CN102824898A - Three-dimensional porous pressure-resistant and expansion-limiting type bentonite adsorbing material and preparation method thereof - Google Patents
Three-dimensional porous pressure-resistant and expansion-limiting type bentonite adsorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a three-dimensional porous pressure-resistant and expansion-limiting type bentonite adsorbing material and a preparation method thereof. The preparation method comprises the following steps of: preparing intercalation carbonized bentonite: selecting bentonite, acrylic acid, an initiator and sodium hydroxide; under the protection of N2, heating raw materials in a water bath manner, and impregnating and intercalating; and adding an emulsifier and a cross-linking agent to carry out cross linkage, centrifugal washing and vacuum extracting, and then roasting and carbonizing to obtain the intercalation carbonized bentonite; and preparing the three-dimensional porous pressure-resistant and expansion-limiting type bentonite adsorbing material: selecting the intercalation carbonized bentonite, a cementing material, a foaming agent, a thickener, a water reducing agent and water to mix; and maintaining by hydrating and curing and crushing, making holes through dilute acid etching, filtering, washing and drying, so as to obtain the three-dimensional porous pressure-resistant and expansion-limiting type bentonite adsorbing material. The material composited by the invention has the advantages of good compatibility, easiness of solid-liquid separation, simple adsorbing process, low cost, and environmental friendless. The adsorbing material is porous, lyophobic and pressure-resistant, and can collaboratively adsorb metal ions and organic matter in sewage.
Description
Technical field
The present invention relates to a kind of novel bentonite sorbing material preparation technology, bloated type bentonite sorbing material of particularly a kind of three-dimensional porous resistance to compression limit and preparation method thereof.
Background technology
Absorption is to remove soluble heavy metal ions and organic common method in the sewage, and this method realizes through using sorbing material.Current, sorbing material commonly used has active carbon and clay mineral.
The charcoal absorption material has huge specific area because of it and good hole attitude distributes; Be widely used in extraordinary sewage or contain in the sewage disposal of the toxic organic compound that is difficult to handle with conventional method; In use the limitation of charcoal absorption material has 2 points; One of which is too high cost, has promoted the cost that water treatment is polluted; It two is the removal efficient that it is low excessively to heavy metal ion.These two drawbacks limit this sorbing material application with extensively promote.A kind of high-quality sorbing material safe, environmental protection, cheap and collaborative adsorb organic compound and heavy metal ion of market demand.
Big, the cheap environmental protection of clay class mineral reserves also has good absorption property concurrently and receives much concern; Become one of preferred material of Recent study and application; Particularly said material has a more modification function; Can carry out the specific aim modification according to the different adsorption process object, make it have better absorption property.Main clay mineral has bentonite, kaolinite, zeolite and diatomite etc.Wherein research the most extensively, the most everybody favor and be expected to that the marketization answers surely belong to bentonite mineral material.
Meet bentonite wastewater treatment preparation methods like the described a kind of organic and inorganic of Chinese patent ZL200410018109.Between bentonite bed, form hydroxy metal, effectively adsorbed phosphate radical and organic matter, and improved solid-liquid separation capability with the surface.
Like the graininess organic clay mixture of U.S. Pat 6093241 described a kind of oil removings from waste water, prescription relates to sepiolite, green sloping stone, quaternary compound and cement adhesive etc., and this sorbing material has the speciality of high-temperature stability.
Bentonite mineral material is a kind of high-quality sorbing material with high activity and high absorption property after purification and modification, and it is with a wide range of applications and application prospect in sewage disposal industry.But mainly there is following problem in this material in study on the modification and application: 1) solid-liquid separation difficulty.Can be known that by correlative study bentonitic grain diameter is more little, specific area and surface tension are big more, and its water treatment adsorption efficiency is high more; But grain diameter is more little, and the rate of settling of particle in liquid is slow more, the relative swellability of its particle bigger (about 10%), and both have all strengthened sedimentation, concentrate and the cost of technology such as dehydration.The way that addresses this problem now mainly contains two kinds, and the one, in the solid-liquid system, add flocculant; The 2nd, improve filter pressure, the former has introduced secondary pollution, and the latter has improved cost of investment.2) deep processing research is not enough.Current; The research of aspects such as adsorption effect the when researcher concentrates on surface modifier to the bentonite in treatment different sewage mostly and industry; Used bentonite material is traditional powdered granule, does not combine the research of raw material deep processing and bentonite modified both correlations.3) introduce secondary pollution.Because after the imbibition of bentonite sorbing material, it is the flocculation attitude, the strength of materials is extremely low, is stirring and is taking off and lose in the technology and will break, and under the bentonite granularity of cracking, sedimentation is extremely slow, in water treatment, has to adopt flocculant to remove these particles; No matter be organic flocculant, or inorganic flocculating agent all can be dissolved in the middle of the water body, like this, causes the rising of cost of water treatment, and has introduced secondary pollution.4) absorption poor compatibility.The pollutant that sorbing material is handled in the water body is broadly divided into two types, i.e. metal ion and harmful organic substance.Metal ion and harmful organic substance are of a great variety separately, and the tool relevant report is when adopting bentonite modified adsorbing metal ions or harmful organic substance; The bentonite that a kind of modification and modification arranged is effective 1 ~ 2 kind of harmful substance in the adsorbed water only, so, to the water body that polluted by multiple harmful substances; With the bentonite after multiple being modified of use; Like this, cause the complicated of water treatment technology, improved cost; This also is that bentonite had not replaced active carbon always and is used for one of reason of water body treating.
Summary of the invention
Technical problem to the existence in research and application of bentonite mineral material; The objective of the invention is to prepare a kind of novel water treatment sorbing material; The present invention selects through specific prescription design and processes parameter, and preparation synthesizes a kind ofly has favorable compatibility, be easy to Separation of Solid and Liquid, absorbing process is simple, three-dimensional resistance to compression limit with low cost, eco-friendly expands type bentonite porous adsorbing material.This sorbing material has porous, hydrophobic, withstand voltage material behavior and can work in coordination with simultaneously and adsorbs metal ion and organic functional characteristic in the sewage.
The objective of the invention is to realize through following technical proposals.
The bloated type bentonite sorbing material of a kind of three-dimensional porous resistance to compression limit, this material is prepared from following weight percentages:
Intercalation charing bentonite 40-75%; Binder Materials 10-20%; Blowing agent 3%; Thickener 1%; Water reducer 1%; Water 10-45%.
Further, in the said material:
Said Binder Materials is portland cement or sulfate cement.
Said blowing agent is ammonium nitrate, ammonium carbonate or sodium acid carbonate.
Said thickener is a CMC.
Said water reducer is sodium lignin sulfonate, melamino-formaldehyde condensation polymer or sulfanilate-sulfonated acetone-formaldehyde condensation products.
Said intercalation charing bentonite is prepared from following weight percentages:
Bentonite 10-20%; Distilled water 60-75%; Acrylic acid 3-8%; Initator 0.03%; NaOH 9-12%; Emulsifying agent 0.05%; Crosslinking agent 0.02%.
Said initator is potassium peroxydisulfate or ammonium persulfate.
Said emulsifying agent is Span60 or Span80.
Said crosslinking agent is N, the N-methylene-bisacrylamide.
Correspondingly, the present invention gives the preparation method of the bloated type bentonite sorbing material of a kind of three-dimensional porous resistance to compression limit, comprises the steps:
The first step, the bentonitic preparation of intercalation charing:
Choose percentage by weight and be 10-20% bentonite, 60-75% distilled water, 3-8% acrylic acid, 0.03% initator, 9-12% NaOH mixes in container; At N
2Protection down, 40-50 ℃ of water-baths heating 1-2h flood, intercalation; Add 0.05% emulsifying agent again and carry out emulsion polymerization; Add 0.02% crosslinking agent then at 30-50 ℃ of crosslinked 1-2h; After centrifuge washing, vacuum extraction, 400-600 ℃ of charing 1-3h in roaster take out and are cooled to room temperature, promptly make intercalation charing bentonite then;
The preparation of second step, the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit:
Choose percentage by weight and be the intercalation charing bentonite that 40-75% step 1 is produced; 10-20% Binder Materials, 3% blowing agent, 1% thickener; 1% water reducer; 10-45% water is mixed with into the porous block material, is 22-30 ℃ in temperature, hydration and hardening maintenance 72-96h under the condition of humidity 95%; With the porous block material pulverize, 200 orders sieve, will sieve down particulate material in concentration is 1% dilute acid soln; At 25 ℃ of following etching drilling 8-10h; Filter out solid particle; To the PH=6 that filtrates-7, the solid particle after the washing is dried 24-36h down for 105-120 ℃ in temperature with distilled water wash solids particle, promptly get the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit.
Further, in the said method, dilute acid soln is hydrochloric acid, dilute sulfuric acid or p-methyl benzenesulfonic acid.
The present invention has following beneficial effect with respect to preparation technology, prescription design and the application etc. of existing bentonite composite material:
1), three-dimensional porousization design
Adopt the three-dimensional porousization bentonite material of " template " and " foaming " preparation, 80% is the mesopore of aperture≤50nm, through later stage etching and activation, estimates that the micropore of aperture≤2nm will reach 60%.
2), the crosslinked charing modification of intercalation
The molecule quantitative change of the crosslinked back of interlayer intercalation polymeric thing is big, and heavy polymer can effectively strut bentonitic interlamellar spacing, from pore structure possibility is provided for bentonite is adsorbed with very big molecule; The bentonite that exists with the granular powder state becomes oleophilic drainage in the surface after the crosslinked charing of intercalation, can improve the adsorption capacity of bentonite to organic matter.
3), micropore etching
There is slightly 25% Ca (OH) in the silicate gel material
2Crystal, entringite and aquation gelinite, Ca (OH)
2Crystal and entringite are displaced a large amount of micropore (about 1.25nm) by sour stripping, are distributed in Ca in the aquation gelinite (OH)
2Crystal be dissolved with entringite after, the aquation gelinite is island shape structure, the centre will interconnect, thereby form netted three-dimensional porous sorbing material.
4), absorption is compatible
Bentonite and carbonated material all have suction-operated to organic matter in the water or metal ion, bentonite since its strong hydrophilicity and minimum interlamellar spacing size absorbing aspect the metal ion because carbonated material; On the contrary, carbonated material is selected the compound of carbonated material and bentonite material because its good oleophylic performance has better suction-operated to organic molecule, can bring into play both characteristics, can absorb organic matter and metal ion in the water simultaneously.
5), " original position " expands
The bentonite imbibition is one of its important attribute; It is the difficult scientific problems that water treatment runs into that the back solid-liquid that expands separates always, and the present invention adopts the means of composite porous design, makes bentonite when the absorption suction; " original position " expands; Do not drift about, the passage of can shutoff liquid not flowing through, thus improved filter efficiency.
6), adsorb big molecule
Silicate-base porous material and hole, charcoal Quito material all exist many connection mesopores (omiting 30%), adsorbable a large amount of organic macromolecule.
7), resistance to compression design
The three-dimensional porous sorbing material design compression strength >=5Mpa of the present invention's preparation has certain crushing resistance and resistance to deformation ability.When material carried out Separation of Solid and Liquid, there was barometric gradient in the sorbing material two ends, if the pressure resistance of material is spent when hanging down; Material itself will be out of shape, and the material after the distortion is with densification, and bulk density raises; Porosity descends, and absorption and liquid communication ability reduce, and filtering rate reduces as a result; The material body distortion that produces because of pressure differential when the present invention can avoid filtering through the resistance to compression design of material does not influence filtering rate, does not influence the adsorption efficiency of material.
Description of drawings
Fig. 1 is a bentonite synthesis process of prepolymer flow chart of the present invention.
Fig. 2 is the preparation flow figure of the three-dimensional porous sorbing material of silicate of the present invention.
The specific embodiment
Below in conjunction with accompanying drawing and embodiment bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit of the present invention and preparation method are made detailed description.
In the preparation of the crosslinked charing modified alta-mud of first step intercalation of the present invention material
1) raw material is chosen
Bentonite (industrial goods), acrylic acid (technical pure), potassium peroxydisulfate (analyzing pure), ammonium persulfate (analyzing pure), NaOH (analyzing pure), N, N '-methylene-bisacrylamide (analyzing pure), nitrogen; Span60 (analyzing pure), Span80 (analyzing pure), distilled water (analyzing pure).
2) preparation technology
It is bentonitic pillared modification monomer that acrylic acid is selected in experiment for use, and persulfate is an initator, and Span60 or Span80 are emulsifying agent, and distilled water is solvent, at N
2Under the protection, the synthetic polyacrylic acid of method of emulsion polymerization is adopted in the water-bath heating, after polyacrylic acid reaches certain degree of polymerization, drips crosslinking agent N, N-methylene-bisacrylamide, the polyacrylic acid of formation crosslinking netization between bentonite bed; After unnecessary monomer in acrylic acid top layer and solvent are removed in washing, extracting, it being carried out charing handles.Through above step, prepare polyacrylic acid modified intercalation charing bentonite material at last.The bentonite synthesis process of prepolymer is shown in accompanying drawing 1.
3), preparation principle
Preparation intercalation charing bentonite material relates generally to solution adsorption and diffusion mechanism, acid activation mechanism, ion-exchange mechanism, mechanism of polymerization or the like.
Bentonite has very strong absorption property, can adsorbs propylene acid, and acrylic acid solution can ionization go out H between bentonite bed
+To solution is acid, but the acid solution activated bentonite.Acid activation is handled can remove the impurity that is distributed in bentonite micropore or interlayer, as the organic matter that mixes, and the duct obtains mediation, the diffusion that helps adsorbing the object minuteness particle.Moreover, H
+Ionic radius is less than Na
+, Mg
2+, K
+, Ca
2+Isoionic radius, so the little H of volume
+Na between the ion exchange bentonite bed
+, Mg
2+, K
+, Ca
2+Behind the plasma, the aperture increases, and has weakened the bonding force between original layer; Layer winding is broken off; Montmorillonite inside connects with hydrogen bond between them along with cationic removal in the octahedron has formed as the same exposed surface of solid acid effect, has stronger chemism, adsorptivity and catalytic.And when acroleic acid polymerization reacted, because of its degree of neutralization has only 75%, so reaction system is acid, and the sodium bentonite particulate was positively charged under sour environment.According to the charges of different polarity principle that attracts each other, think that structural carboxylic acid group of functional group of bentonite particulate and molecular network or amide groups draw each other and adhere on the macromolecule network structure.
Can be through XRD to bentonite d
001The crystal face diffraction maximum is measured, with Bragg formula computation layer spacing d
001The microstructure and the charing degree of the water through TG, dsc analysis intercalation carbonated material characterize; Automatically physical adsorption appearance is measured N
2Adsorption isotherm; Calculate the sample specific area through the BET method; Thereby porosity, pore structure and distribution to material describe, through the microstructure of TEM or SEM bentonite internal crosslinking directly perceived carbonated material, and the connected mode between carbonated material and bentonite lamella.
Can reach following 3 purposes through the crosslinked charing modified alta-mud of intercalation material: first; The molecule quantitative change of the crosslinked back of interlayer intercalation polymeric thing is big; Heavy polymer can effectively strut bentonitic interlamellar spacing, from pore structure possibility is provided for bentonite is adsorbed with very big molecule; The second, the adsorbable small organic molecule of microcosmic pore structure and the metal ion of charing; The 3rd; The bentonite that exists with the granular powder state becomes oleophilic drainage in the surface after the crosslinked charing of intercalation; When follow-up water environment prepares three-dimensional porous sorbing material, its surface will form hydrated films, after three-dimensional porous material aquation (silicate-base) or the curing (high polymer base); Hydrated films disappears; To form hole between matrix and modified alta-mud particle, in case be wrapped in matrix material around the modified particles material after etching, activation processing, matrix material and material modified have just formed intercommunicating pore.
Second step: the preparation of the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit
1) raw material is chosen
The crosslinked charing modified alta-mud of intercalation material (material of first step preparation according to the invention); Portland cement or sulfate cement (PC32.5 or PC42.5 or PC52.5); Water reducer sodium lignin sulfonate, melamino-formaldehyde condensation polymer or sulfanilate-sulfonated acetone-formaldehyde condensation products (technical pure), methylol is newly tieed up element (technical pure); Blowing agent ammonium nitrate, ammonium carbonate or sodium acid carbonate (purity 99.5%, 200 orders, commercially available); Sulfuric acid (analyzing pure); Hydrochloric acid (analyzing pure); P-methyl benzenesulfonic acid (analyzing pure).
2) preparation technology
Be matrix with the Binder Materials, mix raw materials such as blowing agent, thickener, the crosslinked charing modified alta-mud of intercalation and running water and be mixed with by a certain percentage and produce three-dimensional porous sorbing material; Adopt semi-dry pressing to make block porous material; This porous material is behind maintenance, gel, hydration and hardening; Pulverize, sieve, classification; Three-dimensional porous sorbing material after utilizing certain density acid to classification again carries out etching, and is last, after the granular materials after the distilled water washing etching, oven dry, makes the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit.
Technological process is shown in accompanying drawing 2.
3), preparation principle
Prepare the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit and relate to the cement based hydration mechanism, acid-base neutralization reaction mechanism, metal and alkali replacement mechanism etc.Be mainly reflected in two aspects: on the one hand, control mesopore (2nm ~ 50nm) and the porosity of macropore of material through the ratio of regulating foaming agent consumption, water and cement; On the other hand, generate the island gelinite during silicate cement hydration, the Ca (OH) of even distribution about 25% in the middle of the gelinite
2Crystal, size zero point several nanometers between the dozens of nanometer; Ca (OH)
2With inorganic acid (like H
2SO
4, H
3PO
5, H
2CO
3Deng) or organic acid (like oxalic acid, acetate, ethanedioic acid etc.) reaction generation soluble-salt, displacing netted micropore between silicate layer, these interlayer micropores can have good suction-operated to metal ion, and modified alta-mud is wrapped in the grid, as Ca (OH)
2After crystal is dissolved, modified alta-mud interlayer micropore and extraneous porosity communication, bentonitic interlayer adsorption capacity obtains discharging.Adopt automatic physical adsorption appearance to measure N
2Adsorption isotherm; Calculate the sample specific area through the BET method; Microscopic appearance with the sem observation sample; The x-ray diffractometer amalyzing substances is formed; With universal material mechanical test appearance test material mechanical property.
Further specify the present invention through specific embodiment below.
Embodiment 1
The first step, the bentonitic preparation of intercalation charing:
Choose percentage by weight and be 10% bentonite, 75% distilled water, 3% acrylic acid, 0.03% potassium peroxydisulfate, 11.9% NaOH mixes in container; At N
2Protection down, 40 ℃ of water-baths heating 2h flood, intercalation; Add 0.05% Span60 emulsifying agent again and carry out emulsion polymerization; Add 0.02% N then, the N-methylene-bisacrylamide is at 30 ℃ of crosslinked 2h; After centrifuge washing, vacuum extraction, 400 ℃ of charing 3h in roaster take out and are cooled to room temperature, promptly make intercalation charing bentonite then;
The preparation of second step, the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit:
Choose percentage by weight and be the intercalation charing bentonite that 45% step 1 is produced; 20% portland cement, 3% ammonium nitrate, 1% CMC; 1% sodium lignin sulfonate; 30% running water is mixed with into the porous block material, is 22 ℃ in temperature, hydration and hardening maintenance 96h under the condition of humidity 95%; With the porous block material pulverize, 200 orders sieve, will sieve down particulate material in concentration is 1% dilute hydrochloric acid solution; At 25 ℃ of following etching drilling 9h; Filter out solid particle; To the PH=6 that filtrates-7, the solid particle after the washing is dried 36h down for 105 ℃ in temperature with distilled water wash solids particle, promptly get the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit.
Embodiment 2
The first step, the bentonitic preparation of intercalation charing:
Choose percentage by weight and be 16.5% bentonite, 68.8% distilled water, 5.5% acrylic acid, 0.03% ammonium persulfate, 9.1% NaOH mixes in container; At N
2Protection down, 40 ℃ of water-baths heating 1.5h flood, intercalation; Add 0.05% Span80 emulsifying agent again and carry out emulsion polymerization; Add 0.02% N then, the N-methylene-bisacrylamide is at 40 ℃ of crosslinked 1.5h; After centrifuge washing, vacuum extraction, 500 ℃ of charing 2h in roaster take out and are cooled to room temperature, promptly make intercalation charing bentonite then;
The preparation of second step, the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit:
Choose percentage by weight and be the intercalation charing bentonite that 40% step 1 is produced; 10% sulfate cement, 3% ammonium carbonate, 1% CMC; 1% melamino-formaldehyde condensation polymer; 45% running water is mixed with into the porous block material, is 25 ℃ in temperature, hydration and hardening maintenance 72h under the condition of humidity 95%; With the porous block material pulverize, 200 orders sieve, will sieve down particulate material in concentration is 1% dilution heat of sulfuric acid; At 25 ℃ of following etching drilling 8h; Filter out solid particle; To the PH=7 that filtrates, the solid particle after the washing is dried 24h down for 105 ℃ in temperature with distilled water wash solids particle, promptly get the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit.
Embodiment 3
The first step, the bentonitic preparation of intercalation charing:
Choose percentage by weight and be 20% bentonite, 60% distilled water, 7.9% acrylic acid, 0.03% potassium peroxydisulfate, 12% NaOH mixes in container; At N
2Protection down, 50 ℃ of water-baths heating 1h flood, intercalation; Add 0.05% Span60 emulsifying agent again and carry out emulsion polymerization; Add 0.02% N then, the N-methylene-bisacrylamide is at 50 ℃ of crosslinked 1h; After centrifuge washing, vacuum extraction, 600 ℃ of charing 1h in roaster take out and are cooled to room temperature, promptly make intercalation charing bentonite then;
The preparation of second step, the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit:
Choose percentage by weight and be the intercalation charing bentonite that 75% step 1 is produced; 10% portland cement, 3% sodium acid carbonate, 1% CMC; Sulfanilate-sulfonated acetone of 1%-formaldehyde condensation products; 10% running water is mixed with into the porous block material, is 30 ℃ in temperature, hydration and hardening maintenance 48h under the condition of humidity 95%; With the porous block material pulverize, 200 orders sieve, will sieve down particulate material in concentration is 1% p-methyl benzenesulfonic acid solution; At 25 ℃ of following etching drilling 10h; Filter out solid particle; To the PH=7 that filtrates, the solid particle after the washing is dried 48h down for 120 ℃ in temperature with distilled water wash solids particle, promptly get the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit.
Above embodiment only is used to explain the present invention; And be not limitation of the present invention; The those of ordinary skill in relevant technologies field under the situation that does not break away from the spirit and scope of the present invention, can also be made various variations and distortion; Therefore all technical schemes that are equal to also belong to category of the present invention, and scope of patent protection reason claim of the present invention limits.
Claims (10)
1. the type bentonite sorbing material that expands is limit in a three-dimensional porous resistance to compression, it is characterized in that this material is prepared from following weight percentages:
Intercalation charing bentonite 40-75%;
Binder Materials 10-20%;
Blowing agent 3%;
Thickener 1%;
Water reducer 1%;
Water 10-45%.
2. the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit according to claim 1 is characterized in that said Binder Materials is portland cement or sulfate cement.
3. the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit according to claim 1 is characterized in that said blowing agent is ammonium nitrate, ammonium carbonate or sodium acid carbonate; Said thickener is a CMC.
4. the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit according to claim 1 is characterized in that said water reducer is sodium lignin sulfonate, melamino-formaldehyde condensation polymer or sulfanilate-sulfonated acetone-formaldehyde condensation products.
5. the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit according to claim 1 is characterized in that said intercalation charing bentonite is prepared from following weight percentages:
Bentonite 10-20%;
Distilled water 60-75%;
Acrylic acid 3-8%;
Initator 0.03%;
NaOH 9-12%;
Emulsifying agent 0.05%;
Crosslinking agent 0.02%.
6. the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit according to claim 5 is characterized in that said initator is potassium peroxydisulfate or ammonium persulfate.
7. the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit according to claim 5 is characterized in that said emulsifying agent is Span60 or Span80.
8. the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit according to claim 5 is characterized in that said crosslinking agent is N, the N-methylene-bisacrylamide.
9. the preparation method based on the bloated type bentonite sorbing material of the described three-dimensional porous resistance to compression limit of claim 1 is characterized in that this method comprises the steps:
The first step, the bentonitic preparation of intercalation charing:
Choose percentage by weight and be 10-20% bentonite, 60-75% distilled water, 3-8% acrylic acid, 0.03% initator, 9-12% NaOH mixes in container; At N
2Protection down, 40-50 ℃ of water-baths heating 1-2h flood, intercalation; Add 0.05% emulsifying agent again and carry out emulsion polymerization; Add 0.02% crosslinking agent then at 30-50 ℃ of crosslinked 1-2h; After centrifuge washing, vacuum extraction, 400-600 ℃ of charing 1-3h in roaster take out and are cooled to room temperature, promptly make intercalation charing bentonite then;
The preparation of second step, the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit:
Choose percentage by weight and be the intercalation charing bentonite that the step 1 of 40-75% is produced; The Binder Materials of 10-20%, 3% blowing agent, 1% thickener; 1% water reducer; The water of 10-45% is mixed with into the porous block material, is 22-30 ℃ in temperature, hydration and hardening maintenance 72-96h under the condition of humidity 95%; With the porous block material pulverize, 200 orders sieve, will sieve down particulate material in concentration is 1% dilute acid soln; At 25 ℃ of following etching drilling 8-10h; Filter out solid particle; To the PH=6 that filtrates-7, the solid particle after the washing is dried 24-36h down for 105-120 ℃ in temperature with distilled water wash solids particle, promptly get the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit.
10. the preparation method of the bloated type bentonite sorbing material of three-dimensional porous resistance to compression limit according to claim 9 is characterized in that said dilute acid soln is hydrochloric acid, dilute sulfuric acid or p-methyl benzenesulfonic acid.
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| WO2017206579A1 (en) * | 2016-05-31 | 2017-12-07 | 成都新柯力化工科技有限公司 | Graphene micro-sheet having mesh structure and preparation method therefor |
| CN109012642A (en) * | 2018-09-08 | 2018-12-18 | 佛山市森昂生物科技有限公司 | A kind of preparation method of diatomite based composite adsorption material |
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| CN110681371A (en) * | 2019-09-26 | 2020-01-14 | 浙江海洋大学 | Preparation method of natural adsorbent for removing heavy metal ions |
| CN110681360A (en) * | 2019-09-11 | 2020-01-14 | 浙江海洋大学 | Preparation method of natural adsorbent for treating landfill leachate |
| WO2020253271A1 (en) * | 2019-06-21 | 2020-12-24 | 南京云香纳米技术有限公司 | Harmful gas removing medium and preparation method therefor |
| CN114669271A (en) * | 2022-03-21 | 2022-06-28 | 西南石油大学 | Preparation method of efficient, durable, high-temperature-resistant and high-pressure-resistant oil-water separation material |
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| CN103055824A (en) * | 2013-01-07 | 2013-04-24 | 河北工业大学 | Calcium bentonite -AA- (AA-Na) composite cadmium ion adsorbent |
| WO2017206579A1 (en) * | 2016-05-31 | 2017-12-07 | 成都新柯力化工科技有限公司 | Graphene micro-sheet having mesh structure and preparation method therefor |
| CN106669640A (en) * | 2016-11-16 | 2017-05-17 | 西安科技大学 | Polyaniline modified bentonite nano-microsphere adsorption material and preparation method thereof |
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| CN107017476A (en) * | 2017-02-23 | 2017-08-04 | 宁波高新区远创科技有限公司 | A kind of preparation method of the special friction reducer of lightning protection engineering |
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