CN104672046A - Method of increasing ethylene and propylene yields by freshening C-4 olefins in catalytic cracking or pyrolysis process after separation - Google Patents
Method of increasing ethylene and propylene yields by freshening C-4 olefins in catalytic cracking or pyrolysis process after separation Download PDFInfo
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Abstract
The invention discloses a method of increasing ethylene and propylene yields by freshening C-4 olefins in catalytic cracking or pyrolysis process after separation. The technical method is as follows: 1) directly conveying etherified C-4 into a reactor, and firstly reacting with acetic acid under the action of a catalyst to generate sec-butyl acetate; 2) carrying out conventional distillation on materials at the outlet of the reactor to obtain alkane at the tower top and the sec-butyl acetate at the tower bottom; 3) using the material at the tower bottom as a raw material for increasing the propylene yield by cracking, and carrying out a cleavage reaction on the material in a catalytic cracking riser reactor. A mass separating agent (acetic acid) generating no influence on subsequent reaction and needing no separation is added in the invention to strengthen the separation process of alkane and olefin, and under the condition of not separating the mass separating agent, high-selectivity freshening is carried out on olefin components with high reaction activity to solve the problem of efficient separation of alkane and olefin in a traditional manufacturing process and achieve the target of increasing the propylene yield by freshening. The process can be used for utilizing the original device to improve the olefin utilization rate under the condition of small investment.
Description
Technical field
The present invention relates to a kind of method C 4 olefin being separated rear freshening increasing output of ethylene and propylene in catalytic cracking or cracking process, belong to liquefied gas deep processing and petroleum resources efficiency utilization field, be especially applicable to using the mixed c 4 of catalytic cracking unit by-product to produce propylene.
Background technology
Propylene is important petrochemical materials, and along with continually developing of propylene downstream derivative thing new variety, propylene is in great demand in recent years.At present, the propylene of China 54% derives from the steam cracking of petroleum naphtha, and 42% propylene is catalytic cracking unit by-product.Contrast with in world wide, China's catalytic cracking by-product propylene occupies an important position.Domestic catalytic cracking unit is many, and adaptability to raw material is strong, and it is still huge that catalytic cracking process produces propylene potentiality.By catalytic cracking unit, be propylene by C 4 olefin Efficient Conversion be an important channel of improving carbon four resource utilization, increasing economic efficiency.
CN102372608A discloses a kind of Application way of mixed c 4, and in this technique, after ether, carbon four carries out extracting rectifying, obtains mixed butanes and mixed butene, and mixed butene produces the raw material of propylene as scission reaction.In this method, extracting rectifying process adopts the double-column process of extraction tower and stripping tower combination, and the extraction liquid after regeneration loops back extraction tower, and technology controlling and process is complicated; Select acetonitrile comparatively large as toxicity during extraction agent, labor protection condition is harsh; Often process 1 ton of carbon four and produce 300 ~ 400kg containing ethane nitrile wastewater, seriously polluted.
CN102603454A discloses a kind of method of mixed c 4 separating treatment.According to this processing method, mixed c 4 enters the extracting rectifying device be made up of Trimethylmethane extraction tower, normal butane extraction tower and stripping tower, obtains high-purity isobutane, normal butane and butylene product after deviating from carbon three, carbon five component by conventional distillation method.Butylene product can be used for freshening, and propylene is produced in cracking.This technique sepn process needs 5 towers to complete altogether, and extraction column plate reaches 70 ~ 100 pieces; Extraction agent through stripper regenerates divides two-way circulation to enter Trimethylmethane tower, normal butane tower, and extraction rectification technique is complicated, not easy to operate; When adopting morpholine/N-N-formyl morpholine N-mixed solution as extraction agent, stripping bottom temperature is higher, easily cause extraction agent coking loss, and extraction agent price is higher; Investment, process cost is all higher.
CN101928195A discloses the method for a kind of carbon four comprehensive utilization.Mixed c 4 is produced MTBE through catalytic distillation by this technique, after ether, carbon four carries out conventional distillation operation after separating methanol process: after ether, carbon four introduces the first rectifying tower, tower top isolates Trimethylmethane, materials at bottom of tower enters Second distillation column, Second distillation column tower top is separated and obtains high purity butene-1, and at the bottom of tower, 2-butylene concentration is also improved.Adopt the exemplary device of this technology, two rectifiying plate numbers all nearly 200 pieces, be often separated 1 ton of carbon four and consume steam 3.8 tons.Greatly, energy consumption is high for facility investment, process cost.
CN102071054A discloses a kind of method of heavy crude and the cracking of lighter hydrocarbons co-catalysis, and carbon after ether four can be introduced in catalytic cracking riser reactor and carry out freshening by this technique, and normal butylenes is propylene.But this technique is owing to containing fractional saturation alkane in freshening lighter hydrocarbons, cause system loading comparatively large, olefin conversion is low, and process energy consumption is higher.
CN101381272A discloses a kind of method that methyl alcohol and C 4 olefin two-step approach prepare ethene and propylene.According to this processing method, first methyl alcohol, dme and carbon four and above alkene are carried out etherification reaction, then reaction outlet material is carried out scission reaction production ethene, propylene.But what by methanol-to-olefins and carbon four cracking, this technique mainly produced that two kinds, alkene reacts is coupled, and reaches and makes full use of heat, reduce the object of temperature of reaction.Do not relate to the sepn process of alkane and alkene in technological process, if adopt catalytic cracking unit to carry out scission reaction, be still difficult to solve alkane in system, accumulate the problem that device load is large, energy consumption is high caused.In addition, in process described by this patent, use dme to carry out etherificate (generate methyl alkyl ether and also have methyl alcohol) to carbon four and above alkene, then product is carried out the process of freshening, or using the steps necessary of methanol decomposition alkene as whole reaction process.
The technical process of the catalytic pyrolysis producing more propylene technology of the more employing in current domestic refinery: the liquefied gas of catalytic cracking unit output, remove after C2, C3, C5 through gas separation unit, enter ether-based device, be not separated without alkane/olefin containing carbon four after the ether of iso-butylene or the light benzine that is rich in alkene, directly return to catalytic cracking unit and carry out freshening.But because alkane is constantly accumulated in system, finally cause the olefin(e) centent carrying out freshening in system lower.So carbon four lower for some olefin content is discharged system by this process need, in the program, carbon four utilization ratio is lower, and system loading is large, and process energy consumption is high.
Above-mentioned technique relates to the separation problem of mixed c 4 alkane, alkene mostly, and current carbon four separating technology mainly contains conventional distillation technology and extraction and distillation technology.When adopting the method for conventional distillation to process carbon four, because in carbon four, each component boiling point of butylene, butane is close, conventional distillation method is separated exists reflux ratio greatly, and stage number is many, and energy consumption is high, the problem that operation investment cost is high.Butylene yield is there is low when adopting extraction and distillation technology; Flow process is complicated, operational difficulty; Extraction agent is mixed with in product separation butylene; Solvent ratio is large, the problems such as extraction agent usage quantity is large.
In sum, after exploitation ether, carbon four is converted in the technical process of propylene, and improving alkene utilization ratio and improving device benefit aspect needs to coordinate to consider.
Summary of the invention
The object of the invention is to provide a kind of method C 4 olefin being separated rear freshening increasing output of ethylene and propylene in catalytic cracking or cracking process on the basis of existing technology, effective recovery extraction and application method is lacked mainly for current many C 4 olefins as liquefied gas as fuel, there is provided a kind of and alkene and acetic acidreaction in carbon four or other lighter hydrocarbons are generated sec-butyl acetate, make to be easy between alkane with alkene be separated, then sec-butyl acetate is introduced catalytic cracking riser reactor and carry out scission reaction, the method for producing more propylene.The method Propylene Selectivity is high, energy consumption is low, can increase substantially the economy of carbon fourth class lighter hydrocarbons propylene enhancing technique.
For reaching above-mentioned target, the invention provides a kind of method of C 4 olefin highly selective freshening propylene enhancing, concrete grammar is:
1). alkene and acetic acidreaction: enter reactor packed with catalyst after the mixed c 4 material containing alkene mixes with acetic acid, temperature of reaction 30 ~ 200 DEG C, absolute pressure 0.3 ~ 6MPa, mass space velocity is 0.1 ~ 10h
-1, acetic acid: olefin molar feed ratio is react under 0.1 ~ 10:1 condition, generates sec-butyl acetate.Reactor outlet material enters step 2);
2). sepn process: from step 1) reactor outlet material mainly containing alkane, sec-butyl acetate, acetic acid, enter Dealkylater, only need carry out conventional distillation, tower top obtains mixed alkanes, and materials at bottom of tower enters into step 3);
3). scission reaction: from step 2) mainly enter in catalytic cracking riser reactor containing the dealkylate materials at bottom of tower of sec-butyl acetate, unreacted acetic acid, temperature of reaction 350 ~ 650 DEG C, absolute pressure 0.08 ~ 0.4MPa, reactant and catalyst exposure also react, and generate the low-carbon alkene comprising propylene.
Described step 1) reactor that adopts of alkene and acetic acidreaction is fixed-bed reactor or catalytic rectifying tower, can be set to a reactor or multiple tandem reactor, unreacting material also can reenter reactor cycles reaction.The catalyzer that this reaction process adopts is one or more in ion-exchange resin catalyst or its modified product, strong acidic ion liquid, the vitriol oil, carried heteropoly acid, Y zeolite or its modified product, ZSM molecular sieve or its modified product, SAPO molecular sieve or its modified product.All types of catalyzer can be used alone, and also can be combined as mixed catalyst by the mode of bonding or blending.Containing alkane, sec-butyl acetate in the outlet material of reactor, also unreacted acetic acid etc. may be had.
Described step 2) sepn process only need adopt simple conventional distillation to operate, and can realize being separated of alkane and sec-butyl acetate, acetic acid etc., dealkylate tower top isolates alkane, and materials at bottom of tower is primarily of sec-butyl acetate and unreacted acetic acid composition.
Main material boiling point (standard atmosphere pressure) in table 1, Dealkylater
| Component | Acetic acid | Sec-butyl acetate | Normal butane | Trimethylmethane |
| Boiling point DEG C | 117.9 | 112.3 | -0.5 | -11.72 |
In system, each typical material boiling point is known as shown in Table 1, alkane and sec-butyl acetate boiling-point difference comparatively large (close to 100 DEG C), boiling-point difference (shown in table 2) in carbon Four composition between alkane, alkene, be separated easily between component, comparatively the process energy consumption such as extraction and distillation technology is low, simple to operate.
Main material boiling point (standard atmosphere pressure) in table 2, mixed c 4
| Component | Trimethylmethane | Iso-butylene | Normal butane | Butene-1 | C-butene-2 | S-butene-2 |
| Boiling point DEG C | -11.72 | -6.9 | -0.5 | -6.2 | 3.72 | 0.88 |
Removing the acetic acid of non-complete reaction in the material after alkane without the need to being separated with sec-butyl acetate, can enter together with sec-butyl acetate in catalytic cracking riser reactor and carrying out scission reaction.
Described step 3) catalytic cracking reaction process carries out in catalytic cracking riser reactor, the position that in dealkylate materials at bottom of tower, sec-butyl acetate, acetic acid etc. enter riser reactor can be positioned at the top of heavy feed stock oil-in, below or equal height, wherein preferred below.Heavy crude hydro carbons and sec-butyl acetate, acetic acid etc. react in the same space, reach the target improving propene yield.
Catalytic cracking reaction used catalyst be selected from following at least one: Y zeolite or its modified product, ZSM-5 molecular sieve or its modified product, SAPO molecular sieve or its modified product.All types of catalyzer can be used alone, and also can be combined as mixed catalyst by the mode of bonding or blending.
Key point of the present invention is: by C 4 materials and acetic acid being reacted, olefin component is wherein made to generate sec-butyl acetate, the sec-butyl acetate that utilization generates and the feature that boiling point of alkanes differs greatly, alkane is separated with sec-butyl acetate, thus guarantees in the material of freshening propylene enhancing not containing inert components such as alkane.Due to alkane in lighter hydrocarbons freshening process is isolated system in time, the alkane material that purity is higher can be obtained, therefore can reduce catalytic cracking unit load, reduce energy consumption; Improve the production capacity that lighter hydrocarbons produce propylene.Therefore the method Propylene Selectivity is high, energy consumption is low, significantly can improve the economy of carbon fourth class lighter hydrocarbons propylene enhancing production technique.
Compared with prior art, feature of the present invention is:
1) the present invention contains the lighter hydrocarbons logistics of alkene by carbon four or other and acetic acid reacts, and C 4 olefin is changed into sec-butyl acetate, makes the difficult olefin/paraffin be separated realize the separation of highly selective, less energy-consumption, and propylene enhancing target.
2) in the inventive method, sec-butyl acetate and boiling point of alkanes difference are large, and the highly selective only needing conventional distillation can realize alkane/olefin is separated, and do not need to adopt the complicated technologies such as extracting rectifying, simple to operate, energy consumption is low, pollution-free.
3) in the inventive method, alkane isolates system in time, improves device capbility, reduces the load of system, energy efficient.And isolated alkane purity is high, and carbon four utilization of resources is abundant.
4) present method can significantly improve with mixed c 4 selectivity and the productive rate of the process being raw material production propylene.
Accompanying drawing explanation
Fig. 1 is the methodological principle schema of freshening increasing output of ethylene and propylene in catalytic cracking or cracking process after C 4 olefin of the present invention is separated
Fig. 2 is the process flow sheet of comparative example 1 catalytic cracking or cracking process processing carbon Four composition propylene enhancing.
In figure: 1, catalytic cracking (or cracking) device, 2, gas separation unit, 3, MTBE device, 4, acetic ester catalytic synthesis device, 5, Dealkylater, 6, dry gas, gasoline, diesel oil etc., 7, liquefied gas, 8, propylene, 9, mixed c 4,10, MTBE, 11, not containing the mixed c 4 of iso-butylene, 12, acetic acid, 13, reactor outlet material, 14, the low-carbon alkanes of etherification reaction is not participated in, 15, the acetic ester of freshening, 16, stock oil.
Describe the present invention in detail below by accompanying drawing, but do not limit the scope of the invention.
Embodiment
Below by specific embodiment, illustrate effect of the present invention further, but embodiment does not limit the scope of the invention.
As shown in Figure 1, heavy oil feedstock (logistics 16) enters in riser catalytic cracking reactor and cracking reaction occurs, the gasoline generated, diesel oil and dry gas are as product (logistics 6) separating device of catalytic cracking unit, liquefied gas (logistics 7) enters into gas separation unit (module 2), obtain propylene product (logistics 8) and mixed c 4 (logistics 9), after mixed c 4 logistics (logistics 9) transforms in MTBE device (module 3), MTBE product (logistics 10) can be obtained and not containing the mixed c 4 (logistics 11) of iso-butylene, logistics 11 mixes with acetic acid (logistics 12), together introduce the reactor (module 4) that acid cation exchange resin catalyst is housed, temperature of reaction 70 ~ 180 DEG C, reaction gauge pressure 0.5 ~ 6MPa, reaction velocity 0.5 ~ 3h
-1carry out building-up reactions, wherein the raw materials components mole ratio of acetic acid and butylene is 0.5 ~ 3:1, generates sec-butyl acetate.Reactor outlet material (logistics 13) enters Dealkylater (module 5), alkane in mixture is distillated (logistics 14) at tower top, residue materials at bottom of tower (logistics 15) enters in the catalytic cracking riser reactor containing ZSM-5 molecular sieve catalyzer (module 1), temperature of reaction 400 ~ 600 DEG C, gauge pressure 0 ~ 0.1MPa, under catalyzer and reaction mass are less than 0.2 second condition duration of contact, carry out scission reaction, produce propylene.
Embodiment 1
To the fixed bed catalytic reactor (in Fig. 1 module 4) of the acid cation exchange resin catalyst of 200ml be filled with, be heated to 120 DEG C.Acetic acid (logistics 12) and the mixture (logistics 11) containing butane and butene-1 are by acetic acid/alkene mol ratio 1:1, and mass space velocity is 3h
-1enter acetic ester catalytic synthesis device (in Fig. 1 module 4), carry out contacting reacting with catalyzer, temperature 120 DEG C, the outlet of acetic ester catalytic synthesis device obtains the mixture (logistics 13) of reacted sec-butyl acetate and butane.Acetic ester catalytic synthesis device is exported the product liquid obtained, carry out rectifying separation (module 5), tower top obtains unreacted butane (logistics 14), obtains sec-butyl acetate (logistics 15) at the bottom of tower.The fcc riser reactor (module 1) containing H-ZSM-5 molecular sieve catalyst is introduced in this logistics (logistics 15), temperature of reaction 540 DEG C, cracking reaction occurs with heavy oil feedstock (logistics 16) simultaneously.Compared with the operating mode of not participating in reaction with logistics 15, cracking reactor outlet additionally can obtain 83.6% propylene+39.1% ethene (account for charging butene-1 mass percentage, part carbon is from acetic acid, and total carbon effective rate of utilization is 91%).The product that fcc riser reactor (module 1) exports comprises gasoline, diesel oil and dry gas (logistics 6) and liquefied gas (logistics 7), wherein logistics 6 directly goes out device as product, liquefied gas logistics (logistics 7) enters into gas separation unit (module 2), isolate propylene product (logistics 8), obtain mixed c 4 logistics (logistics 9) in addition.This logistics, after MTBE device (module 3) transforms, obtains the mixture (logistics 11) that this example starts described butane and butene-1.
Comparative example 1
As shown in Figure 2, mixture (logistics 11) containing butane and butene-1 directly enters splitter (module 5), obtain the mixture (logistics 14) of one butane going out device and butene-1, and the mixture of the butane of one freshening and butene-1 (logistics 15).The fcc riser reactor (module 1) containing H-ZSM-5 molecular sieve catalyst is introduced in this logistics (logistics 15), temperature of reaction 540 DEG C, cracking reaction occurs with heavy oil feedstock (logistics 16) simultaneously.Compared with the operating mode of not participating in reaction with logistics 15, cracking reactor outlet additionally can obtain 31.6% propylene+16.1% ethene (account for butene-1 mass percentage in logistics 11, total carbon effective rate of utilization is 47.7%).The product that fcc riser reactor (module 1) exports comprises gasoline, diesel oil and dry gas (logistics 6) and liquefied gas (logistics 7), wherein logistics 6 directly goes out device as product, liquefied gas logistics (logistics 7) enters into gas separation unit (module 2), isolate propylene product (logistics 8), obtain mixed c 4 logistics (logistics 9) in addition.This logistics, after MTBE device (module 3) transforms, obtains the mixture (logistics 11) that this example starts described butane and butene-1.The difference of this process and embodiment 1 is, the butylene in logistics 11 is not converted to butylacetate, directly carries out scission reaction.Because the butane-component in the middle of logistics 11 does not react in catalytic cracking/cracking process, for preventing butane-component from accumulating in systems in which, need the material containing butane to discharge system (logistics 14).In logistics 14, understand some butylene discharge system with butane, cause the yield losses of target product propylene.Compared with the scheme of the complete freshening of butylene (embodiment 1), in this process, the effective rate of utilization of carbon is lower, and calculate according to the gauge of butylene contained in logistics 11, the efficiency of recycling is only 47.7%.
As can be seen from the Comparative result of above embodiment with comparative example: the alkene be rich in the light hydrocarbon feedstocks of alkene is first changed into acetic ester and carries out cracking conversion reaction again after being separated, can the remarkable yield of ethene and propylene in split product, improve utilization of resources rate, reduce the volume of reactor, therefore this technological line and the method for conventional direct freshening compare and possess comparatively significantly advantage.
Claims (8)
1. a method for freshening increasing output of ethylene and propylene in catalytic cracking or cracking process after being separated by C 4 olefin, is characterized in that its processing step is as follows:
1). the carbon four containing alkene (positive structure or isomery) under catalyst action with acetic acid, temperature of reaction 30 ~ 200 DEG C, absolute pressure 0.1 ~ 6MPa, mass space velocity is 0.1 ~ 10h
-1react under condition, wherein acetic acid: olefin molar feed ratio is 0.1 ~ 10:1, generate sec-butyl acetate, the material that reactor outlet obtains enters into step 2;
2). the reactor outlet material from step 1 carries out conventional distillation in rectifying tower, does not need to add extraction agent or other quality of assistance separating agent, and tower top isolates alkane, the material that the molecular weight obtaining at the bottom of tower being generated by olefine reaction is larger; Materials at bottom of tower enters step 3;
3). from step 2 at the bottom of rectifying tower sec-butyl acetate enter in catalytic cracking riser reactor, temperature of reaction 350 ~ 650 DEG C, in the environment of absolute pressure 0.08 ~ 0.4MPa, contact with catalyzer and react, generating the low-carbon alkene comprising propylene.
2., according to method according to claim 1, it is characterized in that: step 1) described in C 4 olefin and acetic acid between the catalyzer of reaction that occurs be one or more in ion-exchange resin catalyst or its modified product, ionic liquid, the vitriol oil, carried heteropoly acid, Y zeolite or its modified product, ZSM molecular sieve or its modified product, SAPO molecular sieve or its modified product; All types of catalyzer can be used alone, and also can be combined as composite catalyst system by the mode of bonding, blending or grating.
3. according to method according to claim 1, it is characterized in that: step 1) described in C 4 olefin and acetic acid between the adopted reactor that reacts be fixed-bed reactor or reactive distillation column, can arrange the reactor of one or more series connection, unreacted acetic acid also can reenter reactor and proceed reaction again.
4., according to method according to claim 1, it is characterized in that: step 2) described in sepn process be conventional distillation, the alkane that can not react is separated with by reacting the sec-butyl acetate generated, and obtains the material being stripped of alkane at the bottom of tower.
5. according to method according to claim 1, it is characterized in that: in the material obtained at the bottom of Dealkylater except the sec-butyl acetate that reaction generates, can also containing the acetic acid do not reacted, this strand of material can directly enter catalytic cracking riser reactor and react, without the need to it being thoroughly separated with reaction product.
6., according to method according to claim 1, it is characterized in that: step 3) described in the scission reaction of sec-butyl acetate catalyzer used be selected from following at least one: Y zeolite or its modified product, ZSM molecular sieve or its modified product, SAPO molecular sieve or its modified product; All types of catalyzer can be used alone, and also can be combined as mixed catalyst by the mode of bonding or blending.
7. according to method according to claim 1, it is characterized in that: step 3) in catalytic cracking reaction process be carry out in catalytic cracking riser reactor, reaction raw materials comprises the heavy raw oil of boiling spread more than 350 DEG C, and the position that in dealkylate materials at bottom of tower, sec-butyl acetate, acetic acid etc. enter riser reactor can be positioned at the top of heavy feed stock oil-in, below or equal height; Heavy crude hydro carbons and sec-butyl acetate, acetic acid etc. react in the same space, reach the target improving propene yield.
8. according to method according to claim 7, it is characterized in that: step 3) in catalytic cracking reaction process be carry out in catalytic cracking riser reactor, reaction raw materials comprises the heavy raw oil of boiling spread more than 350 DEG C, and the position that in dealkylate materials at bottom of tower, sec-butyl acetate, acetic acid etc. enter riser reactor is positioned at the below of heavy feed stock oil-in; Heavy crude hydro carbons and sec-butyl acetate, acetic acid etc. react in the same space, reach the target improving propene yield.
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| CN105152833A (en) * | 2015-07-22 | 2015-12-16 | 珠海飞扬新材料股份有限公司 | Method for preparing n-butene |
| CN109096035A (en) * | 2018-07-17 | 2018-12-28 | 天津大学 | Utilize the method and apparatus of kinetics differential separation alkane and alkene |
| CN112225654A (en) * | 2020-11-02 | 2021-01-15 | 中国海洋石油集团有限公司 | Device and method for comprehensively utilizing mixed C4 |
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| CN101432254A (en) * | 2006-02-07 | 2009-05-13 | 塞拉尼斯国际公司 | Integrated process for the production of acetic acid and vinyl acetate |
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| CN105152833A (en) * | 2015-07-22 | 2015-12-16 | 珠海飞扬新材料股份有限公司 | Method for preparing n-butene |
| CN109096035A (en) * | 2018-07-17 | 2018-12-28 | 天津大学 | Utilize the method and apparatus of kinetics differential separation alkane and alkene |
| CN112225654A (en) * | 2020-11-02 | 2021-01-15 | 中国海洋石油集团有限公司 | Device and method for comprehensively utilizing mixed C4 |
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