CN104785295B - A kind of preparation method of high selectivity dopamine platinum carbon catalyst - Google Patents
A kind of preparation method of high selectivity dopamine platinum carbon catalyst Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of high selectivity dopamine platinum carbon catalyst, and dopamine platinum carbon catalyst is prepared as raw material using the platinum precursor solution of dopamine precursor solution and dopped activated carbon.The preparation method of the present invention, not only solves the problems such as traditional precipitation method and infusion process activity is low, poor selectivity and service life are short, and maintain the particle diameter distribution and particle size similar to colloid platinum catalyst.
Description
Technical field
The invention belongs to catalysis technical field, is related to a kind of high selectivity dopamine platinum charcoal of specific aluminum oxide frame carrier
Method for preparing catalyst.
Background technology
Platinum metal catalysts have good catalytic performance, occupy in petrochemical industry and organic synthesis extremely important
Status, it is widely used in the reaction such as hydrogenation, dehydrogenation, oxidation, reduction, isomerization, aromatisation, cracking.The catalytic performance of catalyst, is removed
It is also closely related with the preparation method of catalyst and process conditions etc. outside the composition and content of catalyst, it is same
Raw material, identical composition and content, preparation method is different, and the activity and heat endurance of catalyst may have very big difference.Cause
This, the preparation method of research high selectivity platinum carbon catalyst has particularly important meaning.
The traditional precipitation method or infusion process the particle diameter of active component, decentralization and are urged during platinum carbon catalyst is prepared
Physico-chemical property, the speed of stirring, the temperature of reaction, the concentration of reaction system, reducing agent of the selectivity of agent by Carbon supports
Concentration and its complicated factor such as species influence.Such as platinum nucleus can be in the liquid phase or on carrier surface in precipitation-reduction process
Grow up, reunite, the active component particles scope of prepared catalyst is wide, particle diameter is big, skewness, decentralization are low, it is difficult to
Prepare the platinum carbon catalyst of high selectivity high activity long-life.
The content of the invention
It is an object of the invention to provide a kind of high selectivity dopamine platinum carbon catalyst system with aluminum oxide frame carrier
Preparation Method, the present invention not only solve the problems such as traditional precipitation method and infusion process activity is low, poor selectivity and service life are short, and
And maintain the particle diameter distribution and particle size similar to colloid platinum catalyst.
A kind of preparation method of high selectivity dopamine platinum carbon catalyst, it is characterised in that the step of its preparation method such as
Under：
1) system of platinum precursor solution is matched somebody with somebody
Chloroplatinic acid is weighed, adds deionized water to dilute platinum to 20-50g/L, and lubricant is added into platinum acid chloride solution, is being stirred
Mix down, adjust pH to 1-5, platinum precursor solution is made；
2) system of dopamine precursor solution is matched somebody with somebody
For the raw material used for absolute ethyl alcohol, dopamine, sodium hydroxide, deionized water, dispersant, step is by absolute ethyl alcohol
It is stirred vigorously, dopamine obtained solution A is added dropwise, deionized water, absolute ethyl alcohol, sodium hydroxide, dispersant are uniformly mixed, is made
Solution B；In the case where being stirred vigorously, solution A is added drop-wise in solution B, is added dropwise to complete stopping stirring；
3) it is catalyzed the washing of frame carrier
At normal temperatures, the acid treatment 20 minutes by aluminium oxide ceramics foaming body with the 0.01mol/L of 2 times of volumes, with 2-4 times
The deionized water cleaning of volume, is then cleaned by ultrasonic, the deionized water with 2-4 times of volume is clear with the neutral detergent of 2 times of volumes
Wash, using soaked in absolute ethyl alcohol 2-5 hours, dry；
4) the platinum precursor solution of dopped activated carbon
Nitric acid treatment 4h by active carbon nanoparticles using the 0.5mol/L of 2 times of volumes, filtering, with 2-4 times of quality go from
Sub- water immersion, under agitation, adjusts pH to 1-5, soaks 4-12h, filtering, dries, then put dried active carbon nanoparticles
Enter platinum precursor solution, add macromolecule dispersing agent, form the platinum precursor solution of dopped activated carbon；
5) preparation of platinum catalysis frame carrier
4) the platinum precursor solution of the dopped activated carbon in is put into special plastic bucket, by 3) by the way of the lifting
Aluminium oxide ceramics foaming body be immersed in special plastic bucket, through repeatedly lifting after, by platinum catalysis frame carrier dry in the air naturally
It is dry, the catalysis frame carrier high temperature sintering after then drying, to turning white completely, natural cooling；
6) preparation of dopamine platinum carbon catalyst
5) platinum in is catalyzed in the dopamine precursor solution 2) frame carrier is added in, using multiple lifting
Mode, then the frame carrier after lifting is put into drying box, washed through absolute ethyl alcohol, is dried to obtain dopamine platinum charcoal
Catalyst.
Wherein, the lubricant in the step 1) is that castor oil, silicone oil, fatty acid amide, the one or more of carboxylic acid are matched somebody with somebody
System forms.
Wherein, the dispersant in the step 2) is polyvinylpyrrolidone, triethyl group hexyl phosphoric acid, dodecyl
One of sodium sulphate, methyl anyl alcohol, cellulose derivative, polyacrylamide, guar gum, fatty acid polyethylene glycol ester.
Wherein, the high temperature sintering temperature in the step 5) is 300-450 DEG C.
Wherein, the platinum catalysis frame carrier in the step 5) is that 10-80ppi (pores per inch, is measurement
Unit.Refer to the pore number that per inch length has), the activated carbon supported amount of platinum catalysis frame carrier is 5-10%,
The load capacity of platinum is 0.5-15%.
Wherein, dopamine forms chelated surface with platinum in the dopamine platinum carbon catalyst in the step 6), is formed
Surface key.
Compared with prior art, the invention has the advantages that：
(1) preparation method of the invention, not only solves the low traditional precipitation method and infusion process activity, poor selectivity and use
The problems such as short life, and maintain the particle diameter distribution and particle size similar to colloid platinum catalyst.
(2) preparation method energy-conserving and environment-protective of the invention, easily controllable, stability is good, the platinum carbon catalyst activearm of preparation
Point granulometric range is narrow, particle diameter is small, be evenly distributed, activity is high, selectivity is good, service life length.
(3) product produced by the present invention has good adhesiving effect, temperature tolerance and extremely strong catalytic effect.
Embodiment
The present invention is described further with reference to embodiment：
Embodiment 1
The present invention provides a kind of preparation method of high selectivity dopamine platinum carbon catalyst, it is characterised in that its preparation side
The step of method, is as follows：
1) system of platinum precursor solution is matched somebody with somebody
Chloroplatinic acid 394.74g (platinum content 38.0% in chloroplatinic acid) accurately is weighed, adds deionized water to dilute platinum to 50g/L,
And 150g castor oil (lubricant) is added into platinum acid chloride solution, under stirring, use quality fraction is 5% Na2CO3Solution is adjusted
Its pH to 1 is saved, platinum precursor solution is made；
2) system of dopamine precursor solution is matched somebody with somebody
The raw material used for absolute ethyl alcohol, dopamine, sodium hydroxide, deionized water, polyvinylpyrrolidone, step be by
Absolute ethyl alcohol is stirred vigorously, and dopamine obtained solution A is added dropwise, by deionized water, absolute ethyl alcohol, sodium hydroxide, polyvinyl pyrrole
Alkanone uniformly mixes, obtained solution B；In the case where being stirred vigorously, solution A is added drop-wise in solution B, stopping is added dropwise to complete and stirs
Mix；
3) it is catalyzed the washing of frame carrier
At normal temperatures, the acid treatment 20 minutes by aluminium oxide ceramics foaming body with the 0.01mol/L of 2 times of volumes, with 4 times of bodies
Long-pending deionized water cleaning, is then cleaned by ultrasonic with the neutral detergent of 2 times of volumes, is cleaned, adopted with the deionized water of 4 times of volumes
With soaked in absolute ethyl alcohol 5 hours, dry；
4) the platinum precursor solution of dopped activated carbon
Nitric acid treatment 4h by active carbon nanoparticles using the 0.5mol/L of 2 times of volumes, filtering, with 2-4 times of quality go from
Sub- water immersion, under agitation, adjusts pH to 5, soaks 12h, filtering, dries, dried active carbon nanoparticles then are put into platinum
Precursor solution, macromolecule dispersing agent is added, form the platinum precursor solution of dopped activated carbon；
5) preparation of platinum catalysis frame carrier
4) the platinum precursor solution of the dopped activated carbon in is put into special plastic bucket, by 3) by the way of the lifting
Foaming body be immersed in special plastic bucket, through repeatedly lifting after, by platinum be catalyzed frame carrier naturally dry, then will dry in the air
Catalysis frame carrier high temperature sintering after dry, to turning white completely, natural cooling；
6) preparation of dopamine platinum carbon catalyst
5) platinum in is catalyzed in the dopamine precursor solution 2) frame carrier is added in, using multiple lifting
Mode, then the frame carrier after lifting is put into drying box, washed through absolute ethyl alcohol, is dried to obtain dopamine platinum charcoal
Catalyst.
The activated carbon supported amount of the product is 5%, and the load capacity of platinum is 0.5%.
The product catalyst has good catalytic performance to the reaction of o-chloronitrobenzene preparing o-chloroaniline by catalytic hydrogenation,
O-chloronitrobenzene is 1.6g, isopropanol 15mL, catalyst amount 15.0mg, and reaction temperature is synthesis under normal pressure at 40 DEG C
45min, it is selectively respectively 100% and 97% to obtain o-chloronitrobenzene conversion ratio and o-chloraniline, after recycling 10 times according to
So keep preferable catalytic activity.
Embodiment 2
The present invention provides a kind of preparation method of high selectivity dopamine platinum carbon catalyst, it is characterised in that its preparation side
The step of method, is as follows：
1) system of platinum precursor solution is matched somebody with somebody
Chloroplatinic acid 394.74g (platinum content 38.0% in chloroplatinic acid) accurately is weighed, adds deionized water to dilute platinum to 30g/L,
And 300g fatty acid amides (lubricant) are added into platinum acid chloride solution, under agitation, use quality fraction is 15%
NaHCO3Solution adjusts its pH to 2.5, and platinum precursor solution is made；
2) system of dopamine precursor solution is matched somebody with somebody
The raw material used is absolute ethyl alcohol, dopamine, sodium hydroxide, deionized water, triethyl group hexyl phosphoric acid, step be by
Absolute ethyl alcohol is stirred vigorously, be added dropwise dopamine be made to obtain solution A, by deionized water, absolute ethyl alcohol, sodium hydroxide, triethyl group oneself
Base phosphoric acid uniformly mixes, obtained solution B；In the case where being stirred vigorously, solution A is added drop-wise in solution B, is added dropwise to complete stopping
Stirring；
3) it is catalyzed the washing of frame carrier
At normal temperatures, the acid treatment 20 minutes by aluminium oxide ceramics foaming body with the 0.01mol/L of 2 times of volumes, with 2 times of bodies
Long-pending deionized water cleaning, is then cleaned by ultrasonic with the neutral detergent of 2 times of volumes, is cleaned, adopted with the deionized water of 2 times of volumes
With soaked in absolute ethyl alcohol 2 hours, dry；
4) the platinum precursor solution of dopped activated carbon
Nitric acid treatment 4h by active carbon nanoparticles using the 0.5mol/L of 2 times of volumes, filtering, with 2-4 times of quality go from
Sub- water immersion, under agitation, adjusts pH to 1, soaks 4h, filtering, dries, before dried active carbon nanoparticles then are put into platinum
Liquid solution is driven, adds macromolecule dispersing agent, forms the platinum precursor solution of dopped activated carbon；
5) preparation of platinum catalysis frame carrier
4) the platinum precursor solution of the dopped activated carbon in is put into special plastic bucket, by 3) by the way of the lifting
Foaming body be immersed in special plastic bucket, through repeatedly lifting after, by platinum be catalyzed frame carrier naturally dry, then will dry in the air
Catalysis frame carrier high temperature sintering after dry, to turning white completely, natural cooling；
6) preparation of dopamine platinum carbon catalyst
5) platinum in is catalyzed in the dopamine precursor solution 2) frame carrier is added in, using multiple lifting
Mode, then the catalyst frame carrier after lifting is put into drying box, is washed through absolute ethyl alcohol, is dried to obtain DOPA
Amine platinum carbon catalyst.
The activated carbon supported amount of the product is 10%, and the load capacity of platinum is 15%.
The product catalyst has good catalytic performance to the reaction of o-chloronitrobenzene preparing o-chloroaniline by catalytic hydrogenation,
O-chloronitrobenzene is 1.6g, isopropanol 15mL, catalyst amount 15.0mg, and reaction temperature is synthesis under normal pressure at 40 DEG C
45min, it is selectively respectively 100% and 99.7% to obtain o-chloronitrobenzene conversion ratio and o-chloraniline, after reusing 20 times
Still keep preferable catalytic activity.
Embodiment 3
The present invention provides a kind of preparation method of high selectivity dopamine platinum carbon catalyst, it is characterised in that its preparation side
The step of method, is as follows：
1) system of platinum precursor solution is matched somebody with somebody
Chloroplatinic acid 394.74g (platinum content 38.0% in chloroplatinic acid) accurately is weighed, adds deionized water to dilute platinum to 30g/L,
And 300g fatty acid amides (lubricant) are added into platinum acid chloride solution, under agitation, use quality fraction is 15%
NaHCO3Solution adjusts its pH to 2.5, and platinum precursor solution is made；
2) system of dopamine precursor solution is matched somebody with somebody
The raw material used for absolute ethyl alcohol, dopamine, sodium hydroxide, deionized water, lauryl sodium sulfate, step be by
Absolute ethyl alcohol is stirred vigorously, and dopamine obtained solution A is added dropwise, by deionized water, absolute ethyl alcohol, sodium hydroxide, dodecyl sulphur
Sour sodium uniformly mixes, obtained solution B；In the case where being stirred vigorously, solution A is added drop-wise in solution B, stopping is added dropwise to complete and stirs
Mix；
3) it is catalyzed the washing of frame carrier
At normal temperatures, the acid treatment 20 minutes by aluminium oxide ceramics foaming body with the 0.01mol/L of 2 times of volumes, with 3 times of bodies
Long-pending deionized water cleaning, is then cleaned by ultrasonic with the neutral detergent of 2 times of volumes, is cleaned, adopted with the deionized water of 3 times of volumes
With soaked in absolute ethyl alcohol 3 hours, dry；
4) the platinum precursor solution of dopped activated carbon
Nitric acid treatment 4h by active carbon nanoparticles using the 0.5mol/L of 2 times of volumes, filtering, with 2-4 times of quality go from
Sub- water immersion, under agitation, adjusts pH to 3, soaks 8h, filtering, dries, before dried active carbon nanoparticles then are put into platinum
Liquid solution is driven, adds macromolecule dispersing agent, forms the platinum precursor solution of dopped activated carbon；
5) preparation of platinum catalysis frame carrier
4) the platinum precursor solution of the dopped activated carbon in is put into special plastic bucket, by 3) by the way of the lifting
Foaming body be immersed in special plastic bucket, through repeatedly lifting after, by platinum be catalyzed frame carrier naturally dry, then will dry in the air
Catalysis frame carrier high temperature sintering after dry, to turning white completely, natural cooling；
6) preparation of dopamine platinum carbon catalyst
5) platinum in is catalyzed in the dopamine precursor solution 2) frame carrier is added in, using multiple lifting
Mode, then the catalyst frame carrier after lifting is put into drying box, is washed through absolute ethyl alcohol, is dried to obtain DOPA
Amine platinum carbon catalyst.
The activated carbon supported amount of the product is 7%, and the load capacity of platinum is 8%.
The product catalyst has good catalytic performance to the reaction of o-chloronitrobenzene preparing o-chloroaniline by catalytic hydrogenation,
O-chloronitrobenzene is 1.6g, isopropanol 15mL, catalyst amount 15.0mg, and reaction temperature is synthesis under normal pressure at 40 DEG C
45min, it is selectively respectively 100% and 98% to obtain o-chloronitrobenzene conversion ratio and o-chloraniline, after recycling 15 times according to
So keep preferable catalytic activity.
Embodiments of the invention are the foregoing is only, are not intended to limit the present invention, it is all using equivalent substitution or equivalent transformation
The technical scheme that mode is obtained, all falls within protection scope of the present invention.
Claims (6)
1. a kind of preparation method of high selectivity dopamine platinum carbon catalyst, it is characterised in that as follows the step of its preparation method：
1) system of platinum precursor solution is matched somebody with somebody
Chloroplatinic acid is weighed, adds deionized water to dilute platinum to 20-50g/L, and lubricant is added into platinum acid chloride solution, is being stirred
Under, pH to 1-5 is adjusted, platinum precursor solution is made；
2) system of dopamine precursor solution is matched somebody with somebody
For the raw material used for absolute ethyl alcohol, dopamine, sodium hydroxide, deionized water, dispersant, step is that absolute ethyl alcohol is violent
Stirring, dopamine obtained solution A is added dropwise, deionized water, absolute ethyl alcohol, sodium hydroxide, dispersant are uniformly mixed, obtained solution
B；In the case where being stirred vigorously, solution A is added drop-wise in solution B, is added dropwise to complete stopping stirring；
3) it is catalyzed the washing of frame carrier
At normal temperatures, the acid treatment 20 minutes by aluminium oxide ceramics foaming body with the 0.01mol/L of 2 times of volumes, with 2-4 times of volume
Deionized water cleaning, be then cleaned by ultrasonic with the neutral detergent of 2 times of volumes, cleaned, adopted with the deionized water of 2-4 times of volume
With soaked in absolute ethyl alcohol 2-5 hours, dry；
4) the platinum precursor solution of dopped activated carbon
Nitric acid treatment 4h by active carbon nanoparticles using the 0.5mol/L of 2 times of volumes, filtering, with the deionized water of 2-4 times of quality
Immersion, under agitation, pH to 1-5 is adjusted, soak 4-12h, filtering, dry, dried active carbon nanoparticles are then put into platinum
Precursor solution, macromolecule dispersing agent is added, form the platinum precursor solution of dopped activated carbon；
5) preparation of platinum catalysis frame carrier
4) the platinum precursor solution of the dopped activated carbon in is put into special plastic bucket, by the oxygen in 3) by the way of the lifting
Change aluminium ceramic foam to be immersed in special plastic bucket, after repeatedly lifting, platinum is catalyzed frame carrier naturally dry, so
Catalysis frame carrier high temperature sintering after drying afterwards, to turning white completely, natural cooling；
6) preparation of dopamine platinum carbon catalyst
5) platinum in is catalyzed in the dopamine precursor solution 2) frame carrier is added in, using the side repeatedly lifted
Formula, then the frame carrier after lifting is put into drying box, washed through absolute ethyl alcohol, be dried to obtain the catalysis of dopamine platinum charcoal
Agent.
A kind of 2. preparation method of high selectivity dopamine platinum carbon catalyst according to claim 1, it is characterised in that institute
Lubricant in step 1) is stated to be formulated for castor oil, silicone oil, fatty acid amide, the one or more of carboxylic acid.
A kind of 3. preparation method of high selectivity dopamine platinum carbon catalyst according to claim 1, it is characterised in that institute
The dispersant stated in step 2) is polyvinylpyrrolidone, triethyl group hexyl phosphoric acid, lauryl sodium sulfate, methylpent
One of alcohol, cellulose derivative, polyacrylamide, guar gum, fatty acid polyethylene glycol ester.
A kind of 4. preparation method of high selectivity dopamine platinum carbon catalyst according to claim 1, it is characterised in that institute
It is 300-450 DEG C to state the high temperature sintering temperature in step 5).
A kind of 5. preparation method of high selectivity dopamine platinum carbon catalyst according to claim 1, it is characterised in that institute
It is 10-80ppi to state the catalysis frame carrier of the platinum in step 5), and the activated carbon supported amount of platinum catalysis frame carrier is 5-
10%, the load capacity of platinum is 0.5-15%.
A kind of 6. preparation method of high selectivity dopamine platinum carbon catalyst according to claim 1, it is characterised in that institute
State dopamine in the dopamine platinum carbon catalyst in step 6) and form chelated surface with platinum, form surface key.
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