CN105080506A - Preparation method and application of sodium alginate microspheres - Google Patents

Preparation method and application of sodium alginate microspheres Download PDF

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Publication number
CN105080506A
CN105080506A CN201510603741.3A CN201510603741A CN105080506A CN 105080506 A CN105080506 A CN 105080506A CN 201510603741 A CN201510603741 A CN 201510603741A CN 105080506 A CN105080506 A CN 105080506A
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China
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sodium alginate
reed
micro ball
pcp
phe
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郎印海
彭鹏
王小梅
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Ocean University of China
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Ocean University of China
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Abstract

The invention discloses a preparation method and application of sodium alginate microspheres. After reeds are washed, dried in air and crushed, reed powder is placed in a 600 DEG C muffle furnace (the environment is full of N2) to be subjected to pyrolysis for 2 h, after being cooled, the reed power is sieved through a 100-mesh sieve, and reed biochar is obtained after the reed powder is subjected to chlorohydric acid pickling. Meanwhile, sodium alginate is dissolved in deionized water to be prepared into a 4% sodium alginate solution. A 20g/L reed biochar aqueous solution and the sodium alginate solution are evenly mixed according to the volume ratio of 1:1, a mixed solution is dropped into a CaCl2 solution through a peristaltic pump, and reed biochar-sodium alginate microsphere adsorption materials are made. The sodium alginate microspheres are environment-friendly materials and low in cost, the preparation method is simple and easy to implement, specifications are uniform, the sodium alginate microspheres have a good adsorption effect on pentachlorophenol (PCP) and phenanthrene (Phe) and are easy to recycle and high in acid and alkali resistance. The preparation method can be used for waste water treatment and can also be used as growing carriers of microorganisms, algae and the like.

Description

A kind of preparation method of sodium alginate micro ball and application
Technical field
The invention belongs to technical field of waste water processing, particularly a kind of sodium alginate micro ball preparation method and application.
Background technology
Pentachlorophenol (PCP) is a kind of ionogenic ionic chlorophenols compound, and it is listed in the pollutant of priority acccess control, has the characteristics such as toxicity is large, antibiont degradation capability is strong.The stable chemical nature of PCP, not easily degrade, volatility is very low, be difficult to pass through air migration, there is very strong toxicity, it can cause damage in various degree to the five big systems of human body (respiratory system, internal system, reproductive system, nervous system and integumentary system), and has carcinogenic, the effect such as teratogenesis and mutagenesis.Luxuriant and rich with fragrance (Phenanthrene, Phe) is condensed by three phenyl ring to form, and molecular characterization is a kind of typical polycyclic aromatic hydrocarbon (PAHs) significantly.It is extensively present in environment as the typical organic pollution of one, and polycyclic aromatic hydrocarbon has significant Zhi Ai ﹑ Zhi Ji ﹑ mutagenesis " three cause " effect, and thus the Transport And Transformation of the organic pollution such as PCP and Phe is subject to the extensive concern of Chinese scholars.
Absorption method is used for the removal of organic pollution as a kind of method that cheapness is easy.Mainly contain active carbon, charcoal etc. for the adsorbent removing PCP and Phe at present, and there is very strong absorption property.But the removal that active carbon and charcoal are used for PCP or Phe in water makes adsorbent be difficult to recycling, and in addition, a large amount of charcoals or active carbon are dispersed in water and make the color and luster of water environment be deteriorated, and then cause secondary pollution.
Summary of the invention
The object of the present invention is to provide a kind of utilize waste reed to prepare for raw material charcoal and reed charcoal-sodium alginate micro ball of preparing of sodium alginate compound, for the removal containing PCP and Phe waste water; To solve waste resource problem of management further, and adsorbent reclaims cycling and reutilization problem, thus makes up the deficiencies in the prior art.
Sodium alginate micro ball of the present invention, its preparation method is as follows:
1) 60 mesh sieves are crossed, pyrolysis in Muffle furnace after being pulverized by reed; Be cooled to room temperature to take out, cross 100 mesh sieves, obtained original reed charcoal;
2) by the HCl of original reed charcoal 1mol/L soak 12h, then with deionized water repeatedly rinse to flushing liquor pH be 7, then under 60 DEG C of conditions dry obtain reed charcoal;
3) sodium alginate aqueous solution is mixed with reed charcoal aqueous solution equal-volume, with the CaCl of peristaltic pump by mixed liquor instillation 4% 2in solution, be cross-linked, product is cleaned by deionized water again, namely obtains reed charcoal-sodium alginate micro ball.
Above-mentioned steps 1) in pyrolysis time be filled with nitrogen, pyrolysis heating rate is 15 DEG C/min, and pyrolysis temperature is 600 DEG C.
Above-mentioned steps 2) described in the volume mass of 1mol/LHCl soak and original reed charcoal be 15 ~ 25:1 than mL/g.
Above-mentioned steps 3) described in the concentration of the reed charcoal aqueous solution be 10 ~ 20g/L, the concentration of sodium alginate soln is 2.5% ~ 4.0%.
Sodium alginate micro ball prepared by the present invention is for the adsorption treatment of pollutant in water body;
Described pollutant, for pentachlorophenol PCP or and luxuriant and rich with fragrance Phe;
The present invention also provides a kind of process containing the method for PCP and/or Phe waste water, is be added to by sodium alginate micro ball in the waste water containing PCP and/or Phe to adsorb;
CaCl is placed in as preferred sodium alginate micro ball 2soak 24h in solution, make the performance of microballoon more stable.
The present invention build a kind of reed charcoal-sodium alginate micro ball preparation method and to containing the application of PCP and Phe waste water.The preparation of this microballoon improves the organic efficiency of reed charcoal, reduces cost recovery, avoids secondary pollution.Reed charcoal-sodium alginate micro ball all has better removal effect to PCP and Phe, and power of regeneration is strong, is a kind of environmental protection shaped material of cheapness.
Specific embodiments
Below by embodiment, the present invention is described in further detail.
Embodiment 1
Waste reed is reclaimed, cleans by deionized water, air-dry to constant weight, pulverize with plant pulverizer, crossing 60 mesh sieves, taking reed powder 50g in being full of N 2muffle furnace in pyrolysis, heating rate is 15 DEG C/min, and pyrolysis temperature is 600 DEG C, be cooled to after pyrolysis 2h room temperature take out, cross 100 mesh sieves, namely obtain original reed charcoal.
For the ash content in removal reed charcoal and solable matter, get original reed charcoal 10g, by 1mol/L salt acid soak (V:m=20:1), and be placed in 25 DEG C, constant temperature oscillation 12h under 180rpm condition, filter, discard filtrate, then reed charcoal is repeatedly cleaned by deionized water, until the pH value of filtrate is 7, then dry under 60 DEG C of conditions, obtain reed charcoal.
Accurately taking 2.0g reed charcoal adds in the beaker containing 100mL deionized water, be the sodium alginate soln Homogeneous phase mixing of 4% with 100mL mass fraction after stirring with glass bar, mixed liquor magnetic stirrer makes its Homogeneous phase mixing, and dropwise instilling mass fraction by peristaltic pump (rotating speed is 40rpm) is the CaCl of 4% 2in solution, under room temperature, crosslinked 12h, obtains reed charcoal-sodium alginate micro ball.The particle diameter of this microballoon is 3.8 ± 0.1mm, is dispersed with the reed charcoal particle of black in translucent sodium alginate sphere space equably.
Accurately take the above-mentioned reed charcoal-sodium alginate micro ball of 0.010g in the pentachlorophenol solution of 40mL variable concentrations (2 ~ 30mg/L) at 25 DEG C, vibrate under 210rmp condition 16h in constant temperature oscillator, take out and filter, measure the PCP concentration of filtrate, result shows, and the PCP clearance of this microballoon to variable concentrations reaches 47.8% ~ 86.3%.
Accurately take the above-mentioned reed charcoal-sodium alginate micro ball of 0.010g, joining 40mL concentration is in 20mg/L pentachlorophenol solution, with the hydrochloric acid of 0.1mol/L or sodium hydroxide solution by pH (3 ~ 12) different for solution furnishing, at 25 DEG C, vibrate under 210rmp condition 16h in constant temperature oscillator, take out and filter, measure the PCP concentration of filtrate, result shows that reed charcoal-sodium alginate micro ball has very strong acid and alkali-resistance ability, and the clearance of PCP is raised along with the reduction of pH value of solution, especially, as pH=3, its clearance reaches 95.8%.
Accurately take the above-mentioned reed charcoal-sodium alginate micro ball of 0.015g, join in the Phe solution (100mL) of variable concentrations (0.1 ~ 1.2mg/L) respectively, and at 25 DEG C, under 180rmp condition, vibration 24h, take out and filter, measure the Phe concentration of filtrate, the clearance of result variable concentrations Phe is all greater than 62.8%.
By above-mentioned microballoon reclaiming of having adsorbed PCP or Phe, use deionized water cyclic washing, until PCP and Phe, without detecting, obtains the reed charcoal-sodium alginate micro ball regenerated in cleaning solution;
Accurately take the reed charcoal-sodium alginate micro ball of the above-mentioned regeneration of 0.010g, join the PCP that 40mL concentration is 2mg/L, at 25 DEG C, vibrate under 210rmp condition 16h in constant temperature oscillator, take out and filter, measure the PCP concentration of filtrate, the clearance of result PCP reaches 51.6%.
Embodiment 2
Waste reed is reclaimed, clean by deionized water, air-dry to constant weight, pulverize with plant pulverizer, cross 60 mesh sieves, take reed powder 50g pyrolysis in the Muffle furnace being full of N2, heating rate is 15 DEG C/min, and pyrolysis temperature is 600 DEG C, is cooled to room temperature and takes out after pyrolysis 2h, cross 100 mesh sieves, namely obtain reed charcoal.
Accurately take the above-mentioned reed charcoal of 0.010g, joining 40mL concentration is in the PCP aqueous solution of 20mg/L, and at 25 DEG C, vibrate under 210rmp condition 16h in constant temperature oscillator, takes out and filters, and measure the PCP concentration of filtrate, the clearance of result PCP reaches 22.1%
Accurately take 0.015g sodium alginate, joining 100mL concentration is in the Phe aqueous solution of 0.8mg/L, and at 25 DEG C, vibrate under 210rmp condition 24h in constant temperature oscillator, takes out and filters, and measure the Phe concentration of filtrate, the clearance of result Phe reaches 12.6%.
From above two examples, the present invention prepares the significant removal effect that reed charcoal-sodium alginate micro ball has PCP and Phe in waste water, and reclaiming ability is strong, is a kind of green material efficiently.

Claims (9)

1. a sodium alginate micro ball, is characterized in that, the preparation method of described sodium alginate micro ball is as follows:
1) 60 mesh sieves are crossed, pyrolysis in Muffle furnace after being pulverized by reed; Be cooled to room temperature to take out, cross 100 mesh sieves, obtained original reed charcoal;
2) by the HCl of original reed charcoal 1mol/L soak 12h, then with deionized water repeatedly rinse to flushing liquor pH be 7, then under 60 DEG C of conditions dry obtain reed charcoal;
3) mix long-pending to sodium alginate aqueous solution and the reed charcoal aqueous solution, with peristaltic pump by the CaCl2 solution of mixed liquor instillation 4%, be cross-linked, product is cleaned by deionized water again, namely obtains reed charcoal-sodium alginate micro ball.
2. the method for claim 1, is characterized in that, described step 1) in pyrolytical condition as follows: be filled with nitrogen, pyrolysis heating rate is 15 DEG C/min, and pyrolysis temperature is 600 DEG C.
3. the method for claim 1, is characterized in that, described step 2) in the volume mass of HCl soak and original reed charcoal of 1mol/L be 15 ~ 25:1 than mL/g.
4. the method for claim 1, is characterized in that, described step 3) in the concentration of the reed charcoal aqueous solution be 10 ~ 20g/L, the concentration of sodium alginate soln is 2.5% ~ 4.0%.
5. the application in the pollutant of sodium alginate micro ball according to claim 1 in adsorbed water body.
6. apply as claimed in claim 6, it is characterized in that, described pollutant is pentachlorophenol or and luxuriant and rich with fragrance.
7. process is containing a method for PCP and/or Phe water body, and it is characterized in that, described method is added to by sodium alginate micro ball according to claim 1 in the water body containing PCP and/or Phe to adsorb.
8. method as claimed in claim 7, it is characterized in that, described sodium alginate micro ball is placed in after CaCl2 solution soaks 24h and puts into water body again.
9. a renovation process for sodium alginate micro ball according to claim 1, is characterized in that, described method is that the microballoon of absorption PCP or Phe is spent deionized water.
CN201510603741.3A 2015-09-21 2015-09-21 Preparation method and application of sodium alginate microspheres Pending CN105080506A (en)

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Cited By (17)

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Publication number Priority date Publication date Assignee Title
CN105597691A (en) * 2015-12-19 2016-05-25 中国海洋大学 Preparation method and application of composite microspheres
CN107876020A (en) * 2017-10-20 2018-04-06 福建省农业科学院农业生态研究所 A kind of adsorbent, preparation method and applications
CN108467131A (en) * 2017-12-19 2018-08-31 苏州纳贝通环境科技有限公司 A kind of sanitary wastewater processing method
CN108905999A (en) * 2018-07-20 2018-11-30 武汉沃特工程技术有限公司 A kind of new bio charcoal plural gel and its preparation method and application
CN108940219A (en) * 2018-07-12 2018-12-07 浙江正洁环境科技有限公司 A kind of anti-acid heavy metal absorbent and preparation method thereof
CN110681364A (en) * 2019-10-31 2020-01-14 上海工程技术大学 Loofah sponge based activated carbon hydrogel material and preparation method and application thereof
CN111135800A (en) * 2020-01-10 2020-05-12 景德镇一牧堂陶瓷科技有限公司 Biochar material for efficiently reducing arsenic pollution of soil and preparation method thereof
CN111701568A (en) * 2020-07-10 2020-09-25 西安交通大学 Eggshell straw biochar composite microsphere phosphorus removal adsorbent with high adsorption performance and preparation method and application thereof
CN111729644A (en) * 2020-07-31 2020-10-02 河海大学 Biochar-bentonite porous composite ball and preparation method thereof
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
CN112973630A (en) * 2021-02-18 2021-06-18 山东大学 Biomass-based heavy metal adsorption material and preparation method and application thereof
CN113413882A (en) * 2021-06-23 2021-09-21 兰州大学 Preparation method and application of sodium alginate @ natural mineral/biochar composite gel beads
CN113750976A (en) * 2021-10-09 2021-12-07 东华理工大学 Millimeter-sized sodium alginate/phosphorylated biochar composite bead as well as preparation method and application thereof
CN114591747A (en) * 2022-02-28 2022-06-07 中国科学院南京土壤研究所 Surface functional group amplification biomass charcoal and preparation method and application thereof
CN114849647A (en) * 2022-05-13 2022-08-05 海南师范大学 Method for preparing spherical Cu/Fe biochar composite material by one-step method and application
CN115069214A (en) * 2022-06-29 2022-09-20 桂林理工大学 Preparation method of biochar-based functional material for removing arsenic
CN115739033A (en) * 2022-09-23 2023-03-07 齐鲁工业大学 Carbon material sodium alginate gel ball based on furfural residues, preparation method and application

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Cited By (20)

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Publication number Priority date Publication date Assignee Title
CN105597691A (en) * 2015-12-19 2016-05-25 中国海洋大学 Preparation method and application of composite microspheres
CN107876020A (en) * 2017-10-20 2018-04-06 福建省农业科学院农业生态研究所 A kind of adsorbent, preparation method and applications
CN107876020B (en) * 2017-10-20 2020-10-27 福建省农业科学院农业生态研究所 Adsorbent, preparation method and application thereof
CN108467131A (en) * 2017-12-19 2018-08-31 苏州纳贝通环境科技有限公司 A kind of sanitary wastewater processing method
CN108940219A (en) * 2018-07-12 2018-12-07 浙江正洁环境科技有限公司 A kind of anti-acid heavy metal absorbent and preparation method thereof
CN108905999A (en) * 2018-07-20 2018-11-30 武汉沃特工程技术有限公司 A kind of new bio charcoal plural gel and its preparation method and application
CN110681364B (en) * 2019-10-31 2022-08-23 上海工程技术大学 Loofah sponge based activated carbon hydrogel material and preparation method and application thereof
CN110681364A (en) * 2019-10-31 2020-01-14 上海工程技术大学 Loofah sponge based activated carbon hydrogel material and preparation method and application thereof
CN111135800A (en) * 2020-01-10 2020-05-12 景德镇一牧堂陶瓷科技有限公司 Biochar material for efficiently reducing arsenic pollution of soil and preparation method thereof
CN111701568A (en) * 2020-07-10 2020-09-25 西安交通大学 Eggshell straw biochar composite microsphere phosphorus removal adsorbent with high adsorption performance and preparation method and application thereof
CN111729644A (en) * 2020-07-31 2020-10-02 河海大学 Biochar-bentonite porous composite ball and preparation method thereof
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
CN112973630B (en) * 2021-02-18 2022-05-03 山东大学 Biomass-based heavy metal adsorption material and preparation method and application thereof
CN112973630A (en) * 2021-02-18 2021-06-18 山东大学 Biomass-based heavy metal adsorption material and preparation method and application thereof
CN113413882A (en) * 2021-06-23 2021-09-21 兰州大学 Preparation method and application of sodium alginate @ natural mineral/biochar composite gel beads
CN113750976A (en) * 2021-10-09 2021-12-07 东华理工大学 Millimeter-sized sodium alginate/phosphorylated biochar composite bead as well as preparation method and application thereof
CN114591747A (en) * 2022-02-28 2022-06-07 中国科学院南京土壤研究所 Surface functional group amplification biomass charcoal and preparation method and application thereof
CN114849647A (en) * 2022-05-13 2022-08-05 海南师范大学 Method for preparing spherical Cu/Fe biochar composite material by one-step method and application
CN115069214A (en) * 2022-06-29 2022-09-20 桂林理工大学 Preparation method of biochar-based functional material for removing arsenic
CN115739033A (en) * 2022-09-23 2023-03-07 齐鲁工业大学 Carbon material sodium alginate gel ball based on furfural residues, preparation method and application

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