CN101224896A - Nano gluconic acid montmorillonite and preparation method thereof - Google Patents
Nano gluconic acid montmorillonite and preparation method thereof Download PDFInfo
- Publication number
- CN101224896A CN101224896A CNA2008100734512A CN200810073451A CN101224896A CN 101224896 A CN101224896 A CN 101224896A CN A2008100734512 A CNA2008100734512 A CN A2008100734512A CN 200810073451 A CN200810073451 A CN 200810073451A CN 101224896 A CN101224896 A CN 101224896A
- Authority
- CN
- China
- Prior art keywords
- gluconic acid
- montmorillonite
- nano
- preparation
- alkaline calcium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention relates to a nanometer gluconic acid smectite and a preparation technique, which is characterized in that: an alkali calcium bentonite and a gluconic acid are adopted as materials to react in the existence of the dispersant of ethanol-water solution. The preparation method is that: disperse the alkali calcium bentonite into the ethanol-water solution, add a gluconic acid water solution and stir the mixture for reaction; filter the mixture after the reaction to obtain a filter cake and wash the filter cake with an ethanol-water solution and an absolute ethyl alcohol, then dry the filter cake under vacuum condition at room temperature to obtain the nanometer gluconic acid smectite. Compared with traditional organophilic bentonite, the granular size of the prepared nanometer gluconic acid smectite achieves a nanometer level and has excellent dispersing function and can be applied to the modification of macromolecule material with strong polarity such as starch, sugar, water soluble paint and polyvinyl alcohol and so on to improve the mechanical property of the materials.
Description
Technical field
The present invention relates to a kind of modified alta-mud and preparation method thereof, particularly nano gluconic acid montmorillonite and preparation method thereof.
Background technology
Wilkinite is a kind of mineral clay material, its effective constituent is the silico-aluminate montmorillonite, montmorillonite is one group of 2: 1 type stratified material, by the reactive force between the electronegative silicate layer is Van der Waals force and weak electrostatic force, and the metal ion isomorphous substitution that has similar size and less valence state in the lamella has produced clean negative charge.Be the compensation negative charge, alkali metal cation enters interlayer.By cationic exchange, the modified alta-mud that available can be different.In common interlayer ion exchange modifying process, interlamellar spacing changes according to the size of modifier molecules, and still layer is not peeled off with layer, keeps the laminate structure of montmorillonite.Traditional organic montmorillonite is a kind of modified alta-mud that obtains by the organic cation exchange, after metal ion between montmorillonite layer is exchanged by organic ion, original bentonitic hydrophilic and oleophobic and water-swelling characteristic have been changed, function with hydrophobic oleophylic and adsorb organic compound is in anti-heavy, the modulation of oil drilling mud of the thickening tackify of coating and printing ink, the preparation of high temperature lubricant, the aspect extensive application such as modification of macromolecular material.Chinese patent [application (patent) number] CN200710027154.X discloses bentonite of organic acid and preparation method thereof, this organobentonite is to adopt the modified with organic acids alkaline calcium bentonite synthetic in organic dehydrated solvent, overcome traditional organophilic clay and can only use the organic cation modification, widened the bentonite Application Areas greatly, in the embodiment of this patent, be mentioned to the gluconic acid preparation method for bentonite, because a little less than the solvent polarity that uses, gluconic acid solubleness is little, and modifying process does not make montmorillonite peel off.More than these organic modifications all do not change montmorillonite stratiform structure, resulting organobentonite particle is bigger, disperses relatively difficulty in the polymer modification process.
But when a large amount of fierce thermopositive reaction took place, peeled off, and obtains the big or small montmorillonite sheet of nano-scale that is by the montmorillonite layer sector-meeting in the compound between montmorillonite layer for intercalation.Make the montmorillonite lamella produce the method for peeling off at present, all be that intercalation polymeric is peeled off method, promptly earlier the polymer monomer intercalation between montmorillonite layer, allow monomer polymerization reaction take place between montmorillonite layer then, the montmorillonite synusia is peeled off, CN200610007296.5 discloses polyamide copolymer/clay nano composite material and its production and use as Chinese patent [application (patent) number], adopt two sections continuous polymerization techniques, with monomer of polyamide or polymerizing polyamide catalyzer and chain alkyl ammonium salt Combined Processing clay, the lamella quilt polymerizing catalyst and the monomer intercalation as much as possible of organifying clay realized fully peeling off of matrix material medium clay soil lamella by a large amount of heat of polymerizations and polymer chain.After montmorillonite is peeled off in polymkeric substance, in polymkeric substance, disperse, the mechanical mechanics property of polymkeric substance is greatly improved with the size of nanometer.In theory,, allow the stratified material of the abundant intercalation of monomer,, can realize peeling off of stratified material by intercalation polymeric as long as can find to the macromolecular material of synthetic; But to natural polymer, as carbohydrate, protein etc., very difficult realization montmorillonite portion is within it peeled off the dispersion modification.
Summary of the invention
The inventor's purpose provides a kind of, dispersion easy reach broad-spectrum nano gluconic acid montmorillonite and preparation method thereof good with the hydrophilic macromolecular compounds consistency.This nano montmorillonite is on the basis of bentonite of organic acid preparation, and adopting alkaline calcium bentonite and gluconic acid is raw material, by the reaction conditions between key-course, bentonitic smectite structure is produced peel off, and obtains nano gluconic acid montmorillonite.
Nano gluconic acid montmorillonite of the present invention, its crystal are gluconic acid surface modification type montmorillonite nano sheet, and thickness is that 300～600nm, length are 800～1000nm less than 100nm, width, and organic loss on ignition is 30～40%.
Nano gluconic acid montmorillonite of the present invention is to be raw material with alkaline calcium bentonite and gluconic acid, alkaline calcium bentonite and gluconic acid reaction in the presence of aqueous ethanolic solution, concrete technology are to be that 1.5～2.0mmol/g, granularity are that to be scattered in quantity be that 10～30 times of alkaline calcium bentonite quality, mass content are in 40～75% the aqueous ethanolic solution to 60～200 purpose alkaline calcium bentonites with anion-exchange capacity; 60～85 ℃ and stir under, evenly add quantity in 0.5～2 hour and be the alkaline calcium bentonite quality 25～50%, mass content is 30～50% gluconic acid aqueous solution, add the back and continue reaction 2～5 hours; After-filtration is finished in reaction, and filter cake with 40～60% aqueous ethanolic solutions washing 2～4 times, is used absolute ethanol washing 1～2 time earlier again, the nano gluconic acid montmorillonite that last room temperature vacuum-drying obtains.
The nano gluconic acid montmorillonite that the present invention prepares is compared with traditional organobentonite, and its granular size has reached nano level, has good divergent function.
The preparation method of nano gluconic acid montmorillonite of the present invention, owing to be reflected in the aqueous ethanolic solution and carry out, reacted washing, filtration and dry than being easier to, processing unit is simple, is produced on a large scale.
The nano gluconic acid montmorillonite that the present invention prepares can be used for macromolecular material modifications such as the stronger starch of polarity, sugar, water soluble paint and polyvinyl alcohol, to improve the mechanical mechanics property of these materials.
Embodiment
Embodiment 1
Anion-exchange capacity is that 1.7mmol/g, granularity are that to be scattered in quantity be that 15 times of alkaline calcium bentonite quality, mass content are in 65% the aqueous ethanolic solution to 100 purpose alkaline calcium bentonites; 70 ℃ and stir under, evenly add quantity in 1 hour and be the alkaline calcium bentonite quality 35%, mass content is the 50% gluconic acid aqueous solution, add the back and continue reaction 4 hours; After-filtration is finished in reaction, and filter cake with 60% aqueous ethanolic solution washing 2 times, is used absolute ethanol washing 2 times earlier again, the nano gluconic acid montmorillonite that last room temperature vacuum-drying obtains.
Embodiment 2
Anion-exchange capacity is that 1.8mmol/g, granularity are that to be scattered in quantity be that 20 times of alkaline calcium bentonite quality, mass content are in 70% the aqueous ethanolic solution to 150 purpose alkaline calcium bentonites; 75 ℃ and stir under, evenly add quantity in 1.5 hours and be the alkaline calcium bentonite quality 40%, mass content is the 45% gluconic acid aqueous solution, add the back and continue reaction 3 hours; After-filtration is finished in reaction, and filter cake with 55% aqueous ethanolic solution washing 2 times, is used absolute ethanol washing 2 times earlier again, the nano gluconic acid montmorillonite that last room temperature vacuum-drying obtains.
Embodiment 3
Anion-exchange capacity is that 1.9mmol/g, granularity are that to be scattered in quantity be that 10 times of alkaline calcium bentonite quality, mass content are in 65% the aqueous ethanolic solution to 100 purpose alkaline calcium bentonites; 80 ℃ and stir under, evenly add quantity in 1.5 hours and be the alkaline calcium bentonite quality 45%, mass content is the 50% gluconic acid aqueous solution, add the back and continue reaction 3 hours; After-filtration is finished in reaction, and filter cake with 50% aqueous ethanolic solution washing 3 times, is used absolute ethanol washing 2 times earlier again, the nano gluconic acid montmorillonite that last room temperature vacuum-drying obtains.
Claims (1)
1. the preparation method of a nano gluconic acid montmorillonite, it is characterized in that preparing nano gluconic acid montmorillonite and be with alkaline calcium bentonite and gluconic acid is raw material, alkaline calcium bentonite and gluconic acid reaction in the presence of aqueous ethanolic solution, its preparation method is as follows:
(1) be that 1.5～2.0mmol/g, granularity are that to be scattered in quantity be that 10～30 times of alkaline calcium bentonite quality, mass content are in 40～75% the aqueous ethanolic solution to 60～200 purpose alkaline calcium bentonites with anion-exchange capacity;
(2) 60～85 ℃ and stir under, evenly add quantity in 0.5～2 hour and be the alkaline calcium bentonite quality 25～50%, mass content is 30～50% gluconic acid aqueous solution, add the back and continue reaction 2～5 hours;
(3) after-filtration is finished in reaction, and filter cake is used absolute ethanol washing 1～2 time again with 40～60% aqueous ethanolic solutions washing earlier 2～4 times, the nano gluconic acid montmorillonite that last room temperature vacuum-drying obtains.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2008100734512A CN100556807C (en) | 2008-01-29 | 2008-01-29 | Nano gluconic acid montmorillonite and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2008100734512A CN100556807C (en) | 2008-01-29 | 2008-01-29 | Nano gluconic acid montmorillonite and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101224896A true CN101224896A (en) | 2008-07-23 |
| CN100556807C CN100556807C (en) | 2009-11-04 |
Family
ID=39857138
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2008100734512A Expired - Fee Related CN100556807C (en) | 2008-01-29 | 2008-01-29 | Nano gluconic acid montmorillonite and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100556807C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530973A (en) * | 2012-01-10 | 2012-07-04 | 宁波荣山新型材料有限公司 | Bentonite alkaline activation method for efficiently adsorbing saccharide molecules |
| CN103254470A (en) * | 2013-06-03 | 2013-08-21 | 史莹华 | Trehalose-montmorillonite nano compound and preparation method thereof |
| CN110065948A (en) * | 2018-01-23 | 2019-07-30 | 中国石油天然气股份有限公司 | The preparation method of clay |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103964452B (en) * | 2013-12-17 | 2016-04-13 | 广西大学 | Gluconic acid montmorillonite nano belt and preparation method thereof |
-
2008
- 2008-01-29 CN CNB2008100734512A patent/CN100556807C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530973A (en) * | 2012-01-10 | 2012-07-04 | 宁波荣山新型材料有限公司 | Bentonite alkaline activation method for efficiently adsorbing saccharide molecules |
| CN103254470A (en) * | 2013-06-03 | 2013-08-21 | 史莹华 | Trehalose-montmorillonite nano compound and preparation method thereof |
| CN103254470B (en) * | 2013-06-03 | 2016-01-20 | 史莹华 | A kind of trehalose-montmorillonite nano compound and preparation method thereof |
| CN110065948A (en) * | 2018-01-23 | 2019-07-30 | 中国石油天然气股份有限公司 | The preparation method of clay |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100556807C (en) | 2009-11-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Mu et al. | Adsorption of dyes onto palygorskite and its composites: a review | |
| Xuan et al. | Inhibiting effect of dopamine adsorption and polymerization on hydrated swelling of montmorillonite | |
| CN101049943B (en) | Bentonite of organic acid, and preparation method | |
| CN100556807C (en) | Nano gluconic acid montmorillonite and preparation method thereof | |
| CN105502358B (en) | It is a kind of that the method that graphite material prepares Graphene is peeled off by auto polymerization | |
| CN101469145B (en) | Process for preparing attapulgite based composite material | |
| CN105079887A (en) | Blocky bionic material, method for manufacturing same and application of blocky bionic material | |
| CN102690535A (en) | Organic modified nano-attapulgite particles and preparation method thereof | |
| Wang et al. | Nanoscale clay minerals for functional ecomaterials: Fabrication, applications, and future trends | |
| CN103850152B (en) | Nanometer paper material and preparation method thereof | |
| CN102604433B (en) | Preparation method of aldehyde modified shell micro powder | |
| Detellier et al. | Kaolinite–polymer nanocomposites | |
| WO2015155110A1 (en) | Process for making tiles | |
| CN105126641A (en) | Flexible attapulgite membrane and preparation method thereof | |
| CN104944431B (en) | A kind of inorganic supermolecule electric double layer two-dimensional nano piece and preparation method thereof | |
| CN103897433A (en) | Calcium carbonate-modifier composition and calcium carbonate surface modification method using the same | |
| Mihai et al. | Chitosan based nonstoichiometric polyelectrolyte complexes as specialized flocculants | |
| CN112830497B (en) | Preparation method of high-viscosity attapulgite-based inorganic gel | |
| CN1544538A (en) | Organic modified phyllosilicate and method for preparing same | |
| CN109650400A (en) | A kind of DMF intercalation-removing na-montmorillonite ultrathin nanometer piece and preparation method thereof | |
| CN104610575B (en) | A kind of zinc-aluminium-layered double-hydroxide enveloping carbon nanotube composite powder and preparation method thereof | |
| CN101302294B (en) | Preparation of polyaniline nano-wire/nano-particle compound system | |
| CN1252161C (en) | Organic composite rectorite and preparation process thereof | |
| CN109046046A (en) | A kind of preparation method of nano material/Quorum quenching enzymes hydrogel nanofiltration membrane | |
| CN108502910A (en) | Insoluble inorganic salts micro Nano material and its preparation method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20091104 Termination date: 20140129 |