CN105688896A - Method for preparing palladium-carbon catalyst for producing nilox resin - Google Patents
Method for preparing palladium-carbon catalyst for producing nilox resin Download PDFInfo
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- CN105688896A CN105688896A CN201610058102.8A CN201610058102A CN105688896A CN 105688896 A CN105688896 A CN 105688896A CN 201610058102 A CN201610058102 A CN 201610058102A CN 105688896 A CN105688896 A CN 105688896A
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- 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
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- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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Abstract
The invention discloses a method for preparing a palladium-carbon catalyst for producing nilox resin and belongs to the technical field of nilox resin preparation. The method comprises the following steps: acidizing activated carbon, washing and drying; soaking into a solution prepared by mixing titanium tetrachloride with hexane; filtering, washing and drying, and then alkalizing, washing and drying; soaking into a solution prepared by mixing sodium hypochlorite with palladium acetate, and then filtering, washing and drying; putting into hydrogen for reduction; lastly, burning at high temperature, thereby acquiring the palladium-carbon catalyst. The palladium-carbon catalyst prepared according to the method provided by the invention is high in dispersity, obvious in catalytic activity and reusable.
Description
Technical field
The invention belongs to disproportionated rosin preparing technical field, the preparation method particularly relating to a kind of disproportionated rosin production palladium-carbon catalyst。
Background technology
Disproportionated rosin, mainly with Colophonium for raw material, prepares by carrying out catalytic isomerization with palladium carbon for catalyst。
It is not high enough that existing palladium carbon is that catalyst exists catalysis activity mostly, easily in the process preparing disproportionated rosin, because the impurity such as the hot conditions of its preparation process and organic materials are deposited on the reasons such as palladium-carbon catalyst surface, cause that palladium-carbon catalyst activity reduces, even inactivate, finally cannot again come into operation。
Summary of the invention
Present invention solves the technical problem that the preparation method being to provide a kind of disproportionated rosin production palladium-carbon catalyst, the catalysis activity of the palladium-carbon catalyst that the method prepares is high, it is not easy to inactivation, can Reusability。
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
It comprises the following steps:
A, first activated carbon is put in the salpeter solution that concentration is 60%, acidifying 2 hours～6 hours at 50 DEG C～70 DEG C, then with deionized water wash to neutral, and dry；
B, the activated carbon after step A processes is put in the solution prepared for the ratio mixing of 1:4 in mass ratio by titanium tetrachloride and hexane, dipping 1 hour～4 hours at normal temperatures, then filter, with deionized water wash to neutral, and dry；
C, the activated carbon after step B processes is put in the sodium hydroxide solution that concentration is 15%, alkalize 2 hours～6 hours at 50 DEG C～70 DEG C, then with deionized water wash to neutral；
D, the activated carbon after step C processes is put in the solution prepared for the ratio mixing of 10:1 in mass ratio by sodium hypochlorite and palladium, dipping 4 hours～6 hours at normal temperatures, then filter, with deionized water wash to neutral, and dry；
E, the activated carbon after D step process is placed in temperature be 400 DEG C～500 DEG C, purity be 99.5% hydrogen in 4 hours～8 hours, then calcine 3 hours～6 hours at 1100 DEG C～1200 DEG C, prepare。
Owing to adopting technique scheme, the present invention obtains providing the benefit that:
The palladium-carbon catalyst dispersion that the present invention prepares is high, and catalysis activity is notable, 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 intended to be limited to following example。
Embodiment 1
The preparation method of this disproportionated rosin production palladium-carbon catalyst comprises the following steps:
A, first activated carbon is put in the salpeter solution that concentration is 60%, acidifying 6 hours at 50 DEG C, then with deionized water wash to neutral, and dry；
B, the activated carbon after step A processes is put in the solution prepared for the ratio mixing of 1:4 in mass ratio by titanium tetrachloride and hexane, dipping 1 hour at normal temperatures, then filter, with deionized water wash to neutral, and dry；
C, the activated carbon after step B processes is put in the sodium hydroxide solution that concentration is 15%, alkalize 6 hours at 50 DEG C, then with deionized water wash to neutral；
D, the activated carbon after step C processes is put in the solution prepared for the ratio mixing of 10:1 in mass ratio by sodium hypochlorite and palladium, dipping 4 hours at normal temperatures, then filter, with deionized water wash to neutral, and dry；
E, the activated carbon after D step process is placed in temperature be 400 DEG C, purity be 99.5% hydrogen in 8 hours, then calcine 6 hours at 1100 DEG C, prepare。
Embodiment 2
The preparation method of this disproportionated rosin production palladium-carbon catalyst comprises the following steps:
A, first activated carbon is put in the salpeter solution that concentration is 60%, acidifying 2 hours at 70 DEG C, then with deionized water wash to neutral, and dry；
B, the activated carbon after step A processes is put in the solution prepared for the ratio mixing of 1:4 in mass ratio by titanium tetrachloride and hexane, dipping 4 hours at normal temperatures, then filter, with deionized water wash to neutral, and dry；
C, the activated carbon after step B processes is put in the sodium hydroxide solution that concentration is 15%, alkalize 2 hours at 70 DEG C, then with deionized water wash to neutral；
D, the activated carbon after step C processes is put in the solution prepared for the ratio mixing of 10:1 in mass ratio by sodium hypochlorite and palladium, dipping 6 hours at normal temperatures, then filter, with deionized water wash to neutral, and dry；
E, the activated carbon after D step process is placed in temperature be 500 DEG C, purity be 99.5% hydrogen in 4 hours, then calcine 3 hours at 1200 DEG C, prepare。
Embodiment 3
The preparation method of this disproportionated rosin production palladium-carbon catalyst comprises the following steps:
A, first activated carbon is put in the salpeter solution that concentration is 60%, acidifying 4 hours at 60 DEG C, then with deionized water wash to neutral, and dry；
B, the activated carbon after step A processes is put in the solution prepared for the ratio mixing of 1:4 in mass ratio by titanium tetrachloride and hexane, dipping 3 hours at normal temperatures, then filter, with deionized water wash to neutral, and dry；
C, the activated carbon after step B processes is put in the sodium hydroxide solution that concentration is 15%, alkalize 4 hours at 60 DEG C, then with deionized water wash to neutral；
D, the activated carbon after step C processes is put in the solution prepared for the ratio mixing of 10:1 in mass ratio by sodium hypochlorite and palladium, dipping 4 hours at normal temperatures, then filter, with deionized water wash to neutral, and dry；
E, the activated carbon after D step process is placed in temperature be 450 DEG C, purity be 99.5% hydrogen in 6 hours, then calcine 4 hours at 1100 DEG C, prepare。
The catalysis activity that embodiment 1～3 brings back to life the palladium-carbon catalyst, original new palladium-carbon catalyst and both mixture that obtain is tested, its result such as table 1。
Table 1
。
Claims (1)
1. the preparation method of a disproportionated rosin production palladium-carbon catalyst, it is characterised in that comprise the following steps:
A, first activated carbon is put in the salpeter solution that concentration is 60%, acidifying 2 hours～6 hours at 50 DEG C～70 DEG C, then with deionized water wash to neutral, and dry；
B, the activated carbon after step A processes is put in the solution prepared for the ratio mixing of 1:4 in mass ratio by titanium tetrachloride and hexane, dipping 1 hour～4 hours at normal temperatures, then filter, with deionized water wash to neutral, and dry；
C, the activated carbon after step B processes is put in the sodium hydroxide solution that concentration is 15%, alkalize 2 hours～6 hours at 50 DEG C～70 DEG C, then with deionized water wash to neutral；
D, the activated carbon after step C processes is put in the solution prepared for the ratio mixing of 10:1 in mass ratio by sodium hypochlorite and palladium, dipping 4 hours～6 hours at normal temperatures, then filter, with deionized water wash to neutral, and dry；
E, the activated carbon after D step process is placed in temperature be 400 DEG C～500 DEG C, purity be 99.5% hydrogen in 4 hours～8 hours, then calcine 3 hours～6 hours at 1100 DEG C～1200 DEG C, prepare。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610058102.8A CN105688896A (en) | 2016-01-27 | 2016-01-27 | Method for preparing palladium-carbon catalyst for producing nilox resin |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610058102.8A CN105688896A (en) | 2016-01-27 | 2016-01-27 | Method for preparing palladium-carbon catalyst for producing nilox resin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106111128A (en) * | 2016-06-26 | 2016-11-16 | 广西众昌树脂有限公司 | Hydrogenated rosin production catalyst |
| CN115555014A (en) * | 2021-07-01 | 2023-01-03 | 谷育英 | High-activity palladium-carbon catalyst and preparation method and application thereof |
Citations (5)
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| SU180574A1 (en) * | М. С. Немцов, И. Радченко, М. И. Рыскин, С. Л. ибр , Ф. С. Шендерович | DISPROPORTIONATION METHOD | ||
| CN1565725A (en) * | 2003-06-12 | 2005-01-19 | 中国石化上海石油化工股份有限公司 | Method for preparing hydrogenising selectively palladium/carbon catalyzer |
| 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 |
| CN102626619A (en) * | 2012-03-24 | 2012-08-08 | 中国石油化工股份有限公司 | Preparation method of palladium carbon catalyst |
| 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 CN201610058102.8A patent/CN105688896A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU180574A1 (en) * | М. С. Немцов, И. Радченко, М. И. Рыскин, С. Л. ибр , Ф. С. Шендерович | DISPROPORTIONATION METHOD | ||
| CN1565725A (en) * | 2003-06-12 | 2005-01-19 | 中国石化上海石油化工股份有限公司 | Method for preparing hydrogenising selectively palladium/carbon catalyzer |
| 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 |
| CN102626619A (en) * | 2012-03-24 | 2012-08-08 | 中国石油化工股份有限公司 | Preparation method of palladium carbon catalyst |
| CN103394347A (en) * | 2013-07-23 | 2013-11-20 | 河海大学 | Preparation method of high-activity palladium-carbon catalyst |
Non-Patent Citations (3)
| Title |
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| 厉嘉云等: ""碱处理对活性炭载体及负载钯催化剂性能的影响"", 《石油化工》 * |
| 宋永辉等: "《提金氰化废水处理理论与方法》", 31 March 2015, 冶金工业出版社 * |
| 曾韬等: ""钯/竹炭催化剂的制备及表征"", 《生物质化学工程》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106111128A (en) * | 2016-06-26 | 2016-11-16 | 广西众昌树脂有限公司 | Hydrogenated rosin production catalyst |
| CN115555014A (en) * | 2021-07-01 | 2023-01-03 | 谷育英 | High-activity palladium-carbon catalyst and preparation method and application thereof |
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