CN101190864A - Catalyst for preparing ethene and propene by catalysis cracking - Google Patents

Catalyst for preparing ethene and propene by catalysis cracking Download PDF

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CN101190864A
CN101190864A CNA2006101185320A CN200610118532A CN101190864A CN 101190864 A CN101190864 A CN 101190864A CN A2006101185320 A CNA2006101185320 A CN A2006101185320A CN 200610118532 A CN200610118532 A CN 200610118532A CN 101190864 A CN101190864 A CN 101190864A
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zsm
molecular sieve
propylene
catalyst
zeolite
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CN101190864B (en
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陈亮
谢在库
马广伟
胡永君
姚晖
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
China Petrochemical Corp
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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Abstract

The invention relates to a catalyst used for producing ethylene and propylene by catalytic cracking, and mainly solves the problem that temperature required by the catalyst is high while selectivity to the ethylene and the propylene is low in the existing catalytic cracking reaction. The invention adopts the technical proposal of sieving ZSM-5/beta zeolite accrete molecular as catalyst, and SiO2/Al2O3 mole ratio of which is more than 100 to 500, thereby properly solving the problem. The invention is used for industrial production of the ethylene and the propylene by the catalytic cracking.

Description

The catalyzer that is used for preparing ethylene propylene from catalytic pyrolysis
Technical field
The present invention relates to a kind of catalyzer that is used for preparing ethylene propylene from catalytic pyrolysis.
Background technology
Along with the development of society, the market requirement of China's ethylene, propylene sharply increases, and the import volume of ethylene, propylene and derived product thereof increases year by year, and the home products share of market is less than half.Whole world ethene is raw material with petroleum naphtha (or ethane) mainly at present, adopts steam heat cracking technique (under the temperature about 800 ℃) production, and its output surpasses 90% of ultimate production.Catalytic pyrolysis is compared with the steam heat cracking, and this process reaction temperature is than low 50～200 ℃ approximately of standard scission reactions, and therefore than common steam cracking less energy consumption, cracking furnace pipe inwall coking rate will reduce, thereby but prolong operation cycle increases the boiler tube life-span; Carbon emission also can reduce, and can adjust the product mix flexibly, can increase the total recovery of ethene and propylene, and production cost of ethylene reduces significantly.
U.S. Pat P6211104 and domestic patent CN1504540A adopt a kind of 10～70 weight % clays that contain, 5～85 weight % inorganic oxides, 1～50 weight % molecular sieve is formed catalyzer, to the various raw materials of traditional steam heat cracked, the activity, the especially ethene that well are converted into light olefin have been demonstrated.With molecular sieve be by 0～25 weight %Y zeolite of high silica alumina ratio or have the ZSM molecular sieve of MFI structure, form by P, Al, Mg or Ca dipping, but the ethylene, propylene selectivity of catalyzer and yield are not high.
Japan Asahi Chemical Industry (patent CN1274342A) has announced that a kind of high silica alumina ratio, the aperture molecular sieve between 0.5～0.65 is a catalyzer, be the feedstock production ethylene, propylene with the light hydrocarbons that contains alkene, but the ethylene, propylene yield is lower.
Exxon Mobil (00816642.0) announces that a kind of aperture of a kind of usefulness contains the hydrocarbon raw material of petroleum naphtha less than the zeolite treatment of 0.7 nanometer, produces ethylene, propylene between 550-600 ℃, and conversion of raw material is lower.
Mobil Oil Corp. (CN1413244A) has announced that a kind of mesopore phosphate material with modification is that catalyzer and primary catalytic pyrolysis material combine, the hydrocarbon raw material of catalytic pyrolysis sulfur-bearing prepares micromolecular hydrocarbon mixture, but the use temperature of catalyzer, conversion of raw material and product yield are all lower.
Summary of the invention
Technical problem to be solved by this invention is that the catalyst activity that uses in the existing catalytic cracking reaction is lower, and the problem that the yield of ethylene, propylene is lower, use temperature is high provides a kind of new catalyzer that is used for preparing ethylene propylene from catalytic pyrolysis.This catalyzer has catalytic activity height, ethylene, propylene yield height, advantage that use temperature is low.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of catalyzer that is used for preparing ethylene propylene from catalytic pyrolysis, catalyzer are SiO 2/ Al 2O 3Mol ratio is the coexisting molecular sieve of＞100～500 ZSM-5/ β zeolite.
In the technique scheme, the SiO of ZSM-5/ beta zeolite coexisting molecular sieve 2/ Al 2O 3Mol ratio is that preferable range is＞100～200, and more preferably scope is＞100～150.In the ZSM-5/ beta zeolite coexisting molecular sieve by weight percentage the content preferable range of ZSM-5 molecular sieve be 20～99.5%, more preferably scope is 60～99%.
At least a as in silicate, metasilicate sodium or the silicon sol of the preparation coexisting molecular sieve silicon source of using, the aluminium source is at least a in aluminium salt or the aluminate, template is at least a in quadrol, ethamine, n-Butyl Amine 99, triethylamine, 4-propyl bromide, TPAOH, tetraethyl ammonium hydroxide or the tetraethylammonium bromide, and the pH value of regulating colloidal sol with diluted acid is 10～13.
The synthetic method of coexisting molecular sieve is, get the silicon source and the aluminium source of aequum by material proportion, make solution with dissolved in distilled water respectively, then two kinds of solution are mixed, the powerful stirring adds the template of aequum then, stirs after 30 minutes with rare acid for adjusting pH value in 10～13 scopes, add the β zeolite as crystal seed, supply distilled water again.Colloidal sol is put into autoclave, control required temperature crystallization after 10～100 hours, take out 4 hours, 550 ℃ roastings of 2 times, 120 ℃ oven dry of washing 3 hours, can obtain ZSM-5/ beta zeolite coexisting molecular sieve.With concentration is 5% ammonium nitrate solution, and 70 ℃ of exchanges twice, roasting then makes hydrogen type molecular sieve after repeating twice, then compressing tablet, break into pieces, sieve, get 20～40 purpose particles and put into fixed-bed reactor and check and rate.
Catalyzer involved in the present invention, owing to adopted the coexisting molecular sieve that contains ZSM-5 molecular sieve and β zeolite simultaneously, this molecular sieve is owing to contain acid strong β zeolite, so its acid amount is bigger, acidity is stronger, is suitable for the higher alkane cracking of cracking energy.Because coexisting molecular sieve contains multistage pore canal, can handle the different mixture material of molecular diameter.Because the degree that comes to the surface, acidity, duct and the specific surface of coexisting molecular sieve and having than big difference of two kinds of molecular sieve mechanically mixing so catalytic performance is preferably arranged, are used for the naphtha catalytic pyrolysis preparing ethylene propylene reaction, with C 4～C 10The petroleum naphtha of hydrocarbon is raw material (the raw material physical index sees Table 1), is 12 millimeters down examination of fixed-bed reactor normal pressure with diameter, and range of reaction temperature is 600～700 ℃, and reaction pressure is 0.001MPa～0.5MPa, and mass space velocity is 0.25～2 hour -1, water/stock oil weight ratio is that ethene and propylene total recovery can reach 51.94% and obtain better technical effect under 1～4: 1 the condition.
Description of drawings
Fig. 1 is the XRD figure spectrum of ZSM-5/ beta zeolite coexisting molecular sieve
Curve 1 is the XRD diffracting spectrum of FH-1 sample among Fig. 1, and curve 2 is the XRD diffracting spectrum of FH-12 sample.
Table 1 feed naphtha index
Project Data
Density (20 ℃) kilogram/rice 3 704.6
Boiling range is boiling range ℃ just 40
Whole boiling range ℃ 160
Saturated vapor pressure (20 ℃) kPa 50.2
Alkane % (weight %) 65.18
Normal paraffin % (weight %) in the alkane ＞32.5
Naphthenic hydrocarbon % (weight %) 28.44
Alkene % (weight %) 0.17
Aromatic hydrocarbons % (weight %) 6.21
The present invention is further elaborated below by embodiment.
Embodiment
[embodiment 1]
Get 284 gram Starsos, become solution A with 300 gram dissolved in distilled water, get 5.56 gram Tai-Ace S 150, make solution B with 100 gram distilled water, B solution is slowly poured in the A solution, the powerful stirring, add 12.2 gram quadrols and 29.4 gram tetraethyl ammonium hydroxides (mixed templates is designated as M) then, after stirring for some time, regulate the pH value 11 with dilute sulphuric acid, the mole proportioning of control colloidal sol is: Si: Al: M: H 2O=1: 0.0167: 0.4: 40, add 2.8 gram β zeolite seed crystals, mixing solutions is put into autoclave, 160 ℃ of insulations 40 hours, take out 4 hours, 550 ℃ roastings of 2 times, 120 ℃ oven dry of washing 3 hours then, make ZSM-5/ beta zeolite coexisting molecular sieve, the XRD diffracting spectrum is shown in curve among Fig. 11, with the XRD diffraction quantitatively as can be known in the coexisting molecular sieve ZSM-5 weight percentage be 94.6%, the β zeolite is 5.4%.It with concentration 5% ammonium nitrate solution, twice of 70 ℃ of exchange, 550 ℃ of roastings are 3 hours then, make Hydrogen ZSM-5/ beta zeolite coexisting molecular sieve after repeating twice, then compressing tablet, break into pieces, sieve, getting 20～40 purpose particles and put into fixed-bed reactor, is that 650 ℃, reaction pressure are that 0.02MPa, weight space velocity are 0.5 hour in temperature of reaction -1, water/stock oil weight ratio is to check and rate under 3: 1 the condition, the results are shown in Table 4.
[embodiment 2～4]
According to the method for embodiment 1, the pH of control solution is respectively 10.5,11.5 and 12, synthesizes ZSM-5/ beta zeolite coexisting molecular sieve respectively, is designated as FH-2 respectively, FH-3, FH-4.The ratio of ZSM-5 and β zeolite sees Table 3.Method examination according to embodiment 1 the results are shown in Table 4.
[embodiment 5～11]
According to the method for embodiment 1, the different mole proportionings of control solution, the two constant rate in the mixed templates, synthetic ZSM-5/ beta zeolite coexisting molecular sieve sees Table 2 respectively, and the ratio of ZSM-5 and β zeolite sees Table 3.Method examination according to embodiment 1 the results are shown in Table 4.
Table 2
Embodiment Solution mole proportioning Sample number into spectrum
Embodiment
5 Si∶Al∶M∶H 2O＝1∶0.005∶0.4∶40 FH-5
Embodiment 6 Si∶Al∶M∶H 2O＝1∶0.01∶0.4∶40 FH-6
Embodiment 7 Si∶Al∶M∶H 2O＝1∶0.0111∶0.4∶40 FH-7
Embodiment 8 Si∶Al∶M∶H 2O＝1∶0.0133∶0.4∶40 FH-8
Embodiment 9 Si∶Al∶M∶H 2O＝1∶0.0182∶0.4∶40 FH-9
Embodiment 10 Si∶Al∶M∶H 2O＝1∶0.0167∶0.2∶30 FH-10
Embodiment 11 Si∶Al∶M∶H 2O＝1∶0.0167∶0.5∶60 FH-11
[embodiment 12～15]
Method according to embodiment 1, the mole proportioning of control solution is identical, adding β zeolite seed crystal amount respectively is 5.68 grams, 11.3 grams, 22.6 grams and 28.4 grams, synthetic ZSM-5/ beta zeolite coexisting molecular sieve, be designated as FH-12, FH-13, FH-14, FH-15 respectively, the XRD diffracting spectrum of FH-12 is shown in curve among Fig. 11, and the ratio of ZSM-5 and β zeolite sees Table 3.Method examination according to embodiment 1 the results are shown in Table 4.
[embodiment 16～19]
According to the method for embodiment 1, the mole proportioning of control solution is identical, and mixed templates mol ratio 1: 1 or 1: 1: 1 (selecting three kinds of template for use) are used n-Butyl Amine 99 and tetraethylammonium bromide successively respectively; Ethamine, quadrol and tetraethyl ammonium hydroxide; 4-propyl bromide and tetraethyl ammonium hydroxide; TPAOH, n-Butyl Amine 99 and tetraethyl ammonium hydroxide; Synthetic ZSM-5/ beta zeolite coexisting molecular sieve is designated as FH-16, FH-17, FH-18, FH-19 respectively, and the ratio of ZSM-5 and β zeolite sees Table 3.Method examination according to embodiment 1 the results are shown in Table 4.
[embodiment 20～21]
According to the method for embodiment 1, the mole proportioning of control solution is identical, and crystallization temperature is set to 150 ℃ and 170 ℃ respectively, has synthesized ZSM-5/ beta zeolite coexisting molecular sieve respectively, is designated as FH-20, FH-21, and the ratio of ZSM-5 and β zeolite sees Table 3.Method examination according to embodiment 1 the results are shown in Table 4.
Table 3
Sample number into spectrum Contain ZSM-5 ratio (weight %) Contain β zeolite ratio (weight %)
FH-1 94.6 5.4
FH-2 98.7 1.3
FH-3 92.3 7.7
FH-4 86.4 13.6
FH-5 99.3 0.7
FH-6 99.0 1.0
FH-7 90.1 9.9
FH-8 95.6 4.4
FH-9 98.2 1.8
FH-10 93.4 6.6
FH-11 95.3 4.7
FH-12 89.8 10.2
FH-13 75.6 24.4
FH-14 63.7 36.3
FH-15 50.5 49.5
FH-16 95.2 4.8
FH-17 96.1 3.9
FH-18 94.9 5.1
FH-19 96.4 3.6
FH-20 93.7 6.3
FH-21 95.1 4.9
Table 4
Sample number into spectrum Yield of ethene (weight %) Propene yield (weight %) Total recovery (weight %)
FH-1 23.47 26.25 49.72
FH-4 21.25 22.53 43.78
FH-6 25.11 26.83 51.94
FH-8 24.54 25.37 49.91
FH-12 22.06 24.32 46.38
FH-14 20.52 21.12 41.64
FH-18 24.57 25.73 50.30
FH-20 23.27 25.16 48.43
[comparative example 1]
With the synthesis mode of embodiment 1, do not add the β zeolite seed crystal, template is only used quadrol, synthetic pure ZSM-5 molecular sieve, making the catalyzer postscript is C-1, checks and rates according to the mode of embodiment 1, the results are shown in Table 5.
[comparative example 2]
In the mode of embodiment 1, template is only used tetraethyl ammonium hydroxide, adds 5.68 gram β zeolite seed crystals, synthetic pure β zeolite, and making the catalyzer postscript is C-2, checks and rates according to the mode of embodiment 1, the results are shown in Table 5.
[comparative example 3]
Prepare the two mechanical mixture in the ratio of ZSM-5 among the embodiment 12 and β zeolite, make catalyzer, be designated as C-3, check and rate, the results are shown in Table 5 by the mode of embodiment 1.
Table 5
Sample Yield of ethene (weight %) Propene yield (weight %) Total recovery (weight %)
C-1 21.84 22.62 44.46
C-2 19.12 21.32 40.44
C-3 22.47 23.44 45.91

Claims (5)

1. a catalyzer that is used for preparing ethylene propylene from catalytic pyrolysis is characterized in that catalyzer is SiO 2/ Al 2O 3Mol ratio is＞100～500 ZSM-5/ beta zeolite coexisting molecular sieve.
2. according to the described catalyzer that is used for preparing ethylene propylene from catalytic pyrolysis of claim 1, it is characterized in that the SiO of ZSM-5/ beta zeolite coexisting molecular sieve 2/ Al 2O 3Mol ratio is＞100～200.
3. according to the described catalyzer that is used for preparing ethylene propylene from catalytic pyrolysis of claim 2, it is characterized in that the SiO of ZSM-5/ beta zeolite coexisting molecular sieve 2/ Al 2O 3Mol ratio is＞100～150.
4. according to the described catalyzer that is used for preparing ethylene propylene from catalytic pyrolysis of claim 1, it is characterized in that in the ZSM-5/ beta zeolite coexisting molecular sieve that the content of ZSM-5 molecular sieve is 20～99.5% by weight percentage.
5. according to the described catalyzer that is used for preparing ethylene propylene from catalytic pyrolysis of claim 4, it is characterized in that in the ZSM-5/ beta zeolite coexisting molecular sieve that the content of ZSM-5 molecular sieve is 60～99% by weight percentage.
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9227181B2 (en) 2011-09-13 2016-01-05 Basf Corporation Catalyst to increase propylene yields from a fluid catalytic cracking unit
US10723631B2 (en) 2018-03-14 2020-07-28 Saudi Arabian Oil Company Methods of producing composite zeolite catalysts for heavy reformate conversion into xylenes
US10723630B2 (en) * 2018-03-14 2020-07-28 Saudi Arabian Oil Company Methods of producing composite zeolite catalysts for heavy reformate conversion into xylenes
US10927059B2 (en) 2018-03-14 2021-02-23 Saudi Arabian Oil Company Catalyst for converting heavy reformate to produce BTX compounds
US11091413B2 (en) 2018-03-14 2021-08-17 Saudi Arabian Oil Company Methods of heavy reformate conversion into aromatic compounds
CN113830778A (en) * 2020-06-24 2021-12-24 中国石油化工股份有限公司 ZSM-5/beta core-shell type molecular sieve and synthetic method and application thereof

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1259293C (en) * 2003-10-27 2006-06-14 中国石油化工股份有限公司 Method for producing propene
CN1332759C (en) * 2004-01-19 2007-08-22 中国石油化工股份有限公司 Method for preparing ZSM-5 and beta zeolite mixed crystal material

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9227181B2 (en) 2011-09-13 2016-01-05 Basf Corporation Catalyst to increase propylene yields from a fluid catalytic cracking unit
US10723631B2 (en) 2018-03-14 2020-07-28 Saudi Arabian Oil Company Methods of producing composite zeolite catalysts for heavy reformate conversion into xylenes
US10723630B2 (en) * 2018-03-14 2020-07-28 Saudi Arabian Oil Company Methods of producing composite zeolite catalysts for heavy reformate conversion into xylenes
CN112105457A (en) * 2018-03-14 2020-12-18 沙特阿拉伯石油公司 Process for producing composite zeolite catalyst for converting heavy reformate to xylenes
US10927059B2 (en) 2018-03-14 2021-02-23 Saudi Arabian Oil Company Catalyst for converting heavy reformate to produce BTX compounds
US11091413B2 (en) 2018-03-14 2021-08-17 Saudi Arabian Oil Company Methods of heavy reformate conversion into aromatic compounds
US11472755B2 (en) 2018-03-14 2022-10-18 Saudi Arabian Oil Company Methods of heavy reformate conversion into aromatic compounds
CN112105457B (en) * 2018-03-14 2023-10-24 沙特阿拉伯石油公司 Process for producing composite zeolite catalyst for converting heavy reformate to xylenes
CN113830778A (en) * 2020-06-24 2021-12-24 中国石油化工股份有限公司 ZSM-5/beta core-shell type molecular sieve and synthetic method and application thereof
CN113830778B (en) * 2020-06-24 2023-06-09 中国石油化工股份有限公司 ZSM-5/beta core-shell molecular sieve and synthesis method and application thereof

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