CN108927148A - A kind of preparation method of high activity hydroxide palladium carbon - Google Patents
A kind of preparation method of high activity hydroxide palladium carbon Download PDFInfo
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- CN108927148A CN108927148A CN201810743273.3A CN201810743273A CN108927148A CN 108927148 A CN108927148 A CN 108927148A CN 201810743273 A CN201810743273 A CN 201810743273A CN 108927148 A CN108927148 A CN 108927148A
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- hydroxide
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- UKVIEHSSVKSQBA-UHFFFAOYSA-N methane;palladium Chemical compound C.[Pd] UKVIEHSSVKSQBA-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 230000000694 effects Effects 0.000 title claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 27
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 230000001376 precipitating effect Effects 0.000 claims abstract description 10
- 238000007598 dipping method Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000012805 post-processing Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 30
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 21
- 239000012498 ultrapure water Substances 0.000 claims description 21
- 239000006229 carbon black Substances 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 5
- 229910001854 alkali hydroxide Inorganic materials 0.000 claims description 5
- 150000002940 palladium Chemical class 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- 239000012266 salt solution Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 239000003273 ketjen black Substances 0.000 claims description 2
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 2
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 claims description 2
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 claims description 2
- 238000003828 vacuum filtration Methods 0.000 claims description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 9
- 239000003054 catalyst Substances 0.000 abstract description 6
- 238000006264 debenzylation reaction Methods 0.000 abstract description 5
- 238000005984 hydrogenation reaction Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 229910000510 noble metal Inorganic materials 0.000 abstract description 2
- 235000019241 carbon black Nutrition 0.000 description 13
- LXNAVEXFUKBNMK-UHFFFAOYSA-N acetic acid;palladium Chemical compound [Pd].CC(O)=O.CC(O)=O LXNAVEXFUKBNMK-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 3
- 102000004316 Oxidoreductases Human genes 0.000 description 2
- 108090000854 Oxidoreductases Proteins 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000005711 Benzoic acid Substances 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000012852 risk material Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/44—Palladium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The present invention provides a kind of preparation method of high activity hydroxide palladium carbon, belongs to the preparation method technical field of loaded noble metal catalyst, comprising the following steps: conductive carbon black pretreatment, the dipping of palladium presoma, palladium dydroxide precipitating and post-processing.Preparation method provided by the invention, simple process and low cost, hydroxide palladium carbon obtained are suitable for general hydrogenation reaction system, and especially plus hydrogen debenzylation reaction, uniform particle diameter, activity are high.
Description
Technical field
The invention belongs to the preparation method technical fields of loaded noble metal catalyst, and in particular to a kind of high activity hydrogen-oxygen
Change the preparation method of palladium carbon.
Background technique
Hydroxide palladium carbon has relatively broad application in medical organic synthesis and chemical field, mainly plays catalytic hydrogenation
Effect, including debenzylation, hydrogenation of olefins, benzoic acid reduction, the oxidation of aldehyde etc..Since William M.Pearlman in 1967
After being prepared for hydroxide palladium carbon using ion-exchange, the extensive concern of people is caused due to its excellent catalytic activity,
But the activity of existing hydroxide palladium carbon is still lower.
Existing a kind of palladium-carbon catalyst of application for a patent for invention and the preparation method and application thereof (application No. is
CN201611205052.8) include the following steps: to carry out acid oxidase processing to active carbon raw material；At alkali metal hydroxide
Manage acid oxidase treated activated carbon；Palladium-carbon catalyst is prepared as carrier using the activated carbon obtained after handling.But it prepared
Active carbon is handled using acid solutions such as nitric acid in journey, risk is high, and the palladium-carbon catalyst granular size obtained is inhomogenous, activity
It is low.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of high activity hydroxide palladium carbon, simple process and low cost is obtained
The hydroxide palladium carbon obtained is suitable for general hydrogenation reaction system, and especially plus hydrogen debenzylation reaction, uniform particle diameter, activity are high.
The present invention provides the following technical solutions:
A kind of preparation method of high activity hydroxide palladium carbon, comprising the following steps:
S1, conductive carbon black pretreatment: it weighs 1~100 part of conductive carbon black and is put into container, 1~100 part of organic solvent is added
And 1~500 part of ultrapure water, 10~90min is handled, is then filtered, washed, is dried to obtain processed carbon black；
The dipping of S2, palladium presoma: 1~1000 part of ultrapure water is added in processed carbon black into S1, is subsequently poured into
Palladium salt solution is stirred, 0.5~5h of mixing time with the speed of 100~500rmp；
The precipitating of S3, palladium dydroxide: alkali hydroxide soln or carbonate is added in the mixed solution obtained to S2
Solution adjusts pH to 8~13, is stirred with the speed of 100~500rmp, and microwave heating reaction is aged 12h；
S4, post-processing: the solution after being aged in S3 being filtered, and is cleaned 3~10 times with ultrapure water, until filtrate pH
Value is neutrality, and being then dried under vacuum to moisture content is 10%~80%, obtains high activity hydroxide palladium carbon finished product, Vacuum Package.
Preferably, the organic solvent in the S1 is one of methanol, ethyl alcohol or ethylene glycol or a variety of, is conducive to improve
The dispersing uniformity of conductive black.
Preferably, in the S1 conductive carbon black be Ketjen black series of conductive carbon black, Cabot XC-72 series of conductive carbon black or
One of BP series of conductive carbon black, has good meso-hole structure, and large specific surface area and aperture is moderate is conducive to active particle
Load.
Preferably, the filter method in the S1 is positive press filtration or vacuum filtration, and drying means is vacuum drying, dry
Temperature be 40~100 DEG C, drying time be 10~for 24 hours.
Preferably, the palladium salt solution in the S2 is one of palladium acetate, palladium chloride or palladium nitrate solution.
Preferably, the alkali hydroxide soln in the S3 is sodium hydroxide solution, and the carbonate solution is carbon
Acid sodium solution.
Preferably, the power of microwave heating is 400~900W in the S3, and the reaction time is 5~20min.
Preferably, the filter method in the S4 is positive press filtration, and vacuum drying temperature is 40~100 DEG C.
The beneficial effects of the present invention are:
(1) present invention uses conductive black, has good meso-hole structure, and large specific surface area and aperture is moderate is conducive to
The load of active particle, and raw material is easy to get, compared with other carbon blacks, conductive black be easier to be dispersed in methanol, ethyl alcohol or
In ethylene glycol organic solvent.
(2) present invention does not have risk, and raw material using the organic solvent and Pure water preparation conductive black suitably matched
It is easy to get, it is at low cost.
(3) it in the precipitating of step S3 palladium dydroxide of the present invention, with alkali hydroxide soln or carbonate solution, adjusts
PH to 8~13 makes palladium salt generate palladium dydroxide precipitating in alkaline environment with certain speed responsing；Using microwave heating, add
It is hot rapidly and uniform；It is finally aged, is deposited in palladium dydroxide on conductive black carrier and grows up to active particle, and make active particle
Particle diameter distribution is uniform.
(4) preparation method provided by the invention, simple process are suitble to large-scale production and application.
(5) the hydroxide palladium carbon prepared by the present invention, granularity is uniform, is suitable for general hydrogenation reaction system, especially
It is the utilization rate that its catalytic activity and active component are improved in the hydrogenation process of debenzylation.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the TEM figure for the high activity hydroxide palladium carbon that embodiment 1 prepares.
Specific embodiment
Embodiment 1
A kind of preparation method of high activity hydroxide palladium carbon, comprising the following steps:
S1, conductive carbon black pretreatment: it weighs 4.5g XC-72 conductive carbon black and is put into 250ml container, 10ml methanol is added
And 100ml ultrapure water, 1h is handled, is then filtered, washed, is dried to obtain processed carbon black；
The dipping of S2, palladium presoma: the ultrapure water of 100ml is added in processed carbon black into S1, is subsequently poured into acetic acid
Palladium solution (palladium content 0.5g) is stirred, mixing time 2h with the speed of 100rmp；
The precipitating of S3, palladium dydroxide: the sodium hydroxide solution being added in the mixed solution obtained to S2, adjusting pH to 9~
11, it is stirred with the speed of 100rmp, microwave heating reaction, microwave power 600W, reaction time 10min are aged 12h；
S4, post-processing: the solution after being aged in S3 being filtered, and is cleaned 3~10 times with ultrapure water, until filtrate pH
Value is neutrality, and it is 50% that then 100 DEG C, which are dried under vacuum to moisture content, obtains high activity hydroxide palladium carbon finished product, Vacuum Package.
Fig. 1 is the TEM figure for the high activity hydroxide palladium carbon that the present embodiment prepares, as seen from the figure, the present embodiment preparation
The partial size of palladium dydroxide carbon particle out is smaller and is evenly distributed.
Embodiment 2
A kind of preparation method of high activity hydroxide palladium carbon, comprising the following steps:
S1, conductive carbon black pretreatment: it weighs 4.5g BP2000 conductive carbon black and is put into 250ml container, 10ml methanol is added
And 100ml ultrapure water, 1h is handled, is then filtered, washed, is dried to obtain processed carbon black；
The dipping of S2, palladium presoma: the ultrapure water of 100ml is added in processed carbon black into S1, is subsequently poured into acetic acid
Palladium solution (palladium content 0.5g) is stirred, mixing time 2h with the speed of 100rmp；
The precipitating of S3, palladium dydroxide: the sodium hydroxide solution being added in the mixed solution obtained to S2, adjusting pH to 9~
11, it is stirred with the speed of 100rmp, microwave heating reaction, microwave power 600W, reaction time 10min are aged 12h；
S4, post-processing: the solution after being aged in S3 being filtered, and is cleaned 3~10 times with ultrapure water, until filtrate pH
Value is neutrality, and it is 50% that then 100 DEG C, which are dried under vacuum to moisture content, obtains high activity hydroxide palladium carbon finished product, Vacuum Package.
Embodiment 3
A kind of preparation method of high activity hydroxide palladium carbon, comprising the following steps:
S1, conductive carbon black pretreatment: it weighs 4.5g XC-72 conductive carbon black and is put into 250ml container, 10ml methanol is added
And 100ml ultrapure water, 1h is handled, is then filtered, washed, is dried to obtain processed carbon black；
The dipping of S2, palladium presoma: the ultrapure water of 100ml is added in processed carbon black into S1, is subsequently poured into chlorination
Palladium solution (palladium content 0.5g) is stirred, mixing time 2h with the speed of 100rmp；
The precipitating of S3, palladium dydroxide: the sodium hydroxide solution being added in the mixed solution obtained to S2, adjusting pH to 9~
11, it is stirred with the speed of 100rmp, microwave heating reaction, microwave power 600W, reaction time 10min are aged 12h；
S4, post-processing: the solution after being aged in S3 being filtered, and is cleaned 3~10 times with ultrapure water, until filtrate pH
Value is neutrality, and it is 50% that then 100 DEG C, which are dried under vacuum to moisture content, obtains high activity hydroxide palladium carbon finished product, Vacuum Package.
Embodiment 4
A kind of preparation method of high activity hydroxide palladium carbon, comprising the following steps:
S1, conductive carbon black pretreatment: it weighs 4.5g XC-72 conductive carbon black and is put into 250ml container, 10ml methanol is added
And 100ml ultrapure water, 1h is handled, is then filtered, washed, is dried to obtain processed carbon black；
The dipping of S2, palladium presoma: the ultrapure water of 100ml is added in processed carbon black into S1, is subsequently poured into acetic acid
Palladium solution (palladium content 0.5g) is stirred, mixing time 2h with the speed of 100rmp；
The precipitating of S3, palladium dydroxide: the sodium hydroxide solution being added in the mixed solution obtained to S2, adjusting pH to 9~
11, it is stirred with the speed of 20rmp, microwave heating reaction, microwave power 600W, reaction time 10min are aged 12h；
S4, post-processing: the solution after being aged in S3 being filtered, and is cleaned 3~10 times with ultrapure water, until filtrate pH
Value is neutrality, and it is 50% that then 100 DEG C, which are dried under vacuum to moisture content, obtains high activity hydroxide palladium carbon finished product, Vacuum Package.
Embodiment 5
A kind of preparation method of high activity hydroxide palladium carbon, comprising the following steps:
S1, conductive carbon black pretreatment: it weighs 4.5g XC-72 conductive carbon black and is put into 250ml container, 10ml methanol is added
And 100ml ultrapure water, 1h is handled, is then filtered, washed, is dried to obtain processed carbon black；
The dipping of S2, palladium presoma: the ultrapure water of 100ml is added in processed carbon black into S1, is subsequently poured into acetic acid
Palladium solution (palladium content 0.5g) is stirred, mixing time 2h with the speed of 100rmp；
The precipitating of S3, palladium dydroxide: the sodium hydroxide solution being added in the mixed solution obtained to S2, adjusting pH to 9~
11, it is stirred with the speed of 100rmp, microwave heating reaction, microwave power 900W, reaction time 10min are aged 12h；
S4, post-processing: the solution after being aged in S3 being filtered, and is cleaned 3~10 times with ultrapure water, until filtrate pH
Value is neutrality, and it is 50% that then 100 DEG C, which are dried under vacuum to moisture content, obtains high activity hydroxide palladium carbon finished product, Vacuum Package.
Table 1 is the catalysis debenzylation performance table of hydroxide palladium carbon prepared by embodiment 1-5
As it can be seen from table 1 palladium dydroxide carbon particle partial size is smaller, distribution is more uniform, it is shorter the time required to fully reacting,
Catalyst activity is higher.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although referring to aforementioned reality
Applying example, invention is explained in detail, for those skilled in the art, still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features.It is all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of preparation method of high activity hydroxide palladium carbon, which comprises the following steps:
S1, conductive carbon black pretreatment: weigh 1~100 part of conductive carbon black be put into container, be added 1~100 part of organic solvent and
1~500 part of ultrapure water handles 10~90min, is then filtered, washed, is dried to obtain processed carbon black；
The dipping of S2, palladium presoma: 1~1000 part of ultrapure water is added in processed carbon black into S1, is subsequently poured into palladium salt
Solution is stirred, 0.5~5h of mixing time with the speed of 100~500rmp；
The precipitating of S3, palladium dydroxide: being added alkali hydroxide soln or carbonate solution in the mixed solution obtained to S2,
PH to 8~13 is adjusted, is stirred with the speed of 100~500rmp, microwave heating reaction is aged 12h；
S4, post-processing: the solution after being aged in S3 being filtered, and is cleaned 3~10 times with ultrapure water, until filtrate pH value is
Neutrality, being then dried under vacuum to moisture content is 10%~80%, obtains high activity hydroxide palladium carbon finished product, Vacuum Package.
2. a kind of preparation method of high activity hydroxide palladium carbon according to claim 1, which is characterized in that in the S1
Organic solvent is one of methanol, ethyl alcohol or ethylene glycol or a variety of.
3. a kind of preparation method of high activity hydroxide palladium carbon according to claim 1, which is characterized in that led in the S1
Electrical carbon is black for one of Ketjen black series of conductive carbon black, Cabot XC-72 series of conductive carbon black or BP series of conductive carbon black.
4. a kind of preparation method of high activity hydroxide palladium carbon according to claim 1, which is characterized in that in the S1
Filter method is positive press filtration or vacuum filtration, and drying means is vacuum drying, and drying temperature is 40~100 DEG C, drying time
For 10~for 24 hours.
5. a kind of preparation method of high activity hydroxide palladium carbon according to claim 1, which is characterized in that in the S2
Palladium salt solution is one of palladium acetate, palladium chloride or palladium nitrate solution.
6. a kind of preparation method of high activity hydroxide palladium carbon according to claim 1, which is characterized in that in the S3
Alkali hydroxide soln is sodium hydroxide solution, and the carbonate solution is sodium carbonate liquor.
7. a kind of preparation method of high activity hydroxide palladium carbon according to claim 1, which is characterized in that micro- in the S3
The power of Wave heating is 400~900W, and the reaction time is 5~20min.
8. a kind of preparation method of high activity hydroxide palladium carbon according to claim 1, which is characterized in that in the S4
Filter method is positive press filtration, and vacuum drying temperature is 40~100 DEG C.
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| CN113680362A (en) * | 2021-08-18 | 2021-11-23 | 北京工业大学 | Preparation method of palladium hydroxide carbon catalyst for removing N-benzyl |
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| CN113680362A (en) * | 2021-08-18 | 2021-11-23 | 北京工业大学 | Preparation method of palladium hydroxide carbon catalyst for removing N-benzyl |
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