CN106694054A - Load-type resin catalyst for preparing xylene by virtue of selective toluene disproportionation - Google Patents
Load-type resin catalyst for preparing xylene by virtue of selective toluene disproportionation Download PDFInfo
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- CN106694054A CN106694054A CN201611167229.XA CN201611167229A CN106694054A CN 106694054 A CN106694054 A CN 106694054A CN 201611167229 A CN201611167229 A CN 201611167229A CN 106694054 A CN106694054 A CN 106694054A
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- active component
- maceration extract
- type resin
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/34—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of chromium, molybdenum or tungsten
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/08—Ion-exchange resins
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
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Abstract
The invention discloses a load-type resin catalyst for preparing xylene by virtue of selective toluene disproportionation, which relates to the technical field of resin catalysts. Weak-base anion-exchange resin is adopted as a carrier, molybdenum trioxide is adopted as a main active component, and the loading amount of the molybdenum trioxide is 10 to 25 percent of the mass of the carrier; and cuprous oxide is an auxiliary active component, and the loading amount of the cuprous oxide is 3 to 10 percent of the mass of the carrier. The load-type resin catalyst is particularly used for preparing xylene by virtue of selective toluene disproportionation, the catalytic efficiency is high, and the yield of the xylene reaches 95 percent or higher; the catalyst is little in consumption, and the investment cost of the catalyst can be effectively decreased; and moreover, the catalyst is easy to recycle, the activation method is simple, and the service life of the catalyst is effectively prolonged.
Description
Technical field：
The present invention relates to resin catalyst technical field, and in particular to a kind of selective disproportionation of toluene prepares dimethylbenzene and uses negative
Load type resin catalyst.
Background technology：
Toluene disproportionation reaction refers to the reaction that two molecule toluene generate a molecule benzene and a molecule dimethylbenzene, but actual anti-
Answer and be often accompanied by system side reaction, such as the generation of Toluene Hydrogenation dealkylation benzene and methane, toluene benzene ring hydrogenation generation first
Butylcyclohexane etc., therefore toluene disproportionation process is often the selectivity of benzene apparently higher than dimethylbenzene selective.For this case,
Our company develops a kind of selective disproportionation of toluene and prepares dimethylbenzene support type resin catalyst, and the height using the catalyst is living
Property and selectivity, improve toluene disproportionation generate paraxylene yield, increase toluene conversion ratio.
The content of the invention：
The technical problems to be solved by the invention are a kind of high catalytic efficiency of offer, consumption is few and reclaims easy toluene
Selective disproportionation prepares dimethylbenzene support type resin catalyst.
The technical problems to be solved by the invention are realized using following technical scheme：
A kind of selective disproportionation of toluene prepares dimethylbenzene support type resin catalyst, with weak-base anion-exchange resin
It is carrier, is main active component with molybdenum trioxide, load capacity is the 10-25% of carrier quality；Cuprous oxide is to help active component,
Load capacity is the 3-10% of carrier quality.
Its preparation method comprises the following steps：
(1) preparation of main maceration extract：By the 15-20 parts of positive ammonium molybdate aqueous solution for being configured to 10-30wt% soluble in water, then
1-2 parts of polyethylene glycol oxide and 0.5-1 parts of ammonium citrate are added, is uniformly dispersed after 3h is stood in 0-5 DEG C of environment, be then heated to
Reflux state insulation mixing 15min, i.e. winner's maceration extract；
(2) preparation of maceration extract is helped：By the 10-15 parts of copper acetate aqueous solution for being configured to 5-15wt% soluble in water, then add
Enter 0.5-1 parts of carbomer 934 and 0.5-1 parts of sulfurized lard, and be heated to reflux state insulation mixing 10min, obtain final product and help dipping
Liquid；
(3) load of main active component：During 25-35 parts of weak-base anion-exchange resin impregnated in into main maceration extract, in
Microwave treatment 5min under microwave frequency 2450MHz, power 700W, adds the 0-5 DEG C cold water isometric with main maceration extract, insulation
Mixing 30min, then again in microwave treatment 5min under microwave frequency 2450MHz, power 700W, filtering, gained filter residue in
5h is dried at 100-105 DEG C, gained solid abrasive obtains final product the catalyst for being loaded with main active component into powder；
(4) load of active component is helped：The catalyst that main active component will be loaded with impregnated in and help in maceration extract, and heat
To reflux state insulation mixing 15min, 1-2 parts of polyvinyl alcohol and 0.5-1 parts of ferrocene are added, be sufficiently mixed after Microwave Frequency
Microwave treatment 5min under rate 2450MHz, power 700W, continues under microwave frequency 2450MHz, power 700W after standing 30min
Microwave treatment 5min, filtering, in gained filter residue feeding freeze drier, the grind into powder after fully drying is subsequently adding
In weight portion ethylene glycol, and add a small amount of water to be warming up to 180 DEG C of backflow mixing 3h, filter again, gained filter residue washing three times, most
After 8h is dried at 100-105 DEG C, support type resin catalyst is obtained final product.
The weak-base anion-exchange resin is with styrene diethylene benzene copoly mer Archon as raw material, by work(
Energyization treatment is obtained, and its functionalization method is：2-4 parts of HPO, 1-2 parts of lanonol and 0.5-1 parts of ring five are gathered
Dimethyl siloxane is added in 15-20 parts of ethanol, is heated to reflux state insulation mixing 10min, adds 3-5 parts of sulfamic acid
With 0.5-1 parts of HPMA, continue the insulation mixing 5min that flows back, gained slurry is uniformly then sprayed on 25-35 parts of benzene
The surface of ethene-divinyl benzene copolymer Archon, 30min is at microwave under microwave frequency 2450MHz, power 700W for standing
Reason 5min, gained spherical particle is finally placed in -5-0 DEG C of environment and freezes 2h in 5h is dried at 75-80 DEG C, obtains final product alkalescent cloudy
Ion exchange resin.
The beneficial effects of the invention are as follows：The made support type resin catalyst of the present invention is exclusively used in selective disproportionation of toluene preparation
Dimethylbenzene, high catalytic efficiency makes the yield of dimethylbenzene reach more than 95%；The catalytic amount of the catalyst is few, can effectively reduce
The input cost of catalyst；And reclaim easy, by staticly settling i.e. achievable recovery, the catalyst warp of recovery after use
Can be reused after 130-140 DEG C of heating 2-3h, activation method is simple, effectively the service life of extension catalyst.
Specific embodiment：
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment 1
(1) preparation of main maceration extract：By 15 parts of positive ammonium molybdate aqueous solution for being configured to 25wt% soluble in water, 1 is added
Part polyethylene glycol oxide and 0.5 part of ammonium citrate, are uniformly dispersed after 3h is stood in 0-5 DEG C of environment, are then heated to reflux state
Insulation mixing 15min, i.e. winner's maceration extract；
(2) preparation of maceration extract is helped：By 10 parts of copper acetate aqueous solution for being configured to 10wt% soluble in water, 0.5 is added
Part carbomer 934 and 0.5 part of sulfurized lard, and reflux state insulation mixing 10min is heated to, obtain final product and help maceration extract；
(3) load of main active component：During 30 parts of weak-base anion-exchange resins impregnated in into main maceration extract, in microwave
Microwave treatment 5min under frequency 2450MHz, power 700W, adds the 0-5 DEG C cold water isometric with main maceration extract, insulation mixing
30min, then again in microwave treatment 5min under microwave frequency 2450MHz, power 700W, filters, and gained filter residue is in 100-105
5h is dried at DEG C, gained solid abrasive obtains final product the catalyst for being loaded with main active component into powder；
(4) load of active component is helped：The catalyst that main active component will be loaded with impregnated in and help in maceration extract, and heat
To reflux state insulation mixing 15min, 1 part of polyvinyl alcohol and 0.5 part of ferrocene are added, be sufficiently mixed after microwave frequency
Microwave treatment 5min under 2450MHz, power 700W, stand continue at after 30min it is micro- under microwave frequency 2450MHz, power 700W
Ripple processes 5min, filtering, and in gained filter residue feeding freeze drier, the grind into powder after fully drying is subsequently adding and waits heavy
In amount part ethylene glycol, and add a small amount of water to be warming up to 180 DEG C of backflow mixing 3h, filter again, gained filter residue washing three times, finally
In 8h is dried at 100-105 DEG C, support type resin catalyst is obtained final product.
The preparation of weak-base anion-exchange resin：By 2 parts of HPOs, 2 parts of lanonols and 0.5 part of poly- diformazan of ring five
Radical siloxane is added in 20 parts of ethanol, is heated to reflux state insulation mixing 10min, adds 3 parts of sulfamic acids and 0.5 part of water
Solution HPMA, continues the insulation mixing 5min that flows back, and gained slurry is uniformly then sprayed on into 35 parts of styrene-divinylbenzenes
The surface of copolymer Archon, stands 30min after microwave treatment 5min under microwave frequency 2450MHz, power 700W, and gained is spherical
Particle is finally placed in -5-0 DEG C of environment and freezes 2h in 5h is dried at 75-80 DEG C, obtains final product weak-base anion-exchange resin.
After testing, the load capacity of molybdenum trioxide is carrier quality in the made support type resin catalyst of embodiment 1
20.5%, the load capacity of cuprous oxide is the 5.8% of carrier quality.
Embodiment 2
(1) preparation of main maceration extract：By 20 parts of positive ammonium molybdate aqueous solution for being configured to 25wt% soluble in water, 1 is added
Part polyethylene glycol oxide and 1 part of ammonium citrate, are uniformly dispersed after 3h is stood in 0-5 DEG C of environment, are then heated to reflux state guarantor
Temperature mixing 15min, i.e. winner's maceration extract；
(2) preparation of maceration extract is helped：By 15 parts of copper acetate aqueous solution for being configured to 10wt% soluble in water, 0.5 is added
Part carbomer 934 and 0.5 part of sulfurized lard, and reflux state insulation mixing 10min is heated to, obtain final product and help maceration extract；
(3) load of main active component：During 30 parts of weak-base anion-exchange resins impregnated in into main maceration extract, in microwave
Microwave treatment 5min under frequency 2450MHz, power 700W, adds the 0-5 DEG C cold water isometric with main maceration extract, insulation mixing
30min, then again in microwave treatment 5min under microwave frequency 2450MHz, power 700W, filters, and gained filter residue is in 100-105
5h is dried at DEG C, gained solid abrasive obtains final product the catalyst for being loaded with main active component into powder；
(4) load of active component is helped：The catalyst that main active component will be loaded with impregnated in and help in maceration extract, and heat
To reflux state insulation mixing 15min, 1 part of polyvinyl alcohol and 0.5 part of ferrocene are added, be sufficiently mixed after microwave frequency
Microwave treatment 5min under 2450MHz, power 700W, stand continue at after 30min it is micro- under microwave frequency 2450MHz, power 700W
Ripple processes 5min, filtering, and in gained filter residue feeding freeze drier, the grind into powder after fully drying is subsequently adding and waits heavy
In amount part ethylene glycol, and add a small amount of water to be warming up to 180 DEG C of backflow mixing 3h, filter again, gained filter residue washing three times, finally
In 8h is dried at 100-105 DEG C, support type resin catalyst is obtained final product.
The preparation of weak-base anion-exchange resin：By 2 parts of HPOs, 1 part of lanonol and 0.5 part of poly- diformazan of ring five
Radical siloxane is added in 20 parts of ethanol, is heated to reflux state insulation mixing 10min, adds 5 parts of sulfamic acids and 0.5 part of water
Solution HPMA, continues the insulation mixing 5min that flows back, and gained slurry is uniformly then sprayed on into 35 parts of styrene-divinylbenzenes
The surface of copolymer Archon, stands 30min after microwave treatment 5min under microwave frequency 2450MHz, power 700W, and gained is spherical
Particle is finally placed in -5-0 DEG C of environment and freezes 2h in 5h is dried at 75-80 DEG C, obtains final product weak-base anion-exchange resin.
After testing, the load capacity of molybdenum trioxide is carrier quality in the made support type resin catalyst of embodiment 2
21.8%, the load capacity of cuprous oxide is the 5.6% of carrier quality.
General principle of the invention and principal character and advantages of the present invention has been shown and described above.The technology of the industry
Personnel it should be appreciated that the present invention is not limited to the above embodiments, simply explanation described in above-described embodiment and specification this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appending claims and its
Equivalent thereof.
Claims (3)
1. a kind of selective disproportionation of toluene prepares dimethylbenzene support type resin catalyst, it is characterised in that：With alkalescent it is cloudy from
Sub-exchange resin is carrier, is main active component with molybdenum trioxide, and load capacity is the 10-25% of carrier quality；Cuprous oxide is
Active component is helped, load capacity is the 3-10% of carrier quality.
2. selective disproportionation of toluene according to claim 1 prepares dimethylbenzene support type resin catalyst, and its feature exists
In its preparation method comprises the following steps：
(1) preparation of main maceration extract：By the 15-20 parts of positive ammonium molybdate aqueous solution for being configured to 10-30wt% soluble in water, add
1-2 parts of polyethylene glycol oxide and 0.5-1 parts of ammonium citrate, are uniformly dispersed after 3h is stood in 0-5 DEG C of environment, are then heated to backflow
State insulation mixing 15min, i.e. winner's maceration extract；
(2) preparation of maceration extract is helped：By the 10-15 parts of copper acetate aqueous solution for being configured to 5-15wt% soluble in water, add
0.5-1 parts of carbomer 934 and 0.5-1 parts of sulfurized lard, and reflux state insulation mixing 10min is heated to, obtain final product and help maceration extract；
(3) load of main active component：During 25-35 parts of weak-base anion-exchange resin impregnated in into main maceration extract, in microwave
Microwave treatment 5min under frequency 2450MHz, power 700W, adds the 0-5 DEG C cold water isometric with main maceration extract, insulation mixing
30min, then again in microwave treatment 5min under microwave frequency 2450MHz, power 700W, filters, and gained filter residue is in 100-105
5h is dried at DEG C, gained solid abrasive obtains final product the catalyst for being loaded with main active component into powder；
(4) load of active component is helped：The catalyst that main active component will be loaded with impregnated in and help in maceration extract, and be heated to back
Stream mode insulation mixing 15min, adds 1-2 parts of polyvinyl alcohol and 0.5-1 parts of ferrocene, is sufficiently mixed after microwave frequency
Microwave treatment 5min under 2450MHz, power 700W, stand continue at after 30min it is micro- under microwave frequency 2450MHz, power 700W
Ripple processes 5min, filtering, and in gained filter residue feeding freeze drier, the grind into powder after fully drying is subsequently adding and waits heavy
In amount part ethylene glycol, and add a small amount of water to be warming up to 180 DEG C of backflow mixing 3h, filter again, gained filter residue washing three times, finally
In 8h is dried at 100-105 DEG C, support type resin catalyst is obtained final product.
3. selective disproportionation of toluene according to claim 1 and 2 prepares dimethylbenzene support type resin catalyst, its feature
It is：The weak-base anion-exchange resin is with styrene diethylene benzene copoly mer Archon as raw material, by functionalization
Treatment is obtained, and its functionalization method is：By 2-4 parts of HPO, 1-2 parts of lanonol and the 0.5-1 parts of poly- diformazan of ring five
Radical siloxane add 15-20 part ethanol in, be heated to reflux state insulation mixing 10min, add 3-5 parts of sulfamic acid with
0.5-1 parts of HPMA, continues the insulation mixing 5min that flows back, and gained slurry is uniformly then sprayed on into 25-35 parts of benzene second
The surface of alkene-divinyl benzene copolymer Archon, stands 30min after microwave treatment under microwave frequency 2450MHz, power 700W
5min, gained spherical particle is finally placed in -5-0 DEG C of environment and freezes 2h in 5h is dried at 75-80 DEG C, obtain final product alkalescent it is cloudy from
Sub-exchange resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611167229.XA CN106694054A (en) | 2016-12-16 | 2016-12-16 | Load-type resin catalyst for preparing xylene by virtue of selective toluene disproportionation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611167229.XA CN106694054A (en) | 2016-12-16 | 2016-12-16 | Load-type resin catalyst for preparing xylene by virtue of selective toluene disproportionation |
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| CN201611167229.XA Withdrawn CN106694054A (en) | 2016-12-16 | 2016-12-16 | Load-type resin catalyst for preparing xylene by virtue of selective toluene disproportionation |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101172245A (en) * | 2006-11-02 | 2008-05-07 | 中国石油化工股份有限公司 | Methylbenzene shape-selective disproportionation reaction catalyzer |
| CN101898152A (en) * | 2009-05-25 | 2010-12-01 | 中国石油化工股份有限公司 | Toluene disproportionation and alkyl transfer catalyst and preparation method thereof |
| CN101993332A (en) * | 2009-08-31 | 2011-03-30 | 中国石油化工股份有限公司上海石油化工研究院 | Combined method for joint production of aromatic hydrocarbon |
| CN103121912A (en) * | 2011-11-18 | 2013-05-29 | 中国石油化工股份有限公司 | Method for preparing dimethylbenzene through methylation and transalkylation |
| CN103880584A (en) * | 2012-12-19 | 2014-06-25 | 中国石油化工股份有限公司 | Method for combined production of p-xylene |
| CN104107714A (en) * | 2013-04-16 | 2014-10-22 | 中国石油化工股份有限公司 | High-xylene-selectivity toluene disproportionation catalyst and its application |
| CN104557434A (en) * | 2013-10-28 | 2015-04-29 | 中国石油化工股份有限公司 | Method for producing paraxylene |
| CN106076359A (en) * | 2016-07-14 | 2016-11-09 | 安徽海德石油化工有限公司 | A kind of oil hydrogenation deoxidation nickel-base catalyst |
-
2016
- 2016-12-16 CN CN201611167229.XA patent/CN106694054A/en not_active Withdrawn
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|---|---|---|---|---|
| CN101172245A (en) * | 2006-11-02 | 2008-05-07 | 中国石油化工股份有限公司 | Methylbenzene shape-selective disproportionation reaction catalyzer |
| CN101898152A (en) * | 2009-05-25 | 2010-12-01 | 中国石油化工股份有限公司 | Toluene disproportionation and alkyl transfer catalyst and preparation method thereof |
| CN101993332A (en) * | 2009-08-31 | 2011-03-30 | 中国石油化工股份有限公司上海石油化工研究院 | Combined method for joint production of aromatic hydrocarbon |
| CN103121912A (en) * | 2011-11-18 | 2013-05-29 | 中国石油化工股份有限公司 | Method for preparing dimethylbenzene through methylation and transalkylation |
| CN103880584A (en) * | 2012-12-19 | 2014-06-25 | 中国石油化工股份有限公司 | Method for combined production of p-xylene |
| CN104107714A (en) * | 2013-04-16 | 2014-10-22 | 中国石油化工股份有限公司 | High-xylene-selectivity toluene disproportionation catalyst and its application |
| CN104557434A (en) * | 2013-10-28 | 2015-04-29 | 中国石油化工股份有限公司 | Method for producing paraxylene |
| CN106076359A (en) * | 2016-07-14 | 2016-11-09 | 安徽海德石油化工有限公司 | A kind of oil hydrogenation deoxidation nickel-base catalyst |
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Application publication date: 20170524 |