CN1827706A - Process for preparing nano montmorillonite - Google Patents
Process for preparing nano montmorillonite Download PDFInfo
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- CN1827706A CN1827706A CN 200610042359 CN200610042359A CN1827706A CN 1827706 A CN1827706 A CN 1827706A CN 200610042359 CN200610042359 CN 200610042359 CN 200610042359 A CN200610042359 A CN 200610042359A CN 1827706 A CN1827706 A CN 1827706A
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Abstract
The invention relates to a process for preparing nanomontmorillonite, which includes the following job steps and conditions in turn: a. stirring 2, heating and stirring powdery montmorillonite 1 and adding intercalation agent 3; b. heating 5 to evaporate the adsorbed water 6 ;c. keeping the temperature of 8, intermittently mixing the water-reducing mixture 7, and making intercalation agent 3 into the metasilicate sheet interval of extensive powdery montmorillonite; d. heating 9 to produce column-supported mixture 11; e. keeping the temperature of 12, gradually volatilizing the disintegratable component 10 of intercalation agent 3; f. cooling 13, bulking to bulky montmorillonite 14; g. baiting 15, filling the bulky montmorillonite 14 into a heat-insulating and damp-proof container; h. comminuting 16 by gas stream, comminuting the obtained bulky montmorillonite 14 by nanno-gas stream to produce nanomontmorillonite 17. The intercalation agent used in the said method can be carbamide and polysorbate. The invention is characterized in that it is of simple process, few devices and is liable to control, and the intercalation agent is of wide source, low price, is liable to buy and decompose without reserve and can effectively prevent powders from birdnesting, and the grain diameter of the gained montmorillonite is between 1 and 100 nm and enlarges the applied area.
Description
One. technical field
The present invention relates to a kind of working method of montmorillonite, especially a kind of preparation method of nano montmorillonite.
Two. background technology
Montmorillonite is processed into powder and can be used for technical fields such as casting, iron ore pellets, petroleum drilling, its working method is divided into two kinds of dry method and wet processes: (one) wet processes technology, it is that the early-stage Study that montmorillonite is processed is dominated, its key problem in technology is to adopt the montmorillonite ion exchange technique, because adaptable types of agents is many, consumption is big, so have problems such as stone flour is thick, technical process long, the volume production ability is little, production cost is high and tail washings is unfriendly to environment, intractability is big, almost do not have application prospect; (2) dry process technology, it is based on the rise of nanotechnology and causes nano montmorillonite to can be used as the reality of the senior weighting agent that is applied to nanometer polymer, medicine, makeup etc. and the imagination that proposes: montmorillonite nanoization should be utilized silicate sturcture between montmorillonite layer, make organic or inorganic thing molecule insert between the montmorillonite silicate lamella under certain temperature and static(al) or the shear action and further making its miniaturization.Therefore, various researchs are carried out, but are not to have insertion process and condition question in the technical study, are exactly to have which kind of intercalator problem of selection or follow-up miniaturization working-procedure problem.
Three. summary of the invention
The object of the present invention is to provide a kind of preparation method of nano montmorillonite, make montmorillonite fine, can prevent the serial problem that the wet processes technology produces to nano level.
For reaching this purpose, the present invention mainly finishes in the following way:
1. the preparation method of nano montmorillonite comprises the processing step and the condition of following order:
A. stir, with powdery montmorillonite pack that reactor is heated into, continuously stirring and add intercalator;
B. heat up, the compound that adds intercalator is warming up to 95～105 ℃, make the planar water evaporation of powdery montmorillonite;
C. constant temperature keeps diminishing compound constant temperature 3～5 hours, intermittently stirs, and intercalator is entered between the silicate lamella of powdery montmorillonite, and its interlayer is enlarged;
D. heat up, the diminishing compound is warming up to 200～220 ℃, make the diminishing compound become pillared compound;
E. constant temperature makes in the pillared compound the easy decomposition components of intercalator volatilize gradually, and this time kept 6～8 hours;
F. cooling, water-cooled cooling to 50 ℃ along with the easy decomposition components of intercalator is volatilized and the effect of the component of anti-powder reuniting fully, makes pillared compound expand into bulk montmorillonite;
G. blanking is filled to the heat-holding dampproof container with bulk montmorillonite;
H. comminution by gas stream carries out the ultramicronising comminution by gas stream with the bulk montmorillonite input sulfuration bed formula comminution by gas stream mill in the heat-holding dampproof container, produces nano montmorillonite.
2. stream pressure is 0.8～1.2MPa during described comminution by gas stream.
3. the intercalator used of aforesaid method comprises: easily decompose the B component of the component A and the anti-powder reuniting of noresidue, component A is a kind of urea
B component is a kind of poly-pears acid esters
The weight proportion of each component is: component A1～8, B component 0.001～0.2.
4. described intercalator, preferably the weight proportion of each component is:
Component A2～6, B component 0.01～0.03.
Component (A) urea and the poly-pears acid esters of component (B) that can be used as the intercalator that the inventive method uses are the materials that market is easily purchased.For avoiding pillared compound residual impurity and reduce cost, the preferably poly-pears acid esters-20 of the preferred pure urea component of component (A) (B), component (B).
Reactor and sulfuration bed formula comminution by gas stream mill also for conventional, easily purchase equipment.Reactor should select the model of conduction oil interlayer, horizontal stirring and adjustable rotating speed.Equipment also should be controlled parameter such as air outlet temperature and keep water ratio, oil length, powder directly to minimize when using.
Advantage of the present invention:
1. preparation nano montmorillonite technology is easy, equipment is few, be easy to control.
The component of intercalator source wide, inexpensive, easily purchase.
3. intercalator component A easily decomposes noresidue, B component can effectively prevent powder reuniting.
4. nano montmorillonite has enlarged Application Areas.
5. Zhi Bei nano montmorillonite detects through scanning electron microscope, X ray and laser particle size and shows: the montmorillonite interlayer structure strut and in the form of sheets, 2 θ angles obviously reduce, microtexture homogenizing and fineness reach 389.8nm, promptly particle diameter is in 1～100nm scope.
Four. description of drawings
The concrete grammar and the equipment of invention are provided by the following drawings.
Fig. 1 is preparation method's process flow sheet of the nano montmorillonite of proposition according to the present invention.
Preparation method's temperature control curve figure of the nano montmorillonite that Fig. 2 proposes according to the present invention.
Each sign expression in the accompanying drawing:
1. powdery montmorillonite 2. stirs 3. intercalators, 4. compounds, 5. intensifications, 6. planar water, 7. diminishing compounds, 8. constant temperature, 9. intensifications, 10. easy decomposition components 11. pillared compound 12. constant temperature 13. coolings 14. bulk montmorillonite 15. blankings 16. comminution by gas stream 17. nano montmorillonites
Five. embodiment
1. as shown in Figure 1, the preparation method of nano montmorillonite comprises the processing step and the condition of following order:
B. heat up 5, the compound 4 that adds intercalator is warming up to 95～105 ℃, make planar water 6 evaporations of powdery montmorillonite 1;
C. constant temperature 8, and diminishing compound 7 constant temperature were kept 3～5 hours, intermittently stir, and intercalator 3 is entered between the silicate lamella of powdery montmorillonite 1, and its interlayer is enlarged;
D. heat up 9, diminishing compound 7 is warming up to 200～220 ℃, make diminishing compound 7 become pillared compound 11;
E. constant temperature 12, and the easy decomposition components 10 of intercalator 3 in the pillared compound 11 is volatilized gradually, and this time kept 6～8 hours;
F. lower the temperature 13, water-cooled cooling to 50 ℃ along with the easy decomposition components 10 of intercalator 3 is volatilized and the effect of the component of anti-powder reuniting fully, makes pillared compound 11 expand into bulk montmorillonite 14;
G. blanking 15, and bulk montmorillonite 14 is filled to the heat-holding dampproof container;
H. comminution by gas stream 16, and the 14 input sulfuration bed formula comminution by gas stream mills of the bulk montmorillonite in the heat-holding dampproof container are carried out the ultramicronising comminution by gas stream, produce nano montmorillonite 17.
The intercalator that described method is used is selected the component urea of easy decomposition noresidue and the poly-pears acid esters of component of anti-powder reuniting for use, and the weight proportion of each component is: urea 1～8, poly-pears acid esters 0.001～0.2.
Referring to Fig. 2, preparation method's temperature control of nano montmorillonite is that the powdery montmorillonite under the normal temperature 1 is heated in reactor, temperature rises to 95～105 ℃ of the first constant temperature points gradually, kept 3～5 hours, continue to make temperature to rise to 200～220 ℃ of the second constant temperature points gradually, kept 6～8 hours, water-cooled cooling to 50 ℃ blanking is to next process again.
The following example will further specify the present invention.
Embodiment 1
With 325 order powdery montmorillonite pack that reactor is heated into, continuously stirring and add intercalator urea and poly-pears acid esters simultaneously, weight is: urea 2～6, poly-pears acid esters 0.01～0.03, again through described intensification, constant temperature, intensification, constant temperature, cooling process and condition, transport to sulfuration bed formula comminution by gas stream mill after the blanking and carry out the ultramicronising comminution by gas stream, producing particle diameter is the nano montmorillonite of 1～100nm.
Technology and condition add intercalator urea and poly-pears acid esters with embodiment 1, and weight is: urea 1～8, poly-pears acid esters 0.01～0.2, producing particle diameter is the nano montmorillonite of 1～100nm.
Contrast experiment's example 1
Technology is identical with embodiment 1,2 with condition, only first constant temperature point is brought up to 135 ℃, and the urea volatilization is sent pungent ammonium flavor, the intercalator actual effect.
Contrast experiment's example 2
Technology is identical with embodiment 1,2 with condition, only first constant temperature point is reduced to 90 ℃, is adsorbed water between montmorillonite layer and occupies, and intercalator is difficult to enter interlayer, and does not obviously reduce at 2 θ angles, microtexture is inhomogeneous.
Contrast experiment's example 3
Technology is identical with embodiment 1,2 with condition, only second constant temperature point is brought up to 230 ℃, and water of constitution loses between montmorillonite layer, so that the montmorillonite internal structure changes.
Contrast experiment's example 4
Technology is identical with embodiment 1,2 with condition, only second constant temperature point is reduced to 190 ℃, and the intercalator urea that enters interlayer do not decompose, non-volatile.
Contrast experiment's example 5
Technology is identical with embodiment 1,2 with condition, only respectively first constant temperature is put the thermostatic hold-time shortening or the prolongation of the second constant temperature point, can have influence on planar water evaporation between montmorillonite layer respectively, stop powder reunion degree and urea decomposition evaporable degree.
Claims (4)
1. the preparation method of a nano montmorillonite is characterized in that this method comprises the processing step and the condition of following order:
A. stir (2), with powdery montmorillonite (1) pack that reactor is heated into, continuously stirring and add intercalator (3);
B. heat up (5), the compound (4) that adds intercalator is warming up to 95～105 ℃, make planar water (6) evaporation of powdery montmorillonite (1);
C. constant temperature (8) keeps diminishing compound (7) constant temperature 3～5 hours, intermittently stirs, and intercalator (3) is entered between the silicate lamella of powdery montmorillonite (1), and its interlayer is enlarged;
D. heat up (9), diminishing compound (7) is warming up to 200～220 ℃, make diminishing compound (7) become pillared compound (11);
E. constant temperature (12) volatilizees the easy decomposition components (10) of intercalator (3) in the pillared compound (11) gradually, and this time kept 6～8 hours;
F. cooling (13), water-cooled cooling to 50 ℃ along with the easy decomposition components (10) of intercalator (3) is volatilized and the effect of anti-powder reuniting component fully, makes pillared compound (11) expand into bulk montmorillonite (14);
G. blanking (15) is filled to the heat-holding dampproof container with bulk montmorillonite (14);
H. comminution by gas stream (16) carries out the ultramicronising comminution by gas stream with the input of the bulk montmorillonite (14) in heat-holding dampproof container sulfuration bed formula comminution by gas stream mill, produces nano montmorillonite (17).
2. the preparation method of nano montmorillonite according to claim 1, stream pressure is 0.8～1.2MPa when it is characterized in that described comminution by gas stream (16).
3. preparation method's intercalator of nano montmorillonite according to claim 1, it is characterized in that this intercalator (3) comprising: easily decompose the component (A) of noresidue and the component (B) of anti-powder reuniting, component (A) is a kind of urea
Component (B) is a kind of poly-pears acid esters
The weight proportion of each component is: component (A) 1～8, component (B) 0.001～0.2.
4. preparation method's intercalator of nano montmorillonite according to claim 3 is characterized in that the weight proportion of preferred each component is:
Component (A) 2～6, component (B) 0.01～0.03.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100423590A CN100528979C (en) | 2006-02-05 | 2006-02-05 | Process for preparing nano montmorillonite |
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| CNB2006100423590A CN100528979C (en) | 2006-02-05 | 2006-02-05 | Process for preparing nano montmorillonite |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101999558A (en) * | 2010-12-27 | 2011-04-06 | 双胞胎（集团）股份有限公司 | Compound premix for pigs at different physiological stages |
| CN104381620A (en) * | 2014-11-05 | 2015-03-04 | 辽宁宏泰药业有限公司 | Preparation method of nano stripped montmorillonite for feed |
| CN105176301A (en) * | 2015-08-30 | 2015-12-23 | 常州市鼎日环保科技有限公司 | Preparation method for self-cleaning nano-paint |
-
2006
- 2006-02-05 CN CNB2006100423590A patent/CN100528979C/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101999558A (en) * | 2010-12-27 | 2011-04-06 | 双胞胎（集团）股份有限公司 | Compound premix for pigs at different physiological stages |
| CN101999558B (en) * | 2010-12-27 | 2013-04-17 | 双胞胎（集团）股份有限公司 | Compound premix for pigs at different physiological stages |
| CN104381620A (en) * | 2014-11-05 | 2015-03-04 | 辽宁宏泰药业有限公司 | Preparation method of nano stripped montmorillonite for feed |
| CN105176301A (en) * | 2015-08-30 | 2015-12-23 | 常州市鼎日环保科技有限公司 | Preparation method for self-cleaning nano-paint |
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| Publication number | Publication date |
|---|---|
| CN100528979C (en) | 2009-08-19 |
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