CN109433250A - Reduce the catalyst of high boiling aromatic hydrocarbon solvent bromine index - Google Patents
Reduce the catalyst of high boiling aromatic hydrocarbon solvent bromine index Download PDFInfo
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- CN109433250A CN109433250A CN201811200427.0A CN201811200427A CN109433250A CN 109433250 A CN109433250 A CN 109433250A CN 201811200427 A CN201811200427 A CN 201811200427A CN 109433250 A CN109433250 A CN 109433250A
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- catalyst
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- aromatic hydrocarbon
- hydrocarbon solvent
- high boiling
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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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/40—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively
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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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/18—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the mordenite type
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/148—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound
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Abstract
The invention discloses a kind of catalyst for reducing high boiling aromatic hydrocarbon solvent bromine index, component including following parts by weight: 1.5 ~ 4 parts of carrier, 1 part of active component, 0.1 ~ 1 part of metal oxide, active component is selected from one or more of ZSM-5, Y type molecular sieve, modenite or X-type molecular sieve, and metal is selected from magnesium, sodium, potassium, copper, cobalt, nickel, tin, caesium, palladium, beryllium, manganese, caesium, ferric nitrate, zinc, cerium or lanthanum.The present invention is sieved using unimolecule or composite molecular screen is as catalyst, carry out the technical issues of catalytic efficiency is not up to ideal effect when catalysis BTX aromatic hydrocarbons methyl is combined to pseudocumene, catalyst preparation process is not necessarily to high temperature and pressure, hydrogen is not had in reaction process, catalyst activity is high, removal alkene effect is good, and arene content remains unchanged in product.Rectifying or extraction and separation are not necessarily to after reaction, it is only necessary to which step unit operation reaches effect, small investment.
Description
Technical field
The present invention relates to the catalyst technologies that high boiling aromatic hydrocarbon solvent bromine index is reduced under non-hydrogen state, more specifically relate to
And a kind of catalyst for reducing high boiling aromatic hydrocarbon solvent bromine index.
Background technique
Bromine index content in aromatic hydrocarbons can react the contaminated level of aromatic hydrocarbons.So-called bromine index is according to petrochemical industry row
Industry standard (SH/T 0630-1996), refers in point titration process, to be saturated all unsaturated bonds in every hectogram oil sample
The milligram number of consumed simple substance bromine, unit are mgBr/100g oil.It mainly include unsaturated hydro carbons such as monoolefine, polyenoid
Hydrocarbon and phenylethylene, these hydro carbons produce colloid and undesirable side reaction.It can lead to the biography of covering reaction or operating system
Hot face reduces reaction or operating system efficiency and generates by-product.Therefore, it should will before aroamtic hydrocarbon raw material is for other techniques
These impurity are from wherein removing.
Currently, industrial, there are two types of schemes to remove the olefin impurity in aromatic solvent.One is after reforming reactor
" back end hydrogenation " is carried out to achieve the purpose that remove alkene.Catalyst used is generally the noble metals such as platinum, palladium.
Practice have shown that for single benzene close-cut fraction, no matter it is all relatively good to make catalyst effect with platinum or palladium, still
For the aromatic hydrocarbons long distillate product of trimethylbenzene to durene, " back end hydrogenation " reaction is difficult to take into account comprehensively, and causes aromatic hydrocarbons
It loses larger.This contradiction can be mitigated by carrying out the method that purification removes alkene with Emathlite, it is to from trimethylbenzene to tetramethyl
Alkene is removed in the long distillate of benzene preferable effect.But because carclazyte inactivation is fast, replaces frequently, and be difficult to after inactivating again sharp
With, it will cause serious pollution and biggish labor intensity, and be difficult to handle, it is very unfavorable to environment.In addition, also useful oxidation
Aluminium, magnesium silicate or alumina silicate replace the report that coincides or be copolymerized removing alkene of the carclazyte by alkene.
Summary of the invention
The object of the present invention is to provide a kind of catalyst for reducing high boiling aromatic hydrocarbon solvent bromine index, to overcome the prior art
Existing defect.
The catalyst of the reduction high boiling aromatic hydrocarbon solvent bromine index, the component including following parts by weight:
1.5 ~ 4 parts of carrier
1 part of active component
Preferably, the catalyst of the reduction high boiling aromatic hydrocarbon solvent bromine index, the component including following parts by weight:
1.5 ~ 4 parts of carrier
1 part of active component
0.1 ~ 1 part of metal oxide, most preferably 0.1 ~ 0.3 part
The active component is selected from one or more of ZSM-5, Y type molecular sieve, modenite or X-type molecular sieve；
The metal is selected from magnesium, sodium, potassium, copper, cobalt, nickel, tin, caesium, palladium, beryllium, manganese, caesium, ferric nitrate, zinc, cerium or lanthanum；
Preferably, the metal is caesium, cerium or lanthanum；
Preferably, the active component is the mixture of ZSM-5 and following metal oxide:
Caesium, cerium or lanthanum；
The weight ratio of ZSM-5 and the metal oxide are as follows: 1:0.1 ~ 1
The carrier is selected from carclazyte, diatomite, gama-alumina or SiO2；
The Chinese of term " ZSM-5 " is ZSM-5 molecular sieve, and commercially produced product can be used；
The preparation method of the catalyst of the reduction high boiling aromatic hydrocarbon solvent bromine index, includes the following steps:
(1) active component and carrier are mixed, inorganic binder bonding is added；
The inorganic binder is selected from nitric acid or phosphoric acid, the preferably nitric acid of weight concentration 10% or the phosphorus of weight concentration 10%
Acid, the weight consumption of inorganic binder are as follows:
Active component and total weight of carrier: inorganic binder=1:8 ~ 12；
(2) it then being squeezed into item, sloughs moisture in 90-130 DEG C of drying 2h, 400-600 DEG C of roasting 3-5h of Muffle furnace is activated,
(3) catalyst after activation is ground into the particle of 20-40 mesh, as the reduction high boiling aromatic hydrocarbon solvent bromine index
Catalyst, be put into drying box stand-by.
Preferably, further include following steps:
(4) metal chloride or itrated compound are made into the aqueous solution that weight concentration is 1%-10%, then by the catalyst of step (3)
4 ~ 6h of incipient impregnation, 95 ~ 100 DEG C of drying, 240 ~ 260 DEG C of 1 ~ 3h of roasting, then 380 ~ 420 DEG C of 2 ~ 4 h of roasting, can be obtained
The catalyst of the performance more preferably reduction high boiling aromatic hydrocarbon solvent bromine index；
The metal chloride or itrated compound is selected from magnesium chloride, sodium chloride, potassium chloride, copper chloride, cobalt chloride, nickel chloride, chlorine
Change stannous, cesium chloride, palladium chloride, beryllium chloride or manganese chloride, the metal itrated compound is cesium nitrate, ferric nitrate, copper nitrate, nitric acid
Zinc, cerous nitrate or lanthanum nitrate；
The beneficial effects of the present invention are:
The present invention is sieved using unimolecule or composite molecular screen is as catalyst, is carried out catalysis BTX aromatic hydrocarbons methyl and is combined to inclined front three
Catalytic efficiency is not up to the technical issues of ideal effect when benzene, and catalyst preparation process is not necessarily to high temperature and pressure, in reaction process not
With hydrogen, catalyst activity is high, and removal alkene effect is good, and arene content remains unchanged in product.Rectifying or extraction are not necessarily to after reaction
Take separation, it is only necessary to which step unit operation reaches effect, small investment.
Specific embodiment
1 catalyst A of embodiment
Catalytic component and proportion: (parts by weight)
1 part of active component ZSM-5
1.5 parts of carrier carclazyte
Preparation method:
Active component and carrier carclazyte are uniformly mixed, the nitric acid that weight concentration is 10% is added and bonds,
The addition weight of nitric acid are as follows:
Active component and total weight of carrier: nitric acid=1:8 that weight concentration is 10%；
Then it is squeezed into item, sloughs moisture, 400 DEG C of roasting 5h in 90 DEG C of drying 1h.Catalyst after activation is ground into 20 mesh
Particle, the catalyst of the as described reduction high boiling aromatic hydrocarbon solvent bromine index is put into drying box stand-by.
2 catalyst B of embodiment
Catalytic component and proportion: (parts by weight)
1 part of active component modenite
4 parts of carrier gama-alumina
Preparation method:
Modenite and gama-alumina are mixed, the nitric acid that weight concentration is 10% is added and bonds, the addition weight of nitric acid are as follows: living
Property component and total weight of carrier: nitric acid=1:12 that weight concentration is 10%；
Then it is squeezed into item, sloughs moisture, 600 DEG C of roasting 3h in 130 DEG C of drying 3h.Catalyst after activation is ground into 40 mesh
Particle, the catalyst of the as described reduction high boiling aromatic hydrocarbon solvent bromine index is put into drying box stand-by.
3 catalyst C of embodiment
Catalytic component and proportion: (parts by weight)
1 part of active component zsm-5
3 parts of carrier gama-alumina
The preparation method is the same as that of Example 1, obtains catalyst C.
4 catalyst D of embodiment
Catalytic component and proportion: (parts by weight)
1 part of active component zsm-5
3 parts of carrier gama-alumina
0.2 part of metal oxide cerium
Preparation method:
Zsm-5 and carrier gama-alumina are uniformly mixed, the nitric acid that weight concentration is 10% is added and bonds, the addition weight of nitric acid
Are as follows: active component and total weight of carrier: nitric acid=1:10 that weight concentration is 10%；
It is squeezed into item, then dries 2h at 100 DEG C, sloughs moisture, 400 DEG C of roasting 3h activation are ground into the particle of 30 mesh；
Cerous nitrate is made into 1% aqueous solution, by above-mentioned particle in the medium volume impregnation 5h of cerous nitrate aqueous solution, 100 DEG C of baking ovens dry
Dry, first 250 DEG C of roasting 2h, then 400 DEG C of 3 h of roasting can be obtained the catalyst.
Embodiment 5, catalyst E
Catalytic component and proportion: (parts by weight)
1 part of active component zsm-5
3 parts of carrier gama-alumina
0.1 part of lanthana
Zsm-5 and carrier gama-alumina are uniformly mixed, the nitric acid that weight concentration is 10% is added and bonds, the addition weight of nitric acid
Are as follows: active component and total weight of carrier: nitric acid=1:10 that weight concentration is 10%
It is squeezed into item, then sloughs moisture in 130 DEG C of drying 2h, 600 DEG C of roasting 3h activation are ground into the particle of 20 mesh；
Lanthanum nitrate is made into 10% aqueous solution, by above-mentioned particle in the medium volume impregnation 6h of cerous nitrate aqueous solution, 100 DEG C of baking ovens dry
It is dry, 250 DEG C of roasting 2h, then 400 DEG C of 3 h of roasting, it can be obtained the catalyst.
Embodiment 6, catalyst F
Catalytic component and proportion: (parts by weight)
1 part of active component zsm-5
3 parts of carrier gama-alumina
0.3 part of cesium oxide
Zsm-5 and gama-alumina are mixed, the nitric acid that weight concentration is 10% is added and bonds, the addition weight of nitric acid are as follows: activity
Component and total weight of carrier: nitric acid=1:9 that weight concentration is 10% is squeezed into item, then sloughs moisture in 120 DEG C of drying 2h,
500 DEG C of roasting 4h activation, are ground into the particle of 30 mesh；
Cesium nitrate is made into 5% aqueous solution, dries after exchanging 5h with above-mentioned catalyst incipient impregnation with 100 DEG C of baking ovens, finally puts
Enter first 250 DEG C of roasting 2h, then 400 DEG C of 3 h of roasting in Muffle furnace, can be obtained the catalyst.
Embodiment 7 evaluates embodiment
Reaction carries out in fixed bed reactors.
Catalytic reaction condition is as follows: the catalyst of embodiment 1 ~ 6 and porcelain ball is fitted into reactor, at 180 DEG C of temperature,
Pressure 1.0MPa, weight space velocity 1.5h-1Under conditions of, raw material high boiling aromatic hydrocarbon solvent is passed through into the fixed bed reactors,
Its bromine index is analyzed with bromine valency bromine index instrument.
Raw material high boiling aromatic hydrocarbon solvent contains the component of following mass percent:
Table 1
| Component | Mass fraction (wt.%) |
| Non-aromatics | 0.13 |
| C8 aromatic hydrocarbons | 0.14 |
| Between p-methyl-ethylbenzene | 16.78 |
| Mesitylene | 6.28 |
| O-methylethylbenzene | 9.82 |
| Pseudocumene | 38.79 |
| 1,2,3-trimethylbenzene | 9.97 |
| Indane | 1.77 |
| C10 aromatic hydrocarbons | 15.45 |
So-called bromine index is referred to according to China's oil chemical industry standard (SH/T 0630-1996) in constant-current titration process
In, for the milligram number for being saturated simple substance bromine consumed by all unsaturated keys in every hectogram oil sample, unit is mg Br/100g
Oil.
Catalyst activity X=[(feedstock oil bromine index-discharged oil bromine index)/feedstock oil bromine index] * 100%
Each embodiment corresponds to the catalytic activity such as table 2 of catalyst:
Table 2
| Catalyst title | Catalyst activity X |
| A | 84.44% |
| B | 86.67% |
| C | 88.89% |
| D | 90.00% |
| E | 91.11% |
| F | 93.33% |
Claims (10)
1. reducing the catalyst of high boiling aromatic hydrocarbon solvent bromine index, which is characterized in that the component including following parts by weight:
1.5 ~ 4 parts of carrier
1 part of active component；
The active component is selected from one or more of ZSM-5, Y type molecular sieve, modenite or X-type molecular sieve.
2. reducing the catalyst of high boiling aromatic hydrocarbon solvent bromine index, which is characterized in that the component including following parts by weight:
1.5 ~ 4 parts of carrier
1 part of active component
0.1 ~ 1 part of metal oxide
The active component is selected from one or more of ZSM-5, Y type molecular sieve, modenite or X-type molecular sieve；
The metal is selected from magnesium, sodium, potassium, copper, cobalt, nickel, tin, caesium, palladium, beryllium, manganese, caesium, ferric nitrate, zinc, cerium or lanthanum.
3. the catalyst according to claim 2 for reducing high boiling aromatic hydrocarbon solvent bromine index, which is characterized in that the gold
Belonging to oxide is 0.1 ~ 0.3 part.
4. the catalyst according to claim 2 for reducing high boiling aromatic hydrocarbon solvent bromine index, which is characterized in that the work
Property group is divided into the mixture of ZSM-5 Yu following metal oxide:
Caesium, cerium or lanthanum；
The weight ratio of ZSM-5 and the metal oxide are as follows: 1:0.1 ~ 1.
5. described in any item catalyst for reducing high boiling aromatic hydrocarbon solvent bromine index according to claim 1 ~ 4, which is characterized in that
The carrier is selected from carclazyte, diatomite, gama-alumina or SiO2。
6. according to claim 1 ~ 5 it is described in any item reduce high boiling aromatic hydrocarbon solvent bromine indexs catalyst, preparation method,
It is characterized by comprising the following steps:
(1) active component and carrier are mixed, inorganic binder bonding is added；
(2) it then is squeezed into item, dried, 400-600 DEG C of calcination activation,
(3) catalyst after activation is ground into particle, the catalyst of the as described reduction high boiling aromatic hydrocarbon solvent bromine index.
7. according to the method described in claim 6, it is characterized in that, the inorganic binder is selected from nitric acid or phosphoric acid, weight
The nitric acid of concentration 10% or the phosphoric acid of weight concentration 10%, the weight consumption of inorganic binder are as follows: active component and total weight of carrier:
Inorganic binder=1:8 ~ 12.
8. according to the method described in claim 6, it is characterized in that, item is squeezed into, in 90-130 DEG C of drying, 400-600 DEG C of roasting
Burn 3-5h activation.
9. according to the method described in claim 8, it is characterized in that, further including following steps:
(4) metal chloride or itrated compound are made into the aqueous solution that weight concentration is 1%-10%, then by the catalyst of step (3)
4 ~ 6h of incipient impregnation, 95 ~ 100 DEG C of drying, 240 ~ 260 DEG C of 1 ~ 3h of roasting, then 380 ~ 420 DEG C of 2 ~ 4 h of roasting, can be obtained
The catalyst of the reduction high boiling aromatic hydrocarbon solvent bromine index.
10. according to the method described in claim 9, it is characterized in that, the metal chloride or itrated compound be selected from magnesium chloride,
Sodium chloride, potassium chloride, copper chloride, cobalt chloride, nickel chloride, stannous chloride, cesium chloride, palladium chloride, beryllium chloride or manganese chloride, it is described
Metal itrated compound is cesium nitrate, ferric nitrate, copper nitrate, zinc nitrate, cerous nitrate or lanthanum nitrate.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070112240A1 (en) * | 2005-11-17 | 2007-05-17 | Brown Stephen H | Process for reducing Bromine Index of hydrocarbon feedstocks |
| CN101433856A (en) * | 2007-11-13 | 2009-05-20 | 华东理工大学 | Catalyst for removing trace amounts of olefin hydrocarbon in arene |
| CN102309977A (en) * | 2010-07-07 | 2012-01-11 | 中国石油化工股份有限公司 | Deolefination catalyst and preparation method and application thereof |
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| CN104549472A (en) * | 2013-10-28 | 2015-04-29 | 中国石油化工股份有限公司 | Aromatic alkyl transferring and deolefination catalyst and application thereof |
| CN105080592A (en) * | 2014-05-14 | 2015-11-25 | 中国石油化工股份有限公司 | Aromatic olefin-reducing catalyst and use thereof |
| CN107754845A (en) * | 2016-08-23 | 2018-03-06 | 中国石油化工股份有限公司 | High life reformate olefine lowering catalyst |
-
2018
- 2018-10-16 CN CN201811200427.0A patent/CN109433250A/en not_active Withdrawn
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070112240A1 (en) * | 2005-11-17 | 2007-05-17 | Brown Stephen H | Process for reducing Bromine Index of hydrocarbon feedstocks |
| CN101433856A (en) * | 2007-11-13 | 2009-05-20 | 华东理工大学 | Catalyst for removing trace amounts of olefin hydrocarbon in arene |
| CN102309977A (en) * | 2010-07-07 | 2012-01-11 | 中国石油化工股份有限公司 | Deolefination catalyst and preparation method and application thereof |
| CN102688771A (en) * | 2011-03-23 | 2012-09-26 | 中国石油天然气股份有限公司 | Catalyst for alkylation of benzene and methanol, preparation and application thereof |
| CN104549472A (en) * | 2013-10-28 | 2015-04-29 | 中国石油化工股份有限公司 | Aromatic alkyl transferring and deolefination catalyst and application thereof |
| CN105080592A (en) * | 2014-05-14 | 2015-11-25 | 中国石油化工股份有限公司 | Aromatic olefin-reducing catalyst and use thereof |
| CN107754845A (en) * | 2016-08-23 | 2018-03-06 | 中国石油化工股份有限公司 | High life reformate olefine lowering catalyst |
Non-Patent Citations (1)
| Title |
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| 张蕾 著: "《烟气脱硫脱硝技术及催化剂的研究进展》", 31 July 2016, 中国矿业大学出版社 * |
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