparation easily adsorbs heavy metal ion, and adsorption rate is high.
Mosanom prepared by embodiment 1-3/mussel shell powder microballoon adsorbs a huge sum of money respectively with existing sodium alginate micro ball
Belong to ion, detailed process is:A certain amount of mosanom/mussel shell powder microballoon and heavy metal ion are added in 300mL conical flasks
Solution 100mL, put it into water-bath constant temperature oscillator with 100r/min velocity fluctuation, filtered to the scheduled time, using point
Light photometry measure Bing calculates the adsorption rate of heavy metal ion, and existing sodium alginate micro ball assay method is same as above.
As a result such as following table:
Sorbing material | Embodiment 1 | Embodiment 2 | Embodiment 3 | Sodium alginate micro ball |
Adsorption rate (%) | 74 | 82 | 77 | 65 |
As seen from table, mosanom/mussel shell powder microballoon heavy metal ion prepared by the present invention has excellent absorption property,
The heavy metal ion in water body can effectively be removed.
Routine operation in above-described embodiment 1,2,3 is well known to those skilled in the art, herein without repeating.
Technical scheme is described in detail embodiment described above, it should be understood that it is described above only
For the specific embodiment of the present invention, it is not intended to limit the invention, all any modifications made in the spirit of the present invention,
Supplement or similar fashion replacement etc., should be included in the scope of the protection.
Claims (9)
- A kind of 1. sodium alginate/mussel shell powder microballoon, it is characterised in that:The preparation method of the microballoon is as follows:1)Take atoleine to be placed in conical flask, emulsifying agent is added under water bath condition, be stirred until homogeneous ensuing crop oil phase;2)The aqueous solution is made into sodium alginate, is aqueous phase, adds in oil phase and stirs, forms w/o type emulsion, adds 2 ~ 4wt%'s CaCL2The modification mussel shell powder solution of solution and 30 ~ 45wt%, slow-speed of revolution crosslinking curing add petroleum ether and stirring, and centrifuging and taking is sunk Starch, washed with isopropanol, dry sodium alginate/mussel shell powder microballoon.
- A kind of 2. sodium alginate according to claim 1/mussel shell powder microballoon, it is characterised in that:Breast in the step 1 Agent is the one or more in Arlacel-80, Tween-80, Octoxinol.
- A kind of 3. sodium alginate according to claim 1/mussel shell powder microballoon, it is characterised in that:It is modified in the step 2 The preparation method of oyster shell whiting is:60-100 mesh mussel shell powder was taken to be added to the citric acid solution and 1-3wt% that concentration is 2-4wt% Polyvinylpyrrolidone mixed solution in and stir, solid-to-liquid ratio 1:Sour work is obtained after 2-4, acid activation 0.5-1.5h Change mussel shell powder liquid, above-mentioned acid activation mussel shell powder liquid is subjected to thermal activation at 500 DEG C -680 DEG C, taken out after 0.5-1h To thermal activation mussel shell powder, obtain being modified mussel shell powder after thermal activation mussel shell powder crushed into 180-220 mesh.
- A kind of 4. sodium alginate according to claim 3/mussel shell powder microballoon, it is characterised in that:The citric acid solution 10-15min is stirred under 0.1T to 0.3T magnetic fields, and magnetic direction is parallel to described mixing direction;Described stirring There is electrode in the stirring rod that exchange step uses, and there is electrode in stirring container;Described stirring rod is between stirring container Voltage be 0.3 to 0.4V.
- A kind of 5. sodium alginate according to claim 1/mussel shell powder microballoon, it is characterised in that:The step 2 reclaimed water oil The ratio of phase is 1:0.95-1.03.
- A kind of 6. sodium alginate according to claim 1/mussel shell powder microballoon, it is characterised in that:Stirring in the step 2 It is 480-550r/min to mix speed.
- A kind of 7. sodium alginate according to claim 1/mussel shell powder microballoon, it is characterised in that:Marine alga in the step 2 Acid sodium solution mass fraction is 2%-5%.
- A kind of 8. sodium alginate according to claim 1/mussel shell powder microballoon, it is characterised in that:Contain in the petroleum ether There is 1%-1.5%wt APES.
- A kind of 9. purposes of sodium alginate/mussel shell powder microballoon, it is characterised in that:The sodium alginate/mussel shell powder microballoon is used In the purposes being on adsorbent for heavy metal.
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CN108828141A (en) * | 2018-04-26 | 2018-11-16 | 宁波诺丁汉新材料研究院有限公司 | A kind of heavy metal adsorption performance test methods of mussel shell material |
CN108854990A (en) * | 2018-07-12 | 2018-11-23 | 广安职业技术学院 | Corn clothing complex microsphere and preparation method thereof for adsorbing heavy metal |
CN112551631A (en) * | 2020-12-01 | 2021-03-26 | 长春工业大学 | Method for rapidly reducing concentration of heavy metal chromium ions in water |
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CN112852562A (en) * | 2021-01-13 | 2021-05-28 | 浙江海洋大学 | Powdery tableware detergent based on modified mussel shell powder |
CN113198430A (en) * | 2021-05-15 | 2021-08-03 | 兰州城市学院 | Preparation method of composite nano material |
CN113388325A (en) * | 2021-06-09 | 2021-09-14 | 湖北绿新环保包装科技有限公司 | Laser transfer coating for low-temperature die pressing |
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CN113388325A (en) * | 2021-06-09 | 2021-09-14 | 湖北绿新环保包装科技有限公司 | Laser transfer coating for low-temperature die pressing |
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Application publication date: 20180116 |