CN103120953A - Disproportionation and alkyl transfer catalyst reducing method - Google Patents

Disproportionation and alkyl transfer catalyst reducing method Download PDF

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Publication number
CN103120953A
CN103120953A CN2011103669625A CN201110366962A CN103120953A CN 103120953 A CN103120953 A CN 103120953A CN 2011103669625 A CN2011103669625 A CN 2011103669625A CN 201110366962 A CN201110366962 A CN 201110366962A CN 103120953 A CN103120953 A CN 103120953A
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catalyst
reducing
disproportionation
hydrogen
gas
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CN103120953B (en
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邹薇
孔德金
李华英
李经球
郭宏利
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02P20/52Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

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Abstract

The invention relates to a disproportionation and alkyl transfer catalyst reducing method which mainly solves the problems of low metal dispersity and high hydrogenation activity in the prior art. The reducing method of a catalyst for disproportionation and alkyl transfer reaction includes the steps: drying and dehydrating the catalyst by inert gas containing oxygen to obtain a catalyst I, and using reducing gas to reduce the catalyst I to obtain a catalyst II; and purging the catalyst II for 1-8 hours under the reducing gas and at the temperature of 300-700 DEG C to obtain a needed catalyst. By the technical scheme, the problems are well solved, and the method can be used in disproportionation and alkyl transfer industrial production of toluene and heavy aromatics.

Description

The method of reducing of disproportionation and transalkylation catalyst
Technical field
The present invention relates to the method for reducing of a kind of disproportionation and transalkylation catalyst.
Background technology
Paraxylene in C8 aronmatic is one of main basic organic of petrochemical industry, in numerous chemical production field such as chemical fibre, synthetic resin, agricultural chemicals, medicine, purposes is widely arranged.For increasing production of xylol, utilize toluene disproportionation or toluene and carbon nine and above heavy aromatics (C thereof 9 +A) disproportionation and transalkylation reaction generate benzene and C8 aronmatic, are the effective ways of increasing yield of p-xylene.
Along with day by day becoming heavily of upstream reforming material, the comprehensive utilization of heavy arene becomes the problem that people are concerned about.C9 aromatic (C 9A) the existing more ripe technology of utilizing, by with the transalkylation reaction increasing production of xylol of toluene.And carbon ten and above heavy aromatics (C thereof 10 +A) can only partly be utilized at present, fused ring compound wherein easily aggravates the coking deactivation of catalyst, therefore, in traditional disproportionation and alkyl transfering process to the C in reaction raw materials 10 +A has strict restriction.For improving the stability of catalyst, can introduce the hydrogenation metal component on molecular sieve catalyst.But then, because metal has than the strong hydrogenation performance, can promote the saturated and cracking side-reaction of the hydrogenation of aromatic hydrocarbons, production non-aromatics and light component, thus reduced the dimethylbenzene yield.
The molecular sieve catalyst of carried metal generally need to carry out reduction activation before use, so that metal is converted into reduction-state by oxidation state.In commercial plant, the good no quality that is directly connected to catalyst performance of the reduction of metallic catalyst, and reduction process also is subjected to the impact of factors, as water content, reduction temperature and reduction pressure etc. in reducing atmosphere.
WO2006039316 discloses a kind of method of ex-situ reduction of noble metal catalyst, and the method comprises completes catalyst drying and reduction in single step under the existence of hydrogen and noble gas mixtures.Secondly, the catalyst after reduction is carried out passivation with mineral oil catalyst filling hole.
CN100357025 discloses a kind of method of reducing that contains molecular sieve, noble metal catalyst, and the method contacts catalyst with ammonia with hydrogen with gaseous mixture, and in the reducing metal, ammonia adsorbs shielding to strong acidic site, to suppress the high activity of crossing at driving initial stage.This patent is mainly concerned with the passivation of completing in reduction process the acid position.
Above-mentioned document exists metal dispersion low when metallic catalyst is carried out reduction activation, the problems such as the active height of metal hydrogenation.
Summary of the invention
Technical problem to be solved by this invention is to have in prior art that metal dispersion is low, the problem of metal hydrogenation hyperactivity, and a kind of new disproportionation and the method for reducing of transalkylation catalyst are provided.The method is used for the activation of disproportionation and transalkylation catalyst, and activating catalyst has higher metal dispersion and suitable metal hydrogenation performance, can effectively reduce the aromatic hydrocarbon ring loss.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: the method for reducing of a kind of disproportionation and transalkylation reaction catalyst comprises the following steps:
A) with the inert gas that contains oxygen, catalyst is carried out getting catalyst I after drying and dehydrating;
B) catalyst I is reduced to get catalyst I I with reducibility gas;
C) under reducibility gas and at 300~700 ℃ of temperature, catalyst I I is purged 1~8 hour, get required catalyst.
In technique scheme, inert gas is at least a in nitrogen, carbon dioxide, and in inert gas, oxygen content is 0.5~20vol%, preferred 1~6vol%, the final baking temperature of inert gas is 300~600 ℃, and during dry the end, the water content in the dry gas of outflow is less than 200ppm.Reducibility gas is at least a in hydrogen, hydrogen~ammonia gas mixture, hydrogen~nitrogen mixed air, the Contact Temperature of reducibility gas and catalyst I is 300~500 ℃, be 1~15 hour time of contact, reducibility gas pressure is 0.05~5.0MPa, and the water content in reduction process in eluting gas is lower than 200ppm.Catalyst I I contacts with hydrogen and carries out passivation, and Contact Temperature is 400~650 ℃, and be 2~6 hours time of contact.By weight percentage, catalyst contains at least a in modenite, β zeolite, ZSM-12 molecular sieve of being selected from of 0.01%~0.2% the metal that is selected from VIIIB family and 50%~80%.
In the present invention, with the inert gas that contains certain oxygen, catalyst is carried out drying, to remove the adsorbed water on catalyst, the existence of oxygen simultaneously can be avoided the agglomeration of metal oxide.Dried catalyst contacts to complete the reduction of metal oxide with reducibility gas, optimize the condition such as moisture, reduction temperature in reducing gas by control, avoids reduction process to cause the metallic agglomeration.Catalyst after reduction carries out suitable Passivation Treatment again, and the strong hydrogenation that has suppressed metal is active.
Use method of reducing of the present invention, can improve the carried metal dispersiveness and optimize the metal hydrogenation activity.Reducing catalyst is used for disproportionation and the transalkylation reaction of toluene and heavy aromatics, has the advantages that reactivity is high, the aromatic hydrocarbons loss late is low, has good industrial application value.
The present invention is further elaborated below by embodiment.
The specific embodiment
[embodiment 1]
With Na 20 content is less than 0.1% (weight), SiO 2/ Al 2O 3Molecular proportion is 40 β zeolite 60 grams and Na 2O content is less than the γ-Al of 0.1% (weight) 2O 3H 2O 57.1 grams evenly mix, and then add a certain amount of rare nitric acid, field mountain valley with clumps of trees and bamboo powder to mediate evenly, and carrier is made in extruded moulding, roasting, and pelletizing is placed in steeper.A certain amount of chloroplatinic acid be impregnated in carrier surface, and 4 hours, 500 ℃ roastings of 120 ℃ of dryings made catalyst A (0.05wt%Pt/ β) in 3 hours.Get the 100ml catalyst A, be placed in tubular reactor, pass into nitrogen-air Mixture that oxygenous amount is 3vol.%, be warming up under 400 ℃ dry 3 hours, be cooled to 200 ℃, and carry out abundant nitrogen replacement.Pass into the hydrogen that flow is 500mL/min, reduction is 1 hour under 200 ℃, is warming up to 400 ℃ of reduction 3 hours.Lift temperature to 500 ℃, hydrogen treat was completed metal passivation in 3 hours.
Catalyst carries out reactivity and investigates on the fixed bed reaction evaluating apparatus.Catalyst packing 20 grams, liquid total feed weight air speed is 3.0 hours -1, 375 ℃ of reaction temperatures, reaction pressure 3.0MPa, hydrogen hydrocarbon molecule are than 3.0, and raw material is toluene: C 9 +A=30: 70 (weight), wherein C 9 +Contain 15% (weight) C in A 10 +A。C 9The A raw material weight consists of: propyl benzene 4.2%, the first and second benzene 29.04%, trimethylbenzene 59.6%, C 10 +A weight consists of: diethylbenzene 3.33%, dimethyl ethylbenzene 26.96%, methyl propyl benzene 2.32%, durene 28.84%, methyl naphthalene 14.49, dimethylnaphthalene 11.16%, other 12.90%, evaluation result is as shown in table 1.
[embodiment 2]
With Na 2O content is less than 0.1% (weight), SiO 2/ Al 2O 3Molecular proportion is 40 modenite 60 grams and Na 2O content is less than the γ-Al of 0.1% (weight) 2O 3H 2O 57.1 grams evenly mix, and then add a certain amount of rare nitric acid, field mountain valley with clumps of trees and bamboo powder to mediate evenly, and carrier is made in extruded moulding, roasting, and pelletizing is placed in steeper.A certain amount of palladium bichloride be impregnated in carrier surface, and 4 hours, 500 ℃ roastings of 120 ℃ of dryings made catalyst B (0.2wt%Pd/Mor) in 3 hours.Catalyst reduction condition and active examination condition are as described in Example 1.
[embodiment 3]
Get the 100ml catalyst A, be placed in tubular reactor, pass into nitrogen-air Mixture that oxygenous amount is 3vol.%, be warming up under 300 ℃ dry 3 hours, be cooled to 200 ℃, and carry out abundant nitrogen replacement.Pass into the hydrogen that flow is 500mL/min, reduction is 1 hour under 200 ℃, is warming up to 350 ℃ of reduction 4 hours.Lift temperature to 500 ℃, hydrogen treat was completed metal passivation in 1 hour.Catalyst activity examination condition as described in Example 1.
[embodiment 4]
Get the 100ml catalyst A, be placed in tubular reactor, pass into nitrogen-air Mixture that oxygenous amount is 3vol.%, be warming up under 500 ℃ dry 3 hours, be cooled to 200 ℃, and carry out abundant nitrogen replacement.Pass into the hydrogen that flow is 500mL/min, reduction is 1 hour under 200 ℃, is warming up to 400 ℃ of reduction 4 hours.Lift temperature to 450 ℃, hydrogen treat was completed metal passivation in 3 hours.Catalyst activity examination condition as described in Example 1.
[embodiment 5]
Get the 100ml catalyst A, be placed in tubular reactor, pass into nitrogen-air Mixture that oxygenous amount is 5vol.%, be warming up under 400 ℃ dry 3 hours, be cooled to 200 ℃, and carry out abundant nitrogen replacement.Pass into the hydrogen that flow is 1000mL/min, reduction is 1 hour under 200 ℃, is warming up to 400 ℃ of reduction 3 hours.Lift temperature to 450 ℃, hydrogen treat was completed metal passivation in 5 hours.Catalyst activity examination condition as described in Example 1.
[embodiment 6]
Get the 100ml catalyst A, be placed in tubular reactor, pass into nitrogen-air Mixture that oxygenous amount is 3vol.%, be warming up under 400 ℃ dry 3 hours, be cooled to 200 ℃, and carry out abundant nitrogen replacement.Pass into the hydrogen that flow is 500mL/min, reduction is 1 hour under 200 ℃, is warming up to 450 ℃ of reduction 3 hours.Lift temperature to 550 ℃, hydrogen treat passivation 2 hours.Catalyst activity examination condition as described in Example 1.
[embodiment 7]
Get the 100ml catalyst A, be placed in tubular reactor, pass into nitrogen-air Mixture that oxygenous amount is 3vol.%, be warming up under 400 ℃ dry 3 hours, carry out abundant nitrogen replacement.Pass into the hydrogen that flow is 500mL/min, reduction is 5 hours under 450 ℃.Lift temperature to 550 ℃, hydrogen Passivation Treatment 5 hours.Catalyst activity examination condition as described in Example 1.
[embodiment 8]
Get the 100ml catalyst B, be placed in tubular reactor, pass into nitrogen-air Mixture that oxygenous amount is 3vol.%, be warming up under 400 ℃ dry 3 hours, be cooled to 200 ℃, and carry out abundant nitrogen replacement.Passing into flow is the hydrogen-nitrogen mixture that contains 60vol.% hydrogen of 500mL/min, and reduction is 1 hour under 200 ℃, is warming up to 400 ℃ of reduction 3 hours.Lift temperature to 500 ℃, hydrogen Passivation Treatment 2 hours.Catalyst activity examination condition as described in Example 1.
[embodiment 9]
Get the 100ml catalyst B, be placed in tubular reactor, pass into nitrogen-air Mixture that oxygenous amount is 3vol.%, be warming up under 400 ℃ dry 3 hours, be cooled to 200 ℃, and carry out abundant nitrogen replacement.Passing into flow is the hydrogen-ammonia gas mixture that contains 90vol.% hydrogen of 500mL/min, and reduction is 1 hour under 200 ℃, is warming up to 400 ℃ of reduction 3 hours.Lift temperature to 500 ℃, hydrogen Passivation Treatment 2 hours.Catalyst activity examination condition as described in Example 1.
[embodiment 10]
Get the 100ml catalyst B, be placed in tubular reactor, pass into nitrogen-air Mixture that oxygenous amount is 3vol.%, be warming up under 400 ℃ dry 3 hours, be cooled to 200 ℃, and carry out abundant nitrogen replacement.Pass into the hydrogen that flow is 500mL/min, reduction is 1 hour under 200 ℃, is warming up to 400 ℃ of reduction 3 hours.Catalyst activity examination condition as described in Example 1.
[embodiment 11]
Get the 100ml catalyst B, be placed in tubular reactor, pass into nitrogen-air Mixture that oxygenous amount is 3vol.%, be warming up under 400 ℃ dry 3 hours, be cooled to 200 ℃, and carry out abundant nitrogen replacement.Pass into the hydrogen that flow is 500mL/min, reduction is 1 hour under 200 ℃, is warming up to 400 ℃ of reduction 3 hours.Lift temperature to 600 ℃, hydrogen Passivation Treatment 2 hours.Catalyst activity examination condition as described in Example 1.
[embodiment 12]
Get the 100ml catalyst B, be placed in tubular reactor, pass into nitrogen-air Mixture that oxygenous amount is 3vol.%, be warming up under 400 ℃ dry 3 hours, be cooled to 200 ℃, and carry out abundant nitrogen replacement.Pass into the hydrogen that flow is 500mL/min, reduction is 1 hour under 200 ℃, is warming up to 400 ℃ of reduction 3 hours.Lift temperature to 600 ℃, hydrogen Passivation Treatment 5 hours.Catalyst activity examination condition as described in Example 1.
The Evaluation results of catalyst is as shown in table 1.The metal hydrogenation activity that method of reducing of the present invention can obtain higher metal dispersity and be fit to.Under more excellent condition, conversion ratio is higher than 46wt%, and the aromatic ring loss late is less than 2wt%.
Table 1 evaluating catalyst result

Claims (8)

1. the method for reducing of a disproportionation and transalkylation reaction catalyst comprises the following steps:
A) with the inert gas that contains oxygen, catalyst is carried out getting catalyst I after drying and dehydrating;
B) catalyst I is reduced to get catalyst I I with reducibility gas;
C) under reducibility gas and at 300~700 ℃ of temperature, catalyst I I is purged 1~8 hour, get required catalyst.
2. the method for reducing of disproportionation according to claim 1 and transalkylation catalyst is characterized in that inert gas is selected from least a in nitrogen, carbon dioxide; In inert gas, the oxygen volume content is 0.5~20%; The final baking temperature of inert gas is 300~600 ℃; During dry the end, the water content in the dry gas of outflow is less than 200ppm.
3. the method for reducing of disproportionation according to claim 2 and transalkylation catalyst, is characterized in that in inert gas, the oxygen volume content is 1~6%.
4. the method for reducing of disproportionation according to claim 1 and transalkylation catalyst is characterized in that reducibility gas is at least a in hydrogen, hydrogen~ammonia gas mixture or hydrogen~nitrogen mixed air.
5. the method for reducing of disproportionation according to claim 1 and transalkylation catalyst, the Contact Temperature that it is characterized in that reducibility gas and catalyst I is 300~600 ℃; Be 1~15 hour the time of contact of reducibility gas and catalyst I; Reducibility gas pressure is 0.05~5.0MPa; Water content in reduction process in eluting gas is lower than 200ppm.
6. the method for reducing of disproportionation according to claim 1 and transalkylation catalyst, is characterized in that catalyst I I continues to contact with hydrogen to carry out passivation.
7. the method for reducing of disproportionation according to claim 1 and transalkylation catalyst, is characterized in that catalyst I I and hydrogen Contact Temperature are 400~650 ℃, and be 2~6 hours time of contact.
8. the method for reducing of disproportionation according to claim 1 and transalkylation catalyst is characterized in that catalyst contains by weight percentage:
A) 0.01%~0.2% the metal that is selected from VIIIB family;
B) 50%~80% be selected from least a in modenite, β zeolite, ZSM-12 molecular sieve.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107866265A (en) * 2016-09-23 2018-04-03 中国石油化工股份有限公司 Transalkylation catalyst selectivity passivating method

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CN101121144A (en) * 2006-08-11 2008-02-13 中国石油化工股份有限公司 Catalyst for aromatics alkyl transferring and dealkylation to synthesis benzene and xylene
CN101688124A (en) * 2007-05-04 2010-03-31 沙索技术有限公司 catalysts
CN101703937A (en) * 2009-09-29 2010-05-12 武汉凯迪科技发展研究院有限公司 Method for regenerating cobalt-base catalyst for slurry-phase Fischer-Tropsch synthesis
CN101822985A (en) * 2009-03-04 2010-09-08 中国石油天然气股份有限公司 Pre-treatment method of nickel hydrogenation catalyst
CN102145286A (en) * 2011-01-11 2011-08-10 山西大学 Preparation method of Ni-SiO2/Al2O3 catalyst

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050227866A1 (en) * 2001-10-25 2005-10-13 Berge Peter J V Process for activating cobalt catalysts
CN101121144A (en) * 2006-08-11 2008-02-13 中国石油化工股份有限公司 Catalyst for aromatics alkyl transferring and dealkylation to synthesis benzene and xylene
CN101688124A (en) * 2007-05-04 2010-03-31 沙索技术有限公司 catalysts
CN101822985A (en) * 2009-03-04 2010-09-08 中国石油天然气股份有限公司 Pre-treatment method of nickel hydrogenation catalyst
CN101703937A (en) * 2009-09-29 2010-05-12 武汉凯迪科技发展研究院有限公司 Method for regenerating cobalt-base catalyst for slurry-phase Fischer-Tropsch synthesis
CN102145286A (en) * 2011-01-11 2011-08-10 山西大学 Preparation method of Ni-SiO2/Al2O3 catalyst

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107866265A (en) * 2016-09-23 2018-04-03 中国石油化工股份有限公司 Transalkylation catalyst selectivity passivating method
CN107866265B (en) * 2016-09-23 2020-07-03 中国石油化工股份有限公司 Selective deactivation of transalkylation catalyst

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