CN102000543A - Method for preparing inorganic montmorillonite material - Google Patents
Method for preparing inorganic montmorillonite material Download PDFInfo
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- CN102000543A CN102000543A CN 201010609368 CN201010609368A CN102000543A CN 102000543 A CN102000543 A CN 102000543A CN 201010609368 CN201010609368 CN 201010609368 CN 201010609368 A CN201010609368 A CN 201010609368A CN 102000543 A CN102000543 A CN 102000543A
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Abstract
The invention relates to a method for preparing an inorganic montmorillonite material, which comprises the following steps of: 1, preparing sodium montmorillonite; and 2, preparing the sodium montmorillonite and absolute ethyl alcohol into 0.5 to 4 percent of dispersion, and drying to prepare an inorganic montmorillonite film; or adding the dispersion onto a polyimide non-woven fabric, and drying to prepare a montmorillonite-polyimide composite material. The method has the characteristics of simple technology, high experimental repeatability, low production cost and the like; and the prepared composite material has excellent fireproof thermal insulation and good application prospect.
Description
Technical field
The invention belongs to the preparation field of imvite, particularly a kind of preparation method of inorganic montmorillonite material.
Background technology
Imvite is the stratiform clouds parent form silicate of 2: 1 types, and each unit cell constitutes by carrying an alumina octahedral secretly in the middle of two silicon-oxy tetrahedrons, the about 1nm of every layer thickness, and interlayer is adsorbed with Ca
2+, Mg
2+, Na
+Deng cation, easily by other cation replacements, they exist with the form of hydrated cation usually, and this hydrophilic microenvironment is unfavorable for the intercalation and the absorption of lipophilic polymer or monomer.Carry out ion-exchange with organic cation modifier and imvite, make hydrophilic imvite become oil loving imvite, simultaneously interlamellar spacing is extended, helps organic absorption or makes its intercalation.Can be used for the preparation of nano composite polymer-montmorillonoid material, or be used for waste water treatment as organic adsorbent.
In recent years, research to imvite mainly concentrates on the composite aspect, and great majority are with modified montmorillonoid, the intercalation imvite, or stripping divides imvite, be compounded to form synthetic material with another organic polymer material or inorganic matter, carry out many-side then and use, the application of composite is very extensive, can be used for fire-proof heat-insulating material, also can be used for adsorbent, catalyst, expanded material etc.As, patent CN101564874 provides a kind of preparation method of nanometer heat-insulation composite material, be exactly with nylon PA66, long alkali-free glass fibre, nano titanium oxide, nano imvite, adopt certain technology compound, prepare then have high tensile, high rigidity, forming stability excellent material.Patent CN1769338 provides a kind of preparation method of polyethylene/montmorillonite nanometer composite material, and montmorillonite layer is dispersed in the polyethylene matrix, makes composite by the original position method of formation then.Patent CN101597392 provides a kind of method for making of inorganic ions/foam polyolefin material, and this expanded material mechanical property is good, and preparation cost is low.Patent CN101239325 provides the preparation method of imvite/ZSM-5 molecular sieves compound material.The good hydrothermal stability of this composite is mainly used in all kinds of catalyst and adsorbent, especially the preparation of hydrogenation catalyst.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of inorganic montmorillonite material, and this method has characteristics such as technology is simple, the experiment favorable reproducibility, and production cost is low; The composite fire insulation performance that makes is good, has a good application prospect.
The preparation method of a kind of inorganic montmorillonite material of the present invention comprises:
(1) preparation of sodium imvite
The pure imvite of 2-5g SILVER REAGENT, 0.2-2.2gNaCl and 80-150ml distilled water are mixed, and the quality of NaCl is 2-6 a times of imvite cation exchange capacity CEC, in room temperature-100 ℃ reaction 2-12h, and cooling, centrifuge washing does not have Cl to clear liquid
-
(2) preparation of inorganic imvite film and imvite-composite polyimide material
Above-mentioned sodium imvite is mixed with ethanol and water mixed liquid, be configured to the dispersion liquid that percentage by weight is 0.5-4%, be uniformly dispersed, regulating dispersion liquid pH with the NaOH aqueous solution then is 8-13, and oven dry makes inorganic imvite film; Perhaps dispersion liquid is added on the polyimide nonwoven fabric, oven dry makes imvite-composite polyimide material.
The pure imvite of SILVER REAGENT in the described step (1) replaces with the sodium imvite and then directly carries out step (2), and the CEC of sodium imvite is 90mmol/100g, 110mmol/100g or 113mmol/100g, and purity＞90%, particle diameter are 2.0-10 μ m.
The percent by volume of second alcohol and water is 25%～50%: 50～75% in ethanol in the described step (2) and the water mixed liquid.
NaOH concentration of aqueous solution in the described step (2) is 1M.
The concrete technology that is uniformly dispersed in the described step (2) is handled montmorillonite dispersions 600-3200s for adopting the supersonic cell crusher, and power is 600-800W.
Bake out temperature in the described step (2) is a room temperature-60 ℃.
The percentage by weight 20%-140% of imvite in imvite-composite polyimide material in the described step (2), the thickness 2-3mm of polyimide nonwoven fabric material.
Beneficial effect
The present invention has characteristics such as technology is simple, the experiment favorable reproducibility, and production cost is low; The composite fire insulation performance that makes is good, has a good application prospect.
Description of drawings
Fig. 1 is imvite SEM, wherein, (a) is the SILVER REAGENT imvite; (b) for CEC be the Na-MMT of 90mmol/100g; (c) for CEC be the Na-MMT of 110mmol/100g;
Fig. 2 is pure imvite film SEM, and wherein (a) is pure imvite film front; (b) be pure imvite film side;
Fig. 3 is pure polyimides SEM;
Fig. 4 is imvite-composite polyimide material SEM.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
With pure imvite of 3g SILVER REAGENT and 0.39gNaCl, the quality of NaCl is 2.5 times of imvite CEC, and 100ml distilled water is inserted in the 250ml three-neck flask, and 100 ℃ are reacted 6h down, cooling, and centrifuge washing does not have Cl to clear liquid
-Till; With sodium imvite and ethanol: water (percent by volume 50%: 50%) is configured to the dispersion liquid 200g of percentage by weight 0.5%, using the cell pulverization instrument to handle 1600s under 600-800W is uniformly dispersed dispersion liquid, regulate the pH value to 10.5 of dispersion liquid then with the NaOH aqueous solution of 1M, this dispersion liquid is poured in the shallow mouthful of Flat bottom container, the thick 3mm of dispersion liquid, insert convection oven, flexible inorganic imvite film is promptly made in 40 ℃ of oven dry.
Embodiment 2
With pure imvite of 5g SILVER REAGENT and 0.59gNaCl, the quality of NaCl is 4 times of imvite CEC, and 100ml distilled water is inserted in the 250ml three-neck flask, and 80 ℃ are reacted 2h down, cooling, and centrifuge washing does not have Cl to clear liquid
-Till; With sodium imvite and ethanol: water (percent by volume 50%: 50%) is configured to the dispersion liquid 200g of percentage by weight 0.5%, using the cell pulverization instrument to handle 1600s under 600-800W is uniformly dispersed dispersion liquid, the pH value of regulating dispersion liquid with the NaOH aqueous solution of 1M is 9 then, this dispersion liquid is poured in the shallow mouthful of Flat bottom container, the thick 3mm of dispersion liquid, insert convection oven, 40 ℃ of oven dry promptly can be made into flexible inorganic imvite film.
Embodiment 3
With pure imvite of 2g SILVER REAGENT and 0.98gNaCl, the quality of NaCl is 6 times of imvite CEC, and 100ml distilled water is inserted in the 250ml three-neck flask, reacts 6h down at 100 ℃, cooling, and centrifuge washing does not have Cl to clear liquid
-Till; With sodium imvite and ethanol: water (percent by volume 25%: 75%) is configured to the dispersion liquid 200g of percentage by weight 1%, using the cell pulverization instrument to handle 1600s under 600-800W is uniformly dispersed dispersion liquid, the pH value of regulating dispersion liquid with the NaOH aqueous solution of 1M is 12 then, this dispersion liquid is poured in the shallow mouthful of Flat bottom container, the thick 2mm of dispersion liquid, insert convection oven, 40 ℃ of oven dry promptly can be made into flexible inorganic imvite film.
Embodiment 4
With pure imvite of 3g SILVER REAGENT and 0.39gNaCl, the quality of NaCl is 2.5 times of imvite CEC, and 100ml distilled water is inserted in the 250ml three-neck flask, reacts 12h down at 100 ℃, cooling, and centrifuge washing does not have Cl to clear liquid
-Till; With imvite and ethanol: water (percent by volume 50%: 50%) is configured to the dispersion liquid 200g of percentage by weight 1.5%, using the cell pulverization instrument to handle 600s under 600-800W is uniformly dispersed dispersion liquid, the pH value of regulating dispersion liquid with the NaOH aqueous solution of 1M is 12 then, divide several to drop to smooth polyimide nonwoven fabric material surface this dispersion liquid, insert convection oven, 40 ℃ of oven dry then can be made into imvite-composite polyimide material.
Embodiment 5
With sodium imvite (CEC is the sodium imvite of 90mmol/100g or 110mmol/100g) and ethanol: it is 4% dispersion liquid 200g that water (percent by volume 50%: 50%) is configured to percentage by weight, using the cell pulverization instrument to handle 3200s then under 600-800W is uniformly dispersed dispersion liquid, the pH value of regulating dispersion liquid with the NaOH aqueous solution of 1M is 12, this dispersion liquid is poured in the shallow mouthful of Flat bottom container, the dispersion liquid THICKNESS CONTROL is about 3mm, insert convection oven, 60 ℃ of oven dry promptly can be made into the inorganic imvite film of translucent flexibility.The material rate of body weight gain if being divided into several, this dispersion liquid drops to smooth polyimide nonwoven fabric material surface, if greater than 60%, can obtain having the imvite-composite polyimide material of good refractory heat-insulating performance so.
Claims (7)
1. the preparation method of an inorganic montmorillonite material comprises:
(1) preparation of sodium imvite
The pure imvite of 2-5g SILVER REAGENT, 0.2-2.2gNaCl and 80-150ml distilled water are mixed, and the quality of NaCl is 2-6 a times of imvite cation exchange capacity CEC, in room temperature-100 ℃ reaction 2-12h, and cooling, centrifuge washing does not have Cl to clear liquid
-
(2) preparation of inorganic imvite film and imvite-composite polyimide material
Above-mentioned sodium imvite is mixed with ethanol and water mixed liquid, be configured to the dispersion liquid that percentage by weight is 0.5-4%, be uniformly dispersed, regulating dispersion liquid pH with the NaOH aqueous solution then is 8-13, and oven dry makes inorganic imvite film; Perhaps dispersion liquid is added on the polyimide nonwoven fabric, oven dry makes imvite-composite polyimide material.
2. the preparation method of a kind of inorganic montmorillonite material according to claim 1, it is characterized in that: the pure imvite of SILVER REAGENT in the described step (1) replaces with the sodium imvite and then directly carries out step (2), the CEC of sodium imvite is 90mmol/100g, 110mmol/100g or 113mmol/100g, purity＞90%, particle diameter are 2.0-10 μ m.
3. the preparation method of a kind of inorganic montmorillonite material according to claim 1, it is characterized in that: the percent by volume of second alcohol and water is 25%～50%: 50～75% in ethanol in the described step (2) and the water mixed liquid.
4. the preparation method of a kind of inorganic montmorillonite material according to claim 1, it is characterized in that: the NaOH concentration of aqueous solution in the described step (2) is 1M.
5. the preparation method of a kind of inorganic montmorillonite material according to claim 1 is characterized in that: the concrete technology that is uniformly dispersed in the described step (2) is handled montmorillonite dispersions 600-3200s for adopting the supersonic cell crusher, and power is 600-800W.
6. the preparation method of a kind of inorganic montmorillonite material according to claim 1 is characterized in that: the bake out temperature in the described step (2) is a room temperature-60 ℃.
7. the preparation method of a kind of inorganic montmorillonite material according to claim 1, it is characterized in that: the percentage by weight 20%-140% of imvite in the imvite-composite polyimide material in the described step (2), the thickness 2-3mm of polyimide nonwoven fabric material.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102225335A (en) * | 2011-04-28 | 2011-10-26 | 武汉大学 | Denitration catalyst for flue gas and preparation method thereof |
| CN105983386A (en) * | 2015-02-26 | 2016-10-05 | 天津市四维康环保科技发展有限公司 | Preparation and application of non-woven fabric |
| CN107503122A (en) * | 2017-08-23 | 2017-12-22 | 江西诚达工程咨询监理有限公司 | A kind of preparation method of electric wire fire proofing |
| CN115536313A (en) * | 2022-09-14 | 2022-12-30 | 山西水务物资贸易有限公司 | Modified clay-based water and soil conservation film spraying material, preparation method and use method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000022010A1 (en) * | 1998-10-08 | 2000-04-20 | Basf Aktiengesellschaft | Polyolefin nanocomposites |
| US6613711B2 (en) * | 2001-08-03 | 2003-09-02 | Changchun Institute Of Applied Chemistry, Chinese Academy Of Sciences | Clay-titanium tetrachloride catalyst and the preparation thereof |
| CN1769338A (en) * | 2004-11-05 | 2006-05-10 | 中国科学院化学研究所 | Polyethylene /montmorillonite nanometer composite material and preparation method |
| CN101564874A (en) * | 2009-05-27 | 2009-10-28 | 靳柱山 | Method for preparing nanometer heat-insulation composite material |
-
2010
- 2010-12-28 CN CN 201010609368 patent/CN102000543B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000022010A1 (en) * | 1998-10-08 | 2000-04-20 | Basf Aktiengesellschaft | Polyolefin nanocomposites |
| US6613711B2 (en) * | 2001-08-03 | 2003-09-02 | Changchun Institute Of Applied Chemistry, Chinese Academy Of Sciences | Clay-titanium tetrachloride catalyst and the preparation thereof |
| CN1769338A (en) * | 2004-11-05 | 2006-05-10 | 中国科学院化学研究所 | Polyethylene /montmorillonite nanometer composite material and preparation method |
| CN101564874A (en) * | 2009-05-27 | 2009-10-28 | 靳柱山 | Method for preparing nanometer heat-insulation composite material |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102225335A (en) * | 2011-04-28 | 2011-10-26 | 武汉大学 | Denitration catalyst for flue gas and preparation method thereof |
| CN105983386A (en) * | 2015-02-26 | 2016-10-05 | 天津市四维康环保科技发展有限公司 | Preparation and application of non-woven fabric |
| CN105983386B (en) * | 2015-02-26 | 2019-04-30 | 天津市四维康环保科技发展有限公司 | A kind of preparation method of non-woven fabrics |
| CN107503122A (en) * | 2017-08-23 | 2017-12-22 | 江西诚达工程咨询监理有限公司 | A kind of preparation method of electric wire fire proofing |
| CN107503122B (en) * | 2017-08-23 | 2020-07-28 | 江西诚达工程咨询监理有限公司 | Preparation method of wire and cable flame-retardant material |
| CN115536313A (en) * | 2022-09-14 | 2022-12-30 | 山西水务物资贸易有限公司 | Modified clay-based water and soil conservation film spraying material, preparation method and use method |
| CN115536313B (en) * | 2022-09-14 | 2023-09-29 | 山西水控实业有限公司 | Modified clay-based water and soil conservation spray film material, preparation method and use method |
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