CN101269821A - Ion thermal method for preparing molecular sieve in alcohol amine ion liquid - Google Patents
Ion thermal method for preparing molecular sieve in alcohol amine ion liquid Download PDFInfo
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- CN101269821A CN101269821A CNA2008101059825A CN200810105982A CN101269821A CN 101269821 A CN101269821 A CN 101269821A CN A2008101059825 A CNA2008101059825 A CN A2008101059825A CN 200810105982 A CN200810105982 A CN 200810105982A CN 101269821 A CN101269821 A CN 101269821A
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Abstract
The invention relates to an ion heat method for preparing a molecular sieve in alcohol-amine ionic liquid, and the used alcohol-amine ionic liquid ism ammonium ethanol-acetate and triethanolamine-lactate. Aluminum isopropoxide, phosphoric acid and hydrofluoric acid are used as raw materials, and after an ion heat crystallization process, filtration, washing and drying, aluminophosphate molecular sieves of AEL type, an AFI type and a GIS type which are widely applied are obtained. The synthetic method of the invention has the advantages of simplicity, safety and friendly environment, and has important value in the field of the material science.
Description
Invention field: the present invention relates to a kind of ion thermal method that in alcohol amine ion liquid, prepares molecular sieve of chemical field.The synthetic molecular sieve can be used for ion-exchange, catalysis and gas storage art.
Background of invention:
Because molecular sieve has special pore passage structure, be widely used in the separation etc. of drying, purification and organic alkane isomer of fractionation by adsorption such as gas; A large amount of Industrial Catalysis process in the fields such as refining of petroleum, petrochemical complex, Coal Chemical Industry and fine chemistry industry; In refining of petroleum and the detergent industry as auxiliary agent and be used for the processing of atomic waste and the fields such as processing of storage and factories and miness waste liquid.Along with the intersection of material science and development fast, porous material obtains deep development at high-technology field, and it is more and more getting more and more people's extensive concerning aspect the Subjective and Objective assembling as main body.Since the aluminium phosphate molecular sieve of 1982 non-silicon occurred, the constitutional chemistry and the structural chemistry of crystalline microporous material had greatly been enriched in the structure type sharp increase of molecular sieve.Because aluminium phosphate molecular sieve family not only comprises having macropore, mesopore and small pore molecular sieve, but also can will comprise main group metal and transition metal and nonmetal 13 kinds of elements (Li, Be, B, Mg, Si, Ga, Ge, As, Ti, Mn, Fe, Co, Zn), introduce framework of molecular sieve.
At present, at present most molecular sieve is that water (solvent) by the use of thermal means under different condition obtains.Use organic amine or ammonium salt as structure directing agent in the reaction process, water or alcohol are made solvent.The proposition of ion process for thermosynthesizing is that new approach has been opened up in the development of molecular sieve.The ion process for thermosynthesizing is meant that reaction process intermediate ion liquid both made solvent simultaneously as structure directing agent, avoided reaction under high pressure, strengthened the security of experiment, topmost characteristics have reduced the effect of solvent-skeleton structure and the competition of structure directing agent-skeleton structure effect, the easier target product that obtains.Yet what use in the ion thermal synthesis process at present mainly is glyoxaline ion liquid.It is simple that alcohol amine ion liquid has synthetic method, the raw material cheapness, and advantage such as viscosity is low, and be applied to the molecular sieve that ion thermal synthesis molecular sieve can obtain novel texture.
Summary of the invention
The object of the present invention is to provide a kind of ion thermal method that in alcohol amine ion liquid, prepares molecular sieve.
Alcohol amine ion liquid is synthetic simple, and raw material is cheap and easy to get, reduces synthetic cost, is fit to industrial-scale production.Adopting alcohol amine ion liquid is solvent and structure directing agent synthesis of molecular sieve, can avoid the use of volatile organic solvent, and reaction simultaneously can be carried out under normal pressure; This method makes the condition of synthesis of molecular sieve be easy to control, avoids the appearance of stray crystal phase, improves the quality of product, to satisfy scale operation and industrial application demand.
Concrete grammar of the present invention may further comprise the steps:
Synthesizing of the first step alcohol amine ion liquid
Adopt a step neutralisation to prepare the alcamines ionic liquid.Choose alcamine compound and comprise thanomin and trolamine; Carboxylic acid compound comprises acetate and lactic acid.According to equimolar hydramine and carboxylic acid is that solvent generates alcohol amine ion liquid by a step neutralization reaction with ethanol under normal temperature, normal pressure, is respectively thanomin acetate and trolamine lactic acid salt.
Second step ion thermal synthesis molecular sieve
With alcohol amine ion liquid, aluminum isopropylate, phosphoric acid (85% in H
2O), hydrofluoric acid (40% in H
2O) add according to a certain percentage successively in the 23ml polytetrafluoroethyllining lining stainless steel cauldron, be heated to corresponding temperature 130-180 ℃, reduce to room temperature through nature after the reaction 3-7d, go out product with deionized water behind the still and repeatedly drip washing filtration of ethanol, drying.Obtain AEL type aluminium phosphate molecular sieve in thanomin acetate ions thermal synthesis system, obtain AFI type and GIS type aluminium phosphate molecular sieve in trolamine lactate ions thermal synthesis system.
Phosphorus aluminum ratio in the described reaction system is 0.8-7.0.
Fluorine aluminum ratio in the described reaction system is 1.8-4.5.
Ionic liquid in the described reaction system and aluminum ratio are 5-60.
The temperature of reaction of described reaction system is 130-180 ℃.
The reaction times of described reaction system is 3-7d.
Description of drawings
The XRD spectra of the aluminium phosphate molecular sieve sample that Fig. 1 obtains under 130 ℃ of conditions in HEA
The XRD spectra of the aluminium phosphate molecular sieve sample that Fig. 2 obtains under 140 ℃ of conditions in HEA
The XRD spectra of the aluminium phosphate molecular sieve sample that Fig. 3 obtains under 150 ℃ of conditions in HEA
The XRD spectra of the aluminium phosphate molecular sieve sample that Fig. 4 obtains under the condition of different temperatures in THEAL
Embodiment:
The present invention illustrates with following example, but the present invention is not limited to following embodiment, under the scope of described aim, changes and implements to be included in the technical scope of the present invention before and after not breaking away from.
Embodiment 1
Synthesizing of the first step ethanol ammonium acetate ions liquid
Building-up process places 25 ℃ water bath with thermostatic control for add the alcohol mixed solution that 100ml contains 24g (0.5mol) thanomin in the 500ml there-necked flask of reflux is housed; Agitation and dropping 100ml contains the alcohol mixed solution of 30g (0.5mol) acetate, and it is muddy that mixture becomes gradually, and reaction places Rotary Evaporators to remove ethanol mixing solutions after finishing, and obtains light yellow viscous liquid; Products obtained therefrom is placed 60 ℃ the dry 48h of vacuum drying oven, get lurid ethanol ammonium acetate ions liquid.
Second step ion thermal synthesis molecular sieve
With ethanol ammonium acetate ions liquid HEA, Al[OCH (CH
3)
2]
3, H
3PO
4(85% in H
2O), HF (40% in H
2O) Al according to a certain percentage successively
2O
3: xP
2O
5: (T=130 ℃ of 3.6HF: 40IL (x=0.8-7.0), t=3d) add in the 23ml polytetrafluoroethyllining lining stainless steel cauldron, reacting by heating 3 days is reduced to room temperature through nature afterwards, goes out product with deionized water behind the still and repeatedly drip washing filtration of ethanol, drying.
Embodiment 2
Synthesizing of the first step ethanol ammonium acetate ions liquid
Building-up process places 25 ℃ water bath with thermostatic control for add the alcohol mixed solution that 100ml contains 24g (0.5mol) thanomin in the 500ml there-necked flask of reflux is housed; Agitation and dropping 100ml contains the alcohol mixed solution of 30g (0.5mol) acetate, it is muddy that mixture becomes gradually, reaction places Rotary Evaporators to remove ethanol mixing solutions after finishing, and obtains light yellow viscous liquid, products obtained therefrom is placed 60 ℃ the dry 48h of vacuum drying oven.Get lurid ethanol ammonium acetate ions liquid.
Second step ion thermal synthesis molecular sieve
With ethanol ammonium acetate ions liquid HEA, Al[OCH (CH
3)
2]
3, H
3PO
4(85% in H
2O), HF (40% in H
2O) Al according to a certain percentage successively
2O
3: xP
2O
5: (T=140 ℃ of 3.6HF: 40IL (x=0.8-7.0), t=3d) add in the 23ml polytetrafluoroethyllining lining stainless steel cauldron, reacting by heating 3 days is reduced to room temperature through nature afterwards, goes out product with deionized water behind the still and repeatedly drip washing filtration of ethanol, drying.
Embodiment 3
Synthesizing of the first step ethanol ammonium acetate ions liquid
Building-up process places 25 ℃ water bath with thermostatic control for add the alcohol mixed solution that 100ml contains 24g (0.5mol) thanomin in the 500ml there-necked flask of reflux is housed; Agitation and dropping 100ml contains the alcohol mixed solution of 30g (0.5mol) acetate, it is muddy that mixture becomes gradually, reaction places Rotary Evaporators to remove ethanol mixing solutions after finishing, and obtains light yellow viscous liquid, products obtained therefrom is placed 60 ℃ the dry 48h of vacuum drying oven.Get lurid ethanol ammonium acetate ions liquid.
Second step ion thermal synthesis molecular sieve
With ethanol ammonium acetate ions liquid HEA, Al[OCH (CH
3)
2]
3, H
3PO
4(85%in H
2O), HF (40%in H
2O) Al according to a certain percentage successively
2O
3: xP
2O
5: (T=150 ℃ of 3.6HF: 40IL (x=0.8-7.0), t=3d) add in the 23ml polytetrafluoroethyllining lining stainless steel cauldron, reacting by heating 3 days is reduced to room temperature through nature afterwards, goes out product with deionized water behind the still and repeatedly drip washing filtration of ethanol, drying.
Embodiment 4
Synthesizing of the first step triethanol ammonium lactate ions liquid
Building-up process places 25 ℃ water bath with thermostatic control for add the alcohol mixed solution that 100ml contains 75g (0.5mol) trolamine in the 500ml there-necked flask of reflux is housed; Agitation and dropping 100ml contains the alcohol mixed solution of 45g (0.5mol) lactic acid, it is muddy that mixture becomes gradually, reaction places Rotary Evaporators to remove ethanol mixing solutions after finishing, and obtains light yellow viscous liquid, products obtained therefrom is placed 60 ℃ the dry 48h of vacuum drying oven.Get lurid triethanol ammonium lactate ions liquid.
Second step ion thermal synthesis molecular sieve
With triethanol ammonium lactate ions liquid THEAL, Al[OCH (CH
3)
2]
3, H
3PO
4(85% in H
2O), HF (40% in H
2O) Al according to a certain percentage successively
2O
3: xP
2O
5: (T=130 ℃ of 0.8HF: 40IL (x=0.8-7.0), t=3d) add in the 23ml polytetrafluoroethyllining lining stainless steel cauldron, reacting by heating 3 days is reduced to room temperature through nature afterwards, goes out product with deionized water behind the still and repeatedly drip washing filtration of ethanol, drying.
Embodiment 5
Synthesizing of the first step triethanol ammonium lactate ions liquid
Building-up process places 25 ℃ water bath with thermostatic control for add the alcohol mixed solution that 100ml contains 75g (0.5mol) trolamine in the 500ml there-necked flask of reflux is housed; Agitation and dropping 100ml contains the alcohol mixed solution of 45g (0.5mol) lactic acid, it is muddy that mixture becomes gradually, reaction places Rotary Evaporators to remove ethanol mixing solutions after finishing, and obtains light yellow viscous liquid, products obtained therefrom is placed 60 ℃ the dry 48h of vacuum drying oven.Get lurid triethanol ammonium lactate ions liquid.
Second step ion thermal synthesis molecular sieve
With triethanol ammonium lactate ions liquid THEAL, Al[OCH (CH
3)
2]
3, H
3PO
4(85% in H
2O), HF (40% in H
2O) Al according to a certain percentage successively
2O
3: xP
2O
5: (T=150 ℃ of 0.8 HF: 40IL (x=0.8-7.0), t=3d) add in the 23ml polytetrafluoroethyllining lining stainless steel cauldron, reacting by heating 3 days is reduced to room temperature through nature afterwards, goes out product with deionized water behind the still and repeatedly drip washing filtration of ethanol, drying.
Embodiment 6
The first step triethanol ammonium lactate ions liquid THEAL's is synthetic
Building-up process places 25 ℃ water bath with thermostatic control for add the alcohol mixed solution that 100ml contains 24g (0.5mol) thanomin in the 500ml there-necked flask of reflux is housed; Agitation and dropping 100ml contains the alcohol mixed solution of 30g (0.5mol) acetate, it is muddy that mixture becomes gradually, reaction places Rotary Evaporators to remove ethanol mixing solutions after finishing, and obtains light yellow viscous liquid, products obtained therefrom is placed 60 ℃ the dry 48h of vacuum drying oven.Get lurid ethanol ammonium acetate ions liquid.
Second step ion thermal synthesis molecular sieve
With triethanol ammonium lactate ions liquid THEAL, Al[OCH (CH
3)
2]
3, H
3PO
4(85% in H
2O), HF (40% in H
2O) Al according to a certain percentage successively
2O
3: xP
2O
5: (T=160 ℃ of 0.8 HF: 40IL (x=0.8-7.0), t=3d) add in the 23ml polytetrafluoroethyllining lining stainless steel cauldron, reacting by heating 3 days is reduced to room temperature through nature afterwards, goes out product with deionized water behind the still and repeatedly drip washing filtration of ethanol, drying.
Embodiment 7
Synthesizing of the first step triethanol ammonium lactate ions liquid
Building-up process places 25 ℃ water bath with thermostatic control for add the alcohol mixed solution that 100ml contains 75g (0.5mol) trolamine in the 500ml there-necked flask of reflux is housed; Agitation and dropping 100ml contains the alcohol mixed solution of 45g (0.5mol) lactic acid, it is muddy that mixture becomes gradually, reaction places Rotary Evaporators to remove ethanol mixing solutions after finishing, and obtains light yellow viscous liquid, products obtained therefrom is placed 60 ℃ the dry 48h of vacuum drying oven.Get lurid triethanol ammonium lactate ions liquid.
Second step ion thermal synthesis molecular sieve
With triethanol ammonium lactate ions liquid THEAL, Al[OCH (CH
3)
2]
3, H
3PO
4(85% in H
2O), HF (40% in H
2O) Al according to a certain percentage successively
2O
3: xP
2O
5: (T=170 ℃ of 0.8HF: 40IL (x=0.8-7.0), t=3d) add in the 23ml polytetrafluoroethyllining lining stainless steel cauldron, reacting by heating 3 days is reduced to room temperature through nature afterwards, goes out product with deionized water behind the still and repeatedly drip washing filtration of ethanol, drying.
Embodiment 8
Synthesizing of the first step triethanol ammonium lactate ions liquid
Building-up process places 25 ℃ water bath with thermostatic control for add the alcohol mixed solution that 100ml contains 75g (0.5mol) trolamine in the 500ml there-necked flask of reflux is housed; Agitation and dropping 100ml contains the alcohol mixed solution of 45g (0.5mol) lactic acid, it is muddy that mixture becomes gradually, reaction places Rotary Evaporators to remove ethanol mixing solutions after finishing, and obtains light yellow viscous liquid, products obtained therefrom is placed 60 ℃ the dry 48h of vacuum drying oven.Get lurid triethanol ammonium lactate ions liquid.
Second step ion thermal synthesis molecular sieve
With triethanol ammonium lactate ions liquid THEAL, Al[OCH (CH
3)
2]
3, H
3PO
4(85% in H
2O), HF (40% in H
2O) Al according to a certain percentage successively
2O
3: xP
2O
5: (T=180 ℃ of 0.8HF: 40IL (x=0.8-7.0), t=3d) add in the 23ml polytetrafluoroethyllining lining stainless steel cauldron, reacting by heating 3 days is reduced to room temperature through nature afterwards, goes out product with deionized water behind the still and repeatedly drip washing filtration of ethanol, drying.
Claims (7)
1. the ion thermal method of a preparation molecular sieve in alcohol amine ion liquid is characterized in that comprising the steps: the ion thermal synthesis of the synthetic and molecular sieve of alcohol amine ion liquid; Alcohol amine ion liquid by equimolar hydramine and carboxylic acid with ethanol be solvent at normal temperatures one the step neutralization reaction obtain; Alcohol amine ion liquid, aluminum isopropylate, phosphoric acid, hydrofluoric acid are added in the 23ml polytetrafluoroethyllining lining stainless steel cauldron successively according to a certain percentage, reacting by heating, reduce to room temperature through nature afterwards, again through deionized water and ethanol repeatedly drip washing filter, dry aluminium phosphate molecular sieve.
2. alcohol amine ion liquid according to claim 1 is characterized in that alcohol amine ion liquid is ethanol ammonium acetate and triethanol ammonium lactic acid salt.
3. ion thermal synthesis molecular sieve according to claim 1 is characterized in that the phosphorus aluminum ratio in the reaction system is 0.8-7.0.
4. ion thermal synthesis molecular sieve according to claim 1 is characterized in that the fluorine aluminum ratio in the reaction system is 1.8-4.5.
5. ion thermal synthesis molecular sieve according to claim 1 is characterized in that ionic liquid and the aluminum ratio in the reaction system is 5-60.
6. ion thermal synthesis molecular sieve according to claim 1 is characterized in that temperature of reaction is 130-180 ℃.
7. ion thermal synthesis molecular sieve according to claim 1 is characterized in that the reaction times is 3-7d.
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| CN102299322A (en) * | 2011-07-22 | 2011-12-28 | 合肥工业大学 | Ion hot preparation method for lithium iron phosphate positive electrode material |
| CN102299325A (en) * | 2011-07-29 | 2011-12-28 | 合肥工业大学 | Ionothermal process of manganese lithium phosphate anode material |
| CN102730713A (en) * | 2012-06-29 | 2012-10-17 | 陕西师范大学 | Ionothermal preparation method for rare earth-substituted ZON-structured aluminophosphate molecular sieve UiO-7 |
| CN103318914A (en) * | 2012-03-21 | 2013-09-25 | 中国科学院大连化学物理研究所 | Preparation of AEL structure aluminophosphate molecular sieve membrane supported by porous alumina carrier |
| CN103318917A (en) * | 2012-03-21 | 2013-09-25 | 中国科学院大连化学物理研究所 | Preparation of highly oriented AEL aluminophosphate molecular sieve membrane supported by alumina carrier |
| CN103318916A (en) * | 2012-03-21 | 2013-09-25 | 中国科学院大连化学物理研究所 | Preparation of LTA structure aluminophosphate molecular sieve membrane supported by porous alumina carrier |
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| CN104108721A (en) * | 2013-04-18 | 2014-10-22 | 中国科学院大连化学物理研究所 | Preparation for AEL structural aluminium-phosphate molecular-sieve membrane supported by porous alumina carrier |
| CN105776239A (en) * | 2014-12-17 | 2016-07-20 | 中国科学院大连化学物理研究所 | Preparation method of hierarchical pore AFI structured aluminum phosphate molecular sieve |
| CN109422278A (en) * | 2017-08-31 | 2019-03-05 | 中国科学院大连化学物理研究所 | A method of synthesis has AEL structure hetero atom Metal-aluminophosphate Molecular Siever |
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2008
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| CN102299322A (en) * | 2011-07-22 | 2011-12-28 | 合肥工业大学 | Ion hot preparation method for lithium iron phosphate positive electrode material |
| CN102299325B (en) * | 2011-07-29 | 2015-02-04 | 合肥工业大学 | Ionothermal process of manganese lithium phosphate anode material |
| CN102299325A (en) * | 2011-07-29 | 2011-12-28 | 合肥工业大学 | Ionothermal process of manganese lithium phosphate anode material |
| CN103318916B (en) * | 2012-03-21 | 2015-04-22 | 中国科学院大连化学物理研究所 | Preparation of LTA structure aluminophosphate molecular sieve membrane supported by porous alumina carrier |
| CN103318917B (en) * | 2012-03-21 | 2015-04-22 | 中国科学院大连化学物理研究所 | Preparation of highly oriented AEL aluminophosphate molecular sieve membrane supported by alumina carrier |
| CN103318916A (en) * | 2012-03-21 | 2013-09-25 | 中国科学院大连化学物理研究所 | Preparation of LTA structure aluminophosphate molecular sieve membrane supported by porous alumina carrier |
| CN103318917A (en) * | 2012-03-21 | 2013-09-25 | 中国科学院大连化学物理研究所 | Preparation of highly oriented AEL aluminophosphate molecular sieve membrane supported by alumina carrier |
| CN103318914A (en) * | 2012-03-21 | 2013-09-25 | 中国科学院大连化学物理研究所 | Preparation of AEL structure aluminophosphate molecular sieve membrane supported by porous alumina carrier |
| CN103318914B (en) * | 2012-03-21 | 2015-04-22 | 中国科学院大连化学物理研究所 | Preparation of AEL structure aluminophosphate molecular sieve membrane supported by porous alumina carrier |
| CN102730713B (en) * | 2012-06-29 | 2014-03-05 | 陕西师范大学 | Ionothermal preparation method for rare earth-substituted ZON-structured aluminophosphate molecular sieve UiO-7 |
| CN102730713A (en) * | 2012-06-29 | 2012-10-17 | 陕西师范大学 | Ionothermal preparation method for rare earth-substituted ZON-structured aluminophosphate molecular sieve UiO-7 |
| CN104108722A (en) * | 2013-04-18 | 2014-10-22 | 中国科学院大连化学物理研究所 | Preparation method for ZIF-8 membrane supported by porous alumina carrier |
| CN104108721A (en) * | 2013-04-18 | 2014-10-22 | 中国科学院大连化学物理研究所 | Preparation for AEL structural aluminium-phosphate molecular-sieve membrane supported by porous alumina carrier |
| CN104108721B (en) * | 2013-04-18 | 2016-01-20 | 中国科学院大连化学物理研究所 | The preparation of the AEL structure aluminophosphate molecular sieve membrane that porous alumina carrier supports |
| CN104108722B (en) * | 2013-04-18 | 2016-06-22 | 中国科学院大连化学物理研究所 | The preparation method of the ZIF-8 film that a kind of porous alumina carrier supports |
| CN105776239A (en) * | 2014-12-17 | 2016-07-20 | 中国科学院大连化学物理研究所 | Preparation method of hierarchical pore AFI structured aluminum phosphate molecular sieve |
| CN109422278A (en) * | 2017-08-31 | 2019-03-05 | 中国科学院大连化学物理研究所 | A method of synthesis has AEL structure hetero atom Metal-aluminophosphate Molecular Siever |
| CN109422282A (en) * | 2017-08-31 | 2019-03-05 | 中国科学院大连化学物理研究所 | A kind of method of synthesizing alkanes catalyst for hydroisomerizing carrier |
| CN112320814A (en) * | 2020-10-29 | 2021-02-05 | 中国科学院过程工程研究所 | Method for preparing FAU type small-grain molecular sieve without template agent and solvent under mild condition |
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