CN1563207A - Dry method for preparing intercalation compound of monotomorillonite/urea - Google Patents
Dry method for preparing intercalation compound of monotomorillonite/urea Download PDFInfo
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- CN1563207A CN1563207A CN 200410012903 CN200410012903A CN1563207A CN 1563207 A CN1563207 A CN 1563207A CN 200410012903 CN200410012903 CN 200410012903 CN 200410012903 A CN200410012903 A CN 200410012903A CN 1563207 A CN1563207 A CN 1563207A
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Abstract
A method for preparing intercalation composite of imvite/urea is featured as mixing sodium-base or calcium-base imvite powder material in diamemter of less than 45 micron m with urea powder uniformly, holding the mixture for 1-3 hr. at constant temperature to have urea molecule entered into interlayer of imvite crystal structure and obtaining the intercalation composite by expanding interlayer distance from 1.27nm-1.55 nm to 1.68 nm to 2.17 nm on imvite face.
Description
Technical field
The present invention relates to a kind of method for preparing montmorillonite/urea intercalated compound, specially refer to a kind of dry method intercalation method.
Background technology
Wilkinite (Bentonite) also be otaylite or amargosite.It is found in the ancient stratum of the Wyoming State of the U.S. the earliest, is yellowish green clay, becomes pasty state because of adding the water after, and people just the clay of this character, are referred to as wilkinite.Bentonitic essential mineral composition is a montmorillonite, and content is 85%～90%, and other contains a small amount of feldspar, quartz, beidellite, calcite and volcanic glass.Can be white in color, be when impure pale green, greyish white, pink isochrome.Can become compact mass, also can be loose earthy, sliding sense is arranged when rubbing mill with the hands with finger, volume swelled several times to tens times after small blocks added water, was suspension in water, and water in the pasty state after a little while.China's bentonite resource is very abundant, and mineral products almost spread all over the country, and its reserves occupy the second place of the world.Wilkinite is a kind of nonmetal mineral resource that purposes is wide in the development of the national economy, consumption is big.Bentonitic fundamental property depends on the mineralogical character of montmorillonite; generally have good cohesiveness, swelling property, colloid dispersiveness, suspension, adsorptivity, catalytic activity, thixotropy and cationic exchange etc., be widely used in the field such as absorption, rubber, plastics, papermaking, soil improvement, pottery, building material, electrically insulating material, makeup, soap and food, carrier, fodder additives of petrochemical complex, daily-use chemical industry, coating, environment protection, weaving, medicine, radioactive substance.
Montmorillonite belongs to 2: 1 type clay minerals, be a kind of mineral the most general in the smectite family, its basic structural unit is to be clipped in the laminate structure that forms by public Sauerstoffatom connection between two silicon-oxy tetrahedrons by a slice alumina octahedral, and the thickness of each lamella of montmorillonite is about 1nm; Length and the wide 100nm that respectively is about.The natural montmorillonite lamella is in forming process, a part is positioned at the Al of central core by metal ion (as Fe, Cu, Zn, Li, Cr etc.) at a low price displacement with one heart, cause each lamella to present weak electronegativity, therefore often adsorbing metallic cation (as Na on the surface of lamella
+, K
+, Ca
2+, Mg
2+Or the like) to keep the electric neutrality of whole mineral structure.Form electric dipole between positively charged ion and crystal skeleton between the montmorillonite crystal layer, add that bonding force between the montmorillonite crystal layer a little less than, can adsorb polar water molecules, according to cation type and relative humidity, interlayer can adsorb one deck or two-layer water molecules.In addition, also adsorbed certain water molecules at the montmorillonite grain surface.Water of constitution is present in the lattice with the OH form.
The interlamination region of montmorillonite has characteristics such as interlayer exchange, interlayer absorption, interlayer catalysis, interlayer polymerization, interlayer be pillared.Therefore,, since the sixties, montmorillonite has been carried out a large amount of study on the modification both at home and abroad and used, obtained great achievement in order to open up the new Application Areas of montmorillonite.The method of modifying that adopts has that the artificial natridization handles, acid activation is handled, organic covering handles and the pillared modification of various Al, Li, Ti or the like metallic cation.Various modified products are widely used in fields such as chemical industry, drilling mud, water purification, building, agricultural.Wherein studying maximum is pillared montmorillonite, it is to be the novel class zeolite layer cylindrical catalyst that " post " shape supports contact by pillaring agent (or linking agent) between montmorillonite layer, have wide aperture, high surface area, micropore amount height, good heat resistance, characteristics such as surface acidity is strong have unique effect in macromolecular catalytic cracking such as some heavy oil, residual oil.
Because this distinctive crystal chemistry characteristic of montmorillonite, it is used for medical carrier, fodder additives, soil improvement agent and chemical fertilizer etc. more and more widely, and the particularly application of the mesoporous package technique of sodium rice has improved montmorillonite Application Areas and added value greatly.
Make a general survey of at present the preparation method of montmorillonite/urea intercalated compound, " montmorillonite is as fertilizer slow-release formulation and carrier " (notification number: 1298853); " is the ammonium carbonate fertilizer containing of filler with the wilkinite " (notification number: 1185424); " a kind of slow-release carbamide and preparation method thereof " (notification number: 1408351), these methods all adopt wet method or pack, and their drawback is: adopt wet method, last operation also needs heat drying, urea could be inserted between montmorillonite layer, so wet method is to gather in the unnecessary step; Adopt pack, urea can only be adsorbed on the montmorillonite surface, can not enter montmorillonite crystalline structure interlayer.
Summary of the invention
The object of the present invention is to provide a kind of operation simply to prepare the method for montmorillonite/urea intercalated compound.
To achieve these goals, technical scheme of the present invention is: the method for a kind of dried preparation montmorillonite/urea intercalated compound, it is characterized in that: will and account for the urea powder uniform mixing of montmorillonite weight 10～30% less than the sodium base or the ca-montmorillonite powder of 45 μ m, smectite content 〉=80%, constant temperature between 90～120 ℃, 1～3 hour, obtain montmorillonite/urea intercalated compound.
Aforesaid method is specially: after will and accounting for the urea powder uniform mixing of montmorillonite weight 10～30% less than the sodium base or the ca-montmorillonite powder of 45 μ m, smectite content 〉=80%, put into baking oven, constant temperature between 90～120 ℃, 1～3 hour, obtain montmorillonite/urea intercalated compound.
Described method is specially: will less than the sodium base or the ca-montmorillonite powder of 45 μ m, smectite content 〉=80% and the urea powder that accounts for montmorillonite weight 10～30% put into respectively can heated and stirred the mixing tank uniform mixing, constant temperature between 90～120 ℃, 1～3 hour, obtain montmorillonite/urea intercalated compound.
Aforesaid best constant temperature is 95 ℃.
The present invention adopts aforesaid method, can make urea molecule enter montmorillonite crystalline structure interlayer, and the interlamellar spacing of montmorillonite (001) face is expand into 1.68nm-2.17nm by 1.27nm-1.55nm, obtains montmorillonite/urea intercalated compound.Adopt the dry method intercalation, montmorillonite (001) surface layer spacing is big, operation simple, preparation is quick, energy consumption is low, cost is little, overcome in the wet processing, and when dry, the shortcoming that montmorillonite easily lumps, reunites.
Description of drawings
Fig. 1 is the Henan sodium base na-montmorillonite former state XRD figure of the embodiment of the invention 1
Fig. 2 is the Henan na-montmorillonite/urea intercalated compound XRD figure of the embodiment of the invention 1
Fig. 3 is the Henan na-montmorillonite/urea intercalated compound XRD figure of the embodiment of the invention 2
Fig. 4 is the Henan na-montmorillonite/urea intercalated compound XRD figure of the embodiment of the invention 3
Fig. 5 is the Henan ca-montmorillonite former state XRD figure of the embodiment of the invention 4
Fig. 6 is the Henan ca-montmorillonite/urea intercalated compound XRD figure of the embodiment of the invention 4
Fig. 7 is the Henan ca-montmorillonite/urea intercalated compound XRD figure of the embodiment of the invention 5
Fig. 8 is the Shandong ca-montmorillonite XRD figure of the embodiment of the invention 6
Fig. 9 is the Shandong ca-montmorillonite/urea intercalated compound XRD figure of the embodiment of the invention 6
Embodiment
Embodiment 1:
After mixing with 30Kg, less than Xinyang, Henan na-montmorillonite powder (Fig. 1) of 45 μ m (less than 325 orders), smectite content about 90% and 3Kg urea powder, put into baking oven, constant temperature is 3 hours between 90～120 ℃, obtain montmorillonite/urea intercalated compound (Fig. 2), by X-ray diffraction (XRD) spectrum 1 and Fig. 2 as seen, (001) surface layer spacing of na-montmorillonite former state is 1.27nm, behind the urea molecule intercalation, is expanded to 2.17nm.
The temperature of baking oven or mixing tank can not be higher than 132 ℃, otherwise the urea molecule that enters between montmorillonite layer is decomposed.Content of urea can not surpass 30% of montmorillonite weight, and unnecessary urea can not enter montmorillonite crystalline structure interlayer, can only be adsorbed on the montmorillonite surface.
Embodiment 2:
After mixing with 50Kg, less than Xinyang, Henan na-montmorillonite powder of 45 μ m, smectite content about 90% and 10Kg urea powder, put into baking oven, constant temperature is 3 hours between 90～120 ℃, obtain urea/montmorillonite intercalated compound (Fig. 3), the interlamellar spacing of montmorillonite (001) face expand into 2.03nm by 1.27nm.
Embodiment 3:
After mixing with 2Kg, less than Xinyang, Henan na-montmorillonite powder of 45 μ m, smectite content about 90% and 0.2Kg urea powder, put into baking oven, constant temperature is 1 hour between 90～120 ℃, obtain urea/montmorillonite intercalated compound (Fig. 4), the interlamellar spacing of montmorillonite (001) face expand into 1.83nm by 1.27nm.
Embodiment 4:
After mixing with 1Kg, less than Xinyang, Henan ca-montmorillonite powder (Fig. 5) of 10 μ m (less than 1250 orders), smectite content 90% and 0.1Kg gram urea powder, put into baking oven, constant temperature is 2 hours between 95 ℃, obtain urea/montmorillonite intercalated compound (Fig. 6), the interlamellar spacing of montmorillonite (001) face expand into 1.69nm by 1.53nm.
Embodiment 5:
After mixing with 10Kg, less than Xinyang, Henan ca-montmorillonite powder of 45 μ m, smectite content 95% and 1Kg gram urea powder, put into baking oven, constant temperature is 3 hours between 90～120 ℃, obtain urea/montmorillonite intercalated compound (Fig. 7), the interlamellar spacing of montmorillonite (001) face expand into 1.76nm by 1.53nm.
Embodiment 6:
With Shandong ca-montmorillonite powder (Fig. 8) and the 1Kg urea powder of 10Kg less than 45 μ m, put into the mixing tank of heated and stirred respectively, constant temperature is 2 hours between 90～120 ℃, obtain montmorillonite/urea intercalated compound (Fig. 9), make the interlamellar spacing of montmorillonite (001) face, expand into 1.71nm by 1.55nm.
Claims (4)
1. the method for dried preparation montmorillonite/urea intercalated compound, it is characterized in that: will and account for the urea powder uniform mixing of montmorillonite weight 10～30% less than the sodium base or the ca-montmorillonite powder of 45 μ m, smectite content 〉=80%, constant temperature between 90～120 ℃, 1～3 hour, obtain montmorillonite/urea intercalated compound.
2. the method for a kind of dried preparation montmorillonite according to claim 1/urea intercalated compound, it is characterized in that: after will and accounting for the urea powder uniform mixing of montmorillonite weight 10～30% less than the sodium base or the ca-montmorillonite powder of 45 μ m, smectite content 〉=80%, put into baking oven, constant temperature between 90～120 ℃, 1～3 hour, obtain montmorillonite/urea intercalated compound.
3. the method for a kind of dried preparation montmorillonite according to claim 1/urea intercalated compound, it is characterized in that: will less than the sodium base or the ca-montmorillonite powder of 45 μ m, smectite content 〉=80% and the urea powder that accounts for montmorillonite weight 10～30% put into respectively can heated and stirred the mixing tank uniform mixing, constant temperature between 90～120 ℃, 1～3 hour, obtain montmorillonite/urea intercalated compound.
4. according to the method for claim 1 or 2 or 3 described a kind of dried preparation montmorillonite/urea intercalated compounds, it is characterized in that: described best constant temperature is 95 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410012903 CN1268693C (en) | 2004-03-26 | 2004-03-26 | Dry method for preparing intercalation compound of monotomorillonite/urea |
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|---|---|---|---|
| CN 200410012903 CN1268693C (en) | 2004-03-26 | 2004-03-26 | Dry method for preparing intercalation compound of monotomorillonite/urea |
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| CN1563207A true CN1563207A (en) | 2005-01-12 |
| CN1268693C CN1268693C (en) | 2006-08-09 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100463853C (en) * | 2005-12-30 | 2009-02-25 | 中国地质大学（武汉） | Method for preparing high-purity montmorillonite |
| CN102048739A (en) * | 2010-11-24 | 2011-05-11 | 陕西科技大学 | Cefradine/montmorillonite composite material and preparation method thereof |
| CN103251956A (en) * | 2013-04-19 | 2013-08-21 | 张彩云 | Matrine-montmorillonite nano composite and preparation method thereof |
| CN103877960A (en) * | 2014-04-03 | 2014-06-25 | 常州大学 | Preparation method of bentonite-based catalyst carrier |
| CN104799017A (en) * | 2014-01-24 | 2015-07-29 | 内蒙古润隆化工有限责任公司 | Preparation method of modified montmorillonite powder for feeds |
-
2004
- 2004-03-26 CN CN 200410012903 patent/CN1268693C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100463853C (en) * | 2005-12-30 | 2009-02-25 | 中国地质大学（武汉） | Method for preparing high-purity montmorillonite |
| CN102048739A (en) * | 2010-11-24 | 2011-05-11 | 陕西科技大学 | Cefradine/montmorillonite composite material and preparation method thereof |
| CN103251956A (en) * | 2013-04-19 | 2013-08-21 | 张彩云 | Matrine-montmorillonite nano composite and preparation method thereof |
| CN104799017A (en) * | 2014-01-24 | 2015-07-29 | 内蒙古润隆化工有限责任公司 | Preparation method of modified montmorillonite powder for feeds |
| CN103877960A (en) * | 2014-04-03 | 2014-06-25 | 常州大学 | Preparation method of bentonite-based catalyst carrier |
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| Publication number | Publication date |
|---|---|
| CN1268693C (en) | 2006-08-09 |
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