CN105665038A - Deactivated ethylbenzene catalyst regeneration method - Google Patents
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Abstract
The present invention relates to a deactivated ethylbenzene catalyst regeneration method, and mainly solves the problems of low use rate and poor regeneration effect of deactivated ethylbenzene catalysts in the prior art. The deactivated ethylbenzene catalyst regeneration method well solves the problems, and the deactivated ethylbenzene catalyst regeneration method is as follows: a deactivated ethylbenzene catalyst is treated for 2 to 10 hours with a 0.1-10.0wt% alkaline solution, then dried at 100-200 DEG C under a nitrogen atmosphere for 2 to 10 hours, and then calcined for 2 to 10 hours at 400 to 800 DEG Cunder an air atmosphere, the solid-liquid ratio of the deactivated catalyst to the alkaline solution is (5 to 50): 1, the treatment temperature is 50-120 DEG C, and then method can be for ethylbenzene catalyst industrial application.
Description
Technical field
The present invention relates to a kind of renovation process inactivating ethylbenzene catalyst.
Background technology
Ethylbenzene is important Organic Chemicals, is mainly used to produce styrene, and cinnamic downstream product such as engineering plastics, synthetic resin, synthetic rubber etc. are the important raw and processed materials of the industries such as building, automobile, electronics and article of everyday use, and purposes is widely. Along with the fast development of the related industries such as country's enforcement of Major Engineering Projects and building, traffic and manufacture, drive the quick growth of ethylbenzene and the synthetic material market demand downstream.
The ethylbenzene of the overwhelming majority is to be prepared through alkylated reaction by benzene and ethylene in world wide, and industrialized ethylbenzene synthesis technique mainly has traditional alchlor process, molecular sieve vapor phase method and molecular sieve liquid phase method, and main raw material is petrobenzene and ethylene. At present, the ethylbenzene production capacity of China alreadys more than 6,000,000 tons/year, leaps to and becomes the big ethylbenzene manufacturing country of the first in the world. Usually, the single trip use cycle of ethylbenzene catalyst was in 1～2 year, catalysis activity can be partly recovered after generally going through regeneration, but due to poor effect, about 200 tons of ethylbenzene catalyst are still had to discard because of loss of activity every year, generally these decaying catalysts require over the method process of physics landfill, cause certain wasting of resources and environmental pollution.
In recent years, production and the manufacture of the catalyst of ethylbenzene have been carried out extensive and deep research by the research institution of countries in the world or company, and the improvement being constantly devoted to the raising by catalyst performance or Technology drives the development of Researches in ethylbenzene production technique. But, the document or the patent that relate to ethylbenzene catalyst regeneration are less, hinder the general advance of Researches in ethylbenzene production technique.
Chinese patent ZL03147999.5 discloses the decolouring renovation process of deactivated molecular sieve catalyst in a kind of benzene and ethylene alkylation, after deactivator is processed in decolorising agent aqueous solution or distilled water, processed by the air of 300～700 DEG C and/or oxygen atmosphere, catalyst after regeneration not only appearance color is restored, and ethylbenzene selectivity and diethylbenzene conversion ratio can respectively reach 98% and more than 99%. Document " the regeneration research of synthesizing ethyl benzene molecular sieve decaying catalyst " (Beijing Institute of Clothing Tech's journal, calendar year 2001,21st volume the 4th phase) by external coke-burning regeneration method, the coked catalyst of synthesizing ethyl benzene is regenerated, and fresh and the drawing together property of regeneration catalyzing agent, carbon content, Acidity and acid amount are measured.
Document " coke-burning regeneration of coked zeolite catalyst used in synthesis of ethylbenzene with dry gas of FCC research " (chemistry of fuel journal, 2004,32nd volume the 4th phase) with the ethylene synthase ethylbenzene coked catalyst in benzene and oil refinery dry gas for object of study, the character of carbon deposit on coked catalyst and the situation of making charcoal under different temperatures are studied, has investigated the change of the performances such as the acidity of catalyst, activity, crystalline phase, specific surface and pore structure before and after regeneration.
The renovation process of the inactivation ethylbenzene catalyst that above-mentioned patent or document relate to, all there is the space of raising further in the utilization rate of decaying catalyst and regeneration effect.
Summary of the invention
The technical problem to be solved is the inactivation problem that ethylbenzene catalyst utilization is low, regeneration effect is poor that prior art exists, it is provided that the renovation process of a kind of new inactivation ethylbenzene catalyst. Catalyst after regeneration is used for benzene and ethylene alkylation, there is catalyst utilization height, favorable regeneration effect, feature that conversion of ethylene is high.
For solving above-mentioned technical problem, the technical solution used in the present invention is as follows: a kind of renovation process inactivating ethylbenzene catalyst, in turn includes the following steps:
A) catalyst inactivated in ethylbenzene reactor is drawn off, process 2～10 hours with 0.1～10.0wt% alkaline solution;
B) catalyst after step a) process is dried 2～10 hours in 100～200 DEG C in a nitrogen atmosphere;
C) by the catalyst of step c) in air atmosphere in 400～800 DEG C of roastings 2～10 hours.
Wherein, catalyst and the solid-to-liquid ratio of alkaline solution in described step a) are (5～50): 1, and treatment temperature is 50～120 DEG C.
In technique scheme, described alkaline solution is at least one in sodium hydroxide solution, sodium carbonate liquor, sodium bicarbonate solution, potassium hydroxide solution, solution of potassium carbonate, potassium bicarbonate solution or ammonia spirit; The concentration of described alkaline solution is 0.5～5.0wt%; The time that described alkaline solution processes is 4～8 hours; The solid-to-liquid ratio of described catalyst and alkaline solution is (10～30): 1, and treatment temperature is 60～90 DEG C; The drying temperature that described catalyst is placed in industrial oven is 120～180 DEG C, and drying time is 4～8 hours; It is 500～650 DEG C that described catalyst is placed in the sintering temperature in high-temperature roasting furnace, and roasting time is 4～6 hours. Described decaying catalyst after regeneration, is 320～380 DEG C in reaction temperature, and reaction pressure is 0.5～1.5MPa, and weight ethylene air speed is 0.2～0.8 hour-1, benzene ethylene mol ratio is 3～8, and regeneration catalyzing agent contacts generation ethylbenzene with reaction raw materials.
In the inventive method, inactivation ethylbenzene catalyst is after regeneration, before being used for reaction, adopts the exchange of known ammonium, dry and roasting technology process. Such as, ammonium is exchanged for and processes 0.5～24 hour under 0～100 DEG C of condition with the ammonium salt solution of weight concentration 1～20%. Described ammonium salt at least one in ammonium nitrate, ammonium chloride, ammonium oxalate, ammonium sulfate or ammonium citrate. Described exchange generally also includes filtration, water-washing step. Drying steps is process 1～10 hour at 100～140 DEG C. Calcination steps is process 1～10 hour at 500～550 DEG C.
In technique scheme, described decaying catalyst after regeneration, is 330～370 DEG C in reaction temperature, and reaction pressure is 0.5～1.0MPa, and weight ethylene air speed is 0.2～0.8 hour-1, benzene ethylene mol ratio is 4～5, and regeneration catalyzing agent contacts generation ethylbenzene with reaction raw materials.
In technique scheme, the solid-to-liquid ratio of described catalyst and alkaline solution is (15～25): 1, and treatment temperature is 70～90 DEG C.
The catalyst recovery process that the inventive method adopts, catalyst requires over alkaline solution before high-temperature roasting and processes, on the one hand, by gentle basic treatment, can while the degree of crystallinity maintaining molecular sieve and maintenance framework of molecular sieve integrity, it is possible to the partial impurities composition that Removal of catalyst contains; On the other hand, meeting generating section mesopore orbit after alkaline solution processes, there is the quick diffusion being prone to reactant and product. Catalyst after processing in this way removes after carbon deposit through high-temperature roasting, the regeneration catalyzing agent of gained shows the catalytic performance of excellence in the reaction for benzene and ethylene production ethylbenzene, compared with the catalyst of roasting direct without alkaline solution process, conversion of ethylene can improve 2.6～3.4 percentage points, ethylization selectivity can improve 0.4～1.1 percentage point, and there is the advantage that processing cost is low, achieve good technique effect.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of ethylbenzene catalyst after the regeneration in [embodiment 1].
XRD spectra measures and carries out on polycrystal X ray diffractometer, uses CuK alpha ray, sweep limits 2Theta=5～50 °. It can be seen that obvious characteristic diffraction maximum occurs at 2Theta=7.9 °, 8.7 °, 14.7 °, 23.0 °, 23.9 °, 45.0 ° etc. XRD spectra, illustrate that this catalyst has typical MFI topological structure, and the degree of crystallinity of catalyst is good.
The present invention is further elaborated by the examples below, but the application of the present invention is not restricted by the embodiments.
Detailed description of the invention
[comparative example 1]
After being drawn off by the ethylbenzene catalyst inactivated in reactor, by catalyst 550 DEG C of high-temperature roastings 6 hours in air atmosphere, prepare the ethylbenzene catalyst X of regeneration.
[comparative example 2]
After being drawn off by the ethylbenzene catalyst inactivated in reactor, by catalyst 600 DEG C of high-temperature roastings 4 hours in air atmosphere, prepare the ethylbenzene catalyst Y of regeneration.
[embodiment 1]
After being drawn off by the ethylbenzene catalyst inactivated in reactor, processing 5 hours with the sodium hydroxide solution of 1.0wt%, wherein, the solid-to-liquid ratio of decaying catalyst and sodium hydroxide solution is 20:1, treatment temperature is 80 DEG C; Then catalyst is dried 5 hours in 150 DEG C in a nitrogen atmosphere; Finally by catalyst 550 DEG C of high-temperature roastings 5 hours in air atmosphere, prepare the ethylbenzene catalyst A of regeneration.
[embodiment 2]
After being drawn off by the ethylbenzene catalyst inactivated in reactor, processing 3 hours with the sodium bicarbonate solution of 0.5wt%, wherein, the solid-to-liquid ratio of decaying catalyst and sodium bicarbonate solution is 12:1, treatment temperature is 60 DEG C; Then catalyst is dried 2 hours in 130 DEG C in a nitrogen atmosphere; Finally by catalyst 600 DEG C of high-temperature roastings 6 hours in air atmosphere, prepare the ethylbenzene catalyst B of regeneration.
[embodiment 3]
After being drawn off by the ethylbenzene catalyst inactivated in reactor, processing 3 hours with the solution of potassium carbonate of 3.0wt%, wherein, the solid-to-liquid ratio of decaying catalyst and solution of potassium carbonate is 25:1, treatment temperature is 70 DEG C; Then catalyst is dried 6 hours in 160 DEG C in a nitrogen atmosphere; Finally by catalyst 500 DEG C of high-temperature roastings 2 hours in air atmosphere, prepare the ethylbenzene catalyst C of regeneration.
[embodiment 4]
After being drawn off by the ethylbenzene catalyst inactivated in reactor, processing 4 hours with the sodium hydroxide solution of 2.0wt%, wherein, the solid-to-liquid ratio of decaying catalyst and sodium hydroxide solution is 10:1, treatment temperature is 60 DEG C; Then catalyst is dried 4 hours in 150 DEG C in a nitrogen atmosphere; Finally by catalyst 580 DEG C of high-temperature roastings 6 hours in air atmosphere, prepare the ethylbenzene catalyst D of regeneration.
[embodiment 5]
After being drawn off by the ethylbenzene catalyst inactivated in reactor, processing 9 hours with the potassium hydroxide solution of 9.0wt%, wherein, the solid-to-liquid ratio of decaying catalyst and potassium hydroxide solution is 35:1, treatment temperature is 55 DEG C; Then catalyst is dried 3 hours in 180 DEG C in a nitrogen atmosphere; Finally by catalyst 450 DEG C of high-temperature roastings 3 hours in air atmosphere, prepare the ethylbenzene catalyst E of regeneration.
[embodiment 6]
After being drawn off by the ethylbenzene catalyst inactivated in reactor, processing 8 hours with the solution of potassium carbonate of 1.0wt%, wherein, the solid-to-liquid ratio of decaying catalyst and solution of potassium carbonate is 40:1, treatment temperature is 110 DEG C; Then catalyst is dried 8 hours in 110 DEG C in a nitrogen atmosphere;Finally by catalyst 500 DEG C of high-temperature roastings 8 hours in air atmosphere, prepare the ethylbenzene catalyst F of regeneration.
[embodiment 7]
After being drawn off by the ethylbenzene catalyst inactivated in reactor, processing 5 hours with the sodium carbonate liquor of 2.0wt%, wherein, the solid-to-liquid ratio of decaying catalyst and sodium carbonate liquor is 35:1, treatment temperature is 100 DEG C; Then catalyst is dried 7 hours in 190 DEG C in a nitrogen atmosphere; Finally by catalyst 600 DEG C of high-temperature roastings 5 hours in air atmosphere, prepare the ethylbenzene catalyst G of regeneration.
[embodiment 8]
After being drawn off by the ethylbenzene catalyst inactivated in reactor, processing 4 hours with the ammonia spirit of 4.0wt%, wherein, the solid-to-liquid ratio of decaying catalyst and ammonia spirit is 48:1, treatment temperature is 115 DEG C; Then catalyst is dried 10 hours in 150 DEG C in a nitrogen atmosphere; Finally by catalyst 750 DEG C of high-temperature roastings 9 hours in air atmosphere, prepare the ethylbenzene catalyst H of regeneration.
[embodiment 9]
After being drawn off by the ethylbenzene catalyst inactivated in reactor, processing 5 hours with the potassium hydroxide solution of 5.0wt%, wherein, the solid-to-liquid ratio of decaying catalyst and potassium hydroxide solution is 20:1, treatment temperature is 80 DEG C; Then catalyst is dried 5 hours in 140 DEG C in a nitrogen atmosphere; Finally by catalyst 700 DEG C of high-temperature roastings 4 hours in air atmosphere, prepare the ethylbenzene catalyst I of regeneration.
[embodiment 10]
After being drawn off by the ethylbenzene catalyst inactivated in reactor, processing 6 hours with the potassium bicarbonate solution of 0.2wt%, wherein, the solid-to-liquid ratio of decaying catalyst and potassium bicarbonate solution is 15:1, treatment temperature is 90 DEG C; Then catalyst is dried 8 hours in 160 DEG C in a nitrogen atmosphere; Finally by catalyst 450 DEG C of high-temperature roastings 5 hours in air atmosphere, prepare the ethylbenzene catalyst J of regeneration.
[embodiment 11]
After being drawn off by the ethylbenzene catalyst inactivated in reactor, processing 8 hours with the sodium hydroxide solution of 1.5wt%, wherein, the solid-to-liquid ratio of decaying catalyst and sodium hydroxide solution is 40:1, treatment temperature is 60 DEG C; Then catalyst is dried 7 hours in 130 DEG C in a nitrogen atmosphere; Finally by catalyst 500 DEG C of high-temperature roastings 6 hours in air atmosphere, prepare the ethylbenzene catalyst K of regeneration.
[embodiment 12]
After being drawn off by the ethylbenzene catalyst inactivated in reactor, processing 6 hours with the sodium carbonate liquor of 2.0wt%, wherein, the solid-to-liquid ratio of decaying catalyst and sodium carbonate liquor is 25:1, treatment temperature is 70 DEG C; Then catalyst is dried 5 hours in 150 DEG C in a nitrogen atmosphere; Finally by catalyst 550 DEG C of high-temperature roastings 5 hours in air atmosphere, prepare the ethylbenzene catalyst L of regeneration.
[embodiment 13]
After being drawn off by the ethylbenzene catalyst inactivated in reactor, processing 4 hours with the sodium hydroxide solution of 2.5wt%, wherein, the solid-to-liquid ratio of decaying catalyst and sodium hydroxide solution is 30:1, treatment temperature is 75 DEG C; Then catalyst is dried 4 hours in 160 DEG C in a nitrogen atmosphere; Finally by catalyst 600 DEG C of high-temperature roastings 8 hours in air atmosphere, prepare the ethylbenzene catalyst M of regeneration.
[embodiment 14]
Regeneration ethylbenzene catalyst A～M provided by the invention, adopts the ammonium chloride solution of 10.0wt% exchange 4 hours at 60 DEG C, and dries after 5 hours roasting 3 hours at 500～550 DEG C in 110 DEG C. By regeneration catalyzing agent X, Y of the catalyst of gained and comparative example when benzene and ethylene are raw material, it is alkylated reaction contrast effect.Wherein, reaction temperature is 360 DEG C, and reaction pressure is 0.9MPa, and the mol ratio of benzene ethylene is 5.5, and weight ethylene air speed is 0.4 hour-1, the loadings of catalyst is 5.0 grams, and concrete reaction result is in Table 1.
Table 1
| Ethylbenzene catalyst | Conversion of ethylene (%) | Ethylization selectivity (%) |
| A | 99.8 | 99.6 |
| B | 99.5 | 99.7 |
| C | 99.4 | 99.5 |
| D | 99.5 | 99.7 |
| E | 99.3 | 99.4 |
| F | 99.6 | 99.6 |
| G | 99.7 | 99.5 |
| H | 99.4 | 99.2 |
| I | 99.3 | 99.4 |
| J | 99.4 | 99.5 |
| K | 99.6 | 99.7 |
| L | 99.4 | 99.8 |
| M | 99.6 | 99.7 |
| X | 98.2 | 98.7 |
| Y | 98.1 | 98.8 |
Claims (10)
1. inactivate a renovation process for ethylbenzene catalyst, in turn include the following steps:
A) catalyst inactivated in ethylbenzene reactor is drawn off, process 2～10 hours with 0.1～10.0wt% alkaline solution;
B) catalyst after step a) process is dried 2～10 hours in 100～200 DEG C in a nitrogen atmosphere;
C) by the catalyst of step c) in air atmosphere in 400～800 DEG C of roastings 2～10 hours;
Wherein, catalyst and the solid-to-liquid ratio of alkaline solution in described step a) are (5～50): 1, and treatment temperature is 50～120 DEG C.
2. the renovation process of inactivation ethylbenzene catalyst according to claim 1, it is characterised in that described alkaline solution is at least one in sodium hydroxide solution, sodium carbonate liquor, sodium bicarbonate solution, potassium hydroxide solution, solution of potassium carbonate, potassium bicarbonate solution or ammonia spirit; The concentration of described alkaline solution is 0.5～5.0wt%; The time that described alkaline solution processes is 4～8 hours.
3. the renovation process of inactivation ethylbenzene catalyst according to claim 1, it is characterized in that inactivation ethylbenzene catalyst after regeneration, before being used for reaction, carry out ammonium exchange process, process 0.5～24 hour under 0～100 DEG C of condition with the ammonium salt solution of weight concentration 1～20%, described ammonium salt at least one in ammonium nitrate, ammonium chloride, ammonium oxalate, ammonium sulfate or ammonium citrate.
4. the renovation process of inactivation ethylbenzene catalyst according to claim 1, it is characterised in that the solid-to-liquid ratio of described catalyst and alkaline solution is (10～30): 1, and treatment temperature is 60～90 DEG C.
5. the renovation process of inactivation ethylbenzene catalyst according to claim 1, it is characterised in that inactivation ethylbenzene catalyst after regeneration, before being used for reaction, carries out ammonium ion exchange or acid treatment.
6. the renovation process of inactivation ethylbenzene catalyst according to claim 5, it is characterised in that the ammonium ion exchange ammonium salt solution of weight concentration 1～20% processes 0.5～24 hour under 0～100 DEG C of condition; Described ammonium salt at least one in ammonium nitrate, ammonium chloride, ammonium oxalate, ammonium sulfate or ammonium citrate.
7. the renovation process of inactivation ethylbenzene catalyst according to claim 1, it is characterised in that the drying temperature that described catalyst is placed in industrial oven is 120～180 DEG C, and drying time is 4～8 hours.
8. the renovation process of inactivation ethylbenzene catalyst according to claim 1, it is characterised in that it is 500～650 DEG C that described catalyst is placed in the sintering temperature in high-temperature roasting furnace, and roasting time is 4～6 hours.
9. the renovation process of inactivation ethylbenzene catalyst according to claim 1, it is characterised in that described decaying catalyst after regeneration, is 320～380 DEG C in reaction temperature, and reaction pressure is 0.5～1.5MPa, and weight ethylene air speed is 0.2～0.8 hour-1, benzene ethylene mol ratio is 3～8, and regeneration catalyzing agent contacts generation ethylbenzene with reaction raw materials.
10. the renovation process of inactivation ethylbenzene catalyst according to claim 8, it is characterised in that described decaying catalyst after regeneration, is 330～370 DEG C in reaction temperature, and reaction pressure is 0.5～1.0MPa, and weight ethylene air speed is 0.2～0.8 hour-1, benzene ethylene mol ratio is 4～5, and regeneration catalyzing agent contacts generation ethylbenzene with reaction raw materials.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108126744A (en) * | 2017-12-29 | 2018-06-08 | 镇江巨茂分子筛有限公司 | The regeneration technology of preparing ethylbenzene from dry gas catalyst |
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| CN1565739A (en) * | 2003-06-30 | 2005-01-19 | 中国石油化工股份有限公司 | Decolorizing and reactivating method of inactivated molecular sieve catalyzer in liquid-phase alkylating reaction of benzene and ethene |
| US20070004951A1 (en) * | 2005-06-30 | 2007-01-04 | Chen John Q | Methods for recovering activity of molecular sieve catalysts |
| CN101829597A (en) * | 2009-03-10 | 2010-09-15 | 中国石油天然气股份有限公司 | Dearsenifying regeneration method of deactivated molecular sieve catalyst |
| CN102188994A (en) * | 2011-03-24 | 2011-09-21 | 欧颖 | Method for regenerating titanium silicalite catalyst |
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| CN1131060A (en) * | 1995-11-27 | 1996-09-18 | 南开大学 | Catalyst for preparation of high purity para-diethylbenzene by using ethylbenzene disproportionation and its technology |
| CN1565739A (en) * | 2003-06-30 | 2005-01-19 | 中国石油化工股份有限公司 | Decolorizing and reactivating method of inactivated molecular sieve catalyzer in liquid-phase alkylating reaction of benzene and ethene |
| US20070004951A1 (en) * | 2005-06-30 | 2007-01-04 | Chen John Q | Methods for recovering activity of molecular sieve catalysts |
| CN101829597A (en) * | 2009-03-10 | 2010-09-15 | 中国石油天然气股份有限公司 | Dearsenifying regeneration method of deactivated molecular sieve catalyst |
| CN102188994A (en) * | 2011-03-24 | 2011-09-21 | 欧颖 | Method for regenerating titanium silicalite catalyst |
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| CN108126744A (en) * | 2017-12-29 | 2018-06-08 | 镇江巨茂分子筛有限公司 | The regeneration technology of preparing ethylbenzene from dry gas catalyst |
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