CN105964232B - A kind of synthetic method and application of the polysulfones microcapsules adsorbing indium - Google Patents
A kind of synthetic method and application of the polysulfones microcapsules adsorbing indium Download PDFInfo
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- CN105964232B CN105964232B CN201610421206.0A CN201610421206A CN105964232B CN 105964232 B CN105964232 B CN 105964232B CN 201610421206 A CN201610421206 A CN 201610421206A CN 105964232 B CN105964232 B CN 105964232B
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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
- B01J20/26—Synthetic macromolecular compounds
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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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B58/00—Obtaining gallium or indium
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses the synthetic methods and application of a kind of polysulfones microcapsules for adsorbing indium, using polysulfones as raw material, microcapsules technology is combined with abstraction technique, extractant cladding is got up using microencapsulation method, the purposes of indium is adsorbed for it, propose optimal stirring and emulsifying speed in synthesis extraction process, the concentration of dispersing agent, the composition of oily phase and best water-oil factor, effectively avoid emulsification and the generation of split-phase problem, the smooth densification of polysulfones surface of microcapsule of preparation, preparation method is simple, device simple is at low cost, solvent loss is small, it applies it in the absorption of indium, obtain splendid adsorption effect.
Description
Technical field
The present invention relates to the preparation method of microcapsules more particularly to it is a kind of adsorb indium polysulfones microcapsules synthetic method and
Using.
Background technique
In the 1990s, microcapsules technology is rapidly developed, microcapsules technology is combined with abstraction technique molten
Agent microcapsules technology, causes the concern of lot of domestic and foreign researcher, and has obtained rapid development extractant microcapsules and not only had
There is the advantages of extration resin, moreover it is possible to avoid the problem that emulsification and split-phase, and in extractant covering amount and extractant be prevented to be lost
Etc. have advantage.
Indium is " less noble metal " and a kind of strategic metal in rare metal, has very unique physics and change
Performance is learned, such as fusing point is low, boiling point is high and conductibility is good.Be therefore widely used in electronic computer, the energy, electronics, photoelectricity,
The high-tech areas such as defense military, aerospace, nuclear industry and modern information industry, the effect in national economy are increasingly heavy
It wants, and becomes one of most important backing material in modern electronics industry.And indium is that content is few in the earth's crust, distributed pole dissipates
Rare and scatter element, the high mineral containing indium are difficult to find, this just determines that the extraction of indium has important research significance.
A kind of pair of indium how is synthesized to be of great significance with the polysulfones microcapsules of preferable absorption property.
Summary of the invention
Goal of the invention: in order to overcome problems of the prior art, the invention proposes the absorption properties of a kind of pair of indium
Good, preparation method is simple, and device simple is at low cost, solvent loss is small, avoids the polysulfones of the absorption indium of emulsification and split-phase problem micro-
The synthetic method and application of capsule.
Technical solution: in order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is as follows: a kind of absorption indium (III)
Polysulfones microcapsules synthetic method, comprising the following steps:
(1) preparation of water phase: 600mL distilled water is added into 1000mL, adds 6g gelatin dispersing agent, heating stirring makes
Gelatin is completely dissolved；
(2) preparation of organic phase: 4g polysulfones is weighed in 1000mL three-necked bottle, adds 60mL methylene chloride, use is electronic
Blender is stirred at room temperature, after polysulfones is completely dissolved into three-necked bottle fast drop 3mL25vol%P204；
(3) synthesis of polysulfones microcapsules: water phase being added into organic phase, and water phase is divided 10 times by the total amount of step (1) preparation
Time control is added every time and stirs 3h in 30s, then mixed solution is transferred in the beaker of 1000mL and is stirred to dichloro for addition
Methane volatilization completely, is detected with methylene chloride gas concentration and content leakage detector；It is filtered with Buchner funnel, uses distilled water
Filtered several times are washed, until filtrate is limpid；Filtrate is obtained by drying in 30-40 DEG C of baking oven.
The speed of heating stirring described in step (1) is 600r/min, is emulsified under revolving speed herein, water phase emulsifying effectiveness is most
It is good.
To obtain optimal emulsifying effectiveness and improving microcapsules quality, step (1) the gelatin dispersing agent mass concentration is
1%.
When the film core ratio is 3:2, the smooth consistency of the surface of microcapsule of preparation is best.
The water-oil factor is 10:1, and the smooth consistency of the surface of microcapsule of preparation is best.
The invention also provides above-mentioned synthetic method synthesis absorption indium polysulfones microcapsules application, specifically for pair
When the absorption of indium, equilibration time 25min, adsorption temp plays optimal adsorption effect to indium when being 50 DEG C.
The utility model has the advantages that the synthetic method and application of a kind of polysulfones microcapsules for adsorbing indium provided by the invention, are with polysulfones
Raw material combines microcapsules technology with abstraction technique, and extractant cladding is got up using microencapsulation method, adsorbs indium for it
Purposes, propose optimal stirring and emulsifying speed in synthesis extraction process, the concentration of dispersing agent, the composition of oily phase and best
Water-oil factor effectively avoids emulsification and the generation of split-phase problem, the smooth densification of polysulfones surface of microcapsule of preparation, preparation method letter
Single, device simple is at low cost, solvent loss is small, applies it in the absorption of indium, obtains splendid adsorption effect.
Detailed description of the invention
Fig. 1 is that the embodiment of the present invention 1 prepares microcapsules schematic device；
Fig. 2 is the variation schematic diagram of the adsorbance of the different adsorption times of the embodiment of the present invention 2 and indium；
Fig. 3 is the variation schematic diagram of the adsorbance of the different adsorption temps of the embodiment of the present invention 2 and indium；
Fig. 4 is the variation schematic diagram of the adsorbance of indium under 2 various concentration of the embodiment of the present invention.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail:
Embodiment 1:
A kind of synthetic method for the polysulfones microcapsules adsorbing indium, includes the following steps, specific reaction unit figure is shown in Fig. 1:
(1) preparation of water phase: 600mL distilled water being added into 1000mL, adds the gelatin point that 6g mass concentration is 1%
Powder is completely dissolved gelatin with the speed heating stirring of 600r/min, obtains optimal emulsifying effectiveness；
(2) preparation of organic phase: 4g polysulfones is weighed in 1000mL three-necked bottle, adds 60mL methylene chloride, use is electronic
Blender is stirred at room temperature, after polysulfones is completely dissolved into three-necked bottle fast drop 3mL25vol%P204；
(3) synthesis of polysulfones microcapsules: water phase being added into organic phase, and water phase is divided 10 times by the total amount of step (1) preparation
Time control is added every time and stirs 3h in 30s, then mixed solution is transferred in the beaker of 1000mL and is stirred to dichloro for addition
Completely, methylene chloride is detected with methylene chloride gas concentration and content leakage detector for methane volatilization；It is filtered with Buchner funnel,
Filtered several times are washed with distilled water, until filtrate is limpid；Filtrate is obtained by drying in 30-40 DEG C of baking oven.
The film core ratio is 3:2, and when water-oil factor is 10:1, the smooth consistency of the surface of microcapsule of preparation is best.
Embodiment 2:
A kind of application for the polysulfones microcapsules adsorbing indium:
Prepare respectively 10 μ g/mL, 15 μ g/mL, 20 μ g/mL, 25 μ g/mL, 30 μ g/mL, 35 μ g/mL solution of indium be placed in six
In a ground band plug conical flask, six parts of P204 polysulfones microcapsules for then taking 0.05g embodiment 1 to prepare respectively are respectively put into six
In a conical flask, put in an oscillator.
A) optimal adsorption equilibration time is tested: being taken 10 μ g/mL solution of indium to carry out adsorption test at room temperature, is divided in an oscillator
Not carry out 5min, 10min, 15min, 20min, 25min, 30min, 35min oscillation adsorption test, hunting speed 150r/
Min takes filtering after the completion of oscillation, respectively takes filtrate 1mL, then addition 2mL xylenol orange solution, then with acetic acid-ammonium acetate solution
It is settled to scale, measures its absorbance with spectrophotometry, adsorbance is calculated according to indium standard curve, specific situation of adsorbing is shown in figure
2。
B) optimal adsorption humid test: 10 μ g/mL solution of indium are taken to carry out adsorption test at room temperature, in 25 DEG C, 30 DEG C, 35
DEG C, 40 DEG C, 45 DEG C, cyclotron oscillation at 50 DEG C, concussion speed is 150r/min, vibrates 25min.It filters after the completion of oscillation, respectively takes
Then filtrate 1mL is added 2mL xylenol orange solution, then is settled to scale with acetic acid-ammonium acetate solution, surveyed with spectrophotometry
Its fixed absorbance calculates adsorbance according to indium standard curve, and specific situation of adsorbing is shown in Fig. 3.
C 10 μ g/mL, 15 μ g/mL, 20 μ g/mL, 25 μ g/mL, 30 μ g/mL, 35 μ g/mL) optimal adsorption concentration tests: are taken
Solution of indium carry out oscillation 15min at room temperature, concussion speed is 150r/min, filtered after the completion of oscillation, respectively take filtrate 1mL,
Then 2mL xylenol orange solution is added, then is settled to scale with acetic acid-ammonium acetate solution, measures its extinction with spectrophotometry
Degree calculates adsorbance according to indium standard curve, and specific situation of adsorbing is shown in Fig. 4.
It is obtained from the above conclusion (of pressure testing), polysulfones microcapsules are 25min to the optimal adsorption equilibration time of indium；Adsorbance with
The raising of concentration is substantially in raising trend；Adsorbance constantly increases as the temperature rises within 50 DEG C.
It should be pointed out that the above specific embodiment is only illustrative of the invention and is not intended to limit the scope of the invention,
After having read the present invention, those skilled in the art fall within power appended by the application to the modification of various equivalent forms of the invention
Benefit requires limited range.
Claims (2)
1. a kind of synthetic method for the polysulfones microcapsules for adsorbing indium, it is characterised in that the following steps are included:
(1) preparation of water phase: 600mL distilled water is added into 1000mL beaker, adds 6g gelatin dispersing agent, heating stirring makes
Gelatin is completely dissolved；The speed of the heating stirring is 600r/min；The gelatin dispersing agent mass concentration is 1%；
(2) preparation of organic phase: 4g polysulfones is weighed in 1000mL three-necked bottle, 60mL methylene chloride is added, uses electric stirring
Device is stirred at room temperature, after polysulfones is completely dissolved into three-necked bottle fast drop 3mL 25vol% P204；
(3) synthesis of polysulfones microcapsules: water phase being added into organic phase, and water phase is added by total amount point 10 times of step (1) preparation,
Time control is added every time and stirs 3h in 30s, then mixed solution is transferred in the beaker of 1000mL and is stirred to methylene chloride
Volatilization completely, is detected with methylene chloride gas concentration and content leakage detector；It is filtered, is washed with distilled water with Buchner funnel
Filtered several times, until filtrate is limpid；Filtrate is obtained by drying in 30-40 DEG C of baking oven.
2. the application of the polysulfones microcapsules of the synthetic method synthesis of the polysulfones microcapsules of absorption indium as described in claim 1,
It is characterized in that when for absorption to indium, equilibration time 25min, adsorption temp is 50 DEG C.
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| CN110756162A (en) * | 2019-10-24 | 2020-02-07 | 中国科学院城市环境研究所 | Synthesis of P5O7 composite carbon fiber material and method for adsorbing and separating indium in liquid crystal panel by using same |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101224403A (en) * | 2007-10-26 | 2008-07-23 | 清华大学 | Method for preparing microcapsule |
| CN104831077A (en) * | 2015-04-01 | 2015-08-12 | 郴州雄风环保科技有限公司 | Method for extracting and separating indium and tin from indium-containing leaching residues |
| CN105018753A (en) * | 2015-07-27 | 2015-11-04 | 昆明理工大学 | Composite extraction agent and method for extracting, separating and recycling indium through composite extraction agent |
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- 2016-06-15 CN CN201610421206.0A patent/CN105964232B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101224403A (en) * | 2007-10-26 | 2008-07-23 | 清华大学 | Method for preparing microcapsule |
| CN104831077A (en) * | 2015-04-01 | 2015-08-12 | 郴州雄风环保科技有限公司 | Method for extracting and separating indium and tin from indium-containing leaching residues |
| CN105018753A (en) * | 2015-07-27 | 2015-11-04 | 昆明理工大学 | Composite extraction agent and method for extracting, separating and recycling indium through composite extraction agent |
Non-Patent Citations (2)
| Title |
|---|
| P507聚砜微胶囊的合成及吸附铟的性能;李海梅 等;《中国化学会第15届反应性高分子学术讨论会》;20101231;第43-45页 * |
| 溶剂挥发法制备萃取剂微胶囊;杨伟伟 等;《高分子学报》;20050430(第2期);第207页右栏倒数第1-2段、第208页左栏第1段，第209页图2（c）及对应的文字说明 * |
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