CN100475336C - Alkyltransfering catalyst for increasing yield C8 aromatic hydrocarbons - Google Patents

Alkyltransfering catalyst for increasing yield C8 aromatic hydrocarbons Download PDF

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CN100475336C
CN100475336C CNB2006100250958A CN200610025095A CN100475336C CN 100475336 C CN100475336 C CN 100475336C CN B2006100250958 A CNB2006100250958 A CN B2006100250958A CN 200610025095 A CN200610025095 A CN 200610025095A CN 100475336 C CN100475336 C CN 100475336C
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aronmatic
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CN101045207A (en
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郭宏利
杨德琴
孔德金
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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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Abstract

A transalkylation catalyst for increasing the output of C8 arylhydrocarbon contains the hydrogen-type zeolite containing SiO2/Al2O3 (20-90 Wt portions), adhesive (10-80) and platinum oxide (0.001-5).

Description

The transalkylation catalyst of volume increase C8 aronmatic
Technical field
The present invention relates to a kind of transalkylation catalyst that increases production C8 aronmatic, particularly,, increase production the catalyst of C8 aronmatic to greatest extent by transalkylation and dealkylation about being raw material only with carbon nine and above heavy arene thereof.
Background technology
Paraxylene in the 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, plastics 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 C 8A is by volume increase C8 aronmatic (C 8A) reach the purpose of effective volume increase paraxylene.
People are usually C9 aromatic (C 9A), carbon ten and above heavy aromatics (C thereof 10 +A) be referred to as heavy aromatics.Petroleum Aromatics is mainly derived from the byproduct that light oil cracking is produced ethylene unit; The aromatic hydrocarbons that the oil plant catalytic reforming is produced; The byproduct of toluene disproportionation and transalkylation unit.Along with increasing of heavy arene amount, the comprehensive utilization of heavy arene becomes the problem that people are concerned about, wherein C 9The processing and utilization of A has ripe method, is widely used as the raw material of toluene disproportionation and transalkylation reaction, is used for making benzene and C 8A.Aromatic Hydrocarbon United Plant of producing 22.5 ten thousand tons of paraxylene per year according to estimates, because the difference of feedstock oil, the difference of process, the annual C that produces 10 +A is 1～30,000 ton, and this is a kind of resource of preciousness, and present Aromatic Hydrocarbon United Plant does not also have suitable processing and utilizes method to this.
Along with the development of catalyst technology, can adopt the carbon ten heavy arene (C that sneak into certain content in the reaction raw materials at present 10A) method improves the yield of purpose product, pursues under high conversion, the high-speed deficiency that product yield is on the low side, but C in fact to remedy 10Have only about 20～30% to be utilized among the A, and about 80～70% C 10A discharges at the bottom of the heavy aromatics Tata.
As a kind of important research project of rationally utilizing the heavy arene resource, heavy aromatic hydrocarbon light also more and more has been subjected to people's attention.Heavy aromatic hydrocarbon light is by the hydro-dealkylation reaction, finally generates benzene, toluene and dimethylbenzene.Yet because heavy arene mainly is to produce light aromatic hydrocarbons by pyrolysismethod and catalytic dealkylation method at present, its aromatic hydrocarbons loss is bigger, alkyl takes off alkyl and causes the hydrogen consumption to increase, and the side chain alkyl is not utilized effectively yet, and the yield of purpose product is lower, technical-economic index is relatively poor, and commercialization is restricted.
In the public clear 51-29131 patent of spy, use MoO 3-NiO/Al 2O 3(weight consists of 13%Wo, 5%Ni) is catalyst, with C 9A-C 10A (benzene 0.81%, toluene 0.26%, C 8A0.95%, C 10A15.23%) be raw material, under 6MPa and 550 ℃ of reaction conditions, during product is formed by weight percentage for containing benzene 9.74%, toluene 30.27%, dimethylbenzene 32.33% and non-aromatics 0.16%.
USP5,942,651 disclose a kind of with benzene or toluene and C 9 +The method of the light aromatic hydrocarbons of A transalkylation production, this method is loaded into two beds with two kinds of catalyst, perhaps be seated in the reactor of two polyphones, the described first kind of zeolite of this method mainly is selected from MCM-22, PSH-3, SSZ-25, ZSM-12 or β, second kind of zeolite is selected from ZSM-5, the amount of second kind of catalyst accounts for 1～20% of catalyst total amount, and best 10～15%.When reaction, raw material need be passed through first beds earlier, and the control weight space velocity is at 1.0～7.0 o'clock -1, be preferably at 2.5～4.5 o'clock -1, be 5.0～100.0 o'clock by the weight space velocity of second beds -1, be preferably at 15.0～35.0 o'clock -1, the purpose of this method is to make raw material pass through first catalyst with slower speed, generates intermediate products, then allowing these intermediate products pass through second catalyst with fast speeds, to generate more BTX.
Carbon nine and above heavy arene content thereof more only carry out transalkylation reaction by zeolite itself in raw material, the often very fast inactivation of catalyst.United States Patent (USP) 4723048 discloses a kind of toluene and alkylaromatic hydrocarbon disproportionation/transalkylation catalyst, load Ni or Pd, Ag, Sn, Pt or Ge on modenite.Mainly as hydrogenation metal, its activity is subjected to the control of Sn, Ge metal, to improve the performance of catalyst for nickel or palladium in this patent.
In the above-mentioned document, all include toluene aromatic hydrocarbons in the fresh feed of use, lower, the less stable of the yield of purpose product when perhaps having only heavy arene in the reaction feed, technical-economic index and unreasonable problem such as feasible, thus limit its industrializing implementation.
Summary of the invention
Technical problem to be solved by this invention is that what to exist in the prior art is raw material with carbon nine and above heavy arene thereof, the purpose product yield is low during the preparation light aromatics, problems such as the easy coking and deactivation of catalyst provide a kind of new catalyst with carbon nine and above heavy arene volume increase C8 aronmatic thereof.It is raw material with carbon nine and above heavy aromatics thereof only that this catalyst is used for, and toluene and/or benzene that reaction is generated separate in the Returning reactor charging of back, carry out toluene and/or benzene and C 9 +When disproportionation and transalkylation reaction take place A, have dimethylbenzene productive rate height, catalyst is difficult for the characteristics of inactivation.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of transalkylation catalyst that increases production C8 aronmatic wherein comprises following component in parts by weight:
1) SiO 2/ Al 2O 3Mol ratio is 20～90 parts of 10～100 h-type zeolites;
2) oxide of platinum is 0.001～5 part;
3) be selected from tin or plumbous oxide and composition thereof 0.001-15 part;
4) be selected from 0.02～5 part of cerium, zirconium, lanthanum or cobalt;
5) binding agent is 10～80 parts.
In the technique scheme, the h-type zeolite preferred version is selected from least a among β zeolite, modenite, ZSM-12 or the ZSM-5; In parts by weight, the oxide consumption preferable range of platinum is 0.01～2 part; Tin or plumbous oxide consumption preferable range are 0.05～5 part; The oxide consumption consumption preferable range of cerium, zirconium, lanthanum or cobalt is 0.05～3; Binding agent is selected from aluminium oxide or silica.
The Preparation of catalysts method is through dipping or ion-exchange or mixing or mediate extrusion, after 350～600 ℃ of roastings make by h-type zeolite, aluminium oxide and employed slaine among the present invention.
Catalyst of the present invention uses fixed bed reactors to carry out reactivity worth and investigates.25 millimeters of reactor inside diameter φ, 1200 millimeters of length, stainless steel.Adopt electrical heating, temperature is controlled automatically.5 millimeters beades of reactor bottom filling φ are as supporter, filling catalyst 20 grams in the reactor, and 5 millimeters beades of top filling φ are made for the usefulness of raw material preheating and vaporization.Fresh C in the raw material 9 +A and recycle feed toluene and/or benzene mix with hydrogen, from top to bottom by beds, transalkylation and/or dealkylation take place, and generate C 8More rudimentary aromatic hydrocarbons such as A, and alkane such as a small amount of methane, ethane, propane, butane.The weight content of carbon ten and above heavy arene thereof can be preferably 3～20% up to 0～30% in the reaction raw materials, more preferably 5～15% (weight).
Raw material C 9 +A derives from the petrochemical industry Aromatic Hydrocarbon United Plant, and test data is calculated as follows.
Figure C20061002509500051
Figure C20061002509500052
Catalyst of the present invention, because added the oxide of platinum in catalyst, this catalyst is applicable to that carbon nine and above heavy arene thereof are the disproportionation and the transalkylation reaction of raw material, and has dimethylbenzene productive rate height, the characteristics that catalyst is difficult for inactivation have obtained better technical effect.
The invention will be further elaborated below by embodiment.
The specific embodiment
[embodiment 1]
Use Na 2O content is less than 0.15% (weight), SiO 2/ Al 2O 3Ammonium type modenite powder 66.7 gram and the Na of molecular proportion 21.5 2O content is less than the α-Al of 0.15% (weight) 2O 3H 2O 57.1 grams evenly mix, and are made into the aqueous solution with chloroplatinic acid then and flood.Powder behind the dipping adds the dilute nitric acid solution of plumbi nitras, cerous nitrate again, fully mediates evenly, carries out extruded moulding, catalyst A is made in roasting.
[embodiment 2]
Use Na 2O content is less than 0.15% (weight), SiO 2/ Al 2O 3Ammonium type modenite powder 66.7 gram and the Na of molecular proportion 25.9 2O content is less than the α-Al of 0.15% (weight) 2O 3H 2O 57.1 grams evenly mix, and add a certain amount of dilute nitric acid solution, zirconium oxychloride and stannous chloride then, fully mediate evenly, carry out extruded moulding, roasting, flood platinum acid chloride solution again, and catalyst B is made in roasting.
[embodiment 3]
With certain density chlorination four ammonia platinum or nitric acid four ammonia platinum solution to Na 2O content is less than 0.15% (weight), SiO 2/ Al 2O 3The ammonium type modenite of molecular proportion 18.9 exchanges, and takes by weighing dried powder 66.7 gram and Na after the oven dry 2O content is less than the α-Al of 0.15% (weight) 2O 3H 2O 57.1 gram evenly mixes, and adds a certain amount of dilute nitric acid solution, lead nitrate solution and lanthanum nitrate then, fully mediates evenly, carries out extruded moulding, catalyst C is made in roasting.
[embodiment 4]
Use Na 2O content is less than 0.15% (weight), SiO 2/ Al 2O 3Ammonium type β powder 66.7 gram and the Na of molecular proportion 25.6 2O content is less than the α-Al of 0.15% (weight) 2O 3H 2The even mixing of O 57.1 grams adds a certain amount of dilute nitric acid solution, platinum acid chloride solution and stannous chloride solution then, fully mediates evenly, carries out extruded moulding, roasting, floods cobalt acetate, roasting again, makes the catalyst D of different metal content.
[embodiment 5]
Use Na 2O content is less than 0.15% (weight), 8iO 2/ Al 2O 3Ammonium type β powder 66.7 gram and the Na of molecular proportion 25.6 2O content is less than the α-Al of 0.15% (weight) 2O 3H 2The even mixing of O 57.1 gram adds a certain amount of dilute nitric acid solution, platinum acid chloride solution and stannous chloride, zirconyl chloride solution then, fully mediates evenly, carries out the catalyst E that extruded moulding, roasting are made different metal content.
[embodiment 6]
Use Na 2O content is less than 0.15% (weight), SiO 2/ Al 2O 3Ammonium type β powder 66.7 gram and the Na of molecular proportion 25.6 2O content is less than the α-Al of 0.15% (weight) 2O 3H 2The even mixing of O 57.1 grams adds a certain amount of dilute nitric acid solution, platinum acid chloride solution and stannous chloride solution then, fully mediates evenly, carries out extruded moulding, roasting, floods cobalt acetate solution, roasting again, makes the catalyst F of different metal content.
[embodiment 7]
Use Na 2O content is less than 0.15% (weight), SiO 2/ Al 2O 3The ammonium type modenite of molecular proportion 18.9 and the mixed-powder of β 66.7 gram and Na 2O content is less than the α-Al of 0.15% (weight) 2O 3H 2O 57.1 gram evenly mixes, and adds a certain amount of dilute nitric acid solution, platinum acid chloride solution and plumbi nitras, lanthanum nitrate hexahydrate then, fully mediates evenly, carries out extruded moulding, catalyst G is made in roasting.
[embodiment 8]
With certain density platinum acid chloride solution dipping Na 2O content is less than 0.15% (weight), SiO 2/ Al 2O 3The ammonium type ZSM-5 of molecular proportion 25.6 and the mixed-powder of β 66.7 grams, after oven dry, the roasting with Na 2O content is less than the α-Al of 0.15% (weight) 2O 3H 2O 57.1 gram evenly mixes, and adds chemical pure dilute nitric acid solution and lanthanum nitrate, stannous chloride solution of tin again, fully mediates evenly, carries out extruded moulding, catalyst H is made in roasting.
[embodiment 9]
Use Na 2O content is less than 0.15% (weight), SiO 2/ Al 2O 3The ammonium type modenite of molecular proportion 18.9 and the mixed-powder of ZSM-5 66.7 gram and Na 2O content is less than the α-Al of 0.15% (weight) 2O 3H 2O 57.1 grams evenly mix, and add a certain amount of dilute nitric acid solution, chlorination four ammonia platinum solution and stannous chloride solutions then, fully mediate evenly, carry out extruded moulding, roasting, flood cobalt acetate solution, roasting again, make catalyst I.
[embodiment 10]
With 33 gram Na 2O content is less than 0.15% (weight), SiO 2/ Al 2O 3The ZSM-12 zeolite of molecular proportion 18.9 and 33.6 gram Na 2O content is less than 0.15% (weight), SiO 2/ Al 2O 3The β of molecular proportion 24.9 and Na 2O content is less than the α-Al of 0.15% (weight) 2O 3H 2O 57.1 gram evenly mixes, and adds a certain amount of dilute nitric acid solution, chlorination four ammonia platinum solution and lead nitrate solution then, fully mediates evenly, carries out extruded moulding, roasting, floods cerous chlorate solution again, catalyst J is made in roasting.
[embodiment 11]
Use Na 2O content is less than 0.15% (weight), SiO 2/ Al 2O 3Ammonium type modenite powder 66.7 gram and the Na of molecular proportion 21.5 2O content evenly mixes less than silica 57.1 grams of 0.05% (weight), is made into the aqueous solution with chloroplatinic acid then and floods.After the oven dry of powder behind the dipping again with the dilute nitric acid solution of stannous chloride, zirconium oxychloride, fully mediate evenly, carry out extruded moulding, catalyst K is made in roasting.
[embodiment 12]
Use Na 2O content is less than 0.15% (weight), SiO 2/ Al 2O 3Ammonium type β powder 66.7 gram and the Na of molecular proportion 25.6 2O content is less than the α-Al of 0.15% (weight) 2O 3H 2The even mixing of O 57.1 grams adds a certain amount of platinum acid chloride solution then and lead nitrate solution is carried out incipient impregnation, fully mediates with the dilute nitric acid solution of lanthanum nitrate after the oven dry again, carries out extruded moulding, roasting, makes the catalyst L that contains three kinds of metals.
The catalyst that makes with embodiment 1～12 carries out disproportionation and the active investigation of transalkylation reaction on the fixed bed reaction evaluating apparatus.Loaded catalyst is 20 grams, and weight space velocity is 2.5 hours -1, 375 ℃ of reaction temperatures, reaction pressure 3.0MPa, hydrogen hydrocarbon molecule are than 3.5, and fresh feed is C 9 +A, wherein C in the raw material 9A weight consists of: propyl benzene 3.45%, first and second benzene 35.14%, trimethylbenzene 63.40%, C 10 +Hydrocarbon weight consists of: diethylbenzene 2.33%, dimethyl ethylbenzene 26.96%, methyl propyl benzene 2.32%, durene 27.84%, methyl naphthalene 14.49%, dimethylnaphthalene 11.16%, other 12.90%, evaluation result such as table 1.
Table 1. evaluation result (unit: weight)
Embodiment Catalyst Zeolite Binding agent Pt/％ M 2/％ M 3/％ Conversion ratio/% Mixed XYLENE selectivity/%
1 A Modenite Aluminium oxide 1.0 Pb/2.0 Ce/1.5 74.55 54.56
2 B Modenite Aluminium oxide 0.15 Sn/0.32 Zr/0.25 65.21 75.36
3 C Modenite Aluminium oxide 0.16 Pb/0.35 La/0.30 63.90 78.17
4 D β Aluminium oxide 0.8 Sn/1.6 Co/1.2 66.78 65.84
5 E β Aluminium oxide 0.23 Sn/0.50 Zr/0.4 68.35 82.87
6 F β Aluminium oxide 0.1 Sn/0.5 Co/1.5 54.57 84.91
7 G Modenite+β zeolite Aluminium oxide 2.0 Pb/4.5 La/2.0 70.91 59.35
8 H ZSM-5+ β zeolite Aluminium oxide 1.5 Sn/1.5 La/3.0 73.26 61.19
9 I Modenite+ZSM-5 Aluminium oxide 0.8 Sn/1.5 Co/1.0 69.48 78.18
10 J ZSM-12+ β zeolite Aluminium oxide 0.8 Pb/1.5 Ce/1.0 75.64 82.06
11 K Modenite Silica 0.15 Sn/0.32 Zr/ 68.35 80.90
12 L β Aluminium oxide 0.16 Pb/0.35 La/0.75 69.42 83.51
Evaluation result shows, metal or the oxide and at least a tin that is selected from of load platinum on h-type zeolite that the present invention makes, cerium, lanthanum, the catalyst that metal in lead or the cobalt or oxide are made, this catalyst can be with carbon nine and above heavy aromatic hydrocarbon light and transalkylation reaction, improve the conversion ratio of carbon nine and above aromatic hydrocarbons thereof effectively, and by adding metal or the oxide that platinum is had the control activity, under the prerequisite that suitably suppresses catalysqt deactivation, can reach best mixed xylenes productive rate, the characteristics that under the big situation of carbon ten and above aromatic hydrocarbons treating capacity thereof, can keep catalyst activity for a long time, simultaneously, the ability that also has stronger anti-sulphur poisonous substance.
The invention is not restricted to above embodiment, those skilled in the art can make various changes and distortion according to the present invention, only otherwise break away from spirit of the present invention, all should belong to scope of the present invention.

Claims (6)

1, a kind of transalkylation catalyst that increases production C8 aronmatic comprises following component in parts by weight:
1) SiO 2/ Al 2O 3Mol ratio is 20～90 parts of 10～100 h-type zeolites;
2) oxide of platinum is 0.001～5 part;
3) be selected from tin or plumbous oxide and composition thereof 0.001-15 part;
4) be selected from 0.02～5 part of cerium, zirconium, lanthanum or cobalt.
5) binding agent is 10～80 parts.
2,, it is characterized in that h-type zeolite is selected from least a among β zeolite, modenite, ZSM-12 or the ZSM-5 according to the transalkylation catalyst of the described volume increase C8 aronmatic of claim 1.
3,, it is characterized in that the oxide consumption in parts by weight platinum is 0.01～2 part according to the transalkylation catalyst of the described volume increase C8 aronmatic of claim 1.
4,, it is characterized in that in parts by weight tin or plumbous oxide are 0.05～5 part in the catalyst according to the transalkylation catalyst of the described volume increase C8 aronmatic of claim 1.
5,, it is characterized in that in parts by weight the oxide consumption of cerium, zirconium, lanthanum or cobalt is 0.05～3 part in the catalyst according to the transalkylation catalyst of the described volume increase C8 aronmatic of claim 1.
6,, it is characterized in that binding agent is selected from aluminium oxide or silica gel according to the transalkylation catalyst of the described volume increase C8 aronmatic of claim 1.
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KR101743293B1 (en) * 2010-10-22 2017-06-05 에스케이이노베이션 주식회사 Hydrocracking catalyst for preparing valuable light aromatic hydrocarbons from polycyclic aromatic hydrocarbons
CN106316738B (en) * 2015-06-19 2019-06-11 中国石油化工股份有限公司 The composition that the method and this method for producing aromatic hydrocarbons obtain
CN106582792B (en) * 2015-10-14 2019-07-05 中国石油化工股份有限公司 The catalyst of benzene and ethane alkylated reaction
CN106582790B (en) * 2015-10-14 2019-01-25 中国石油化工股份有限公司 The catalyst reacted is alkylated with ethane for benzene
CN106588533B (en) * 2015-10-19 2020-02-07 中国石油化工股份有限公司 Method for increasing yield of xylene by lightening heavy aromatics
CN108786902B (en) * 2017-05-02 2021-03-05 中国石油化工股份有限公司 Heavy aromatic hydrocarbon conversion catalyst and preparation method thereof

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