CN105478110A - Preparing method of palladium-charcoal catalyst for producing disproportionation rosin - Google Patents
Preparing method of palladium-charcoal catalyst for producing disproportionation rosin Download PDFInfo
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- CN105478110A CN105478110A CN201610054427.9A CN201610054427A CN105478110A CN 105478110 A CN105478110 A CN 105478110A CN 201610054427 A CN201610054427 A CN 201610054427A CN 105478110 A CN105478110 A CN 105478110A
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- Prior art keywords
- hours
- palladium
- active carbon
- neutral
- deionized water
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- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000003054 catalyst Substances 0.000 title claims abstract description 19
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 title claims abstract description 14
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 14
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 title claims abstract description 14
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 238000007323 disproportionation reaction Methods 0.000 title abstract 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 12
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 6
- 239000001257 hydrogen Substances 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- UKVIEHSSVKSQBA-UHFFFAOYSA-N methane;palladium Chemical compound C.[Pd] UKVIEHSSVKSQBA-UHFFFAOYSA-N 0.000 claims description 15
- 230000007935 neutral effect Effects 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 5
- 229910052763 palladium Inorganic materials 0.000 claims description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 238000001035 drying Methods 0.000 abstract 2
- 238000005406 washing Methods 0.000 abstract 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 2
- 230000002779 inactivation Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000002994 raw material Substances 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09F—NATURAL RESINS; FRENCH POLISH; DRYING-OILS; OIL DRYING AGENTS, i.e. SICCATIVES; TURPENTINE
- C09F1/00—Obtaining purification, or chemical modification of natural resins, e.g. oleo-resins
- C09F1/04—Chemical modification, e.g. esterification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparing method of a palladium-charcoal catalyst for producing disproportionation rosin, and belongs to the technical field of preparing of the disproportionation rosin. The preparing method includes the steps that active carbon is acidized, washed and dried; aluminum nitrate is loaded, and then alkalifying, washing and drying are carried out; the product is soaked into a solution prepared by mixing hydrogen peroxide and palladium acetate, and filtering, washing and drying are carried out; then the product is put into nitrogen and hydrogen in sequence to be reduced, and the palladium-charcoal catalyst is prepared. The palladium-charcoal catalyst prepared with the method is high in dispersity and remarkable in catalytic activity, and can be recycled.
Description
Technical field
The invention belongs to disproportionated rosin preparing technical field, particularly relate to a kind of preparation method of disproportionated rosin production palladium-carbon catalyst.
Background technology
Disproportionated rosin is mainly raw material with rosin, by obtaining for catalyst carries out catalytic isomerization with palladium carbon.
It is not high enough that existing palladium carbon is that catalyst exists catalytic activity mostly, easily in the process preparing disproportionated rosin, because the Impurity depositions such as the hot conditions of its preparation process and organic materials are in reasons such as palladium-carbon catalyst surfaces, palladium-carbon catalyst activity is caused to reduce, even inactivation, finally cannot come into operation again.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of preparation method of disproportionated rosin production palladium-carbon catalyst, and the catalytic activity of the palladium-carbon catalyst that the method obtains is high, is not easy inactivation, can Reusability.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
It comprises the following steps:
A, first active carbon is put into the salpeter solution that concentration is 60%, acidifying 2 hours ~ 6 hours at 50 DEG C ~ 70 DEG C, then spend deionized water to neutral;
B, aluminum nitrate to be loaded on the active carbon after step A process, and to dry;
C, the active carbon after step B process is put into the sodium hydroxide solution that concentration is 15%, alkalize 2 hours ~ 6 hours at 50 DEG C ~ 70 DEG C, then spend deionized water to neutral;
D, the active carbon after step C process to be put into by hydrogen peroxide and palladium in mass ratio for the ratio of 10:1 mixes obtained solution, flood 4 hours ~ 6 hours at normal temperatures, then filter, spend deionized water to neutral, and dry;
E, the active carbon after D step process is placed in the nitrogen stream 20 hours ~ 24 hours that temperature is 70 DEG C ~ 90 DEG C, then taken out, be then placed in that temperature is 400 DEG C ~ 500 DEG C, purity be 99.5% hydrogen 4 hours ~ 8 hours, obtained.
Owing to adopting technique scheme, the beneficial effect that the present invention obtains is:
The palladium-carbon catalyst decentralization that the present invention obtains is high, and catalytic activity is remarkable, reusable.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described, and protection scope of the present invention is not only confined to following examples.
Embodiment 1
The preparation method of this disproportionated rosin production palladium-carbon catalyst comprises the following steps:
A, first active carbon is put into the salpeter solution that concentration is 60%, acidifying 6 hours at 50 DEG C, then spend deionized water to neutral;
B, aluminum nitrate to be loaded on the active carbon after step A process, and to dry;
C, the active carbon after step B process is put into the sodium hydroxide solution that concentration is 15%, alkalize 6 hours at 50 DEG C, then spend deionized water to neutral;
D, the active carbon after step C process to be put into by hydrogen peroxide and palladium in mass ratio for the ratio of 10:1 mixes obtained solution, flood 4 hours at normal temperatures, then filter, spend deionized water to neutral, and dry;
E, the active carbon after D step process is placed in the nitrogen stream 24 hours that temperature is 70 DEG C, then taken out, be then placed in that temperature is 400 DEG C, purity be 99.5% hydrogen 8 hours, obtained.
Embodiment 2
The preparation method of this disproportionated rosin production palladium-carbon catalyst comprises the following steps:
A, first active carbon is put into the salpeter solution that concentration is 60%, acidifying 2 hours at 70 DEG C, then spend deionized water to neutral;
B, aluminum nitrate to be loaded on the active carbon after step A process, and to dry;
C, the active carbon after step B process is put into the sodium hydroxide solution that concentration is 15%, alkalize 2 hours at 70 DEG C, then spend deionized water to neutral;
D, the active carbon after step C process to be put into by hydrogen peroxide and palladium in mass ratio for the ratio of 10:1 mixes obtained solution, flood 6 hours at normal temperatures, then filter, spend deionized water to neutral, and dry;
E, the active carbon after D step process is placed in the nitrogen stream 20 hours that temperature is 90 DEG C, then taken out, be then placed in that temperature is 500 DEG C, purity be 99.5% hydrogen 4 hours, obtained.
Embodiment 3
The preparation method of this disproportionated rosin production palladium-carbon catalyst comprises the following steps:
A, first active carbon is put into the salpeter solution that concentration is 60%, acidifying 4 hours at 60 DEG C, then spend deionized water to neutral;
B, aluminum nitrate to be loaded on the active carbon after step A process, and to dry;
C, the active carbon after step B process is put into the sodium hydroxide solution that concentration is 15%, alkalize 4 hours at 60 DEG C, then spend deionized water to neutral;
D, the active carbon after step C process to be put into by hydrogen peroxide and palladium in mass ratio for the ratio of 10:1 mixes obtained solution, flood 5 hours at normal temperatures, then filter, spend deionized water to neutral, and dry;
E, the active carbon after D step process is placed in the nitrogen stream 22 hours that temperature is 80 DEG C, then taken out, be then placed in that temperature is 450 DEG C, purity be 99.5% hydrogen 6 hours, obtained.
The catalytic activity that embodiment 1 ~ 3 is brought back to life the palladium-carbon catalyst obtained, original new palladium-carbon catalyst and both mixtures is tested, and its result is as table 1.
Table 1
。
Claims (1)
1. a preparation method for disproportionated rosin production palladium-carbon catalyst, is characterized in that comprising the following steps:
A, first active carbon is put into the salpeter solution that concentration is 60%, acidifying 2 hours ~ 6 hours at 50 DEG C ~ 70 DEG C, then spend deionized water to neutral;
B, aluminum nitrate to be loaded on the active carbon after step A process, and to dry;
C, the active carbon after step B process is put into the sodium hydroxide solution that concentration is 15%, alkalize 2 hours ~ 6 hours at 50 DEG C ~ 70 DEG C, then spend deionized water to neutral;
D, the active carbon after step C process to be put into by hydrogen peroxide and palladium in mass ratio for the ratio of 10:1 mixes obtained solution, flood 4 hours ~ 6 hours at normal temperatures, then filter, spend deionized water to neutral, and dry;
E, the active carbon after D step process is placed in the nitrogen stream 20 hours ~ 24 hours that temperature is 70 DEG C ~ 90 DEG C, then taken out, be then placed in that temperature is 400 DEG C ~ 500 DEG C, purity be 99.5% hydrogen 4 hours ~ 8 hours, obtained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610054427.9A CN105478110A (en) | 2016-01-27 | 2016-01-27 | Preparing method of palladium-charcoal catalyst for producing disproportionation rosin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610054427.9A CN105478110A (en) | 2016-01-27 | 2016-01-27 | Preparing method of palladium-charcoal catalyst for producing disproportionation rosin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105478110A true CN105478110A (en) | 2016-04-13 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610054427.9A Pending CN105478110A (en) | 2016-01-27 | 2016-01-27 | Preparing method of palladium-charcoal catalyst for producing disproportionation rosin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105478110A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1672787A (en) * | 2005-01-07 | 2005-09-28 | 贵研铂业股份有限公司 | Rosin-disproportionating high activity Pd/C catalyst preparing process |
| CN101433839A (en) * | 2008-12-19 | 2009-05-20 | 长沙荣星贵金属有限公司 | Method for preparing palladium carbon catalyst of high activity |
| CN103007962A (en) * | 2012-12-14 | 2013-04-03 | 北京格林凯默科技有限公司 | Metal oxide assisted palladium carbon catalyst and preparation method thereof |
| CN103394347A (en) * | 2013-07-23 | 2013-11-20 | 河海大学 | Preparation method of high-activity palladium-carbon catalyst |
-
2016
- 2016-01-27 CN CN201610054427.9A patent/CN105478110A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1672787A (en) * | 2005-01-07 | 2005-09-28 | 贵研铂业股份有限公司 | Rosin-disproportionating high activity Pd/C catalyst preparing process |
| CN101433839A (en) * | 2008-12-19 | 2009-05-20 | 长沙荣星贵金属有限公司 | Method for preparing palladium carbon catalyst of high activity |
| CN103007962A (en) * | 2012-12-14 | 2013-04-03 | 北京格林凯默科技有限公司 | Metal oxide assisted palladium carbon catalyst and preparation method thereof |
| CN103394347A (en) * | 2013-07-23 | 2013-11-20 | 河海大学 | Preparation method of high-activity palladium-carbon catalyst |
Non-Patent Citations (1)
| Title |
|---|
| 邹澎澎等: "钯炭催化剂的研究进展", 《石油学报（石油加工）》 * |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160413 |
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| RJ01 | Rejection of invention patent application after publication |