CN107511140A - A kind of preparation method of high dephosphorization amount diatomite adsorbing material - Google Patents
A kind of preparation method of high dephosphorization amount diatomite adsorbing material Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of high dephosphorization amount diatomite adsorbing material, belong to field of material technology.Flyash and diatomite are stirred, ball milling, sieved to obtain ball-milled powder, and ball-milled powder is placed in Muffle furnace, activation, then is heated up, and insulation calcining, standing is cooled to room temperature, obtains roasting matrix powder；Weigh tetraethyl ammonium hydroxide solution, sodium hydroxide and sodium metaaluminate to be placed in beaker, stir to obtain matrix liquid, weigh deionized water Ludox, tetraethyl ammonium hydroxide solution and sodium oxide molybdena and be placed in beaker, stir to obtain modification liquid；Modification liquid, acetone, styrene maleic anhydride copolymer and 2 dimethylaminoethylamines are taken respectively, are stirred, and obtain mixing dropping liquid；Roasting matrix powder is added in modification liquid, ultrasonic disperse obtains dispersion liquid, mixing dropping liquid is added dropwise in dispersion liquid, then insulation reaction, standing are cooled to room temperature, filter filter cake and to wash, vacuum drying can be prepared into a kind of high dephosphorization amount diatomite adsorbing material.
Description
Technical field
The present invention relates to a kind of preparation method of high dephosphorization amount diatomite adsorbing material, belong to field of material technology.
Background technology
The system of global fresh water is transported to due to excessive nutrient causes outrophication risk to increase.The input of excessive nitrogen phosphorus causes
Surface water, which is degenerated, causes drinking water safety and ecosystem health problem so as to by global concern.Although in decades, point source
The control of pollution, which is administered, to be greatly improved, therefore the research pipe management in face source is oriented by emphasis.In industrialized country
In, most of face source desorption researchs show, scope is big, intermittent, row occurs because it is produced for pollution of area source caused by agricultural production
The features such as uncertainty when putting, turn into waters nutrition pollution source main at present.Chemical fertilizer that agricultural production uses, agricultural chemicals etc.
Nutrition leakage in goods and materials is the main factor that causes eutrophication, due to the leakage of fertilizer, arable land with water system be combined with
And rainwater transfer, rainwater carry the sewage containing high nutrition and are imported into surface water and groundwater, pollute its water quality.Moreover, with regard to mesh
Preceding global energy environment situation judges that, due to the scarcity and limitation of non-renewable energy resources, biomass energy is because of its circulation effect
Can CO that is high, and discharging2And the matter emissions that can pollute such as CO, HC, PM only have respectively it is original it is general even
Less etc. obvious advantage is as the outstanding figure in regenerative resource, by very big concern.But during manufacture bio-fuel, to environment
Bring certain harm.Wherein, the maximum effect to caused by water environment of the production to bio-fuel is to cause body eutrophication,
Due to can mainly be planted as the crop of bio-fuel in the soil of low nutrition or non-agricultural soil, so can largely make
Use fertilizer and pesticide.Therefore while alleviating energy crisis, the problem of also making global eutrophication, is more serious.Eutrophy dissolves
Wawter bloom now is shown as in lake, reservoir, is then red tide phenomenon in marine site.Investigation on Environment Management of Eutrophication both at home and abroad
Illustrate, the present situation of the ocean situation also allows of no optimist.From the 1960s, due to red tide phenomenon caused by the eutrophication of ocean just
The whole world is generally appeared in, has been one of global Oceanic disasters so far, during the decaying of red tide, release comes in and goes out vulcanization
Thing gas and toxin can polluted seawater, be that many still wants to biology and hidden flee from, so as to form in " dead band ".Such as U.S.'s Publishing Study
Report display, the Gulf of Mexico " dead band " phase size is equivalent to the Connecticut State in the U.S.；The Hangzhou Wan in China Zhejiang
Occur " dead band " of nearly 100 sq-km and 20 sq-kms respectively with the Communities of The Jinzhou Bay in Liaoning.In marine site
Sea grass bed can be the growth of the fish species with very high commercial value with biological support diversity and be ecosystems services
Hotbed, therefore be protect coastal ecosystems key.Eutrophication can cause fungi to grow and limit sunlight,
So as to cause the degeneration of sea grass even to disappear.In summary, it is exactly to administer rich battalion to repair one of important measure of water environment
Fosterization.In the absorbent extraneous nutrient of plant, a kind of minimum upgrowth situation for determining plant of content.Phosphorus is in algae molecule
Middle proportion is minimum, then, phosphorus is the key factor of algal grown.When the nitrogen surplus in water body, made by biochemistry
With nitrogen being made to be converted into the form of gaseous nitrogen, and overflowed from water body.P elements do not have common gas form, certainly
The circulation on right boundary belongs to appositional pattern, if being present in water body, can only just be circulated with different shape in water body, had with nitrogen cycle
Very big difference.Moreover, when the phosphorus content in every liter of water reaches 0.02mg, eutrophication is easy for occurring.In Curacao
Investigation with Bonaire finds that N is 0.91~2.4% in the general content of nutrient density in original sea grass bed blade and P is
Between 0.05~0.18%, and in the system of eutrophication, the content of leaf nutrient concentration is that N is 1.87~3.02%, and P is
0.14~0.70%.Also, the data and SUMMARY OF THE RELEVANT LITERATURE of monitoring illustrate, the nutrient content of blade in sea grass bed（Especially
P）, be typically due near source of nutrition and raise, so generally may be used as be nutrition pollution important indicator.Due in water
Whether the conduct containing phosphorus concentration, which eutrophication occurs, is put into pacing factor, then reducing the concentration of phosphorus just turns into alleviation eutrophication
Breach.
The content of the invention
The technical problems to be solved by the invention：Phosphorus poor-performing is inhaled for diatomite adsorbing material, can not be met existing
A kind of the problem of sorbing material uses, there is provided preparation method of high dephosphorization amount diatomite adsorbing material.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）In mass ratio 1:5, flyash and diatomite ball milling are sieved to obtain ball-milled powder, ball-milled powder is placed in Muffle furnace,
Heated up again after insulation activation, after insulation calcining, standing is cooled to room temperature, obtains roasting matrix powder；
（2）Count in parts by weight, respectively 45~50 parts of tetraethyl ammonium hydroxide solution of weighing, 2~3 parts of sodium hydroxides and 3~5 parts
Sodium metaaluminate is stirred to obtain matrix liquid, then counts in parts by weight, and it is molten to weigh 55~60 parts of deionized waters, 5~8 parts of silicon respectively
Glue, 1~2 part of tetraethyl ammonium hydroxide solution and 1~2 sodium oxide molybdena are stirred to obtain modification liquid；
（3）Count in parts by weight, take 45~50 parts of modification liquids, 50~55 parts of acetone, 10~15 parts of phenylethylene-maleic anhydrides respectively
Copolymer and 5~8 parts of 2- dimethylaminoethylamines are stirred, and obtain mixing dropping liquid；
（4）In mass ratio 1:5, roasting matrix powder is added in modification liquid, ultrasonic disperse obtains dispersion liquid, then by volume 1:
5, mixing dropping liquid is added dropwise in dispersion liquid, after being added dropwise to complete, insulation reaction, standing is cooled to room temperature, washing, dries,
A kind of high dephosphorization amount diatomite adsorbing material can be prepared into.
Step（1）Described insulation activation temperature is 120~150 DEG C.
Step（1）Described insulation calcining heat is 780~850 DEG C.
Step（2）Described described Ludox solid content is 25%.
Step（3）Described is 2mL/min by mixing dropping liquid drop rate.
Compared with other method, advantageous effects are the present invention：
（1）The present invention makes complex matrix produce the singly-bound of metal salt and oxygen by flyash and composite diatomite, through high-temperature roasting
Or the compound group of hydroxyl, the absorption property of material matrix is effectively improved, while molecular screen membrane is coated in matrix surface, pass through molecule
Sieve membrane has excellent pore structure and higher specific surface area, makes matrix material more excellent to phosphorus absorbent properties；
（2）The present invention to its charge by while to blapharoplast Surface coating molecular screen membrane, being modified, passing through benzene
Containing the group for being easy to be reacted with hydroxyl and amino on ethylene-maleic acid strand, carried out with diatomite particle effective
With reference to and grafting, then the 2- dimethylaminoethylamines containing tertiary amine group are grafted on composite material surface, make its cross-linking reaction simultaneously
Quaternary ammonium salt structure is formed, the elecrtonegativity lotus of carboxylic group institute band is counteracted by the positive charge of the quaternary ammonium salt group institute band of introducing,
Effectively improve the absorption property of diatomite adsorbing material.
Embodiment
In mass ratio 1:5, flyash and diatomite are stirred and are placed in ball grinder, under 200~300r/min
After 3~5h of ball milling, cross 200 mesh sieves and obtain ball-milled powder, ball-milled powder is placed in Muffle furnace, activation is incubated at 120~150 DEG C
After 25~30min, then by 10 DEG C/min it is warming up to 780~850 DEG C, after 1~2h of insulation calcining, standing is cooled to room temperature, must roast
Burn matrix powder；Count in parts by weight, respectively weigh 45~50 parts of tetraethyl ammonium hydroxide solution of mass fraction 10%, 2~3 parts
Sodium hydroxide and 3~5 parts of sodium metaaluminates are placed in beaker, are stirred to obtain matrix liquid, then are counted in parts by weight, weigh 55 respectively
~60 parts of deionized waters, 5~8 parts of Ludox, 1~2 part of tetraethyl ammonium hydroxide solution of mass fraction 10% and 1~2 sodium oxide molybdena
It is placed in beaker, is stirred to obtain modification liquid；Count in parts by weight, take 45~50 parts of modification liquids, 50~55 parts of acetone, 10 respectively
~15 parts of styrene-maleic anhydride copolymers and 5~8 parts of 2- dimethylaminoethylamines, are stirred at 45~50 DEG C, must mix
Dropping liquid；In mass ratio 1:5, will roasting matrix powder be added to modification liquid in, under 200~300W ultrasonic disperse 10~
15min, obtains dispersion liquid, then by volume 1:5, mixing dropping liquid is added dropwise in dispersion liquid, it is 2mL/ to control drop rate
Min, after being added dropwise to complete, then 20~24h of insulation reaction under the conditions of 75~85 DEG C, 10~20MPa, standing are cooled to room temperature,
Filter cake and with deionized water rinsing 3~5 times is filtered to obtain, vacuum drying can be prepared into a kind of high dephosphorization amount diatom soil matrix adsorption material
Material；Described Ludox solid content is 25%.
Example 1
In mass ratio 1:5, flyash and diatomite are stirred and are placed in ball grinder, under 200r/min after ball milling 3h,
Cross 200 mesh sieves and obtain ball-milled powder, ball-milled powder is placed in Muffle furnace, at 120 DEG C insulation activation 25min after, then by 10 DEG C/
Min is warming up to 780 DEG C, after 1h is calcined in insulation, and standing is cooled to room temperature, obtains roasting matrix powder；Count, claim respectively in parts by weight
45 parts of tetraethyl ammonium hydroxide solution of mass fraction 10% of amount, 2 parts of sodium hydroxides and 3 parts of sodium metaaluminates are placed in beaker, are stirred
Matrix liquid is mixed to obtain, then is counted in parts by weight, weighs 55 parts of deionized waters respectively, 5 parts of solid contents are 25% Ludox, 1 part of matter
The amount tetraethyl ammonium hydroxide solution of fraction 10% and 1 sodium oxide molybdena are placed in beaker, are stirred to obtain modification liquid；In parts by weight
Meter, takes 45 parts of modification liquids, 50 parts of acetone, 10 parts of styrene-maleic anhydride copolymers and 5 parts of 2- dimethylaminoethylamines respectively,
It is stirred at 45 DEG C, obtains mixing dropping liquid；In mass ratio 1:5, roasting matrix powder is added in modification liquid, under 200W
Ultrasonic disperse 10min, obtains dispersion liquid, then by volume 1:5, mixing dropping liquid is added dropwise in dispersion liquid, controls drop rate
For 2mL/min, after being added dropwise to complete, then the insulation reaction 20h under the conditions of 75 DEG C, 10MPa, standing are cooled to room temperature, filtered
Filter cake and with deionized water rinsing 3 times, vacuum drying can be prepared into a kind of high dephosphorization amount diatomite adsorbing material.
Example 2
In mass ratio 1:5, flyash and diatomite are stirred and are placed in ball grinder, under 250r/min after ball milling 4h,
Cross 200 mesh sieves and obtain ball-milled powder, ball-milled powder is placed in Muffle furnace, at 135 DEG C insulation activation 27min after, then by 10 DEG C/
Min is warming up to 815 DEG C, after 1h is calcined in insulation, and standing is cooled to room temperature, obtains roasting matrix powder；Count, claim respectively in parts by weight
47 parts of tetraethyl ammonium hydroxide solution of mass fraction 10% of amount, 2 parts of sodium hydroxides and 4 parts of sodium metaaluminates are placed in beaker, are stirred
Matrix liquid is mixed to obtain, then is counted in parts by weight, weighs 57 parts of deionized waters respectively, 6 parts of solid contents are 25% Ludox, 1 part of matter
The amount tetraethyl ammonium hydroxide solution of fraction 10% and 1 sodium oxide molybdena are placed in beaker, are stirred to obtain modification liquid；In parts by weight
Meter, takes 47 parts of modification liquids, 52 parts of acetone, 12 parts of styrene-maleic anhydride copolymers and 6 parts of 2- dimethylaminoethylamines respectively,
It is stirred at 47 DEG C, obtains mixing dropping liquid；In mass ratio 1:5, roasting matrix powder is added in modification liquid, under 250W
Ultrasonic disperse 12min, obtains dispersion liquid, then by volume 1:5, mixing dropping liquid is added dropwise in dispersion liquid, controls drop rate
For 2mL/min, after being added dropwise to complete, then the insulation reaction 22h under the conditions of 80 DEG C, 15MPa, standing are cooled to room temperature, filtered
Filter cake and with deionized water rinsing 4 times, vacuum drying can be prepared into a kind of high dephosphorization amount diatomite adsorbing material.
Example 3
In mass ratio 1:5, flyash and diatomite are stirred and are placed in ball grinder, under 300r/min after ball milling 5h,
Cross 200 mesh sieves and obtain ball-milled powder, ball-milled powder is placed in Muffle furnace, at 150 DEG C insulation activation 30min after, then by 10 DEG C/
Min is warming up to 850 DEG C, after 2h is calcined in insulation, and standing is cooled to room temperature, obtains roasting matrix powder；Count, claim respectively in parts by weight
50 parts of tetraethyl ammonium hydroxide solution of mass fraction 10% of amount, 3 parts of sodium hydroxides and 5 parts of sodium metaaluminates are placed in beaker, are stirred
Matrix liquid is mixed to obtain, then is counted in parts by weight, weighs 60 parts of deionized waters respectively, 8 parts of solid contents are 25% Ludox, 2 parts of matter
The amount tetraethyl ammonium hydroxide solution of fraction 10% and 2 sodium oxide molybdenas are placed in beaker, are stirred to obtain modification liquid；In parts by weight
Meter, takes 50 parts of modification liquids, 55 parts of acetone, 15 parts of styrene-maleic anhydride copolymers and 8 parts of 2- dimethylaminoethylamines respectively,
It is stirred at 50 DEG C, obtains mixing dropping liquid；In mass ratio 1:5, roasting matrix powder is added in modification liquid, under 300W
Ultrasonic disperse 15min, obtains dispersion liquid, then by volume 1:5, mixing dropping liquid is added dropwise in dispersion liquid, controls drop rate
For 2mL/min, after being added dropwise to complete, then the insulation reaction 24h under the conditions of 85 DEG C, 20MPa, standing are cooled to room temperature, filtered
Filter cake and with deionized water rinsing 5 times, vacuum drying can be prepared into a kind of high dephosphorization amount diatomite adsorbing material.
The sorbing material that the high dephosphorization amount diatomite adsorbing material being prepared into and Dongguan City company produce is examined
Survey, specific detection is as follows：
（1）Grafting rate is tested
Reflection modified effect directly perceived, grafting rate is represented using the rate of body weight gain of weight method calculating graft modification product.Specific behaviour
It is before graft modification, to weigh and dry baby's algae king's former state quality, and carry out graft modification as method.After the completion of graft modification, first will
Product cleaning and constant weight is dried under vacuum to, then to Weighed product, records its weight.Calculated using following equation：
G=（mg-mr)/mr
G in formula：Grafting rate（%）
mr：The quality of sample before graft modification（mg）
mg：The quality of sample after graft modification（mg）
（2）Phosphorus absorption test
Accurate to weigh after 0.8788g di(2-ethylhexyl)phosphate ammonia clocks fully dissolve with deionized water, the constant volume in volumetric flask, obtaining concentration is
The 100mg/L skilful storing solution of phosphoric acid diamino, the phosphorus solution of the various concentrations used in adsorption experiment dilutes by storing solution to be obtained,
The pH value of solution is adjusted using concentration 1mol/L HCl and 1mol/L NaOH.Adsorption experiment operating process is as follows, takes
Volume is that 20mL vial with cover makees container, 0.01gDE_FeLa and l0mL phosphorus solutions are added into bottle, then will be small
Bottle is moved into constant temperature oscillation case, 25 DEG C of frequency of oscillation 200rpm of set water temperature.After constant temperature oscillation 6h, mixed liquor is through 0.45 μm of filter membrane
Filter filtering, filtrate carry out phosphorus concentration measure,
Specific test result such as table 1.
The high dephosphorization amount diatomite adsorbing material performance characterization of table 1
As shown in Table 1, a kind of high dephosphorization amount diatomite adsorbing material is made in the present invention, and grafting rate is obviously improved
Effectively combined and be grafted with diatomite particle, the concentration of phosphorus reduces, and effectively increases the suction of diatomite adsorbing material
Attached performance.
Claims (5)
1. a kind of preparation method of high dephosphorization amount diatomite adsorbing material, it is characterised in that specifically preparation process is：
（1）In mass ratio 1:5, flyash and diatomite ball milling are sieved to obtain ball-milled powder, ball-milled powder is placed in Muffle furnace,
Heated up again after insulation activation, after insulation calcining, standing is cooled to room temperature, obtains roasting matrix powder；
（2）Count in parts by weight, respectively 45~50 parts of tetraethyl ammonium hydroxide solution of weighing, 2~3 parts of sodium hydroxides and 3~5 parts
Sodium metaaluminate is stirred to obtain matrix liquid, then counts in parts by weight, and it is molten to weigh 55~60 parts of deionized waters, 5~8 parts of silicon respectively
Glue, 1~2 part of tetraethyl ammonium hydroxide solution and 1~2 sodium oxide molybdena are stirred to obtain modification liquid；
（3）Count in parts by weight, take 45~50 parts of modification liquids, 50~55 parts of acetone, 10~15 parts of phenylethylene-maleic anhydrides respectively
Copolymer and 5~8 parts of 2- dimethylaminoethylamines are stirred, and obtain mixing dropping liquid；
（4）In mass ratio 1:5, roasting matrix powder is added in modification liquid, ultrasonic disperse obtains dispersion liquid, then by volume 1:
5, mixing dropping liquid is added dropwise in dispersion liquid, after being added dropwise to complete, insulation reaction, standing is cooled to room temperature, washing, dries,
A kind of high dephosphorization amount diatomite adsorbing material can be prepared into.
A kind of 2. preparation method of high dephosphorization amount diatomite adsorbing material according to claim 1, it is characterised in that：Step
Suddenly（1）Described insulation activation temperature is 120~150 DEG C.
A kind of 3. preparation method of high dephosphorization amount diatomite adsorbing material according to claim 1, it is characterised in that：Step
Suddenly（1）Described insulation calcining heat is 780~850 DEG C.
A kind of 4. preparation method of high dephosphorization amount diatomite adsorbing material according to claim 1, it is characterised in that：Step
Suddenly（2）Described described Ludox solid content is 25%.
A kind of 5. preparation method of high dephosphorization amount diatomite adsorbing material according to claim 1, it is characterised in that：Step
Suddenly（3）Described is 2mL/min by mixing dropping liquid drop rate.
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