CN102627285A - Novel montmorillonite nanometer complex and preparation method thereof - Google Patents
Novel montmorillonite nanometer complex and preparation method thereof Download PDFInfo
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- CN102627285A CN102627285A CN2012101244220A CN201210124422A CN102627285A CN 102627285 A CN102627285 A CN 102627285A CN 2012101244220 A CN2012101244220 A CN 2012101244220A CN 201210124422 A CN201210124422 A CN 201210124422A CN 102627285 A CN102627285 A CN 102627285A
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Abstract
The invention relates to a novel montmorillonite nanometer complex, in particular to the montmorillonite nanometer complex consisting of a polyether ammonium cation, Ti4<+> or/and Sb3<+> ions and montmorillonite as well as a preparation method of the montmorillonite nanometer complex. According to the montmorillonite nanometer complex, the polyether ammonium cation accounts for 5-80 percent by weight of the total amount of the polyether ammonium cation, and the Ti4<+> ion or the Sb3<+> ion or the Ti4<+> and the Sb3<+> ions account for 0.00001-2 percent by weight of the total amount of the montmorillonite nanometer complex. Under the conditions of normal pressure and room temperature of 100DEG C, polyether ammonium salt, titanium tetrachloride or/and antimony trichloride ion are intercalated into the montmorillonite to obtain the montmorillonite nanometer complex. The montmorillonite nanometer complex is simple in preparation process, is mild in conditions and easy in industrial production.
Description
Technical field
The present invention relates to a kind of new modified polynite, particularly a kind of by polyethers ammonium cation, Ti
4+Or/and Sb
3+Common modified montmorillonoid complex body of forming of ion and polynite and preparation method thereof.
Background technology
Inorganic column clay specific surface area is big, thermostability is high, is the one type of porous new function material that receives extensive concern in recent decades and obtain developing rapidly.They are to natural clay and the big specific surface area of Yan Yougeng and unique pore structure, thereby have shown wide application potential in petrochemical complex and environmental protection field as selected adsorbent, catalyzer and support of the catalyst etc.In the 1980s, having prepared aluminium at first is the intercalation polynite, but its specific surface area is not ideal enough.Afterwards, it is found that the titanium pillared montmorillonite has bigger duct, higher heat or hydrothermal stability, and good photocatalytic activity have obtained using widely.
Publication number is that the patent of CN102258993A has prepared titanium oxide polynite photocatalyst, and polynite is compared, and the porosity of this photocatalyst, specific surface area and pore volume significantly improve.Publication number is that the patent of CN1872908A is inserted polynite with titanium tetrachloride, has prepared titanium-montmorillonite catalyst, is used to prepare the matrix material of Vilaterm and multipolymer and polynite.Publication number is that the patent of CN1330101A also is that titanium tetrachloride is inserted polynite, has prepared the montmorillonite load titanium catalyst, is used to prepare the matrix material of polyolefine such as Vilaterm, Vestolen PP 7052 and polynite.BJ University of Aeronautics & Astronautics developed the antimony pillared montmorillonite in 2010, and used it in the preparation of polyester/Nano composite material of montmorillonite, had obtained good effect.Yet, less to the patent report of antimony pillared montmorillonite.
The characteristics of polyethers ammonium salt modified montmorillonoid are that the interlamellar spacing of polynite is bigger, can reach more than the 8nm.Adopt polyetheramine D2000 salt manufacturing, the polyethers ammonium modified montmorillonoid that intercalation obtains like calendar year 2001 Lin J.J..Salahuddin N.A. adopted the polynite of polyetheramine T5000 salt manufacturing intercalation in 2004, and modified montmorillonoid is used for the preparation of high-performance epoxy resin.Yet, less about the patent of polyethers ammonium modified montmorillonoid.Publication number is that the patent of CN1693549A is used the modified by polyether glycol polynite, is used for the preparation of montmorillonite/polyurethane nano composite material.
Yet, about polyethers ammonium cation, Ti
4+Or/and Sb
3+The modified montmorillonoid of common intercalation polynite preparation will have polyethers ammonium modified montmorillonoid and Ti concurrently
4+Ion is or/and Sb
3+The performance of ion modification polynite, the research and the related patent U.S. Patent No. of this respect are not at home and abroad appeared in the newspapers as yet.
Summary of the invention
One of the object of the invention provides a kind of by polyethers ammonium cation, Ti
4+Or/and Sb
3+The common montmorillonite-based nano complex body of forming of ion and polynite.
Another object of the present invention provides a kind of preparation by polyethers ammonium cation, Ti
4+Or/and Sb
3+The method of the common montmorillonite-based nano complex body of forming of ion and polynite.
Novel montmorillonite-based nano complex body involved in the present invention is by polyethers ammonium cation, Ti
4+Or/and Sb
3+Ion and polynite are formed jointly.Wherein, the polyethers ammonium cation accounts for the 5wt%～80wt% of montmorillonite-based nano complex body total amount, Ti
4+Ion or Sb
3+The summation of ion or this two metal ion species accounts for the 0.00001wt%～2wt% of montmorillonite-based nano complex body total amount.
The preparation method of novel montmorillonite-based nano complex body involved in the present invention is: under the temperature condition of normal pressure, room temperature～100 ℃; With polyethers ammonium salt, titanium tetrachloride or/and butter of antimony under certain kind and certain amount of solvent condition; The intercalation polynite; Reflux 0.5-8 hour, obtain the montmorillonite-based nano complex body.
Described novel montmorillonite-based nano complex body, the polyethers ammonium cation accounts for the 10wt%～40wt% of montmorillonite-based nano complex body total amount, Ti
4+Ion or Sb
3+The total amount of ion or this two metal ion species accounts for the 0.001wt%～1wt% of montmorillonite-based nano complex body total amount.
Described polyethers ammonium salt is by polyether diamine or polyethers triamine and hydrochloride aqueous solution prepared in reaction.The molecular-weight average of described polyether diamine or polyethers triamine is 400～6000.Fig. 1 is several kinds of commodity polyether diamines and polyethers triamine.
The mixing solutions that water or acetone or water and acetone are adopted in described polyethers ammonium cation and polynite reaction is as dispersion medium, and temperature of reaction is 60～80 ℃.
Described Ti
4+Ion or Sb
3+Ion or this two metal ion species are common during with the polynite reaction, and employing ethanol or water or water and alcoholic acid mixing solutions are as dispersion medium, and temperature of reaction is 60～80 ℃.
The intercalation of described positively charged ion and polynite is: earlier with the polynite of polyethers ammonium salt intercalation, use titanium tetrachloride again or/and the polynite of butter of antimony intercalation; Or earlier with titanium tetrachloride or/and the polynite of polyethers ammonium salt intercalation is used in the polynite of butter of antimony intercalation again.
Novel montmorillonite-based nano complex body of the present invention; Have characteristics such as specific surface area is big, Heat stability is good; The additive that can be used as sorbent material, catalyzer and high-performance nano polymkeric substance; Under 200-300 ℃ temperature condition, still have certain stability, can satisfy relatively harsher actual environment for use or high temperature adding technology condition.And the preparation technology of this novel montmorillonite-based nano complex body is simple, mild condition, does not use the difficult Fatty Alcohol(C12-C14 and C12-C18) of removing, and does not relate to complicated aftertreatment technology, is easy to suitability for industrialized production.
Description of drawings
Embodiment
The 5.6g titanium tetrachloride is dissolved in the Hydrogen chloride that 100ml concentration is 1mol/L, is configured to the titanium intercalation solution.The 15g sodium-based montmorillonite is dispersed in the deionized water of 750ml, is mixed with montmorillonite suspension liquid.Under the condition of room temperature, magnetic agitation, the titanium intercalation solution is slowly splashed in the montmorillonite suspension liquid, dropwise the afterreaction system and be warming up to 80 ℃, magnetic agitation refluxed 0.5 hour obtains titanium intercalation polynite mixed solution.Reaction mixture is centrifugal, obtain titanium-polynite.
1.7g polyetheramine D400 is dissolved in the 36ml acetone, and 1.5g hydrochloric acid soln (37wt%) mixes with the 12ml deionized water, and under the magnetic agitation, dripping hydrochloric acid solution in the D400 acetone soln dropwises continued magnetic agitation 3h, obtains polyethers ammonium salt D400 solution.Above-mentioned titanium-polynite is dispersed in the deionized water of 1000ml, drips D400 polyethers ammonium salt solution under the room temperature while stirring, after dropwising, reaction system is warming up to 80 ℃, magnetic agitation refluxed 0.5 hour.Reaction mixture is centrifugal, separate obtaining D400 polyethers ammonium cation and Ti
4+The montmorillonite-based nano complex body of modified synergic.
Embodiment 2
The 2.8g titanium tetrachloride is dissolved in the Hydrogen chloride that 100ml concentration is 1mol/L, is configured to the titanium intercalation solution.The 15g sodium-based montmorillonite is dispersed in the absolute ethyl alcohol of 100ml, is mixed with montmorillonite suspension liquid.Under the condition of room temperature, magnetic agitation, the titanium intercalation solution is slowly splashed in the montmorillonite suspension liquid, dropwise the afterreaction system and be warming up to 60 ℃, magnetic agitation refluxed 8 hours obtains titanium intercalation polynite mixed solution.Reaction mixture is centrifugal, isolate the polynite of titanium intercalation.
After 25g polyetheramine D2000,2.6g hydrochloric acid soln (37wt%) mixed with the 20mL deionized water, magnetic agitation 3h obtained D2000 polyethers ammonium salt.The polynite of titanium intercalation is dispersed in the deionized water of 1000ml and the mixed solvent of acetone (volume ratio 1: 1), drips D2000 polyethers ammonium salt solution under the room temperature while stirring, after dropwising, reaction system is warming up to 60 ℃, magnetic agitation refluxed 8 hours.Reaction mixture is centrifugal, separate obtaining D2000 polyethers ammonium salt and Ti
4+The montmorillonite-based nano complex body.
Embodiment 3
25g polyetheramine T5000 is dissolved in the 48ml acetone, adds 1.5g hydrochloric acid soln (37wt%) and 20mL deionized water mixed solution under the room temperature magnetic agitation, continue magnetic agitation 3h, obtain T5000 polyethers ammonium salt intercalation solution.The 15g sodium-based montmorillonite is dispersed in the acetone of 1000ml, is mixed with montmorillonite suspension liquid.Under the condition of room temperature, magnetic agitation, T5000 polyethers ammonium salt intercalation solution is slowly splashed in the montmorillonite suspension liquid, after dropwising, reaction system is warming up to 70 ℃, magnetic agitation refluxed 4 hours obtains T5000 polyethers ammonium salt intercalation polynite mixed solution.Reaction mixture is centrifugal, isolate the polynite of T5000 polyethers ammonium salt intercalation.
The 0.07g titanium tetrachloride is dissolved in the Hydrogen chloride that 100ml concentration is 1mol/L, is configured to the titanium intercalation solution.The polynite of T5000 polyethers ammonium salt intercalation is dispersed in 1000ml deionized water and the ethanol mixed solvent (volume ratio 1: 1), obtains the suspension-s of T5000 polyethers ammonium salt intercalation polynite.Under room temperature, magnetic agitation condition, the titanium intercalation solution is slowly splashed in the T5000 polyethers ammonium salt intercalation montmorillonite suspension liquid; Dropwise the afterreaction system and be warming up to 70 ℃; Magnetic agitation refluxed 4 hours, reaction mixture is centrifugal, separate obtaining T5000 polyethers ammonium salt and Ti
4+The montmorillonite-based nano complex body.
Embodiment 4
The 2.8g titanous chloride is dissolved in the Hydrogen chloride that 100ml concentration is 1mol/L, is configured to the titanium intercalation solution.The 15g sodium-based montmorillonite is dispersed in the deionized water of 750ml, is mixed with montmorillonite suspension liquid.Under the condition of room temperature, magnetic agitation, the titanium intercalation solution is slowly splashed in the montmorillonite suspension liquid, dropwise the afterreaction system and be warming up to 80 ℃, magnetic agitation refluxed 1 hour obtains titanium intercalation polynite mixed solution.Reaction mixture is centrifugal, obtain titanium-polynite.
3.3g polyetheramine D400 is dissolved in the 72ml acetone, and 1.5g hydrochloric acid soln (37wt%) mixes with the 12ml deionized water,
Under the magnetic agitation, dripping hydrochloric acid solution in the D400 acetone soln dropwises continued magnetic agitation 3h, obtains polyethers ammonium salt D400 solution.Above-mentioned titanium-polynite is dispersed in the deionized water of 1000ml, drips D400 polyethers ammonium salt solution under the room temperature while stirring, after dropwising, reaction system is warming up to 80 ℃, magnetic agitation refluxed 1 hour.Reaction mixture is centrifugal, separate obtaining D400 polyethers ammonium cation and Ti
3+The montmorillonite-based nano complex body of modified synergic.
Embodiment 5
2g titanium tetrachloride and 2g butter of antimony are dissolved in the Hydrogen chloride that 100ml concentration is 1mol/L, are configured to titanium/antimony intercalation solution.The 15g sodium-based montmorillonite is dispersed in the absolute ethyl alcohol of 750ml, is mixed with montmorillonite suspension liquid.Under the condition of room temperature, magnetic agitation, titanium/antimony intercalation solution is slowly splashed in the montmorillonite suspension liquid, dropwise the afterreaction system and be warming up to 60 ℃, magnetic agitation refluxed 5 hours obtains titanium/antimony intercalation polynite mixed solution.Reaction mixture is centrifugal, isolate Ti
4+And Sb
3+The intercalation polynite.
After 25g polyetheramine T3000,2.6g hydrochloric acid soln (37wt%) mixed with the 20mL deionized water, magnetic agitation 3h obtained T3000 polyethers ammonium salt.Titanium/antimony intercalation polynite is dispersed in the deionized water of 1000ml and the mixed solvent of acetone (volume ratio 1: 1), drips T3000 polyethers ammonium salt solution under the room temperature while stirring, after dropwising, reaction system is warming up to 70 ℃, magnetic agitation refluxed 2 hours.Reaction mixture is centrifugal, separate obtaining T3000 polyethers ammonium salt, Ti
4+And Sb
3+The montmorillonite-based nano complex body.
Embodiment 6
25g polyetheramine D4000 is dissolved in the 48ml acetone, adds 1.5g hydrochloric acid soln (37wt%) and 20mL deionized water mixed solution under the room temperature magnetic agitation, continue magnetic agitation 3h, obtain D4000 polyethers ammonium salt intercalation solution.The 15g sodium-based montmorillonite is dispersed in the acetone of 1000ml, is mixed with montmorillonite suspension liquid.Under the condition of room temperature, magnetic agitation, D4000 polyethers ammonium salt intercalation solution is slowly splashed in the montmorillonite suspension liquid, after dropwising, reaction system is warming up to 70 ℃, magnetic agitation refluxed 6 hours obtains D4000 polyethers ammonium salt intercalation polynite mixed solution.Reaction mixture is centrifugal, isolate the polynite of D4000 polyethers ammonium salt intercalation.
The 8g butter of antimony is dissolved in the Hydrogen chloride that 100ml concentration is 1mol/L, is configured to the antimony intercalation solution.The polynite of D4000 polyethers ammonium salt intercalation is dispersed in 1000ml deionized water and the ethanol mixed solvent (volume ratio 1: 1), obtains the suspension-s of D4000 polyethers ammonium salt intercalation polynite.Under room temperature, magnetic agitation condition, the antimony intercalation solution is slowly splashed in the D4000 polyethers ammonium salt intercalation montmorillonite suspension liquid; Dropwise the afterreaction system and be warming up to 70 ℃; Magnetic agitation refluxed 6 hours, reaction mixture is centrifugal, separate obtaining D4000 polyethers ammonium salt and Sb
3+The montmorillonite-based nano complex body.
Embodiment 7
The 0.2g butter of antimony is dissolved in the Hydrogen chloride that 100ml concentration is 1mol/L, is configured to the antimony intercalation solution.The 15g sodium-based montmorillonite is dispersed in the deionized water of 500ml, is mixed with montmorillonite suspension liquid.Under the condition of room temperature, magnetic agitation, the antimony intercalation solution is slowly splashed in the montmorillonite suspension liquid, dropwise the afterreaction system and be warming up to 50 ℃, magnetic agitation refluxed 5 hours obtains antimony intercalation polynite mixed solution.Reaction mixture is centrifugal, isolate Sb
3+The intercalation polynite.
After 25g polyetheramine D2000,2.6g hydrochloric acid soln (37wt%) mixed with the 20mL deionized water, magnetic agitation 3h obtained D2000 polyethers ammonium salt.The polynite of antimony intercalation is dispersed in the deionized water of 1000ml and the mixed solvent of acetone (volume ratio 1: 1), drips D2000 polyethers ammonium salt solution under the room temperature while stirring, after dropwising, reaction system is warming up to 50 ℃, magnetic agitation refluxed 5 hours.Reaction mixture is centrifugal, separate obtaining D2000 polyethers ammonium salt and Sb
3+The montmorillonite-based nano complex body.
Embodiment 8
6g polyetheramine D400 is dissolved in the 100ml acetone, and 3g hydrochloric acid soln (37wt%) mixes with the 20ml deionized water, and under the magnetic agitation, dripping hydrochloric acid solution in the D400 acetone soln dropwises continued magnetic agitation 3h, obtains polyethers ammonium salt D400 solution.The 15g sodium-based montmorillonite is dispersed in the deionized water of 750ml, drips D400 polyethers ammonium salt solution under the room temperature while stirring, after dropwising, magnetic agitation is 7 hours at ambient temperature.Reaction mixture is centrifugal, separate obtaining the polynite of D400 polyethers ammonium cation intercalation.
0.1g titanium tetrachloride and 8g butter of antimony are dissolved in the Hydrogen chloride that 100ml concentration is 1mol/L, are configured to titanium/antimony intercalation solution.The polynite of D400 polyethers ammonium cation intercalation is dispersed in the deionized water of 750ml, is mixed with montmorillonite suspension liquid.Under the condition of room temperature, magnetic agitation, titanium/antimony intercalation solution is slowly splashed in the montmorillonite suspension liquid, dropwise the afterreaction system and continue to keep room temperature, magnetic agitation 7 hours obtains polyethers ammonium salt and titanium/antimony intercalation polynite mixed solution.Reaction mixture is centrifugal, isolate D400 polyethers ammonium cation, Ti
4+And Sb
3+The montmorillonite-based nano complex body.
Claims (9)
1. montmorillonite-based nano complex body, it is characterized in that: this montmorillonite-based nano complex body is by polyethers ammonium cation, Ti
4+Or/and Sb
3+Ion and polynite are formed jointly, and wherein the polyethers ammonium cation accounts for the 5wt%～80wt% of montmorillonite-based nano complex body total amount, Ti
4+Ion or Sb
3+The total amount of ion or this two metal ion species accounts for the 0.00001wt%～2wt% of montmorillonite-based nano complex body total amount.
2. montmorillonite-based nano complex body according to claim 1 is characterized in that: the polyethers ammonium cation accounts for the 10wt%～40wt% of montmorillonite-based nano complex body total amount, Ti
4+Ion or Sb
3+The total amount of ion or this two metal ion species accounts for the 0.001wt%～1wt% of montmorillonite-based nano complex body total amount.
3. the preparation method of a montmorillonite-based nano complex body according to claim 1; It is characterized in that: under the temperature condition of normal pressure, room temperature～100 ℃; With polyethers ammonium salt, titanium tetrachloride or/and the polynite of butter of antimony intercalation obtains the montmorillonite-based nano complex body.
4. method according to claim 2 is characterized in that: the polyethers ammonium salt is by polyether diamine or polyethers triamine and hydrochloride aqueous solution prepared in reaction.
5. polyether diamine according to claim 3 or polyethers triamine is characterized in that: the molecular-weight average of polyether diamine or polyethers triamine is 400～6000.
6. method according to claim 2; It is characterized in that: the mixing solutions that water or acetone or water and acetone are adopted in polyethers ammonium cation and polynite reaction is as dispersion medium; The polyethers ammonium cation is 0.5～2 with the CEC ratio of polynite, and temperature of reaction is that 60～80 ℃ of reaction times are 0.5～8 hour.
7. method according to claim 2; It is characterized in that: when metals ion and polynite reaction, adopt ethanol or water or water and alcoholic acid mixing solutions as dispersion medium, metallic cation is 0.1～8 with the CEC ratio of polynite; Temperature of reaction is 60～80 ℃, and the reaction times is 0.5～8 hour.
8. method according to claim 2 is characterized in that: earlier with the polynite of polyethers ammonium salt intercalation, use titanium tetrachloride again or/and the polynite of butter of antimony intercalation.
9. method according to claim 2 is characterized in that: earlier with titanium tetrachloride or/and the polynite of polyethers ammonium salt intercalation is used in the polynite of butter of antimony intercalation again.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103193242A (en) * | 2013-04-09 | 2013-07-10 | 苏州旭达环保科技有限公司 | Montmorillonoid loaded polyethyleneimine water treatment agent as well as preparation method and application thereof |
| CN105419262A (en) * | 2014-09-02 | 2016-03-23 | 允友成(宿迁)复合新材料有限公司 | Polylactic acid/montmorillonite nanometer composite material preparation method |
| CN105732962A (en) * | 2014-12-11 | 2016-07-06 | 中国石油天然气股份有限公司 | Preparation method of polyethylene glycol terephthalate/montmorillonite nano composite material |
| CN105732961A (en) * | 2014-12-11 | 2016-07-06 | 中国石油天然气股份有限公司 | Preparation method of polyethylene glycol terephthalate nano composite material |
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| CN1872908A (en) * | 2005-05-31 | 2006-12-06 | 中国石油天然气股份有限公司 | Method for preparing catalyst of montmorillonite-titanium tetrachloride, and composite material of polyethylene/montmorillonite |
| US20090146107A1 (en) * | 2007-12-07 | 2009-06-11 | National Taiwan University | Inorganic/organic dispersant and application thereof |
| CN101717562A (en) * | 2009-11-27 | 2010-06-02 | 北京航空航天大学 | Transparent high-barrier polyethylene glycol terephthalate composite material product |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103193242A (en) * | 2013-04-09 | 2013-07-10 | 苏州旭达环保科技有限公司 | Montmorillonoid loaded polyethyleneimine water treatment agent as well as preparation method and application thereof |
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| CN105419262A (en) * | 2014-09-02 | 2016-03-23 | 允友成(宿迁)复合新材料有限公司 | Polylactic acid/montmorillonite nanometer composite material preparation method |
| CN105732962A (en) * | 2014-12-11 | 2016-07-06 | 中国石油天然气股份有限公司 | Preparation method of polyethylene glycol terephthalate/montmorillonite nano composite material |
| CN105732961A (en) * | 2014-12-11 | 2016-07-06 | 中国石油天然气股份有限公司 | Preparation method of polyethylene glycol terephthalate nano composite material |
| CN105732961B (en) * | 2014-12-11 | 2018-06-01 | 中国石油天然气股份有限公司 | The preparation method of polyethylene terephthalate nanocomposite |
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