CN105562123A - Prereduction method for catalyst for synthesizing rubber antioxidant - Google Patents
Prereduction method for catalyst for synthesizing rubber antioxidant Download PDFInfo
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- CN105562123A CN105562123A CN201410551834.1A CN201410551834A CN105562123A CN 105562123 A CN105562123 A CN 105562123A CN 201410551834 A CN201410551834 A CN 201410551834A CN 105562123 A CN105562123 A CN 105562123A
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Abstract
The invention belongs to the technical field of fine chemical engineering, and relates to a prereduction method for a catalyst for synthesizing a rubber antioxidant. The problems that in existing industrial production and laboratory tests, due to the fact that a large quantity of prereduction solvents are used for conducting prereduction on the catalyst, not only are the raw material production cost and the post-treatment production cost increased, but also a large number of unqualified products are produced at the initial reaction stage are mainly solved. According to the prereduction method for the catalyst for synthesizing the rubber antioxidant, nitrogen and hydrogen are adopted to conduct catalyst reduction, cleanliness is achieved, the prereduction solvents such as isopropyl alcohol and 4-methyl-2-pentanol are saved, the number of semi-finished products is decreased, or the semi-finished products are not produced, cleaning production is achieved, consumed raw materials are saved, and the prereduction method can be well applied to the industrial production process of rubber antioxidants 6PPD and IPPD.
Description
Technical field
The invention belongs to technical field of fine, relate to a kind of synthetic rubber age resistor 6PPD and IPPD catalyst prereduction method.
Background technology
Rubber antioxidant 6PPD and IPPD is high-efficiency multi-function low-toxicity product, is mainly used in rubber industry, is most important kind in current rubber antioxidant, and they are in natural and synthetic rubber, to ozone with subdue and agingly have good protective benefits.Adopt isopropyl alcohol to carry out prereduction in current production technology, producing upper isopropyl alcohol reduction at least needs one week, and carries out initial production production and can produce underproof product reducing end.Therefore the research of synthesis age resistor 6PPD and 4010NA catalyst prereduction method is also got more and more.
Describe the activation method of the Cu-series catalyst for the synthesis of rubber antioxidant 6PPD in patent CN10231185A, namely adopt 4-methyl-2-amylalcohol to be solvent, pass into hydrogen continuously and heat up gradually and granulated copper series catalysts carried out prereduction.
Not only the present invention adopts nitrogen hydrogen reduction catalyst, clean but also save the prereduction solvent such as isopropyl alcohol, 4-methyl-2-amylalcohol, also reduces half-finished amount or does not produce semi-finished product.Preferably method of reducing concerning nitrogen hydrogen reduction catalysis production, not only cleaner production but also the consumption that economizes in raw materials.
Summary of the invention
The invention provides a kind of catalyst prereduction method of synthetic rubber age resistor.
The present invention uses a large amount of prereduction solvents to carry out prereduction to catalyst mainly in the existing current industrial production of solution and laboratory test, the production cost not only increasing raw material and post processing existed, also can produce the problem of a large amount of defective works in initial reaction stage.
Main technical schemes of the present invention: a kind of prereduction method for the synthesis of rubber antioxidant catalyst, adopts nitrogen and hydrogen to carry out prereduction reaction to the catalyst for the synthesis of rubber antioxidant.
Usually, the main technical schemes of the inventive method comprises the steps:
1. load in fixed-bed reactor and treat catalyst pre-reduction, nitrogen is with the pressure of 0.1 ~ 3MPa, and flow is the air that 0.1 ~ 3L/min replaces whole fixed bed reaction system;
2., after replacement completion, heat up, nitrogen, hydrogen flowing quantity are 0.1 ~ 3L/min, and prereduction pressure is: 0.1 ~ 3MPa;
3. pre-reduction temperature heats up by the temperature program set and carries out the prereduction of catalyst, and pre-reduction temperature is 80 ~ 350 DEG C;
4. prereduction EP (end of program), reaction system temperature drops to reaction temperature, carries out synthetic reaction.
Synthetic rubber age resistor of the present invention is 6PPD and IPPD.
In the present invention, catalyst is copper system, nickel system, palladium system, platinum group catalyst.
Employing nitrogen hydrogen reducing catalyst of the present invention, not only clean but also save isopropyl alcohol, also reduce half-finished amount or do not produce semi-finished product.Preferably method of reducing concerning nitrogen hydrogen reduction catalysis production, not only cleaner production but also the consumption that economizes in raw materials.
Detailed description of the invention
Further illustrate feature of the present invention below by example, but the protection domain of this patent is not by the restriction of embodiment.
embodiment 1
Cu-series catalyst is loaded in fixed-bed reactor, nitrogen is full of with 0.5MPa pressure, 0.5L/min flow and replaces air in whole fixed bed reaction system, after reaction system displacement, heat up, nitrogen, hydrogen flowing quantity are 0.5L/min, and pre-reduction temperature heats up by the temperature program set and carries out the prereduction of catalyst, prereduction EP (end of program), reaction system temperature drops to reaction temperature, carries out the synthetic test of IPPD.
embodiment 2
Nickel catalyst is loaded fixed-bed reactor, nitrogen is full of with 0.5MPa pressure, 0.5L/min flow and replaces whole fixed bed reaction system, after reaction system displacement, heat up, nitrogen, hydrogen flowing quantity are 0.5L/min, and pre-reduction temperature heats up by the temperature program set and carries out the prereduction of catalyst, prereduction EP (end of program), reaction system temperature drops to reaction temperature, carries out the synthetic test of 6PPD.
embodiment 3
Cu-series catalyst is loaded fixed-bed reactor, nitrogen is full of with 0.5MPa pressure, 0.5L/min flow and replaces whole fixed bed reaction system, after reaction system displacement, heat up, nitrogen, hydrogen flowing quantity are 0.5L/min, and pre-reduction temperature heats up by the temperature program set and carries out the prereduction of catalyst, prereduction EP (end of program), reaction system temperature drops to reaction temperature, carries out the synthetic test of IPPD.
embodiment 4
Nickel catalyst is loaded fixed-bed reactor, nitrogen is full of with 0.5MPa pressure, 0.5L/min flow and replaces whole fixed bed reaction system, after reaction system displacement, heat up, nitrogen, hydrogen flowing quantity are 0.5L/min, and pre-reduction temperature heats up by the temperature program set and carries out the prereduction of catalyst, prereduction EP (end of program), reaction system temperature drops to reaction temperature, carries out the synthetic test of 6PPD.
Claims (4)
1., for the synthesis of a prereduction method for rubber antioxidant catalyst, it is characterized in that adopting nitrogen hydrogen to carry out prereduction to catalyst.
2. catalyst prereduction method as claimed in claim 1, it is characterized in that comprising the steps: to load in fixed-bed reactor to treat catalyst pre-reduction, nitrogen is with the pressure of 0.1 ~ 3MPa, and flow is the air that 0.1 ~ 3L/min replaces whole fixed bed reaction system; After replacement completion, heat up, nitrogen, hydrogen flowing quantity are 0.1 ~ 3L/min, and prereduction pressure is: 0.1 ~ 3MPa; Pre-reduction temperature heats up by the temperature program set and carries out the prereduction of catalyst, and pre-reduction temperature is 80 ~ 350 DEG C; Prereduction EP (end of program), reaction system temperature drops to reaction temperature, carries out synthetic reaction.
3. catalyst prereduction method as claimed in claim 1, is characterized in that synthetic rubber age resistor is 6PPD and IPPD.
4. catalyst prereduction method as claimed in claim 1, is characterized in that described catalyst is for being copper system, nickel system, palladium system, platinum group catalyst.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410551834.1A CN105562123A (en) | 2014-10-17 | 2014-10-17 | Prereduction method for catalyst for synthesizing rubber antioxidant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410551834.1A CN105562123A (en) | 2014-10-17 | 2014-10-17 | Prereduction method for catalyst for synthesizing rubber antioxidant |
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| CN105562123A true CN105562123A (en) | 2016-05-11 |
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| CN201410551834.1A Pending CN105562123A (en) | 2014-10-17 | 2014-10-17 | Prereduction method for catalyst for synthesizing rubber antioxidant |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4043942A (en) * | 1969-12-03 | 1977-08-23 | The Goodyear Tire & Rubber Company | Modified nickel catalyst systems and their use in reductive alkylation reactions |
| CN101733169A (en) * | 2009-12-14 | 2010-06-16 | 王农跃 | Pretreating process for preparing copper base catalyst of p-phenylenediamine anti-aging agent |
| CN102146042A (en) * | 2011-01-31 | 2011-08-10 | 江苏扬农化工集团有限公司 | Method for preparing p-phenylenediamine rubber aging inhibitor |
| CN103877991A (en) * | 2012-12-19 | 2014-06-25 | 中国石油化工股份有限公司 | Preparation method for trans-1,4-cyclohexanedimethanol, and catalyst used therefor |
-
2014
- 2014-10-17 CN CN201410551834.1A patent/CN105562123A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4043942A (en) * | 1969-12-03 | 1977-08-23 | The Goodyear Tire & Rubber Company | Modified nickel catalyst systems and their use in reductive alkylation reactions |
| CN101733169A (en) * | 2009-12-14 | 2010-06-16 | 王农跃 | Pretreating process for preparing copper base catalyst of p-phenylenediamine anti-aging agent |
| CN102146042A (en) * | 2011-01-31 | 2011-08-10 | 江苏扬农化工集团有限公司 | Method for preparing p-phenylenediamine rubber aging inhibitor |
| CN103877991A (en) * | 2012-12-19 | 2014-06-25 | 中国石油化工股份有限公司 | Preparation method for trans-1,4-cyclohexanedimethanol, and catalyst used therefor |
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Application publication date: 20160511 |