CN109012642A - A kind of preparation method of diatomite based composite adsorption material - Google Patents
A kind of preparation method of diatomite based composite adsorption material Download PDFInfo
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- 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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- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- 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
- B01J20/28054—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 surface properties or porosity
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
Abstract
The invention discloses a kind of preparation methods of diatomite based composite adsorption material, belong to environment-friendly materials technical field.Diatomite based composite adsorption material blank is mixed with composition metal salting liquid 1:10~1:12 in mass ratio, and the chitosan solution of 0.1~0.2 times of diatomite based composite adsorption material blank quality is added into the mixture of diatomite based composite adsorption material blank and composition metal salting liquid, after impregnating 2~3h under room temperature, filtering, obtain filter cake, after filter cake is washed with deionized 8~10 times, under conditions of being 90~100 DEG C in temperature after dry 1~2h, diatomite based composite adsorption material is obtained.The diatomite based composite adsorption material of technical solution of the present invention preparation has the characteristics that excellent phosphor-removing effect and mechanical property, has broad prospects in the development of environment-friendly materials technology of preparing industry.
Description
Technical field
The invention discloses a kind of preparation methods of diatomite based composite adsorption material, belong to environment-friendly materials technical field.
Background technique
Adsorbent is also referred to as absorbent, and this substance can make active constituent be attached to its particle surface, makes the micro chemical combination of liquid
Object additive becomes solid compounds, is conducive to implement uniformly to mix.It is that one kind can be adsorbed effectively from gas or liquid
The solid matter of some of them ingredient.With big specific surface, suitable pore structure and surface texture；Have to adsorbate strong
Adsorption capacity；It is not chemically reacted with adsorbate and medium generally；Easily manufactured, regenerating easily；Have fabulous adsorptivity and
Mechanicalness characteristic.Adsorbent generally has following characteristics: big specific surface, suitable pore structure and surface texture；Have to adsorbate
Strong adsorption capacity；It is not chemically reacted with adsorbate and medium generally；Easily manufactured, regenerating easily；There is fabulous suction
Attached property and mechanicalness characteristic.Adsorbent can classify by pore size, grain shape, chemical component, surface polarity etc., such as gross porosity and
Pore adsorbent, powdery, granular, strip adsorbent, carbonaceous and oxide adsorbent, polarity and non-polar adsorbent etc..It is common
Adsorbent have using carbonaceous as the various acticarbons and metal of raw material, nonmetal oxide class adsorbent (such as silica gel, oxygen
Change aluminium, molecular sieve, natural clay etc.).Most representative adsorbent is active carbon, and absorption property is fairly good, but cost ratio
It is higher, once applied the toluene being used in adsorbed water body in the event of Song Hua River.Secondly there are also molecular sieve, silica gel, activated aluminum, polymerizations
Object adsorbent and biological adsorption agent etc..Adsorbent is typically used in the industrial production, therefore can according to the common property of industry
Adsorbent is divided into six major class.Silica gel, it is mainly used for dry, admixture of gas and separation of petroleum component etc.；Aluminium oxide,
It is also a kind of adsorbent of dehydration；Active carbon is mainly used for water process, decoloration and gas treatment；Polyacrylamide, it is main to use
In sanitary sewage and organic wastewater；Zeolite molecular sieve, it is dry for gas absorption separation, gas and liquid；Carbon molecular sieve, mainly
Transport channeling is played, micropore then plays molecular sieve.Adsorbent is generally also classified into two class of organic matter and inorganic matter, organic matter
Class such as wheat-germ meal, the maize powder of degreasing, corncob fragment, bran, soybean fine powder and bibulous cereals etc..
Inorganic species then include silica, vermiculite, calcium silicates etc..
And what traditional diatomite based composite adsorption material can not be further increased there is also phosphor-removing effect and mechanical property
Therefore how disadvantage improves traditional diatomite based composite adsorption material phosphor-removing effect and mechanical property can not further increase
Disadvantage, developing the diatomite based composite adsorption material with good comprehensive performance in the hope of exploration is problem to be solved.
Summary of the invention
The present invention solves the technical problem of: for traditional diatomite based composite adsorption material phosphor-removing effect and mechanics
The shortcomings that performance can not further increase provides a kind of preparation method of diatomite based composite adsorption material.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of diatomite based composite adsorption material, specific preparation step are as follows:
(1) alkyl glucoside quaternary ammonium compound is mixed with water 1:10~1:12 in mass ratio, and alkyl glucoside quaternary ammonium compound matter is added
2~4 times of sodium bentonite and 0.3~0.5 times of alkyl glucoside quaternary ammonium compound quality of Aluminium chloride hexahydrate are measured, is stirred to react
Afterwards, it is centrifuged, filters, wash, it is dry, obtain organobentonite；
(2) aniline solution is mixed with graphene 10:2~10:3 in mass ratio, after ultrasonic disperse, aniline mixture is obtained, by benzene
Amine blends are mixed with organobentonite 5:1~5:2 in mass ratio, after being stirred to react, are filtered, are washed, dry, and it is swollen to obtain pre- modification
Profit soil, pre- modified alta-mud is mixed with water 1:4~1:5 in mass ratio, and after adjusting pH to 6.5~6.8, pre- bentone is added
The ferric trichloride that 0.02~0.05 times of soil property amount, after being stirred to react, filtering washing is dry, obtains modified alta-mud；
(3) pretreatment diatomite is mixed with pre- modified alta-mud 2:1~3:1 in mass ratio, and it is diatomaceous that pretreatment is added
The binder of 0.2~0.4 times of amount, after being stirred, is granulated, and calcining obtains diatomite based composite adsorption material blank；
(4) diatomite based composite adsorption material blank is mixed with composition metal salting liquid 1:10~1:12 in mass ratio, and added
Enter 0.1~0.2 times of quality of diatomite based composite adsorption material blank of chitosan solution, impregnate, filter, washs, it is dry, obtain silicon
Diatomaceous earth based composite adsorption material.
Step (1) alkyl glucoside quaternary ammonium compound is eight alkyl glucoside quaternary ammonium compounds or dodecane alkyl polyglucosides quaternary ammonium salt
In any one.
Step (2) aniline solution is to mix aniline with dehydrated alcohol 1:10~2:10 in mass ratio, stirring and dissolving
Afterwards, aniline solution is obtained.
The preparation method of step (3) the pretreatment diatomite is to crush diatomite, crosses 50 meshes, must pre-process diatom
Soil.
Step (3) described binder is the sodium silicate solution that mass fraction is 20~40% or mass fraction is 25~40%
Attapulgite dispersion liquid.
Step (4) the composition metal salting liquid is to mix calcium nitrate with water 1:10~1:12 in mass ratio, and be added
The magnesium chloride that 0.2~0.4 times of calcium nitrate quality after being stirred, obtains composition metal salting liquid.
Step (4) described chitosan solution is the ice for being 2~4% by the chitosan of deacetylation 70~85% and mass fraction
Acetic acid 1:5~1:6 in mass ratio mixing, obtains chitosan solution.
The beneficial effects of the present invention are:
Modified alta-mud is added when preparing diatomite based composite adsorption material in the present invention, firstly, using benzene in modified alta-mud
Amine carries out intercalation modifying to organic base bentonite, and in subsequent preparation process, is formed aniline under the action of iron chloride and handed over
Connection improves bentonitic hole spacing, and then propose the adsorbance of product to be inserted into polyaniline in organobentonite
Height, dephosphorization efficiency and dephosphorization effect improve, secondly, the polyaniline being added can carbonize in product blank calcination process, form gas
The gas of body and carbon fiber, formation can be used as pore-foaming agent, improve the porosity of product, and then improve the adsorptivity of product,
Dephosphorization effect improves, and forms carbon fiber and may be present in bentonitic interlayer structure, and with the graphene of addition in bentonite
Interlayer structure in form porous sponge structure, and then improve the adsorptivity of product, dephosphorization effect improves, and due to sea
The presence of continuous structure can make product with it is porous simultaneously, improve the mechanical property of product；Furthermore in subsequent processing
It is impregnated using composition metal salting liquid, the metal ion in metal salt can be made to be adsorbed by product, thus in product use process
In, Phosphate Adsorption is formed in interiors of products, and then improve the dephosphorization effect of product.
Specific embodiment
Aniline is mixed with dehydrated alcohol 1:10~2:10 in mass ratio, in temperature be 30~50 DEG C, revolving speed be 200~
Under conditions of 300r/min, after 30~60min of stirring and dissolving, aniline solution is obtained；Alkyl glucoside quaternary ammonium compound and water are pressed into quality
It is mixed in beaker than 1:10~1:12, and 2~4 times of alkyl glucoside quaternary ammonium compound quality of sodium bentonite is added into beaker
With 0.3~0.5 times of Aluminium chloride hexahydrate of alkyl glucoside quaternary ammonium compound quality, in temperature be 45~65 DEG C, revolving speed be 250~
Under conditions of 350r/min, after being stirred to react 1~2h, by material in beaker under conditions of revolving speed is 2000~3000r/min
After being centrifuged 10~20min, filtering obtains organobentonite blank, after organobentonite blank is washed with deionized 5~8 times,
Under conditions of being 105~110 DEG C in temperature after dry 1~2h, organobentonite is obtained；In mass ratio by aniline solution and graphene
10:2~10:3 mixing obtains aniline mixture, by benzene under conditions of frequency is 45~65kHz after 30~50min of ultrasonic disperse
Amine blends are mixed with organobentonite 5:1~5:2 in mass ratio, are 70~90 DEG C in temperature, revolving speed is 280~350r/min
Under conditions of, after being stirred to react 1~2h, filtering obtains pre- modified alta-mud blank, by pre- modified alta-mud blank deionized water
After washing 5~8 times, under conditions of being 80~100 DEG C in temperature after dry 1~2h, pre- modified alta-mud is obtained, by pre- bentone
Soil is mixed in flask with water 1:4~1:5 in mass ratio, and the acetic acid for being 2~8% with mass fraction adjusts material in flask
After pH to 6.5~6.8, the ferric trichloride of 0.02~0.05 times of pre- modified alta-mud quality is added into flask, in temperature be 0~
2 DEG C, under conditions of revolving speed is 280~400r/min, after being stirred to react 2~3h, filtering obtains modified alta-mud blank, will be modified
After bentonite blank is washed with water 8~10 times, under conditions of being 100~105 DEG C in temperature after dry 60~80min, modification is obtained
Bentonite；Pretreatment diatomite and pre- modified alta-mud 2:1~3:1 in mass ratio are mixed in blender, and to blender
The middle binder that 0.2~0.4 times of diatomite quality of pretreatment is added is 45~55 DEG C in temperature, and revolving speed is 250~300r/min
Under conditions of, after being stirred 30~40min, it is granulated, diatomite based composite adsorption material blank must be pre-processed, silicon will be pre-processed
After diatomaceous earth based composite adsorption material blank calcines 1~2h under conditions of being 700~800 DEG C in temperature, the compound suction of diatom soil matrix is obtained
Enclosure material blank；Diatomite based composite adsorption material blank is mixed with composition metal salting liquid 1:10~1:12 in mass ratio,
And diatom soil matrix composite adsorption material is added into the mixture of diatomite based composite adsorption material blank and composition metal salting liquid
The chitosan solution of 0.1~0.2 times of material base material quality, after impregnating 2~3h under room temperature, filtering obtains filter cake, filter cake is used
After deionized water is washed 8~10 times, under conditions of being 90~100 DEG C in temperature after dry 1~2h, diatom soil matrix composite adsorption is obtained
Material.The alkyl glucoside quaternary ammonium compound is any one in eight alkyl glucoside quaternary ammonium compounds or dodecane alkyl polyglucosides quaternary ammonium salt
Kind.The preparation method of the pretreatment diatomite is to crush diatomite, crosses 50 meshes, obtains pretreatment diatomite.The bonding
The attapulgite dispersion liquid that agent is the sodium silicate solution that mass fraction is 20~40% or mass fraction is 25~40%.It is described compound
Metal salt solution is to mix calcium nitrate with water 1:10~1:12 in mass ratio, and 0.2~0.4 times of calcium nitrate quality of chlorine is added
Change magnesium, after being stirred, obtains composition metal salting liquid.The chitosan solution be by the chitosan of deacetylation 70~85% with
Glacial acetic acid 1:5~1:6 in mass ratio that mass fraction is 2~4% is mixed, and obtains chitosan solution.
Aniline is mixed with dehydrated alcohol 2:10 in mass ratio, is 50 DEG C in temperature, under conditions of revolving speed is 300r/min, is stirred
After mixing dissolution 60min, aniline solution is obtained；Alkyl glucoside quaternary ammonium compound and water 1:12 in mass ratio are mixed in beaker, and to
4 times of alkyl glucoside quaternary ammonium compound quality of sodium bentonite and the six of 0.5 times of alkyl glucoside quaternary ammonium compound quality is added in beaker
Aluminium chlorohydrate, in temperature be 65 DEG C, revolving speed be 350r/min under conditions of, after being stirred to react 2h, by material in beaker in turn
Speed be 3000r/min under conditions of be centrifuged 20min after, filtering, obtain organobentonite blank, by organobentonite blank spend from
After sub- water washing 8 times, under conditions of being 110 DEG C in temperature after dry 2h, organobentonite is obtained；Aniline solution and graphene are pressed
Mass ratio 10:3 mixing obtains aniline mixture, by aniline mixture under conditions of frequency is 65kHz after ultrasonic disperse 50min
Mixed with organobentonite 5:2 in mass ratio, in temperature be 90 DEG C, revolving speed be 350r/min under conditions of, after being stirred to react 2h,
Filtering, obtains pre- modified alta-mud blank, after pre- modified alta-mud blank is washed with deionized 8 times, in temperature be 100 DEG C
Under the conditions of after dry 2h, obtain pre- modified alta-mud, pre- modified alta-mud and water 1:5 in mass ratio be mixed in flask, are used in combination
In the acetic acid adjusting flask that mass fraction is 8% after the pH to 6.8 of material, pre- modified alta-mud quality 0.05 is added into flask
Ferric trichloride again is 2 DEG C in temperature, and under conditions of revolving speed is 400r/min, after being stirred to react 3h, filtering obtains bentone
Sun-dried mud brick material after modified alta-mud blank is washed with water 10 times, under conditions of being 105 DEG C in temperature after dry 80min, obtains modification
Bentonite；Pretreatment diatomite and pre- modified alta-mud 3:1 in mass ratio are mixed in blender, and are added into blender
The binder of 0.4 times of diatomite quality of pretreatment is 55 DEG C in temperature, under conditions of revolving speed is 300r/min, is stirred
It after 40min, is granulated, diatomite based composite adsorption material blank must be pre-processed, diatomite based composite adsorption material base will be pre-processed
Expect in temperature be 800 DEG C under conditions of calcine 2h after, obtain diatomite based composite adsorption material blank；By diatom soil matrix composite adsorption
Material blank is mixed with composition metal salting liquid 1:12 in mass ratio, and to diatomite based composite adsorption material blank and compound gold
Belong to the chitosan solution that 0.2 times of diatomite based composite adsorption material blank quality is added in the mixture of salting liquid, in room temperature item
After impregnating 3h under part, filtering obtains filter cake, dry under conditions of being 100 DEG C in temperature after filter cake is washed with deionized 10 times
After 2h, diatomite based composite adsorption material is obtained.The alkyl glucoside quaternary ammonium compound is eight alkyl glucoside quaternary ammonium compounds.The pre- place
The preparation method of reason diatomite is to crush diatomite, crosses 50 meshes, obtains pretreatment diatomite.The binder is mass fraction
The attapulgite dispersion liquid that sodium silicate solution or mass fraction for 40% are 40%.The composition metal salting liquid is by calcium nitrate
It is mixed with water 1:12 in mass ratio, and 0.4 times of calcium nitrate quality of magnesium chloride is added, after being stirred, it is molten to obtain composite metal salt
Liquid.The chitosan solution is that the glacial acetic acid 1:6 in mass ratio for being 4% with mass fraction by the chitosan of deacetylation 85% is mixed
It closes, obtains chitosan solution.
Alkyl glucoside quaternary ammonium compound and water 1:12 in mass ratio are mixed in beaker, and alkyl polysaccharide is added into beaker
The sodium bentonite and 0.5 times of alkyl glucoside quaternary ammonium compound quality of Aluminium chloride hexahydrate of 4 times of glycosides quaternary ammonium salt quality be in temperature
65 DEG C, under conditions of revolving speed is 350r/min, after being stirred to react 2h, by material in beaker in the condition that revolving speed is 3000r/min
After lower centrifugation 20min, filtering obtains organobentonite blank, after organobentonite blank is washed with deionized 8 times, Yu Wen
Degree after dry 2h, obtains organobentonite under conditions of being 110 DEG C；Graphene ultrasonic disperse under conditions of frequency is 65kHz
After 50min, obtain mixture, mixture mixed with organobentonite 5:2 in mass ratio, in temperature be 90 DEG C, revolving speed 350r/
Under conditions of min, after being stirred to react 2h, filtering obtains pre- modified alta-mud blank, by pre- modified alta-mud blank deionized water
After washing 8 times, under conditions of being 100 DEG C in temperature after dry 2h, pre- modified alta-mud is obtained, pre- modified alta-mud and water are pressed into matter
Amount is mixed in flask than 1:5, and the acetic acid for being 8% with mass fraction is adjusted in flask after the pH to 6.8 of material, into flask
The ferric trichloride of 0.05 times of pre- modified alta-mud quality is added, is 2 DEG C in temperature, under conditions of revolving speed is 400r/min, stirs
After reacting 3h, filtering obtains modified alta-mud blank, after modified alta-mud blank is washed with water 10 times, in temperature be 105 DEG C
Under the conditions of after dry 80min, obtain modified alta-mud；Pretreatment diatomite is mixed in pre- modified alta-mud 3:1 in mass ratio
In blender, and addition pre-processes 0.4 times of diatomite quality of binder into blender, is 55 DEG C in temperature, revolving speed is
Under conditions of 300r/min, after being stirred 40min, it is granulated, diatomite based composite adsorption material blank must be pre-processed, will be located in advance
It manages after calcining 2h under conditions of diatomite based composite adsorption material blank is 800 DEG C in temperature, obtains diatom soil matrix composite adsorption material
Material base material；Diatomite based composite adsorption material blank is mixed with composition metal salting liquid 1:12 in mass ratio, and to diatomite
Diatomite based composite adsorption material blank quality is added in the mixture of based composite adsorption material blank and composition metal salting liquid
0.2 times of chitosan solution, after impregnating 3h under room temperature, filtering obtains filter cake, filter cake is washed with deionized 10 times
Afterwards, under conditions of being 100 DEG C in temperature after dry 2h, diatomite based composite adsorption material is obtained.The alkyl glucoside quaternary ammonium compound
For eight alkyl glucoside quaternary ammonium compounds.The preparation method of the pretreatment diatomite is to crush diatomite, crosses 50 meshes, obtains pre- place
Manage diatomite.The attapulgite dispersion that the binder is the sodium silicate solution that mass fraction is 40% or mass fraction is 40%
Liquid.The composition metal salting liquid is to mix calcium nitrate with water 1:12 in mass ratio, and 0.4 times of calcium nitrate quality of chlorine is added
Change magnesium, after being stirred, obtains composition metal salting liquid.The chitosan solution is by the chitosan and quality of deacetylation 85%
The glacial acetic acid 1:6 in mass ratio that score is 4% is mixed, and obtains chitosan solution.
Aniline is mixed with dehydrated alcohol 2:10 in mass ratio, is 50 DEG C in temperature, under conditions of revolving speed is 300r/min, is stirred
After mixing dissolution 60min, aniline solution is obtained；Alkyl glucoside quaternary ammonium compound and water 1:12 in mass ratio are mixed in beaker, and to
4 times of alkyl glucoside quaternary ammonium compound quality of sodium bentonite and the six of 0.5 times of alkyl glucoside quaternary ammonium compound quality is added in beaker
Aluminium chlorohydrate, in temperature be 65 DEG C, revolving speed be 350r/min under conditions of, after being stirred to react 2h, by material in beaker in turn
Speed be 3000r/min under conditions of be centrifuged 20min after, filtering, obtain organobentonite blank, by organobentonite blank spend from
After sub- water washing 8 times, under conditions of being 110 DEG C in temperature after dry 2h, organobentonite is obtained；It is in frequency by aniline solution
Under conditions of 65kHz after ultrasonic disperse 50min, aniline mixture is obtained, by aniline mixture and organobentonite 5:2 in mass ratio
Mixing is 90 DEG C in temperature, and under conditions of revolving speed is 350r/min, after being stirred to react 2h, filtering obtains pre- bentone sun-dried mud brick
Material after pre- modified alta-mud blank is washed with deionized 8 times, under conditions of being 100 DEG C in temperature after dry 2h, obtains pre- change
Property bentonite, pre- modified alta-mud and water 1:5 in mass ratio are mixed in flask, and the acetic acid adjusting for being 8% with mass fraction
In flask after the pH to 6.8 of material, the ferric trichloride of 0.05 times of pre- modified alta-mud quality is added into flask, in temperature be 2
DEG C, under conditions of revolving speed is 400r/min, after being stirred to react 3h, filtering obtains modified alta-mud blank, by modified alta-mud blank
After being washed with water 10 times, under conditions of being 105 DEG C in temperature after dry 80min, modified alta-mud is obtained；Will pretreatment diatomite with
Pre- modified alta-mud 3:1 in mass ratio is mixed in blender, and is added into blender and is pre-processed 0.4 times of diatomite quality
Binder is 55 DEG C in temperature, under conditions of revolving speed is 300r/min, after being stirred 40min, is granulated, must pre-process diatom
Soil matrix composite adsorbing material blank is forged under conditions of being 800 DEG C in temperature by pretreatment diatomite based composite adsorption material blank
After burning 2h, diatomite based composite adsorption material blank is obtained；By diatomite based composite adsorption material blank and composition metal salting liquid
The mixing of 1:12 in mass ratio, and silicon is added into the mixture of diatomite based composite adsorption material blank and composition metal salting liquid
The chitosan solution that 0.2 times of quality of diatomaceous earth based composite adsorption material blank, after impregnating 3h under room temperature, filtering obtains filter cake,
After filter cake is washed with deionized 10 times, under conditions of being 100 DEG C in temperature after dry 2h, diatom soil matrix composite adsorption material is obtained
Material.The alkyl glucoside quaternary ammonium compound is eight alkyl glucoside quaternary ammonium compounds.The preparation method of the pretreatment diatomite is by silicon
Diatomaceous earth crushes, and crosses 50 meshes, obtains pretreatment diatomite.The binder is the sodium silicate solution or quality that mass fraction is 40%
The attapulgite dispersion liquid that score is 40%.The composition metal salting liquid be calcium nitrate is mixed with water 1:12 in mass ratio, and
0.4 times of calcium nitrate quality of magnesium chloride is added, after being stirred, obtains composition metal salting liquid.The chitosan solution is that will take off
The chitosan of acetyl degree 85% is mixed with the glacial acetic acid 1:6 in mass ratio that mass fraction is 4%, obtains chitosan solution.
Aniline is mixed with dehydrated alcohol 2:10 in mass ratio, is 50 DEG C in temperature, under conditions of revolving speed is 300r/min, is stirred
After mixing dissolution 60min, aniline solution is obtained；Alkyl glucoside quaternary ammonium compound and water 1:12 in mass ratio are mixed in beaker, and to
4 times of alkyl glucoside quaternary ammonium compound quality of sodium bentonite and the six of 0.5 times of alkyl glucoside quaternary ammonium compound quality is added in beaker
Aluminium chlorohydrate, in temperature be 65 DEG C, revolving speed be 350r/min under conditions of, after being stirred to react 2h, by material in beaker in turn
Speed be 3000r/min under conditions of be centrifuged 20min after, filtering, obtain organobentonite blank, by organobentonite blank spend from
After sub- water washing 8 times, under conditions of being 110 DEG C in temperature after dry 2h, organobentonite is obtained；Aniline solution and graphene are pressed
Mass ratio 10:3 mixing obtains aniline mixture, by aniline mixture under conditions of frequency is 65kHz after ultrasonic disperse 50min
Mixed with organobentonite 5:2 in mass ratio, in temperature be 90 DEG C, revolving speed be 350r/min under conditions of, after being stirred to react 2h,
Filtering, obtains pre- modified alta-mud blank, after pre- modified alta-mud blank is washed with deionized 8 times, in temperature be 100 DEG C
Under the conditions of after dry 2h, obtain pre- modified alta-mud, pre- modified alta-mud and water 1:5 in mass ratio be mixed in flask, are used in combination
In the acetic acid adjusting flask that mass fraction is 8% after the pH to 6.8 of material, pre- modified alta-mud quality 0.05 is added into flask
Ferric trichloride again is 2 DEG C in temperature, and under conditions of revolving speed is 400r/min, after being stirred to react 3h, filtering obtains bentone
Sun-dried mud brick material after modified alta-mud blank is washed with water 10 times, under conditions of being 105 DEG C in temperature after dry 80min, obtains modification
Bentonite；Pretreatment diatomite and pre- modified alta-mud 3:1 in mass ratio are mixed in blender, and are added into blender
The binder of 0.4 times of diatomite quality of pretreatment is 55 DEG C in temperature, under conditions of revolving speed is 300r/min, is stirred
It after 40min, is granulated, diatomite based composite adsorption material blank must be pre-processed, diatomite based composite adsorption material base will be pre-processed
Expect in temperature be 800 DEG C under conditions of calcine 2h after, obtain diatomite based composite adsorption material blank；And to the compound suction of diatom soil matrix
The shell of 0.2 times of diatomite based composite adsorption material blank quality is added in the mixture of enclosure material blank and composition metal salting liquid
Glycan solution, after impregnating 3h under room temperature, filtering obtains filter cake, after filter cake is washed with deionized 10 times, is in temperature
Under conditions of 100 DEG C after dry 2h, diatomite based composite adsorption material is obtained.The alkyl glucoside quaternary ammonium compound is eight alkyl polysaccharides
Glycosides quaternary ammonium salt.The preparation method of the pretreatment diatomite is to crush diatomite, crosses 50 meshes, obtains pretreatment diatomite.Institute
Stating binder is the sodium silicate solution that mass fraction is 40% or the attapulgite dispersion liquid that mass fraction is 40%.The compound gold
Belonging to salting liquid is to mix calcium nitrate with water 1:12 in mass ratio, and 0.4 times of calcium nitrate quality of magnesium chloride is added, and is stirred
Afterwards, composition metal salting liquid is obtained.The chitosan solution is the ice vinegar for being 4% by the chitosan of deacetylation 85% and mass fraction
Acid 1:6 in mass ratio mixing, obtains chitosan solution.
Comparative example: the diatomite based composite adsorption material of Wuxi chemical materials production Co., Ltd production.
Example 1 to the resulting diatomite based composite adsorption material of example 4 and comparative example product are subjected to performance detection, specifically
Detection method is as follows:
Porosity is measured using mercury injection apparatus (Autopore9500)；And survey its specific surface area.Hole is measured when pressure is 500N
Rate.
It takes ground conical flask to number, accurately weighs 0.1g test specimen, 100mL potassium dihydrogen phosphate is injected into conical flask
Ground conical flask is sealed with preservative film, is placed in constant temperature oscillator by (phosphorus content 100mg/L, solution ph 7), control
25 DEG C of water temperature processed, oscillation rate 200rp/min, time of contact 12h, utilize the syringe separation adsorbate with filtering needle and examination
Part measures phosphorus content.
Specific testing result is as shown in table 1:
1 diatomite based composite adsorption material performance test results of table
By 1 testing result of table it is found that the diatomite based composite adsorption material of technical solution of the present invention preparation has excellent dephosphorization
The characteristics of effect and mechanical property, has broad prospects in the development of environment-friendly materials technology of preparing industry.
Claims (7)
1. a kind of preparation method of diatomite based composite adsorption material, which is characterized in that specific preparation step are as follows:
(1) alkyl glucoside quaternary ammonium compound is mixed with water 1:10~1:12 in mass ratio, and alkyl glucoside quaternary ammonium compound matter is added
2~4 times of sodium bentonite and 0.3~0.5 times of alkyl glucoside quaternary ammonium compound quality of Aluminium chloride hexahydrate are measured, is stirred to react
Afterwards, it is centrifuged, filters, wash, it is dry, obtain organobentonite；
(2) aniline solution is mixed with graphene 10:2~10:3 in mass ratio, after ultrasonic disperse, aniline mixture is obtained, by benzene
Amine blends are mixed with organobentonite 5:1~5:2 in mass ratio, after being stirred to react, are filtered, are washed, dry, and it is swollen to obtain pre- modification
Profit soil, pre- modified alta-mud is mixed with water 1:4~1:5 in mass ratio, and after adjusting pH to 6.5~6.8, pre- bentone is added
The ferric trichloride that 0.02~0.05 times of soil property amount, after being stirred to react, filtering washing is dry, obtains modified alta-mud；
(3) pretreatment diatomite is mixed with pre- modified alta-mud 2:1~3:1 in mass ratio, and it is diatomaceous that pretreatment is added
The binder of 0.2~0.4 times of amount, after being stirred, is granulated, and calcining obtains diatomite based composite adsorption material blank；
(4) diatomite based composite adsorption material blank is mixed with composition metal salting liquid 1:10~1:12 in mass ratio, and added
Enter 0.1~0.2 times of quality of diatomite based composite adsorption material blank of chitosan solution, impregnate, filter, washs, it is dry, obtain silicon
Diatomaceous earth based composite adsorption material.
2. a kind of preparation method of diatomite based composite adsorption material according to claim 1, it is characterised in that: step
(1) alkyl glucoside quaternary ammonium compound is any one in eight alkyl glucoside quaternary ammonium compounds or dodecane alkyl polyglucosides quaternary ammonium salt.
3. a kind of preparation method of diatomite based composite adsorption material according to claim 1, it is characterised in that: step
(2) aniline solution is to mix aniline with dehydrated alcohol 1:10~2:10 in mass ratio, and after stirring and dissolving, it is molten to obtain aniline
Liquid.
4. a kind of preparation method of diatomite based composite adsorption material according to claim 1, it is characterised in that: step
(3) preparation method of the pretreatment diatomite is to crush diatomite, crosses 50 meshes, obtains pretreatment diatomite.
5. a kind of preparation method of diatomite based composite adsorption material according to claim 1, it is characterised in that: step
(3) binder is the sodium silicate solution that mass fraction is 20~40% or the attapulgite that mass fraction is 25~40% dispersion
Liquid.
6. a kind of preparation method of diatomite based composite adsorption material according to claim 1, it is characterised in that: step
(4) the composition metal salting liquid is to mix calcium nitrate with water 1:10~1:12 in mass ratio, and calcium nitrate quality 0.2 is added
~0.4 times of magnesium chloride after being stirred, obtains composition metal salting liquid.
7. a kind of preparation method of diatomite based composite adsorption material according to claim 1, it is characterised in that: step
(4) chitosan solution be by the chitosan of deacetylation 70~85% and mass fraction be 2~4% glacial acetic acid in mass ratio
1:5~1:6 mixing, obtains chitosan solution.
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