CN104085898B - Method of preparing tubular clay by polar polymer intercalation - Google Patents
Method of preparing tubular clay by polar polymer intercalation Download PDFInfo
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- CN104085898B CN104085898B CN201410330738.4A CN201410330738A CN104085898B CN 104085898 B CN104085898 B CN 104085898B CN 201410330738 A CN201410330738 A CN 201410330738A CN 104085898 B CN104085898 B CN 104085898B
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- clay
- mud
- tubulose
- intercalation
- slurry
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- Compositions Of Macromolecular Compounds (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
- Preparation Of Clay, And Manufacture Of Mixtures Containing Clay Or Cement (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention relates to a method of preparing tubular clay by polar polymer intercalation and belongs to the field of functional ceramic materials. The clay used by the functional ceramic material is Suzhou soil which mainly comprises mineral compositions of millite and kaolinite; the intercalator is polar low molecular polyacrylic acid, of which the viscosity average molecular weigh is 1800-2400g/mol and the additive amount is 0.5-1wt%. The preparation method comprises the following steps: weighing a certain amount of Suzhou soil and mixing with a proper amount of distilled water to obtain slurry, wherein the distilled water is weighed in a mass ratio of distilled water to clay of 1 to 1; adding 0.5-1wt% of stronger ammonia water based on mass of slurry, wherein the mass fraction of NH3 in stronger ammonia water is 25.0-28.0%; pouring into a ball mill tank to grind for 12 hours; then, adding 0.5-1wt% of polyacrylic acid based on mass of slurry, and grinding for 24 hours to obtain intercalated slurry; grinding the intercalated slurry by a millstone mill for 1 hour; then, drying and dispersing to obtain the dry powder tubular clay. The clay provided by the invention can be used as a harmful substance adsorbent, a clarifying agent for turbid water and a sealant for radioactive wastes and toxic materials and has important meaning in the field of environmental protection, water safety and the like.
Description
Technical field
The invention belongs to ceramic material field, and in particular to a kind of polar polymer intercalation prepares the side of tubulose clay
Method.
Technical background
The industry such as textile printing and dyeing, papermaking, plastics and leather all produces substantial amounts of waste water from dyestuff every year, because many dyestuffs are
Complicated organic matter containing azo bond, poly aromatic rings, can teratogenesis, carcinogenic, mutagenesis, therefore, the removal of this kind of Wastewater Dyes
It is extremely important.Many dyestuffs are anti-oxidant, difficult degradation, have greater advantage using the dyestuff in adsorbent removal waste water.Activated carbon
It is a kind of effective adsorbent, but it is expensive, limit its extensive use.
Clay mineral has the characteristics such as adsorptivity, ion exchangeable, dispersiveness, in terms of environmental improvement, clay pit with it
Thing can be used as noxious substance agent, the fining agent of muddy water, sealant of radioactive waste and poisonous material etc..But, glue
Adsorptivity, ion exchangeable, dispersiveness of soil particle etc. are influenceed very big by clay particle microscopic appearance.And natural clay mineral its
More than the microscopic appearance of particle in the form of sheets, it is bar-shaped, particle size is generally tens microns, limit clay in environmental improvement should
With.
The present invention is by the working process to natural clay mineral, increasing specific surface area, reduction particle size, change particle
Pattern etc., obtains high adsorption, macroion exchangeability, the tubulose clay of polymolecularity, and the tubulose clay is in environmental protection and water
The fields such as purified treatment have a good application prospect.
The content of the invention
It is an object of the invention to be directed to the deficiency that natural clay is applied in environmental improvement, there is provided a kind of high-ratio surface
The preparation method of long-pending, low particle diameter, the tubulose clay of high absorption property.
Technical scheme is with technical characteristic：
It is intercalation object with clay, intercalator is polar low molecular polyacrylic acid, and polyacrylic acid viscosity average molecular weigh is 1800
~2400g/mol, addition are ‰~10wt of 5wt ‰, weigh a certain amount of Suzhou soil and are mixed into mud with appropriate distilled water, are steamed
The amount of distilled water is pressed with clay mass ratio as measure at 1: 1, adds the concentrated ammonia liquor of the ‰~10wt of 5wt ‰ of quality of mud fluid to pour into ball grinder
In mill 12h.The polyacrylic acid for adding the ‰~10wt of 5wt ‰ of quality of mud fluid obtains intercalation mud through the 24h that mills, using disk
Mill mills 1h intercalation mud, then dry powder tubulose clay is obtained after drying and dispersion.
Clay used is with raw clay that kaolinite and illite are main mineral composition.
Concentrated ammonia liquor used is the ‰~10wt of 5wt ‰ of quality of mud fluid, NH3 mass fractions content 25.0% in concentrated ammonia liquor~
28.0%.
Low-molecular polypropylene acid viscosity average molecular weigh used is 1800~2400g/mol.
5~20 μm of the length of obtained tubulose clay, 100~200nm of diameter.
Specific embodiment
Embodiment 1
Selection is intercalation object with the Suzhou soil that illite and kaolinite are main mineral composition, weighs 150g Suzhou soils,
150ml distilled water is measured, the amount of distilled water is pressed with clay mass ratio as measure at 1: 1, in addition ball grinder.It is guiding with ammoniacal liquor
Agent, measures 1.5ml concentrated ammonia liquors, in concentrated ammonia liquor, NH3Mass fraction is content 25.0%~28.0%, pours into ball grinder and mills
12h obtains mud, weighs the polyacrylic acid that 2g viscosity average molecular weighs are 1800g/mol and pours into ball grinder, then the 24h that mills is inserted
Layer mud, using mill by the 1h that milled in intercalation mud, then obtains dry powder tubulose clay after drying and dispersion.
, through laser particle size analysis, clay particle differential volume median particle diameter is in 5.60 μm, differential volume peak for the tubulose clay
Value particle diameter is 4.05 μm；Scanned electronic microscope photos and projection electronic microscope photos, length is 5~10 μm, directly more than clay particle in a tubular form
100~150nm of footpath.And the blank sample without intercalation processing, clay particle differential volume median particle diameter at 13.08 μm, differential
Volumetric peak particle diameter is 34.58 μm；Scanned electronic microscope photos and projection electronic microscope photos, many stratiforms of clay particle, particle size is
30~50 μm.Therefore the method can effectively reduce clay particle diameter, form the effect of tubular structure.
Embodiment 2
Selection is intercalation object with the Suzhou soil that illite and kaolinite are main mineral composition, weighs 150g Suzhou soils,
150ml distilled water is measured, the amount of distilled water is pressed with clay mass ratio as measure at 1: 1, in addition ball grinder.It is guiding with ammoniacal liquor
Agent, measures 1.5ml concentrated ammonia liquors, in concentrated ammonia liquor, NH3Mass fraction is content 25.0%~28.0%, pours into ball grinder and mills
12h obtains mud, weighs the polyacrylic acid that 2g viscosity average molecular weighs are 2400g/mol and pours into ball grinder, then the 24h that mills is inserted
Layer mud, using mill by the 1h that milled in intercalation mud, then obtains dry powder tubulose clay after drying and dispersion.
, through laser particle size analysis, clay particle differential volume median particle diameter is in 9.03 μm, differential volume peak for the tubulose clay
Value particle diameter is 5.37 μm；Scanned electronic microscope photos and projection electronic microscope photos, length is 8~15 μm, directly more than clay particle in a tubular form
130~200nm of footpath.Compare with the blank sample without intercalation processing, the method can effectively reduce clay particle diameter, form tubulose knot
The effect of structure.And with intercalator molecular weight for 1800g/mol samples are contrasted, intercalator molecular weight is to clay particle particle diameter and tubulose
Structure has a significant effect, and intercalator viscosity average molecular weigh is advisable for 1800g/mol.
Embodiment 3
Selection is intercalation object with the Suzhou soil that illite and kaolinite are main mineral composition, weighs 150g Suzhou soils,
150ml distilled water is measured, the amount of distilled water is pressed with clay mass ratio as measure at 1: 1, in addition ball grinder.It is guiding with ammoniacal liquor
Agent, measures 1.5ml concentrated ammonia liquors, in concentrated ammonia liquor, NH3Mass fraction is content 25.0%~28.0%, pours into ball grinder and mills
12h obtains mud, weighs the polyacrylic acid that 3g viscosity average molecular weighs are 1800g/mol and pours into ball grinder, then the 24h that mills is inserted
Layer mud, using mill by the 1h that milled in intercalation mud, then obtains dry powder tubulose clay after drying and dispersion.
, through laser particle size analysis, clay particle differential volume median particle diameter is in 5.89 μm, differential volume peak for the tubulose clay
Value particle diameter is 4.43 μm；Scanned electronic microscope photos and projection electronic microscope photos, length is 10~20 μm more than clay particle in a tubular form,
150~200nm of diameter.Compare with the blank sample without slotting treatment, the method can effectively reduce clay particle diameter, form tubulose knot
The effect of structure.And be 2g with intercalator addition, intercalator addition is contrasted for the sample of 5wt ‰, and intercalator addition is to right
Clay particle particle diameter and tubular structure have a significant effect, and intercalator addition is advisable for 5wt ‰.
Embodiment 4
Selection is intercalation object with the Suzhou soil that illite and kaolinite are main mineral composition, weighs 150g Suzhou soils,
150ml distilled water is measured, the amount of distilled water is pressed with clay mass ratio as measure at 1: 1, in addition ball grinder.It is guiding with ammoniacal liquor
Agent, measures 1.5ml concentrated ammonia liquors, in concentrated ammonia liquor, NH3Mass fraction is content 25.0%~28.0%, pours into ball grinder and mills
12h obtains mud, weighs the polyacrylic acid that 2g viscosity average molecular weighs are 1800g/mol and pours into ball grinder, then the 24h that mills is inserted
Layer mud, using mill by the 1h that milled in intercalation mud, then obtains dry powder tubulose clay after drying and dispersion.
The tubulose clay, through the test of cation exchange specific surface area and volume test, test result is：Tubulose clay always than
Surface area is 220m2/ g, cation exchange capacity is 86.3 milliequivalents/100g.And without the blank sample of slotting treatment, always than
Surface area is 135m2/ g, cation exchange capacity is 59.6 milliequivalents/100g.Contrasted with the blank sample without slotting treatment,
Tubulose clay its total specific surface area being obtained through intercalation processing and improve 63%, cation exchange capacity improves 45%, it is seen that
The total specific surface area and cation exchange capacity for obtaining tubulose clay through intercalation processing are significantly improved.
Claims (4)
1. a kind of method that polar polymer intercalation prepares tubulose clay, it is characterised in that with principal component as illite and kaolinite
Clay be intercalation object, in clay essential mineral composition for kaolinite content be 70wt%~80wt%, illite content is
5wt%~10wt%, other compositions are 10wt%~25wt%, and particle diameter is 30~50 μm, is with polar low molecular polyacrylic acid
Intercalator, the preparation method of the tubulose clay is comprised the following steps：Slurrying；Clay intercalated treatment；Machine-shaping；Dry and divide
Dissipate；
The method of clay intercalated treatment be by viscosity average molecular weigh for 1800g/mol polyacrylic acid by quality of mud fluid 5wt ‰~
10wt ‰ is added in mud, then by mud in ball mill ball milling 24h, obtain intercalation clay mud；
The scattered method of drying be by tubulose clay mortar in toasting 12h at 80 DEG C, then through ball milling 1h, obtain length of tube be 5~
20 μm, the tubulose clay of a diameter of 100~200nm.
2. the method that a kind of polar polymer intercalation as claimed in claim 1 prepares tubulose clay, it is characterised in that pole used
Property low-molecular polypropylene acid viscosity average molecular weigh be 1800g/mol, addition for quality of mud fluid ‰~10wt of 5wt ‰.
3. the method that a kind of polar polymer intercalation as claimed in claim 1 prepares tubulose clay, it is characterised in that mud system
Standby method be clay account for the 49.5wt%~49.75wt% of quality of mud fluid, distilled water account for the 49.5wt% of quality of mud fluid~
49.75wt%, ammoniacal liquor account for the ‰~10wt of 5wt ‰ of quality of mud fluid, and NH3 mass fractions content 25.0wt% in ammoniacal liquor~
28.0wt%, above-mentioned three kinds of raw materials are milled 12h in ball mill.
4. the method that a kind of polar polymer intercalation as claimed in claim 1 prepares tubulose clay, it is characterised in that be processed into
The method of type is that intercalation mud is milled 1h through mill, obtains tubulose clay mortar.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410330738.4A CN104085898B (en) | 2014-07-08 | 2014-07-08 | Method of preparing tubular clay by polar polymer intercalation |
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|---|---|---|---|
| CN201410330738.4A CN104085898B (en) | 2014-07-08 | 2014-07-08 | Method of preparing tubular clay by polar polymer intercalation |
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| CN104085898B true CN104085898B (en) | 2017-05-24 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401566A (en) * | 2002-09-24 | 2003-03-12 | 华南理工大学 | Intercalation type or amorphous kaoline and preparing process thereof |
| CN103880032A (en) * | 2014-04-13 | 2014-06-25 | 北京化工大学 | Thiourea intercalation modified kaolin and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7273899B2 (en) * | 2002-09-25 | 2007-09-25 | Eastman Kodak Company | Materials and method for making splayed layered materials |
| US20060122309A1 (en) * | 2004-12-02 | 2006-06-08 | Grah Michael D | Intercalated layered silicate |
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2014
- 2014-07-08 CN CN201410330738.4A patent/CN104085898B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401566A (en) * | 2002-09-24 | 2003-03-12 | 华南理工大学 | Intercalation type or amorphous kaoline and preparing process thereof |
| CN103880032A (en) * | 2014-04-13 | 2014-06-25 | 北京化工大学 | Thiourea intercalation modified kaolin and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 插层改性粘土的可加工性能研究;曾雄丰等;《中国陶瓷》;20140630;第60页"1 实验过程" * |
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