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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 PDF

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CN107511140A
CN107511140A CN201710928926.0A CN201710928926A CN107511140A CN 107511140 A CN107511140 A CN 107511140A CN 201710928926 A CN201710928926 A CN 201710928926A CN 107511140 A CN107511140 A CN 107511140A
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parts
liquid
diatomite
adsorbing material
preparation
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季美
史玉兰
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Wang Min
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Changzhou Jian Xuan Textile Co Ltd
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/14Diatomaceous earth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/041Oxides or hydroxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06Solid 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
    • B01J20/08Solid 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 comprising aluminium oxide or hydroxide; comprising bauxite
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16Alumino-silicates
    • B01J20/18Synthetic zeolitic molecular sieves
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26Synthetic macromolecular compounds
    • B01J20/261Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/285Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/105Phosphorus compounds
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/30Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37Wastewater or sewage treatment systems using renewable energies using solar energy

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  • Analytical Chemistry (AREA)
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  • Hydrology & Water Resources (AREA)
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  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

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

A kind of preparation method of high dephosphorization amount diatomite adsorbing material
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.
CN201710928926.0A 2017-10-09 2017-10-09 A kind of preparation method of high dephosphorization amount diatomite adsorbing material Pending CN107511140A (en)

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CN110550691A (en) * 2019-09-30 2019-12-10 长安大学 dual-modified aluminum sludge, and preparation method and application thereof

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