CN109174059A - Embed modified meerschaum/nano-titanium dioxide microsphere adsorbing agent preparation method - Google Patents
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- CN109174059A CN109174059A CN201811118463.2A CN201811118463A CN109174059A CN 109174059 A CN109174059 A CN 109174059A CN 201811118463 A CN201811118463 A CN 201811118463A CN 109174059 A CN109174059 A CN 109174059A
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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
- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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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
- B01J20/28002—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 physical properties
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
- B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
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Abstract
The invention discloses a kind of embedding modified meerschaum/nano-titanium dioxide microsphere adsorbing agent preparation methods, it is related to a kind of adsorbent, it is lower to be intended to existing natural sepiolite mine grade, the technical issues of smaller, the acid weak and thermal stability of natural specific surface area is poor, the easy difficult recycling of dispersion etc. limits its practical application comprising following steps: (1) sepiolite purifying；(2) sepiolite is modified；(3) it coats.The present invention provides a kind of processing step is simple, strong operability, it is few to equipment investment, it is suitble to embedding modified meerschaum/nano-titanium dioxide microsphere adsorbing agent preparation method of industrialized production, by cladding so that nano-titanium dioxide and sepiolite are combined into microballoon, embedding modified meerschaum/nano-titanium dioxide microsphere adsorbing agent obtained is at low cost, large specific surface area, it is easy to use, it is without secondary pollution, thermal stability is good with salt-resistance, is easy recycling, has broad application prospects in heavy metal containing wastewater treatment field.
Description
Technical field
The present invention relates to a kind of adsorbents, more particularly, to a kind of embedding modified meerschaum/nano-titanium dioxide microballoon
Sorbent preparation method.
Background technique
Heavy metal wastewater thereby becomes global problem of environmental pollution because of its toxic action, exploitation new process, new method and new
Material becomes the research hotspot of heavy metal containing wastewater treatment.Absorption method is the typical process of heavy metal containing wastewater treatment, in the process,
Core link is exactly to seek high absorption property, highly selective, cheap and efficient adsorbent material.
Sepiolite belongs to natural mineral resources, and rich reserves are a kind of novel water pollution control materials.Its structure list of sepiolite
The natural bed that member is made of two layers of oxygen-octahedron and intermediate one layer of magnesia octahedron, is chain transiens structure, theory compares table
Area is 900m2/ g belongs to fibrous rich magnesium silicate clay mineral, the knot with good zeolite aquaporin and high-specific surface area
Structure feature has very strong absorption property and ion-exchange capacity with the presence of high degree of dispersion suspended state in water body.Sepiolite
Special construction determines that it has many advantages, such as good physical and chemical performance (i.e. adsorptivity, rheological characteristic and catalytic performance), in heavy metal
The application prospect of field of waste water treatment is very extensive.However since natural sepiolite mine grade is lower, natural specific surface area
Smaller, acid weak and thermal stability is poor, difficult recycle etc. of easy dispersion limits its practical application, due to current technology problem,
Cause universal utilization rate low.
Summary of the invention
The present invention is to provide a kind of technique step to solve above-mentioned technical problem present in the sepiolite of the prior art
Rapid simple, strong operability is few to equipment investment, is suitble to embedding modified meerschaum/nano-titanium dioxide of industrialized production
Microsphere adsorbing agent preparation method, embedding modified meerschaum/nano-titanium dioxide microsphere adsorbing agent obtained is at low cost, compares table
Area is big, easy to use, without secondary pollution, and thermal stability is good with salt-resistance, recycling is easy, in heavy metal containing wastewater treatment field
It has broad application prospects.
To achieve the goals above, the invention adopts the following technical scheme:
Embedding modified meerschaum/nano-titanium dioxide microsphere adsorbing agent preparation method of the invention, comprising the following steps:
(1) sepiolite purifies: sepiolite is add to deionized water, is staticly settled after stirring at least 30min, upper layer sea
For the suspension of afrodite after suction filtration, deionized water are washed repeatedly, the Asia of mass concentration 3~5% is added in vacuum drying after crushing
Sodium radio-phosphate,P-32 solution, after stirring at low speed 20~30min, high-speed stirred disperses 1~2h, while appropriate filter aid calcium hydroxide is added,
After staticly settling, upper layer suspension is filtered, deionized water washing, drying, is pulverized and sieved, the sepiolite of purifying is obtained.The present invention
In purification process has been carried out to improve its taste to sepiolite, by it is secondary staticly settle, secondary agitation disperses, and is aided with simultaneously
For filter aid to remove the impurity such as the talcum in sepiolite, calcite, filter aid calcium hydroxide can be such that sepiolite is formed when filtering
The very high filter cake of porosity, advantageously reduces suction filtration resistance, while also easily reacting and being removed with acid in the follow-up process, simultaneously
It is added to dispersing agent sodium phosphite, by the way that sodium phosphite is added to improve the degree of scatter of sepiolite, to be conducive to improve it
Purification effect.
(2) sepiolite is modified: the sepiolite of purifying being added in deionized water, is heated to 160 in the case where sealing stirring
~200 DEG C, and 3~5h is kept the temperature, after filtering, drying, it is added in the dilute hydrochloric acid that mass concentration is 10~15%, is heated to boiling simultaneously
3~4h is stirred, modified meerschaum is obtained after washing, dry through deionized water, pulverizing and sieving.Hydrochloric acid is used to sepiolite in the present invention
It is modified, first heats and sepiolite is swollen, so that lumen pore borehole enlargement in sepiolite, opens sepiolite inner passage,
The dissolution of impurity is not only improved, while being also beneficial to improve the specific surface area of sepiolite, then by by acid and sepiolite
Carbonate effect makes carbonate impurities that corrosion occur, and guarantees that the cavity in sepiolite is unobstructed, on the other hand, the H that acid is assigned+
With the Ca of sepiolite interlayer2+、Mg2+、Na+And K+Replace, improve sepiolite surface and lumen pore characteristic, increase specific surface area and
Micro-porosity improves the absorption property of sepiolite, and during sour modification, acid concentration, processing time and treatment temperature can be right
The structure of sepiolite produces bigger effect, therefore condition modified to acid in the present invention has carried out considered critical.
(3) it coats: nano-titanium dioxide is added in deionized water, after adjustment pH is 8.5~9, ultrasonic disperse is rear to be added
Modified meerschaum is added after heating for dissolving in polyvinyl alcohol and sodium alginate, after mixing evenly cooling suspension；Again by suspension
It is continuously added dropwise in the saturation boric acid solution containing 2% calcium chloride and is solidified, after solidifying at least 20h, filtering is drying to obtain embedding
Modified meerschaum/nano-titanium dioxide microsphere adsorbing agent.By cladding so that nano-titanium dioxide be combined into sepiolite it is micro-
Ball, microballoon are easy to be separated from water, convenient for recycling, and it is easy to use；Nano-titanium dioxide itself have excellent absorption property with
Thermal stability can improve the adsorption effect and thermal stability of microballoon, in addition, nano-titanium dioxide, which is adsorbed on sepiolite surface, to send
Bear several adsorption sites so that the surface of sepiolite more it is more coarse, increase the specific surface area of sepiolite, be conducive to inhale
Attached capacity improves.
Preferably, the mass ratio of sepiolite and deionized water is 1:3~5 in step (1).
Preferably, the mass ratio of sepiolite and sodium phosphite solution is 1:5~10 in step (1).
Preferably, in step (1), the revolving speed stirred at low speed is 50~100r/min, the revolving speed of high-speed stirred is 150~
200r/min。
Preferably, the mass ratio of sepiolite and dilute hydrochloric acid is 1:5~10 in step (2).
Preferably, in step (3), modified meerschaum, polyvinyl alcohol, nano-titanium dioxide, sodium alginate mass ratio
For 100:(20~40): (4~6): (1~3).
Therefore, the invention has the following beneficial effects: simple, the strong operabilitys that provides a kind of processing step, to equipment
Small investment is suitble to embedding modified meerschaum/nano-titanium dioxide microsphere adsorbing agent preparation method of industrialized production, passes through
For cladding so that nano-titanium dioxide and sepiolite are combined into microballoon, embedding modified meerschaum/nano-titanium dioxide obtained is micro-
Ball adsorbent cost is low, and large specific surface area is easy to use, without secondary pollution, and thermal stability is good with salt-resistance, is easy recycling,
Heavy metal containing wastewater treatment has broad application prospects in field.
Specific embodiment
Below by specific embodiment, the present invention will be further described.
Embodiment 1
(1) sepiolite purifies: sepiolite is add to deionized water, the mass ratio of sepiolite and deionized water is 1:3,
It is staticly settled after stirring at least 30min, for the suspension of upper layer sepiolite after suction filtration, deionized water are washed repeatedly, vacuum is dry
It is dry, the sodium phosphite solution of mass concentration 3% is added after crushing, the mass ratio of sepiolite and sodium phosphite solution is 1:5, low speed
After stirring 20min, high-speed stirred disperses 1h, and the revolving speed stirred at low speed is 50r/min, and the revolving speed of high-speed stirred is 150r/min,
Appropriate filter aid calcium hydroxide is added simultaneously, after staticly settling, upper layer suspension is filtered, deionized water washing, dry, crushing
Sieving, obtains the sepiolite of purifying；
(2) sepiolite is modified: the sepiolite of purifying being added in deionized water, is heated to 160 in the case where sealing stirring
DEG C, and 3h is kept the temperature, after filtering, drying, it is added in the dilute hydrochloric acid that mass concentration is 10%, the mass ratio of sepiolite and dilute hydrochloric acid is
1:5 is heated to the 3h that boils and stir, and modified meerschaum is obtained after washing, dry through deionized water, pulverizing and sieving；
(3) it coats: nano-titanium dioxide is added in deionized water, after adjustment pH is 8.5, ultrasonic disperse is added poly- afterwards
Modified meerschaum, modified meerschaum, polyvinyl alcohol, nano-titanium dioxide, sea is added after heating for dissolving in vinyl alcohol and sodium alginate
The mass ratio of mosanom is 100:20:4:1, after mixing evenly cooling suspension；Suspension is continuously added dropwise to containing 2% chlorine again
Change and solidified in the saturation boric acid solution of calcium, after solidifying at least 20h, filtering is drying to obtain embedding modified meerschaum/nanometer two
The microsphere adsorbing agent of titanium oxide.
Comparative example 1
Compared with Example 1, difference is not purify sepiolite comparative example 1, remaining and the complete phase of embodiment 1
Together.
Comparative example 2
Compared with Example 1, difference is not to be modified sepiolite comparative example 2, remaining and the complete phase of embodiment 1
Together.
The adsorption experiment of chromate waste water and cadmium wastewater, tool are carried out to the microballoon in embodiment 1, comparative example 1, comparative example 2
Body experimental method are as follows:
Chromate waste water adsorption experiment: under conditions of temperature is 25 DEG C, pH value is 3, using embodiment 1, comparative example 1, right
Microballoon difference adsorption treatment 100ml in ratio 2 contains Cr6+The waste water of 35mg/L, microballoon additional amount is 0.4g/100ml, when absorption
Between be 8h.
Cadmium wastewater adsorption experiment: under conditions of temperature is 25 DEG C, pH value is 8, using embodiment 1, comparative example 1, right
Microballoon difference adsorption treatment 100ml in ratio 2 contains Cd2+The waste water of 4.58mg/L, the additional amount 2g/100ml of microballoon, when absorption
Between be 8h.
The Adsorption experimental results of chromate waste water and cadmium wastewater are as shown in table 1
1 chromate waste water of table and cadmium wastewater Adsorption experimental results
As seen from Table 1, the purifying of sepiolite, the modified absorption property to microballoon have larger impact, wherein modified shadow
Ring the influence for being greater than purifying, still further it can be seen that, the microballoon tool of embedding modified meerschaum/nano-titanium dioxide obtained of the invention
There is excellent absorption property, has broad application prospects in heavy metal containing wastewater treatment field.
Embodiment 2
(1) sepiolite purifies: sepiolite is add to deionized water, the mass ratio of sepiolite and deionized water is 1:4,
It is staticly settled after stirring at least 30min, for the suspension of upper layer sepiolite after suction filtration, deionized water are washed repeatedly, vacuum is dry
It is dry, the sodium phosphite solution of mass concentration 4% is added after crushing, the mass ratio of sepiolite and sodium phosphite solution is 1:8, low speed
After stirring 25min, high-speed stirred disperses 1.2h, and the revolving speed stirred at low speed is 80r/min, and the revolving speed of high-speed stirred is 180r/
Min, while appropriate filter aid calcium hydroxide is added, after staticly settling, upper layer suspension suction filtration, deionized water are washed, is dry,
It pulverizes and sieves, obtains the sepiolite of purifying；
(2) sepiolite is modified: the sepiolite of purifying being added in deionized water, is heated to 180 in the case where sealing stirring
DEG C, and 4h is kept the temperature, after filtering, drying, it is added in the dilute hydrochloric acid that mass concentration is 12%, the mass ratio of sepiolite and dilute hydrochloric acid is
1:8 is heated to the 3.5h that boils and stir, and modified meerschaum is obtained after washing, dry through deionized water, pulverizing and sieving；
(3) it coats: nano-titanium dioxide is added in deionized water, after adjustment pH is 8.8, ultrasonic disperse is added poly- afterwards
Modified meerschaum, modified meerschaum, polyvinyl alcohol, nano-titanium dioxide, sea is added after heating for dissolving in vinyl alcohol and sodium alginate
The mass ratio of mosanom is 100:30:5:2, after mixing evenly cooling suspension；Suspension is continuously added dropwise to containing 2% chlorine again
Change and solidified in the saturation boric acid solution of calcium, after solidifying at least 20h, filtering is drying to obtain embedding modified meerschaum/nanometer two
The microsphere adsorbing agent of titanium oxide.
Embodiment 3
(1) sepiolite purifies: sepiolite is add to deionized water, the mass ratio of sepiolite and deionized water is 1:5,
It is staticly settled after stirring at least 30min, for the suspension of upper layer sepiolite after suction filtration, deionized water are washed repeatedly, vacuum is dry
It is dry, the sodium phosphite solution of mass concentration 5% is added after crushing, the mass ratio of sepiolite and sodium phosphite solution is 1:10, low
After speed stirring 30min, high-speed stirred disperses 2h, and the revolving speed stirred at low speed is 100r/min, and the revolving speed of high-speed stirred is 200r/
Min, while appropriate filter aid calcium hydroxide is added, after staticly settling, upper layer suspension suction filtration, deionized water are washed, is dry,
It pulverizes and sieves, obtains the sepiolite of purifying；
(2) sepiolite is modified: the sepiolite of purifying being added in deionized water, is heated to 200 in the case where sealing stirring
DEG C, and 5h is kept the temperature, after filtering, drying, it is added in the dilute hydrochloric acid that mass concentration is 15%, the mass ratio of sepiolite and dilute hydrochloric acid is
1:10 is heated to the 4h that boils and stir, and modified meerschaum is obtained after washing, dry through deionized water, pulverizing and sieving；
(3) it coats: nano-titanium dioxide is added in deionized water, after adjustment pH is 9, poly- second is added in ultrasonic disperse afterwards
Modified meerschaum, modified meerschaum, polyvinyl alcohol, nano-titanium dioxide, seaweed is added after heating for dissolving in enol and sodium alginate
The mass ratio of sour sodium is 100:40:6:3, after mixing evenly cooling suspension；Suspension is continuously added dropwise to containing 2% chlorination again
Solidified in the saturation boric acid solution of calcium, after solidifying at least 20h, filtering is drying to obtain embedding modified meerschaum/nano-silica
Change the microsphere adsorbing agent of titanium.
Above-mentioned embodiment is only a preferred solution of the present invention, not the present invention is made in any form
Limitation, there are also other variations and modifications on the premise of not exceeding the technical scheme recorded in the claims.
Claims (6)
1. embedding modified meerschaum/nano-titanium dioxide microsphere adsorbing agent preparation method, which is characterized in that including following step
It is rapid:
(1) sepiolite purifies: sepiolite being add to deionized water, is staticly settled after stirring at least 30min, upper layer sepiolite
Suspension after filtering, deionized water wash repeatedly, vacuum drying, the phosphorous acid of addition mass concentration 3~5% after crushing
Sodium solution, after stirring at low speed 20~30min, high-speed stirred disperses 1~2h, while appropriate filter aid calcium hydroxide is added, and stands
After precipitating, upper layer suspension is filtered, deionized water washing, drying, is pulverized and sieved, the sepiolite of purifying is obtained；
(2) sepiolite is modified: the sepiolite of purifying being added in deionized water, is heated to 160~200 in the case where sealing stirring
DEG C, and 3~5h is kept the temperature, after filtering, drying, it is added in the dilute hydrochloric acid that mass concentration is 10~15%, is heated to boiling and stirs 3
~4h obtains modified meerschaum after washing, dry through deionized water, pulverizing and sieving；
(3) it coats: nano-titanium dioxide is added in deionized water, after adjustment pH is 8.5~9, poly- second is added in ultrasonic disperse afterwards
Modified meerschaum is added after heating for dissolving in enol and sodium alginate, after mixing evenly cooling suspension；It is again that suspension is continuous
It is added dropwise in the saturation boric acid solution containing 2% calcium chloride and is solidified, after solidifying at least 20h, filtering is drying to obtain embedding and is modified
Sepiolite/nano-titanium dioxide microsphere adsorbing agent.
2. embedding modified meerschaum/nano-titanium dioxide microsphere adsorbing agent preparation method according to claim 1, special
Sign is, in step (1), the mass ratio of sepiolite and deionized water is 1:3~5.
3. embedding modified meerschaum/nano-titanium dioxide microsphere adsorbing agent preparation method according to claim 2, special
Sign is, in step (1), the mass ratio of sepiolite and sodium phosphite solution is 1:5~10.
4. embedding modified meerschaum/nano-titanium dioxide microsphere adsorbing agent preparation method according to claim 1 or 2,
It is characterized in that, the revolving speed stirred at low speed is 50~100r/min in step (1), the revolving speed of high-speed stirred is 150~200r/
min。
5. embedding modified meerschaum/nano-titanium dioxide microsphere adsorbing agent preparation method according to claim 1, special
Sign is, in step (2), the mass ratio of sepiolite and dilute hydrochloric acid is 1:5~10.
6. embedding modified meerschaum/nano-titanium dioxide microsphere adsorbing agent preparation method according to claim 1, special
Sign is, in step (3), modified meerschaum, polyvinyl alcohol, nano-titanium dioxide, sodium alginate mass ratio be 100:(20~
40): (4~6): (1~3).
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|---|---|---|---|---|
| CN112875831A (en) * | 2021-01-20 | 2021-06-01 | 苏州础润生态科技有限公司 | Water quality improver for aquaculture, preparation method thereof and application thereof in water purification |
| CN113634236A (en) * | 2021-08-13 | 2021-11-12 | 河北省易县海泡石开发有限公司 | Modification process of sepiolite and application of modified sepiolite |
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