CN103263915A - Hydrotalcite-loaded nanometer platinum catalyst as well as preparation method and application thereof - Google Patents
Hydrotalcite-loaded nanometer platinum catalyst as well as preparation method and application thereof Download PDFInfo
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- CN103263915A CN103263915A CN2013101725386A CN201310172538A CN103263915A CN 103263915 A CN103263915 A CN 103263915A CN 2013101725386 A CN2013101725386 A CN 2013101725386A CN 201310172538 A CN201310172538 A CN 201310172538A CN 103263915 A CN103263915 A CN 103263915A
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Abstract
The invention provides hydrotalcite-loaded nanometer platinum catalyst as well as a preparation method and application thereof. The preparation method of the hydrotalcite-loaded nanometer platinum catalyst comprises the following steps of: preparing magnesium-aluminum hydrotalcite crystal nucleus by utilizing an all-return liquid mixing membrane reactor, dispersing the crystal nucleus in an aqueous solution; adding an chloroplatinic acid aqueous solution and tetradecyl trimethyl ammonium bromide (TTAB) as well as a proper proportion reducing agent of NaBH4; controlling the reducing velocity and the growth of Pt nanometer particles by utilizing the protecting and stabilizing effect of the TTAB to the Pt<4+> ion; and gradually crystallizing the hydrotalcite while reducing the Pt<4+> ion to obtain the hydrotalcite-loaded nanometer platinum catalyst. The catalyst is obtained by loading nanometer particles on a hydrotalcite carrier, wherein the chemical formula of the hydrotalcite is as follows: MgxAly(OH)16CO3 nH2O; the platinum nanometer particle dimension is 2 nm-8nm; the nanometer particles are polyhedral or ellipsoidal in appearance; the loading capacity of the platinum is 0.5%-3%; and the dispersion degree on the carrier is 20%-50%. The hydrotalcite-loaded nanometer platinum catalyst can be used for catalytic hydrogenation reaction of unsaturated aldehyde (cinnamyl aldehyde), wherein water is used as solvent, the conversation rate of the reactant cinnamyl aldehyde is 75%-95% and the selectivity of the product cinnamyl alcohol is 75%-95%.
Description
Technical field
The invention belongs to metal nano Preparation of Catalyst field, be specifically related to loaded platinum catalyst and preparation method thereof, and used as can be used as the unsaturated aldehyde hydrogenation catalyst.
Background technology
Platinum metal catalyst has been found to be catalyst for hydrogenation preferably, shows high activity in multiple organic molecule hydrogenation reaction, for example: the hydrogenation of unsaturated aldehyde/ketone molecule, ester through hydrogenation, nitroreduction etc.The principal element that influences the platinum metal catalyst catalytic performance has: metal particle size, bearer type and metal-[Urbano, F.J. such as carrier interaction; Hidalgo-Carrillo, J.; Aramendia, M.A.; Marinas, A.; Marinas, J.M., Appl.Catal.A-Gen2010,385,190-200.].The method for preparing loaded platinum catalyst of bibliographical information mainly contains at present: infusion process and reducing process.The common dispersiveness of the platinum catalyst that infusion process makes is bad, the platinum particles size is difficult to accurate control, thereby influences its catalytic performance.For reducing process, used reducing agent and reducing condition have material impact to metal particle size, pattern and dispersity.Reducing agent commonly used has sodium borohydride, polyalcohol, hydrazine, the biological sugar of reproducibility, citrate, ascorbic acid etc.Have the reducing agent of strong reducing power, can in the short time metal ion be restored from its solution at the utmost point as sodium borohydride, hydrazine etc., but because reduction rate is too fast, the metal particle size that causes obtaining distributes wide; And gentle reducing agent, as reproducibility carbohydrate, polyalcohol, ascorbic acid etc., though rate of reduction is slowed down, the growth of control metallic particles, but often need higher temperature, take longer, expend the more energy [Z.Guo, Y.Chen, L.Li, X.Wang, G.L.Haller, Y.Yang.J.Catal.2010,276,314-326.].In addition, for load type metal catalyst, present method is normally separated [Bhogeswararao, S. with preparing carriers with the metal loading process; Srinivas, D.Intramolecular J.Catal.2012,285,31-40; J.Zhu, Y.Jia, M.Li, M.Lu, J.Zhu.Ind.Eng.Chem.Res.2013,52,1224-1233.], namely at first prepare carrier and carry out the load of metallic again, or prepare carrier and metal nanoparticle respectively, and then in solution, be mixed into the row metal load, this preparation process makes that the adhesion between metallic and the carrier is relatively poor, move, assemble easily, thereby influence catalytic reaction and stability.
Hydrotalcite is a kind of anion type laminated clay material, and its chemical formula is: Mg
6Al
2(OH)
16CO
3NH
2O is by positively charged class shepardite (shepardite: Mg (OH)
2) laminate and electronegative interlayer carbonate anion formation.Hydrotalcite is because stable layer structure and surface hydrophilic character is commonly used for the carrier material for preparing metallic catalyst under the aqueous phase reactions environment.
Utilize hydrotalcite as carrier, development prepares the method for load platinum catalyst under the aqueous phase reactions condition of gentleness, in regulation and control metal ion rate of reduction, improve metal-carrier and interact, obtain high activity, stable load type platinum metallic catalyst is significant.
Summary of the invention
The purpose of this invention is to provide a kind of hydrotalcite loaded with nano platinum catalyst and preparation method thereof, and used as the catalyst of unsaturated aldehyde hydrogenation reaction in the pure water solvent.
Preparation method of the present invention is: utilize full back-mixing liquid film reactor (referring to patent CN1358691) preparation magnalium hydrotalcite nucleus earlier, this nucleus is dispersed in the aqueous solution, add chloroplatinic acid (H again
2PtCl
6) aqueous solution and TTAB (TTAB), and the reducing agent NaBH of proper proportion
4, reaction utilizes the Pt of TTAB at a certain temperature
4+The protection of ion and stabilization, the growth of control rate of reduction and Pt nano particle is at reduction Pt
4+In the time of ion, hydrotalcite is crystallization gradually, obtains the nanometer Pt of the controllable size of hydrotalcite load.This method is with Pt
4+The deposition of the reduction of ion, the crystallization of hydrotalcite supports and nanometer Pt be integrated into one the step finish, do not use any toxic reagent and organic solvent, the reaction condition gentleness is suitable for the extensive controlled preparation of loaded with nano platinum catalyst.
Hydrotalcite loaded with nano platinum catalyst provided by the present invention: this catalyst is that platinum particles is carried on the hydrotalcite supports; The chemical formula of hydrotalcite is: Mg
xAl
y(OH)
16CO
3NH
2O, wherein the mol ratio of x:y is 2-4:1, n represents crystallization water number; Nano platinum particle is polyhedron or elliposoidal, and particle size is 2-8nm; Wherein the load capacity of nano platinum particle is 0.5-3%, and the decentralization on carrier is 20-50%.
The concrete preparation process of this hydrotalcite loaded with nano platinum catalyst is as follows:
A. with solubility magnesium salts and aluminum soluble salt preparation mixing salt solution, wherein aluminum ions molar concentration is 0.05-0.2mol/L, and the molar concentration of magnesium ion is 2-4 times of aluminium ion molar concentration; Described solubility magnesium salts is magnesium nitrate, magnesium chloride, and a kind of in the magnesium sulfate, aluminum soluble salt is aluminum nitrate, a kind of in the aluminum sulfate;
Preparation NaOH and Na
2CO
3Mixed ammonium/alkali solutions, identical with the volume of above-mentioned mixing salt solution; And in the mixed ammonium/alkali solutions NaOH molar concentration be metal ion molar concentration sum in the mixing salt solution 1-2 doubly, Na
2CO
3Concentration is 2-3 times of aluminium ion molar concentration;
Mixing salt solution and mixed ammonium/alkali solutions are at room temperature added in the full back-mixing liquid film reactor simultaneously, stator and gap between rotor size are decided to be 15-18 μ m; Rotate back-mixing at a high speed in 4000-5000 rev/min rotating speed, reactant liquor is fully contacted mix 2-5min, obtain hydrotalcite suspension, centrifugal, washing 1-2 time; Again the precipitation of cleaning is dispersed in and is made into the hydrotalcite suspension that solid content is 4-32g/L in the water;
B. the platinum acid chloride solution that with concentration is 1-10mmol/L joins in the hydrotalcite suspension of steps A, and make that the mol ratio of magnesium ion and chloroplatinic acid is 150-300:1 in the solution, add TTAB (TTAB) again, wherein the mol ratio of TTAB and chloroplatinic acid is 10-200:1, and more excellent mol ratio is 25-150:1; Solution is warmed up to 40-70 ° of C, stirs 10-20min;
C. with NaBH
4Join in the solution of step B NaBH
4With the mol ratio of chloroplatinic acid be 10-30:1, solution was 40-70 ° of C stirring reaction 4-10 hour, centrifugation goes out sediment, washing 3-5 time then, at 60-80 ℃ time dry 6-12 hour, namely obtains hydrotalcite loaded with nano platinum catalyst.
Adopt JEOL JEM-2100 type transmission electron microscope (HRTEM) to observe pattern and the metal particle size of catalyst, as shown in drawings, the nano platinum particle size is at 2-8nm, and particle is polyhedron shape or elliposoidal;
Adopting the load capacity of platinum on the Z-8000 type atomic absorption spectrometry catalyst is 0.5-3%.
The platinum catalyst that the present invention makes can be used as the unsaturated aldehyde hydrogenation catalyst, be example with the hydrogenation on cinnamic aldehyde reaction, cinnamic acid is a kind of typical α, beta-unsaturated aldehyde, its liquid-phase hydrogenatin reaction obtains multiple product, wherein a kind of hydrogenation products---cinnamyl alcohol is the important chemical intermediate feed, is widely used in industries such as spices, medicine, food interpolation.Concrete catalysis experiment is as follows: take by weighing the 0.05g catalyst, be dispersed in the 15mL water, transferring to the volume that has magnetic agitation is in the reactor of 100mL, the cinnamic acid of measuring 4mmol adds reactor, reactor is airtight, fill, put the air in 10 displacement stills of hydrogen, behind the air in the emptying still, after reactor put into constant temperature bath and be heated to 40-80 ° of C, charge into the hydrogen of 0.5-2MPa, keep temperature constant, reacted 0.5-4 hour, after question response is finished, take out the liquid in the reactor, utilize the gas chromatograph assay products to form and content.The result shows: be solvent with water, the conversion ratio of reactant cinnamic acid reaches 75-95%, and catalyst is 75-95% to the selective of product cinnamyl alcohol.And traditional catalyst is when the spirit catalytic of cinnamaldehyde hydrogenation obtains cinnamyl alcohol, (temperature is lower than 80 ° of C under the reaction condition of gentleness, pressure is lower than 2MPa), conversion ratio＜80% or cinnamyl alcohol are selectively＜75%, and normally used solvent is organic solvent (ethanol, isopropyl alcohol, benzene, cyclohexane), there is pollution risk in environment, seldom uses pure water as solvent.
The present invention has following remarkable result:
(1) in the aqueous solution, the reduction chloroplatinic acid obtains metal platinum nano-particle under the gentle reaction condition, utilize the growth of surfactant TTAB control rate of reduction and nano platinum particle, whole process is not used any toxic reagent and organic solvent, not needing to carry out high-temperature process, is the method for preparing catalyst of a kind of green, gentleness, controlled, low energy consumption.
(2) reduction of metal platinum ion, platinum particles deposition are carried out simultaneously with the crystallization of carrier, are conducive to pay(useful) load and the high degree of dispersion of platinum particles on carrier, improve metal-carrier and interact, and strengthen catalyst stability.
(3) the nano platinum particle size can increase with surfactant (TTAB) addition with the amount modulation that adds surfactant, and the platinum particles size reduces.
(4) in hydrogenation reaction, not with an organic solvent, be green solvent with the pure water, platinum catalyst has high activity and high cinnamyl alcohol selectivity of product to unsaturated aldehyde (cinnamic acid) hydrogenation.
Description of drawings
The HRTEM image of the load platinum catalyst that Fig. 1: embodiment 2 obtains
The platinum particles size distribution plot of the load platinum catalyst that Fig. 2: embodiment 2 obtains
The HRTEM image of the load platinum catalyst that Fig. 3: embodiment 3 obtains
The platinum particles size distribution plot of the load platinum catalyst that Fig. 4: embodiment 3 obtains
The specific embodiment
Take by weighing 1.536gMg (NO
3)
26H
2O and 1.125gAl (NO
3)
39H
2O is dissolved in the 30mL deionized water and prepares mixing salt solution, claims 0.576gNaOH and 0.636gNa
2CO
3Preparation mixed ammonium/alkali solutions 30mL, wherein the NaOH molar concentration is (Mg
2++ Al
3+) 1.6 times of concentration sum, Na
2CO
3Concentration is Al
3+2 times of concentration.
The mixing salt solution and the mixed ammonium/alkali solutions that prepare are at room temperature poured in the full back-mixing liquid film reactor, the rotating speed of liquid film reactor is 4500 rev/mins, and rotation back-mixing 3min obtains hydrotalcite suspension, after centrifugal, the washing 1 time, will precipitate and be dispersed in again in the 80mL water; Be that the platinum acid chloride solution of 10mmol/L adds water in the talcum suspension with 3mL concentration, add TTAB again, wherein TTAB is 50:1 with the ratio of the molal quantity of chloroplatinic acid, is warmed up to 60 ° of C, stirs 10min; Again with NaBH
4Join in the above solution NaBH rapidly
4With the mol ratio of chloroplatinic acid be 20:1, solution is 60 ° of C stirring reactions 6 hours, centrifugal, washing is 3 times then, 70 ℃ dry 8 hours down, obtain hydrotalcite loaded with nano platinum catalyst.
Utilize HRTEM to observe catalyst cupport platinum particles Size Distribution at 3-4.5nm, the load capacity that Atomic Absorption Spectrometer records platinum is 1.1%.The decentralization of nano platinum particle on carrier is 31.4%.
Catalytic performance test: take by weighing the 0.05g catalyst, be dispersed in the 15mL water, transferring to the volume that has magnetic agitation is in the reactor of 100mL, the cinnamic acid of measuring 4mmol adds reactor, reactor is airtight, fill, put the air in 10 displacement stills of hydrogen, behind the air in the emptying still, after reactor put into constant temperature bath and be heated to 60 ° of C, charge into 1MPa hydrogen, keep temperature constant, reacted 3 hours, after question response is finished, take out the liquid in the reactor, utilize the gas chromatograph assay products to form and content.Evaluation result: the conversion ratio of reactant cinnamic acid is 81%, and catalyst selectively is 80% to cinnamyl alcohol.
Take by weighing 2.304gMg (NO
3)
26H
2O and 1.125gAl (NO
3)
39H
2O is dissolved in the 30mL deionized water and prepares mixing salt solution, claims 0.72gNaOH and 0.954gNa
2CO
3Preparation mixed ammonium/alkali solutions 30mL, wherein the NaOH molar concentration is (Mg
2++ Al
3+) 1.5 times of concentration sum, Na
2CO
3Concentration is Al
3+3 times of concentration.
The mixing salt solution and the mixed ammonium/alkali solutions that prepare are at room temperature poured in the full back-mixing liquid film reactor, the rotating speed of liquid film reactor is 4200 rev/mins, and rotation back-mixing 4min obtains hydrotalcite suspension, after centrifugal, the washing 2 times, will precipitate and be dispersed in again in the 60mL water; Be that the platinum acid chloride solution of 10mmol/L adds water in the talcum suspension with 5mL concentration, add TTAB again, wherein TTAB is 25:1 with the ratio of the molal quantity of chloroplatinic acid, is warmed up to 60 ° of C, stirs 15min; Again with NaBH
4Join in the above solution NaBH rapidly
4With the mol ratio of chloroplatinic acid be 15:1, solution is 60 ° of C stirring reactions 6 hours, centrifugal, washing is 3 times then, 70 ℃ dry 12 hours down, obtain hydrotalcite loaded with nano platinum catalyst.
Utilize HRTEM to observe the catalyst cupport platinum particles, the results are shown in Figure 1,2, the platinum particles Size Distribution is at 4-6nm.The load capacity that Atomic Absorption Spectrometer records platinum is 1.5%.The decentralization of nano platinum particle on carrier is 22.6%.
Catalytic performance test: take by weighing the 0.05g catalyst, be dispersed in the 15mL water, transferring to the volume that has magnetic agitation is in the reactor of 100mL, the cinnamic acid of measuring 4mmol adds reactor, reactor is airtight, fill, put the air in 10 displacement stills of hydrogen, behind the air in the emptying still, after reactor put into constant temperature bath and be heated to 60 ° of C, charge into 1MPa hydrogen, keep temperature constant, reacted 2 hours, after question response is finished, take out the liquid in the reactor, utilize the gas chromatograph assay products to form and content.Evaluation result: the conversion ratio of reactant cinnamic acid is 80%, and catalyst selectively is 85% to cinnamyl alcohol.
Take by weighing 3.072gMg (NO
3)
26H
2O and 1.125gAl (NO
3)
39H
2O is dissolved in the 30mL deionized water and prepares mixing salt solution, claims 1.08gNaOH and 0.636gNa
2CO
3Preparation mixed ammonium/alkali solutions 30mL, wherein the NaOH molar concentration is (Mg
2++ Al
3+) 1.8 times of concentration sum, Na
2CO
3Concentration is Al
3+2 times of concentration.
The mixing salt solution and the mixed ammonium/alkali solutions that prepare are at room temperature poured in the full back-mixing liquid film reactor, the rotating speed of liquid film reactor is 4000 rev/mins, and rotation back-mixing 2min obtains hydrotalcite suspension, after centrifugal, the washing 1 time, will precipitate and be dispersed in again in the 50mL water; Be that the platinum acid chloride solution of 10mmol/L adds water in the talcum suspension with 6mL concentration, add TTAB again, wherein TTAB is 100:1 with the ratio of the molal quantity of chloroplatinic acid, is warmed up to 50 ° of C, stirs 20min; Again with NaBH
4Join in the above solution NaBH rapidly
4With the mol ratio of chloroplatinic acid be 25:1, solution is 50 ° of C stirring reactions 8 hours, centrifugal, washing is 4 times then, 60 ℃ dry 12 hours down, obtain hydrotalcite loaded with nano platinum catalyst.
Utilize HRTEM to observe the catalyst cupport platinum particles, the results are shown in Figure 3,4, the platinum particles Size Distribution is at 2-4nm.The load capacity that Atomic Absorption Spectrometer records platinum is 1.2%.The decentralization of nano platinum particle on carrier is 33.2%.
Catalytic performance test: take by weighing the 0.05g catalyst, be dispersed in the 15mL water, transferring to the volume that has magnetic agitation is in the reactor of 100mL, the cinnamic acid of measuring 4mmol adds reactor, reactor is airtight, fill, put the air in 10 displacement stills of hydrogen, behind the air in the emptying still, after reactor put into constant temperature bath and be heated to 70 ° of C, charge into 0.5MPa hydrogen, keep temperature constant, reacted 2.5 hours, after question response is finished, take out the liquid in the reactor, utilize the gas chromatograph assay products to form and content.Evaluation result: the conversion ratio of reactant cinnamic acid is 87%, and catalyst selectively is 78% to cinnamyl alcohol.
Take by weighing 4.608gMg (NO
3)
26H
2O and 2.25gAl (NO
3)
39H
2O is dissolved in the 30mL deionized water and prepares mixing salt solution, claims 1.728gNaOH and 1.272gNa
2CO
3Preparation mixed ammonium/alkali solutions 30mL, wherein the NaOH molar concentration is (Mg
2++ Al
3+) 1.8 times of concentration sum, Na
2CO
3Concentration is Al
3+2 times of concentration.
The mixing salt solution and the mixed ammonium/alkali solutions that prepare are at room temperature poured in the full back-mixing liquid film reactor, the rotating speed of liquid film reactor is 4500 rev/mins, and rotation back-mixing 3min obtains hydrotalcite suspension, after centrifugal, the washing 1 time, will precipitate and be dispersed in again in the 60mL water; Be that the platinum acid chloride solution of 10mmol/L adds water in the talcum suspension with 6mL concentration, add TTAB again, wherein TTAB is 125:1 with the ratio of the molal quantity of chloroplatinic acid, is warmed up to 70 ° of C, stirs 10min; Again with NaBH
4Join in the above solution NaBH rapidly
4With the mol ratio of chloroplatinic acid be 15:1, solution is 70 ° of C stirring reactions 5 hours, centrifugal, washing is 4 times then, 70 ℃ dry 10 hours down, obtain hydrotalcite loaded with nano platinum catalyst.
Utilize HRTEM to observe catalyst cupport platinum particles Size Distribution at 2.5-4nm, the load capacity that Atomic Absorption Spectrometer records platinum is 1.0%.The decentralization of nano platinum particle on carrier is 40.3%.
Catalytic performance test: take by weighing the 0.05g catalyst, be dispersed in the 15mL water, transferring to the volume that has magnetic agitation is in the reactor of 100mL, the cinnamic acid of measuring 4mmol adds reactor, reactor is airtight, fill, put the air in 10 displacement stills of hydrogen, behind the air in the emptying still, after reactor put into constant temperature bath and be heated to 60 ° of C, charge into 1.5MPa hydrogen, keep temperature constant, reacted 2 hours, after question response is finished, take out the liquid in the reactor, utilize the gas chromatograph assay products to form and content.Evaluation result: the conversion ratio of reactant cinnamic acid is 89%, and catalyst selectively is 76% to cinnamyl alcohol.
Claims (4)
1. the preparation method of a hydrotalcite loaded with nano platinum catalyst, concrete preparation process is as follows:
A. with solubility magnesium salts and aluminum soluble salt preparation mixing salt solution, wherein aluminum ions molar concentration is 0.05-0.2mol/L, and the molar concentration of magnesium ion is 2-4 times of aluminium ion molar concentration; Described solubility magnesium salts is magnesium nitrate, magnesium chloride, and a kind of in the magnesium sulfate, aluminum soluble salt is aluminum nitrate, a kind of in the aluminum sulfate;
Preparation NaOH and Na
2CO
3Mixed ammonium/alkali solutions, identical with the volume of above-mentioned mixing salt solution; And in the mixed ammonium/alkali solutions NaOH molar concentration be metal ion molar concentration sum in the mixing salt solution 1-2 doubly, Na
2CO
3Concentration is 2-3 times of aluminium ion molar concentration;
Mixing salt solution and mixed ammonium/alkali solutions are at room temperature added in the full back-mixing liquid film reactor simultaneously, stator and gap between rotor size are decided to be 15-18 μ m; Rotate back-mixing at a high speed in 4000-5000 rev/min rotating speed, reactant liquor is fully contacted mix 2-5min, obtain hydrotalcite suspension, centrifugal, washing 1-2 time; Again the precipitation of cleaning is dispersed in and is made into the hydrotalcite suspension that solid content is 4-32 g/L in the water;
B. the platinum acid chloride solution that with concentration is 1-10mmol/L joins in the hydrotalcite suspension of steps A, and make that the mol ratio of magnesium ion and chloroplatinic acid is 150-300:1 in the solution, add TTAB again, wherein the mol ratio of TTAB and chloroplatinic acid is 10-200:1; This solution is warmed up to 40-70
oC stirs 10-20 min;
C. with NaBH
4Join in the solution of step B, make NaBH
4With the mol ratio of chloroplatinic acid be 10-30:1, solution is at 40-70
oC stirring reaction 4-10 hour, centrifugation goes out sediment, washing 3-5 time then, descends dry 6-12 hour at 60-80 ℃, namely obtains hydrotalcite loaded with nano platinum catalyst.
2. the preparation method of hydrotalcite loaded with nano platinum catalyst according to claim 1 is characterized in that the mol ratio of TTAB and chloroplatinic acid is 25-150:1 among the step B.
3. the hydrotalcite loaded with nano platinum catalyst of a method according to claim 1 preparation, this catalyst is that platinum particles is carried on the hydrotalcite supports; The chemical formula of hydrotalcite is: Mg
xAl
y(OH)
16CO
3NH
2O, wherein the mol ratio of x:y is 2-4:1, n represents crystallization water number; Nano platinum particle is polyhedron or elliposoidal, and particle size is 2-8 nm; Wherein the load capacity of nano platinum particle is 0.5-3%, and the decentralization on carrier is 20-50%.
With the described hydrotalcite loaded with nano of claim 3 platinum catalyst as in the unsaturated aldehyde hydrogenation reaction, make the conversion ratio of reactant reach 75-95%, catalyst reaches 75-95% to product selectivity.
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