CN102649572A - Preparation method for attapulgite clay inorganic gel - Google Patents
Preparation method for attapulgite clay inorganic gel Download PDFInfo
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- CN102649572A CN102649572A CN2011100472117A CN201110047211A CN102649572A CN 102649572 A CN102649572 A CN 102649572A CN 2011100472117 A CN2011100472117 A CN 2011100472117A CN 201110047211 A CN201110047211 A CN 201110047211A CN 102649572 A CN102649572 A CN 102649572A
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Abstract
The invention discloses a preparation method for attapulgite clay inorganic gel. The preparation method comprises the following steps of: preparing attapulgite clay into suspension; reacting the suspension with phosphate and then reacting with magnesium salt; and centrifuging, drying and crushing, thereby obtaining the attapulgite clay inorganic gel. The preparation method has the advantages that the production technology is simple and safe; the production process is easily controlled; the raw material is easily obtained; the preparation method is non-toxic and harmless; the preparation method has the characteristics of low cost, low energy consumption and environmental protection; and the large-scale production is easily realized.
Description
Technical field
The present invention relates to a kind of preparation method of attapulgite clay inorganic gel, belong to nonmetalliferous ore deep processing field.
Background technology
The mineral inorganic gel is a kind of extraordinary silicate colloid series products of layer chain and the frame shape structure of being made up of inorganic elementss such as silicon, magnesium, aluminium and sodium.Because of it has stronger swelling capacity in water, and can take useful rheological property in the Aquo System to and be widely used in industries such as fine chemistry industry, daily use chemicals, medicine and oil, as uses such as thixotropic agent, thickening material, dispersion agent, suspension agent and stablizers.
At present, the mineral inorganic gel mainly is to be the product of raw material deep processing or the product of synthetic with the high purity wilkinite.Veegum-T, Vangel and Magnabrite series product like the production of U.S. Vanderbilt Co. R. T.; The Laponite product that Britain Laporte company produces; The SM series that domestic Zhejiang Feng Hong clay chemical industry ltd produces, Anji County is the YH series bentonite inorganic gel produced of the Hong Pengruntuchang ES series of producing and the grand clay chemical industry of Anji space ltd etc. forever.The mineral inorganic gel has the added value of product advantages of higher, and the external product price is up to 3000-7000 dollar/ton, and home products is also at 5000-20000 unit/ton.
Attapulgite clay be a kind of with the attapulgite be main ingredient have a special rod-like fibre article body structure contain Shuifu County's zeopan mineral.The fibrous crystalline structure of attapulgite clay helps forming fiber mesh, and the noble potential of its plane of crystal helps aquation, Al
3+And Mg
2+Between extensively the having to be beneficial to and produce the active surface position and strengthen hydrating capacity of different valency isomorphous replacement.Therefore, it can form the thixotropy gel of quasi-viscous liquid type in the aqueous solution.Compare with other clays; Attapulgite clay has better colloidal property; Under quite low concentration, can form full-bodied suspension-s, dry post-shrinkage ratio is less, and particularly influenced by ionogen less for the attapulgite soliquid; Even in saturated brine, still can keep colloidal property preferably, be comparatively ideal inorganic gel material.
Summary of the invention
The object of the invention is to provide a kind of technology simple, and good product performance is easy to realize the preparation method of the attapulgite clay inorganic gel of scale operation.
The technical problem that the present invention will solve realizes through following scheme:
We process suspension-s with attapulgite clay, then with phosphate reaction, with the magnesium salts reaction, obtain the attapulgite clay inorganic gel through centrifugal, dry, pulverizing again.
A kind of preparation method of attapulgite clay inorganic gel is characterized in that preparing through the following step successively:
The preparation of A attapulgite clay suspension-s: under whipped state, attapulgite clay is added in the entry, process the suspension-s of concentration at 5-20wt%;
B attapulgite clay and phosphate reaction: under whipped state, in attapulgite clay suspension-s, add phosphoric acid salt, reacted 1～4 hour down at 50-80 ℃;
The C gelation reaction: under whipped state, in above-mentioned system, add magnesium salts, continue reaction 2-4 hour, cooling is after centrifugal, dry, pulverizing obtains the attapulgite clay inorganic gel.
Phosphoric acid salt is any one or more in sodium phosphate, Sodium phosphate, dibasic, SODIUM PHOSPHATE, MONOBASIC, the Sodium hexametaphosphate 99.
The phosphoric acid salt add-on is 2%～10% of an attapulgite clay siccative weight.
Magnesium salts be in Natural manganese dioxide, Marinco H, sal epsom, the magnesiumcarbonate any or more than one.
The add-on of magnesium salts is 1～20% of an attapulgite clay siccative weight percent.
Below be principle explanation of the present invention: the crystalline structure of attapulgite clay contains the 3 D stereo chain; After in water, disperseing, its bar-shaped brilliant bundle disperses and forms mixed and disorderly grid, and very strong gel-formation power is arranged; Under relatively low concentration, just can form than steady suspension; This suspension-s has the characteristic of non-Newtonian fluid, but its character depends on attapulgite clay self character, concentration and shearing force size and pH value etc., and the attapulgite clay self character is the most key.Mg in the attapulgite clay crystalline structure
2+, owing to Al in becoming the ore deposit process
3+Or Fe
3+To Mg
2+Isomorphous replacement; Can also get into 1 or 2 hydrogen ions or other Equivalents in the system, just can make attapulgite clay ability stable suspersion in water medium, but 1 or 2 hydrogen ions of direct compensation or other Equivalents; Just at the interlayer of attapulgite clay, what obtain is the metastable state structure.For this reason, in attapulgite clay suspension-s, earlier with phosphoric acid salt and the tradable Mg of attapulgite clay interlayer
2+, Al
3+Or Fe
3+Exchange; Be adsorbed on the interlayer of attapulgite clay with the form of chemisorption; Increase the electronegativity of the interlayer of attapulgite clay, and pass through the extension of phosphate molecule chain, the steric hindrance repulsive interaction and the aquation repulsive interaction that increase the attapulgite clay interlayer; Make the brilliant bundle of attapulgite clay rod form more mixed and disorderly grid, improve the dispersing property of attapulgite clay in water.In order to increase suspension stability, must further mate positive charge.Therefore, after adding magnesium salts, the magnesium salts that has positive charge is dispersed among the attapulgite frame shape structure that has negative charge; Rely on the electrostatic attraction between the charges of different polarity and the attapulgite frame shape structure that has negative charge is formed booster action, make the ability of this other ion damaged of structure opposing strengthen, yielding stress increases; The resistance increase of flowing relatively and being out of shape; Viscosity improves, and thixotropy strengthens, and shows stronger gellifying property.
The crystalline structure unit of inorganic gel is brilliant in the rod of nanometer, and rod is about 500～2000 nanometers, the wide about 20-40 nanometer of rod.The brilliant surface of rod has been covered with tradable positively charged ion, and when gel particle mixed with water, water contacted with exchangeable cation and is adsorbed to the brilliant surface of rod.Because excellent crystal layer is worn negative charge; End face is positively charged, and water forms three-dimensional colloidal structure rapidly with the back, and the viscosity of system is increased; And have suspension, thickening property, thixotropy and excellent compatibility, the chemicalstability of height, be ideal aqueous systems thickener rheology agent.
The present invention has the following advantages:
Phosphatic effect is the absolute value that improves excellent brilliant surface potential, thereby produces strong electrostatic double layer electrostatic repulsion effect, and adsorption layer can also produce very strong steric exclusion effect simultaneously, prevents the reunion that rod is brilliant effectively.
Attapulgite clay carries out gel on phosphoric acid salt modification basis handles, and attapulgite clay suspension-s force-at-yield is increased, and viscosity improves, and thixotropy strengthens, and shows stronger gellifying property.2.5% inorganic gel water dispersion viscosity＞800mpa.s.Because most organic thickening agents are not had a YV, thus product can with the compound use of organic thickening agent, viscosity, YV and the flowability of system are effectively regulated.
Product has excellent pH stability and chemicalstability and thermostability, with other organic colloids consistency and compatibility is preferably arranged, and oil-in-water and invert emulsion system are had stability preferably.The solvent that its dispersion liquid can dissolve with water is like methyl alcohol, ethanol, glycerine and Ucar 35 and polyoxyethylene glycol.Suspension stability is preferably arranged simultaneously, can satisfy the demand of coating and cosmetics of everyday use thickening.
Production technique is simple and safe, and production process is easy to control, and desired raw material is simple and easy to, and is nontoxic, has low cost, less energy-consumption and eco-friendly characteristics, is easy to realize scale operation.
Embodiment
Comparison sample
Under whipped state, attapulgite clay is added in the entry, process concentration and be 7% attapulgite clay suspension-s; At 70 ℃ of following stirring reactions after 5 hours, cooling is after centrifugal, dry, pulverizing obtains the attapulgite clay product.
Embodiment 1
Under whipped state, attapulgite clay is added in the entry, processing concentration is the attapulgite clay suspension-s of 7wt%; The Sodium hexametaphosphate 99 that adds attapulgite clay mass percent 2.0%; 70 ℃ of following stirring reactions add the Natural manganese dioxide of attapulgite clay mass percent 10% after 3 hours; Continue reaction 2 hours, cooling is after centrifugal, dry, pulverizing obtains attapulgite clay inorganic gel product.
Embodiment 2
Under whipped state, attapulgite clay is added in the entry, processing concentration is the attapulgite clay suspension-s of 10wt%; The SODIUM PHOSPHATE, MONOBASIC that adds attapulgite clay mass percent 5.0%; 80 ℃ of following stirring reactions add the Marinco H of attapulgite clay mass percent 8% after 2 hours; Continue reaction 2 hours, cooling is after centrifugal, dry, pulverizing obtains attapulgite clay inorganic gel product.
Embodiment 3
Under whipped state, attapulgite clay is added in the entry, processing concentration is the attapulgite clay suspension-s of 15wt%; The sodium phosphate that adds attapulgite clay mass percent 2.0%; 70 ℃ of following stirring reactions add the magnesiumcarbonate of attapulgite clay mass percent 12% after 4 hours; Continue reaction 3 hours, cooling is after centrifugal, dry, pulverizing obtains attapulgite clay inorganic gel product.
Embodiment 4
Under whipped state, attapulgite clay is added in the entry, processing concentration is the attapulgite clay suspension-s of 8wt%; Add the sodium phosphate of attapulgite clay mass percent 1.0% and 2.0% SODIUM PHOSPHATE, MONOBASIC; 80 ℃ of following stirring reactions add the sal epsom of attapulgite clay mass percent 3% after 1 hour; Continue reaction 2 hours, cooling is after centrifugal, dry, pulverizing obtains attapulgite clay inorganic gel product.
Embodiment 5
Under whipped state, attapulgite clay is added in the entry, processing concentration is the attapulgite clay suspension-s of 8wt%; The sodium phosphate that adds attapulgite clay mass percent 5.0%; 70 ℃ of following stirring reactions add the sal epsom of attapulgite clay mass percent 3% and 10% Natural manganese dioxide after 1 hour; Continue reaction 3 hours, cooling is after centrifugal, dry, pulverizing obtains attapulgite clay inorganic gel product.
As shown in table 1 with this physical and chemical performance index of inventing the attapulgite clay inorganic gel for preparing.
The physical and chemical performance index of table 1 attapulgite clay inorganic gel
Annotate: viscosity is NDJ rotary viscosity design determining data, is 5.0% water dispersion (25 ℃);
YV is six fast rotational viscosimeter 600r/min readings, is 5.0% water dispersion (25 ℃).
Claims (5)
1. the preparation method of an attapulgite clay inorganic gel is characterized in that preparing through the following step successively:
The preparation of A attapulgite clay suspension-s: under whipped state, attapulgite clay is added in the entry, process the suspension-s of concentration at 5-20wt%;
B attapulgite clay and phosphate reaction: under whipped state, in attapulgite clay suspension-s, add phosphoric acid salt, reacted 1～4 hour down at 50-80 ℃;
The C gelation reaction: under whipped state, in above-mentioned system, add magnesium salts, continue reaction 2-4 hour, cooling is after centrifugal, dry, pulverizing obtains the attapulgite clay inorganic gel.
2. the method for claim 1 is characterized in that phosphoric acid salt is any one or more in sodium phosphate, Sodium phosphate, dibasic, SODIUM PHOSPHATE, MONOBASIC, the Sodium hexametaphosphate 99.
3. like the method for claim 1 or 2, it is characterized in that the phosphoric acid salt add-on is 2%～10% of an attapulgite clay siccative weight.
4. the method for claim 1 is characterized in that magnesium salts is any one or more in Natural manganese dioxide, Marinco H, sal epsom, the magnesiumcarbonate.
5. like the method for claim 1 or 4, the add-on that it is characterized in that magnesium salts is 1～20% of an attapulgite clay siccative weight percent.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103691371A (en) * | 2013-11-29 | 2014-04-02 | 苏州中材非金属矿工业设计研究院有限公司 | Electrolyte-resistant composite mineral gel |
| CN103818916A (en) * | 2014-02-28 | 2014-05-28 | 中国科学院兰州化学物理研究所 | Method for preparing attapulgite nanometer inorganic gel by phytic acid modification |
| CN104096520A (en) * | 2014-07-15 | 2014-10-15 | 淮阴工学院 | Preparation method of fibrous inorganic mineral gel |
| CN104478238A (en) * | 2014-12-17 | 2015-04-01 | 苏州中材非金属矿工业设计研究院有限公司 | Bentonite-based mineral gel and preparation method thereof |
| CN104911230A (en) * | 2015-07-07 | 2015-09-16 | 中科院广州能源所盱眙凹土研发中心 | Bacterial cellulose in-situ fermentation production method |
| CN112830497A (en) * | 2021-03-03 | 2021-05-25 | 中国科学院兰州化学物理研究所 | Preparation method of high-viscosity attapulgite-based inorganic gel |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103691371A (en) * | 2013-11-29 | 2014-04-02 | 苏州中材非金属矿工业设计研究院有限公司 | Electrolyte-resistant composite mineral gel |
| CN103691371B (en) * | 2013-11-29 | 2016-03-16 | 苏州中材非金属矿工业设计研究院有限公司 | A kind of Electrolyte-resistancomposite composite mineral gel |
| CN103818916A (en) * | 2014-02-28 | 2014-05-28 | 中国科学院兰州化学物理研究所 | Method for preparing attapulgite nanometer inorganic gel by phytic acid modification |
| CN103818916B (en) * | 2014-02-28 | 2015-09-30 | 中国科学院兰州化学物理研究所 | The method of palygorskite nano inorganic gel is prepared in phytic acid modification |
| CN104096520A (en) * | 2014-07-15 | 2014-10-15 | 淮阴工学院 | Preparation method of fibrous inorganic mineral gel |
| CN104096520B (en) * | 2014-07-15 | 2015-11-25 | 淮阴工学院 | The preparation method of fibrous type inorganic mineral gel |
| CN104478238A (en) * | 2014-12-17 | 2015-04-01 | 苏州中材非金属矿工业设计研究院有限公司 | Bentonite-based mineral gel and preparation method thereof |
| CN104911230A (en) * | 2015-07-07 | 2015-09-16 | 中科院广州能源所盱眙凹土研发中心 | Bacterial cellulose in-situ fermentation production method |
| CN104911230B (en) * | 2015-07-07 | 2018-03-09 | 中科院广州能源所盱眙凹土研发中心 | The method that in-situ fermentation prepares bacteria cellulose |
| CN112830497A (en) * | 2021-03-03 | 2021-05-25 | 中国科学院兰州化学物理研究所 | Preparation method of high-viscosity attapulgite-based inorganic gel |
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Application publication date: 20120829 |