CN109351350A - A kind of method that emulsion polymerization prepares sodium alginate micro ball adsorbent - Google Patents
A kind of method that emulsion polymerization prepares sodium alginate micro ball adsorbent Download PDFInfo
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- CN109351350A CN109351350A CN201811616685.7A CN201811616685A CN109351350A CN 109351350 A CN109351350 A CN 109351350A CN 201811616685 A CN201811616685 A CN 201811616685A CN 109351350 A CN109351350 A CN 109351350A
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- Prior art keywords
- sodium alginate
- micro ball
- adsorbent
- emulsion polymerization
- alginate micro
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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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
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- 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
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- 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
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention discloses a kind of methods that emulsion polymerization prepares sodium alginate micro ball adsorbent, belong to adsorption of metal ions technical field.Then this method is added glacial acetic acid and discharges calcium ion, generate sodium alginate micro ball under high speed agitation by the way that the sodium alginate soln of chemical modification and calcium carbonate, paraffin oil and 85 surfactant of Span are thoroughly mixed to form lotion.By adjusting dosing and stirring condition, different-grain diameter, and the sodium alginate micro ball of narrow particle size distribution can be made.Compared with traditional sodium alginate is the adsorbent of raw material, microsphere adsorbing agent made from the method has the characteristics that size uniformity, high mechanical strength, selection adsorption capacity are strong.Microsphere adsorbing agent prepared by the present invention has preferable selectivity to noble metal in acid condition, there is preferable selectivity to heavy metal under acidity to neutrallty condition, and application can be successfully loaded in ADSORPTION IN A FIXED BED column, thus there is good prospects for commercial application.
Description
Technical field
The invention belongs to adsorption of metal ions technical fields, and in particular to a kind of using sodium alginate as the porous absorption of raw material
Agent preparation method.
Background technique
It is the research hotspot of biomass absorbent material using sodium alginate as the adsorbent of raw material, but alginic acid common at present
Sodium is that raw material adsorbent is mostly powdered or water-setting is gluey.Wherein These powdered adsorbents due to its particle it is too thin, in practical fortune
It is excessive to will cause pressure drop when used in adsorption column, causes to block.Water-setting glue adsorbent is generally by drop-method, by sodium alginate soln
Instill in the solution of calcium chloride and be made, diameter generally in 1mm or more, when being seated in adsorption column due to size it is slightly larger so as to cause
Short circuit, and the specific surface area as caused by large scale is smaller, and adsorbance is relatively low.Microspheroidal adsorbent can be simultaneous at this time
Shape and performance are cared for, there is apparent superiority in practical applications.However sodium alginate micro ball preparation is more difficult, it is main former
Because being that calcium chloride solution can be soluble in the aqueous phase, it is difficult to apply in emulsion polymerization.
Summary of the invention
The technical problem to be solved in the present invention is to provide one kind using sodium alginate as raw material, is prepared by emulsion polymerization micro-
The method of ball-type metal ion adsorbent is adsorbed to overcome the limitation on sodium alginate sorbent structure for sodium alginate
The industrial application of agent provides possibility.
In order to solve the above technical problems, the present invention is achieved by the following technical programs.
The present invention uses calcium carbonate powder as the medicament of calcium ion is provided, by the way that glacial acetic acid is added in lotion, thus
The calcium ion in calcium carbonate powder is discharged, under high-speed stirred and sodium alginate cross-linking forms microballoon.By adjusting dosing and
Different-grain diameter, and the sodium alginate micro ball of narrow particle size distribution can be made in stirring condition.
Specific step is as follows:
(1) sodium hydroxide solution that 10mL carbon disulfide and 250mL mass concentration are 14% is mixed first, adds 5-
10g sodium alginate stirs 24 hours under conditions of being maintained at 30 DEG C.
(2) acquired solution and 6g calcium carbonate powder are mixed, is stirred under 400-800rpm revolving speed with electric mixer
15min.Then 100mL paraffin oil and 85 emulsifier of 2-5mL Span is added, continues to stir 20min.
(3) 10-15mL glacial acetic acid is added into obtained lotion, revolving speed is kept to stir 30min.It is eventually adding 200mL
Deionized water, stand.Thus obtained microsphere shape solid ethyl alcohol and deionized water are rinsed, the microballoon that sodium alginate is raw material can be obtained
Adsorbent.
As a kind of optimization, in the step (1): the additional amount of sodium alginate is 5g；In the step (2): calcium carbonate
The usage amount of powder is 6g, and the additional amount of 85 emulsifier of Span is 2mL；In the step (3): the additional amount of glacial acetic acid is
10mL。
All medicaments in above-mentioned reaction are analytical reagents.
The present invention prepares microspheroidal adsorbent by primary raw material of sodium alginate, and key technology is by glacial acetic acid and carbon
Sour calcium powder releases the calcium ion in lotion, as the crosslinking agent for solidifying ball processed, is controlled by high-speed stirred and generates microballoon
Size.The characteristics of this method is the controllability for generating Microsphere Size, and does not need complicated device and can be carried out preparing.
Compared with prior art, the present invention has following technical effect that
1, compared with traditional sodium alginate is the adsorbent of raw material, microsphere adsorbing agent made from the method has size equal
One, the strong feature of high mechanical strength, selection adsorption capacity.
2, thus obtained microsphere shape adsorbent size of the present invention is smaller (about 200-300 μm), for adsorption of metal ions rate
Fastly, adsorbance is higher.
3, microspheroidal adsorbent produced by the present invention has very uniform size, is not easy out in the filling of ADSORPTION IN A FIXED BED column
Existing short circuit phenomenon, is conducive to separation and enrichment of the metal ion in adsorption column.It is tested by complete adsorption-desorption, it can be with
Reach complete regeneration, reuses the no apparent absorption property decaying of 5 circulations.
4, microballoon prepared by the present invention has preferable selectivity to noble metal in acid condition, arrives neutrallty condition in acidity
Under have a preferable selectivity to heavy metal, and can the successfully filling application in ADSORPTION IN A FIXED BED column, thus have good
Prospects for commercial application.
Detailed description of the invention
Fig. 1 is the stereoscan photograph of sodium alginate micro ball adsorbent prepared by the embodiment of the present invention 1；
As seen from Figure 1, gained adsorbent size is uniform and regular shape.
Specific embodiment
The present invention is described in detail below in conjunction with specific embodiment, but the present invention is not limited to following embodiments.
Embodiment 1
(1) sodium hydroxide solution that 10mL carbon disulfide and 250mL mass concentration are 14% is mixed first, adds 5g
Sodium alginate stirs 24 hours under conditions of being maintained at 30 DEG C.
(2) acquired solution and 6g calcium carbonate powder are mixed, stirs 15min under 400rpm revolving speed with electric mixer.
Then 100mL paraffin oil and 85 emulsifier of 2mL Span is added, continues to stir 20min.
(3) 10mL glacial acetic acid is added into obtained lotion, revolving speed is kept to stir 30min.It is eventually adding going for 200mL
Ionized water is stood for 24 hours.By thus obtained microsphere shape solid ethyl alcohol and deionized water repeated flushing, can obtain sodium alginate is raw material
Microsphere adsorbing agent (its scanning electron microscope (SEM) photograph is as shown in Figure 1).
Embodiment 2
(1) sodium hydroxide solution that 10mL carbon disulfide and 250mL mass concentration are 14% is mixed first, adds 8g
Sodium alginate stirs 24 hours under conditions of being maintained at 30 DEG C.
(2) acquired solution and 8g calcium carbonate powder are mixed, stirs 15min under 600rpm revolving speed with electric mixer.
Then 100mL paraffin oil and 85 emulsifier of 3mL Span is added, continues to stir 20min.
(3) 15mL glacial acetic acid is added into obtained lotion, revolving speed is kept to stir 30min.It is eventually adding going for 200mL
Ionized water is stood for 24 hours.By thus obtained microsphere shape solid ethyl alcohol and deionized water repeated flushing, can obtain sodium alginate is raw material
Microsphere adsorbing agent.
Embodiment 3
(1) sodium hydroxide solution that 10mL carbon disulfide and 250mL mass concentration are 14% is mixed first, is added
10g sodium alginate stirs 24 hours under conditions of being maintained at 30 DEG C.
(2) acquired solution and 10g calcium carbonate powder are mixed, stirs 15min under 800rpm revolving speed with electric mixer.
Then 100mL paraffin oil and 85 emulsifier of 4mL Span is added, continues to stir 20min.
(3) 15mL glacial acetic acid is added into obtained lotion, revolving speed is kept to stir 30min.It is eventually adding going for 200mL
Ionized water is stood for 24 hours.By thus obtained microsphere shape solid ethyl alcohol and deionized water repeated flushing, can obtain sodium alginate is raw material
Microsphere adsorbing agent.
Claims (2)
1. a kind of method that emulsion polymerization prepares sodium alginate micro ball adsorbent, it is characterised in that include the following steps:
(1) sodium hydroxide solution that 10mL carbon disulfide and 250mL mass concentration are 14% is mixed first, adds 5~10g
Sodium alginate stirs 24 hours under conditions of being maintained at 30 DEG C；
(2) step (1) acquired solution and 6~10g calcium carbonate powder are mixed, with electric mixer in 200~600rpm revolving speed
Lower stirring 15min；Then 100mL paraffin oil and 2~5mL Span, 85 emulsifier is added, continues to stir 20min；
(3) 10~15mL glacial acetic acid is added into lotion obtained by step (2), revolving speed is kept to stir 30min；It is eventually adding
200mL deionized water is stood；It is raw material that thus obtained microsphere shape solid ethyl alcohol and deionized water, which are rinsed to get sodium alginate,
Microsphere adsorbing agent.
2. a kind of method that emulsion polymerization prepares sodium alginate micro ball adsorbent as described in claim 1, which is characterized in that
In the step (1): the additional amount of sodium alginate is 5g；In the step (2): the usage amount of calcium carbonate powder is 6g, Span
The additional amount of 85 emulsifiers is 2mL；In the step (3): the additional amount of glacial acetic acid is 10mL.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811616685.7A CN109351350A (en) | 2018-12-27 | 2018-12-27 | A kind of method that emulsion polymerization prepares sodium alginate micro ball adsorbent |
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| CN201811616685.7A CN109351350A (en) | 2018-12-27 | 2018-12-27 | A kind of method that emulsion polymerization prepares sodium alginate micro ball adsorbent |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111672479A (en) * | 2020-06-10 | 2020-09-18 | 安徽工业大学 | Alginate-based metal photocatalytic reduction material, preparation method and application |
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| CN104907051A (en) * | 2015-05-21 | 2015-09-16 | 江南大学 | Preparation method and application of heavy metal ion absorbent |
| CN106049047A (en) * | 2016-05-24 | 2016-10-26 | 马鞍山中创环保科技有限公司 | Method for preparing sodium alginate-polypropylene functional heavy metal adsorption fiber |
| CN106732431A (en) * | 2017-01-03 | 2017-05-31 | 福州大学 | A kind of metal ion adsorbent based on algal polysaccharides and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111672479A (en) * | 2020-06-10 | 2020-09-18 | 安徽工业大学 | Alginate-based metal photocatalytic reduction material, preparation method and application |
| CN111672479B (en) * | 2020-06-10 | 2022-09-09 | 安徽工业大学 | Alginate-based metal photocatalytic reduction material, preparation method and application |
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Application publication date: 20190219 |