CN102335633B - Rapid reducing method of catalyst - Google Patents
Rapid reducing method of catalyst Download PDFInfo
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- CN102335633B CN102335633B CN 201010228300 CN201010228300A CN102335633B CN 102335633 B CN102335633 B CN 102335633B CN 201010228300 CN201010228300 CN 201010228300 CN 201010228300 A CN201010228300 A CN 201010228300A CN 102335633 B CN102335633 B CN 102335633B
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Abstract
The invention relates to a rapid reducing method of a catalyst. In order to solve the problems of long catalyst reduction time and large hydrogen consumption quantity in the industrial production at present, the inventor provides the method comprising the steps of: in a reduction process of the catalyst, online-analyzing concentrations of hydrogen in gas at an inlet of a reduction furnace and gas in an outlet of the reduction furnace in real time, loading an online analysis result to a catalyst reduction control system, and regulating the reduction temperature of the reduction furnace by the reduction control system according to the change of the online-analyzed concentrations of the hydrogen. By using the method, the automatic reduction control of the catalyst reduction furnace can be realized, the whole reduction process can be monitored, the whole reduction time of the catalyst is reduced, the consumption of the hydrogen is reduced, thus the processing period of the catalyst is greatly shortened and the processing cost of the catalyst is reduced.
Description
Technical field
The present invention relates to a kind of catalyst reduction method, more particularly, relate to a kind of method for the catalyst fast restore.
Background technology
Modern age chemical engineering industry, particularly coal and petrochemical industry develop rapidly, thousands of chemical raw materials and commodity production are all closely related with the exploitation of industrial catalyst.The existence of catalyst has not only promoted the technological innovation in the industrial production, and provides great scope of land for the mankind's activity in production.The catalyst majority that uses in the petrochemical production process belongs to solid catalyst, is comprised of carrier, auxiliary agent and active component three parts, and wherein the precursor of active component mostly is metallic salt.Most catalyst activity components only have for metallic atom loads on the carrier and just can have catalytic activity in commercial Application, therefore carry out pyrolytic and become oxidation state with regard to must loading on the carrier slaine, then reduce the catalyst finished product that just can obtain having active sites.The reduction effect of metal oxide is determining the quality of catalyst catalytic performance in the catalyst.Thereby the catalyst reduction process is the step of an outbalance in the industrial catalyst finished product production process.
At present, mostly the reduction process factory of catalyst is to adopt under certain hydrogen flowing quantity temperature-programmed technique to carry out.These temperature programming programs are obtained by the laboratory experience basically, can be divided into manual adjustments and automatically adjusting according to temperature regulation mechanism.Manual adjustments is that the temperature and time of the prior predetermined section of basis carries out manually piecemeal temperature programmed reduction; Automatically adjusting then is that set heating schedule is set on the instrument, and the centre can not be adjusted.Although above-mentioned dual mode all has separately advantage, drawback be the recovery time of catalyst long, hydrogen gas consumption is large etc., and then will cause long and high in cost of production of catalyst process-cycle.
Summary of the invention
The long and large problem of hydrogen gas consumption for the ubiquitous catalyst reduction time in the present industrial production, the inventor is on the basis of existing operation, density of hydrogen in the on-line analysis reduction furnace entrance and exit gas utilizes the reduction control program to analyze data variation trend program and adjusts the reduction furnace furnace temperature.Result of the test is found, uses fast restore method of the present invention, can be original 70%～85% with the catalyst reduction time shorten, and then hydrogen gas consumption is also along with decline.This has not only shortened the recovery time of catalyst, has improved the annual production of reduction furnace, and reduces the reduction cost of catalyst.
Concrete technical scheme is as follows:
The method of catalyst fast restore of the present invention, in the catalyst reduction process, density of hydrogen in on-line analysis reduction furnace inlet gas and the exit gas, the on-line analysis result is written in the catalyst reduction control system, and the reduction control system is adjusted the reduction temperature of reduction furnace according to the variation of on-line analysis density of hydrogen.
Preferably, if the difference of density of hydrogen 〉=2.0% in density of hydrogen and the exit gas in the reduction furnace inlet gas then keeps reduction temperature constant; If in the inlet gas in density of hydrogen and the exit gas difference of density of hydrogen then improve reduction temperature with 5～20 ℃/hour heating rate less than 2.0%; When the highest reduction temperature that reduction temperature is adjusted to that catalyst allows, kept reduction temperature 1～2 hour, the catalyst reduction process finishes.
Preferably, the air speed of reduction furnace inlet gas is 1～1000h
-1, density of hydrogen is 75%.
More preferably, the density of hydrogen of reduction control system in inlet gas of 10～30min analysis and exit gas.
Preferably, described heating rate is 10～15 ℃/hour.
More preferably, the highest described reduction temperature is 440 ℃.
In the present invention, if do not particularly point out, described concentration all refers to volume percent content.
In reduction control program of the present invention, the foundation of its adjusting is the variation of density of hydrogen in reduction furnace inlet gas and the exit gas.The reduction control program calculates the two difference automatically according to the on-line analysis data of density of hydrogen in the reduction furnace entrance and exit gas, is automatically regulated the temperature programming of reduction furnace by variation tendency.
Catalyst fast restore process is minute three steps generally: the reducing program starting stage; The reduction furnace heating reduction stage; Reduction furnace reduction termination phase.The idiographic flow of fast restore control method is as follows:
1, the reducing program starting stage
After the reduction control program starts, the built-in variables such as the hydrogen flowing quantity in the at first given reduction process and heating rate, and the analysis result signal of identification reduction furnace entrance and exit online analytical instrument.
Confirm that all execute-in-places all are finished, on-the-spot on-line analysis device data access is normal, and has been ready to enter automatic control reduction rank.
2, the reduction furnace heating reduction stage
After entering the reduction control program, the reduction control program obtains the inlet gas of field assay instrument on-line analysis and the density of hydrogen in the exit gas, judge whether to need to adjust the furnace temperature of reduction furnace according to the two difference every 5-30min, realize the automatic control of reduction process, until whole reduction process finishes.
3, reduction furnace reduction termination phase
When the reduction control program monitored catalyst and reaches the highest reduction temperature, the cooling of program automatic alarm reduction apparatus entered the catalyst structure stage.Manually stop reducing control program by operating personnel.
The method of catalyst fast restore of the present invention can be used for the reduction of various catalyst, such as the reduction of nickel-base catalyst, cobalt-base catalyst etc., be exemplified as particularly reduction for the synthesis of the nickel-base catalyst of isopropylamine, for the synthesis of the reduction of the cobalt-base catalyst of ethamine.
Catalyst reduction method of the present invention is compared with conventional method, has the advantage of saving time and saving hydrogen, because the recovery time lacks so that the active component particle of catalyst is grown up not obvious.
The specific embodiment
Further describe the present invention below in conjunction with embodiment.Scope of the present invention is not subjected to the restriction of following embodiment.
Embodiment 1
Method of the present invention is applied to the nickel-base catalyst reduction process.The nickel-base catalyst loadings is 1.0m
3, heating rate is 10 ℃/h, reduction furnace inlet gas flow is 500m
3/ h, density of hydrogen are 75%, and the concrete steps of traditional method of reducing and the inventive method see Table 1.Catalyst through reduction is 0.5h at 152 ℃, acetone volume space velocity
-1, acetone: hydrogen: the mol ratio of ammonia is 1: 3: 3, catalyst amount is that evaluation result sees Table 2 on the isopropylamine evaluating apparatus of 50ml.
Adopt the concrete operation of method of the present invention as follows: setting the reduction furnace rate of heat addition is 10 ℃/h, and the inlet gas flow is 500m
3/ h, density of hydrogen is 75%, opening the reduction control program heats up, carry out simultaneously density of hydrogen in the on-line analysis reduction furnace entrance and exit gas every 10min, when furnace temperature rises to 220 ℃, the difference of analyzing and testing density of hydrogen in the entrance and exit gas 〉=2.0%, keep temperature 2.5h post analysis record＜2.0%; The control program that then reduces begins to heat up, and when temperature rose to 340 ℃, on-line analysis detected the difference of density of hydrogen in the entrance and exit gas 〉=2.0%, and it is constant that the control program that then reduces begins to keep furnace temperature, detects the two difference＜2.0% behind the insulation 3h; And then the control program that reduces heats up and reduces, when being warming up to 390 ℃, and the difference of density of hydrogen 〉=2.0% in the analyzing and testing entrance and exit gas, it is constant that the control program that then reduces begins to keep furnace temperature, detects behind the insulation 2.5h and learn the two difference＜2.0%; Reducing program continues to heat up 440 ℃, keeps reducing behind the 1h, and reducing program stops, and the whole reduction of catalyst is finished.
The table 1 catalyst reduction step table of comparisons
Table 2 evaluating catalyst result contrast
Can be found out that by data in the table 1 total recovery time and hydrogen consumption total amount that method of the present invention is used are 82.3% of traditional reduction process.Found out by table 2 again, utilize the catalyst catalytic performance of method reduction of the present invention to be better than original method.Therefore, reduction control method of the present invention has also reduced the reduction cost of catalyst guaranteeing not only to have shortened the recovery time of catalyst on the basis that catalyst fully reduces.
Claims (5)
1. the method for a catalyst fast restore, it is characterized in that, in the catalyst reduction process, density of hydrogen in on-line analysis reduction furnace inlet gas and the exit gas, the on-line analysis result is written in the catalyst reduction control system, and the reduction control system is adjusted the reduction temperature of reduction furnace according to the variation of on-line analysis density of hydrogen; If the difference of density of hydrogen 〉=2.0% in density of hydrogen and the exit gas in the reduction furnace inlet gas then keeps reduction temperature constant; If in the inlet gas in density of hydrogen and the exit gas difference of density of hydrogen then improve reduction temperature with 5～20 ℃/hour heating rate less than 2.0%; When the highest reduction temperature that reduction temperature is adjusted to that catalyst allows, kept reduction temperature 1～2 hour, the catalyst reduction process finishes.
2. the method for claim 1 is characterized in that, the air speed of reduction furnace inlet gas is 1-1000h
-1, density of hydrogen is 75%.
3. the method for claim 1 is characterized in that, the density of hydrogen difference of reduction control system in inlet gas of 10～30min analysis and exit gas.
4. the method for claim 1 is characterized in that, described heating rate is 10～15 ℃/hour.
5. the method for claim 1 is characterized in that, the highest described reduction temperature is 440 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 201010228300 CN102335633B (en) | 2010-07-16 | 2010-07-16 | Rapid reducing method of catalyst |
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| CN 201010228300 CN102335633B (en) | 2010-07-16 | 2010-07-16 | Rapid reducing method of catalyst |
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| CN102335633A CN102335633A (en) | 2012-02-01 |
| CN102335633B true CN102335633B (en) | 2013-02-27 |
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| CN106397219B (en) * | 2016-08-26 | 2018-03-27 | 安徽昊源化工集团有限公司 | A kind of method of acetone hydrogenation ammonification synthesizing isopropamide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1827218A (en) * | 2006-03-30 | 2006-09-06 | 上海工程技术大学 | Method for preparing supported nano copper nickel catalyst and application thereof in oxidative dehydrogenation reaction of alkylol amine |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1827218A (en) * | 2006-03-30 | 2006-09-06 | 上海工程技术大学 | Method for preparing supported nano copper nickel catalyst and application thereof in oxidative dehydrogenation reaction of alkylol amine |
Non-Patent Citations (4)
| Title |
|---|
| CO低温变换催化剂的还原过程分析;张传玉;《安庆师范学院学报(自然科学版)》;20040229;第10卷(第1期);59-62 * |
| 张传玉.CO低温变换催化剂的还原过程分析.《安庆师范学院学报(自然科学版)》.2004,第10卷(第1期),59-62. |
| 杜鹃.甲醇催化剂快速升温还原的研究.《安徽化工》.2004,(第5期), |
| 甲醇催化剂快速升温还原的研究;杜鹃;《安徽化工》;20041231(第5期);44-45 * |
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