US20190002765A1 - Process for converting mixed waste plastic into liquid fuels by catalytic cracking - Google Patents

Process for converting mixed waste plastic into liquid fuels by catalytic cracking Download PDF

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Publication number
US20190002765A1
US20190002765A1 US16/062,702 US201616062702A US2019002765A1 US 20190002765 A1 US20190002765 A1 US 20190002765A1 US 201616062702 A US201616062702 A US 201616062702A US 2019002765 A1 US2019002765 A1 US 2019002765A1
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Prior art keywords
waste plastic
catalyst
mixed waste
process according
weight
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US16/062,702
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Inventor
Stéphane Streiff
Marco PICCININI
Emmanuel Marx
Avelino Corma
Miriam CERRO-ALARCÓN
Jesús MENGUAL
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Solvay SA
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Solvay SA
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Assigned to SOLVAY SA reassignment SOLVAY SA ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CERRO-ALARCON, MIRIAM, CORMA, AVELINO, MENGUAL, JESUS, STREIFF, STEPHANE, MARX, EMMANUEL, PICCININI, MARCO
Publication of US20190002765A1 publication Critical patent/US20190002765A1/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
    • C10G1/10—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal from rubber or rubber waste
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
    • C10G1/08—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal with moving catalysts
    • C10G1/086—Characterised by the catalyst used
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10—Feedstock materials
    • C10G2300/1003—Waste materials
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/70—Catalyst aspects
    • C10G2300/701—Use of spent catalysts

Definitions

  • the present invention relates to a process for converting mixed waste plastic into liquid fuels by catalytic cracking.
  • the process comprises the steps of introducing mixed waste plastic and a catalyst comprising an amorphous-type catalyst within a reactor; allowing at least a portion of the mixed waste plastic to be converted to liquid fuels within the reactor; and removing a product stream containing said liquid fuels from the reactor.
  • the volatile compounds can be either relatively high boiling liquid hydrocarbons useful as fuel oils or fuel oil supplements or light to medium boiling hydrocarbons useful as gasoline-type fuels or as other chemicals.
  • Catalytic cracking of mixed waste plastic is a process well known to the person skilled in the art.
  • U.S. Pat. No. 5,216,149 discloses a method for controlling the pyrolysis of a complex waste stream of plastics to convert such stream into useful high-value monomers or other chemicals, by identifying catalyst and temperature conditions that permit decomposition of a given polymer in the presence of others, without substantial decomposition of the other polymers.
  • K.-H. Lee, et al. disclose in Polymer Degradation and Stability 84 (2004) 123-127 the liquid-phase catalytic degradation of mixtures of waste high-density polyethylene and polystyrene over spent FCC catalyst.
  • the effect of the mixing proportions of polyethylene to polystyrene was studied and the authors found that an increase of polystyrene content in the reactants showed an increase of gasoline fraction and a decrease in kerosene and diesel fraction in the obtained liquid product.
  • the fraction of aromatic components in the liquid product dramatically increased to 70% and more even at a polystyrene content of only about 40%. This finding is confirmed in the publication of K.-H. Lee in Polymer Degradation and Stability 93 (2008) 1284-1289 where at a polystyrene content of 40% even 90% aromatics were obtained.
  • the experiments reported by K.-H. Lee were conducted using 20 g of catalyst per 200 g of plastic.
  • the present inventors found that this and other problems as described below can surprisingly by solved by selecting a certain ratio of polystyrene to polyolefin in the mixed waste plastic and increasing the ratio of catalyst comprising an amorphous-type catalyst to waste plastic in the reactor.
  • the present invention therefore relates to a process for converting mixed waste plastic into liquid fuels by catalytic cracking, the process comprising:
  • the gasoline fraction contains compounds having a low boiling point of for example below 216° C. This fraction includes compounds having 5 to 11 carbon atoms.
  • the kerosene and diesel fraction has a higher boiling point of for example 216° C. to 359° C. This fraction generally contains compounds having 12 to 21 carbon atoms.
  • the even higher boiling fraction is generally designated as wax (Heavy Cycle Oil or HCO).
  • the compounds are hydrocarbons which optionally comprise heteroatoms, such as N, O, etc. “Liquid fuels” in the sense of the present invention therefore are fuels like gasoline and diesel but may also be used as other valuable chemicals or solvents.
  • a plastic is mostly constituted of a particular polymer and the plastic is generally named by this particular polymer.
  • a plastic contains more than 25% by weight of its total weight of the particular polymer, preferably more than 40% by weight and more preferably more than 50% by weight.
  • Other components in plastic are for example additives, such as fillers, reinforcers, processing aids, plasticizers, pigments, light stabilizers, lubricants, impact modifiers, antistatic agents, inks, antioxidants, etc.
  • a plastic comprises more than one additive.
  • Plastics used in the process of the present invention are polyolefins and polystyrene, such as high density polyethylene (HDPE), low density polyethylene (LDPE), polypropylene (PP) and polystyrene (PS).
  • Mixed plastics mostly constituted of polyolefin and polystyrene are preferred.
  • “mostly constituted” is to be understood such that the concentration of the polyolefin and the polystyrene in the mixed plastic is above 50% by weight, more preferably above 75% by weight, each based on the total weight of the dry mixed plastic.
  • the mixed plastic may be constituted of polyolefin and polystyrene.
  • the mixed plastic contains less than 99.5% by weight, more preferably less than 99% by weight of polyolefin and polystyrene, based on the total weight of the dry mixed plastic.
  • plastics such as polyvinylchloride, polyvinylidene chloride, polyethylene terephthalate, polyurethane (PU), acrylonitrile-butadiene-styrene (ABS), nylon and fluorinated polymers are less desirable. If present in the waste plastic, they are preferably present in a minor amount of less than 50% by weight, preferably less than 30% by weight, more preferably less than 20% by weight, even more preferably less than 10% by weight of the total weight of the dry waste plastic. Preferably, the individual content of any less desirable plastic is less than 5% by weight, more preferably less than 2% by weight based on the total weight of the dry waste plastic.
  • the plastics waste starting material comprises one or more thermoplastic polymers and is essentially free of thermosetting polymers.
  • Essentially free in this regard is intended to denote a content of thermosetting polymers of less than 15, preferably less than 10 and even more preferably less than 5 wt % of the composition.
  • waste plastic contains other non-desired components, namely foreign material, such as paper, glass, stone, metal, etc.
  • the weight of the waste plastic or the weight of the polystyrene and polyolefin in the mixed waste plastic, this weight relates to the weight of the dry plastic without any foreign material being admixed with the plastic.
  • the weight includes any components in the plastic, such as the above described additives.
  • the present inventors found that when using a catalyst comprising an amorphous-type catalyst, the addition of polystyrene to polyolefin raw material increases the reaction rate of the de-polymerization reaction of the polyolefins. There is, however, an optimum polystyrene to polyolefin ratio that maximizes the rate kinetic constant of the polyolefin's de-polymerization reaction.
  • the increase of rate kinetic constant is a significant advantage for an industrial process as it allows higher conversions as well as higher productivity.
  • the rate kinetic constant of the polyolefin's de-polymerization reaction has a maximum when the mixed waste plastic contains about 20% by weight of polystyrene based on the total weight of polystyrene and polyolefin in the mixed waste plastic. Still good values are achieved if the mixed waste plastic contains from 5 to 50% by weight of polystyrene, preferably from 5 to 40% by weight, more preferably from 5 to 30% by weight and even more preferably from 10 to 30% by weight of polystyrene, each based on the total weight of polystyrene and polyolefin in the mixed waste plastic. Most preferably, the mixed waste plastic contains from 15 to 25% by weight, such as about 20% by weight of polystyrene based on the total weight of polystyrene and polyolefin in the mixed waste plastic.
  • the inventors found that the gasoline quality in particular at a concentration of about 20% by weight of polyolefin in the mixed waste plastic is increased with respect to an increase in Research Octane Number (RON) and Motor Octane Number (MON).
  • RON Research Octane Number
  • MON Motor Octane Number
  • the process of the present invention therefore is also characterized in that the weight ratio of catalyst to mixed waste plastic in the reactor is above 1:10.
  • the weight ratio of catalyst to mixed waste plastic in the reactor is above 1:9, more preferably above 1:8, more preferably above 1:7, more preferably above 1:6, more preferably above 1:5, more preferably above 1:4 and even more preferably above 1:3, such as above 1:2.
  • a particularly preferred weight ratio of catalyst to mixed waste plastic in the reactor is about 1:1.5.
  • the weight ratio of catalyst to mixed waste plastic in the reactor can be below 10:1, preferably below 7:1.
  • the weight ratio of catalyst to mixed waste plastic in the reactor can be for example in the range of from 1:9 to 10:1, preferably from 1:8 to 10:1, preferably from 1:7 to 10:1, preferably from 1:6 to 10:1, preferably from 1:5 to 10:1, preferably from 1:4 to 10:1, preferably from 1:3 to 10:1 and even more preferably from 1:2 to 10:1 or from 1:2 to 7:1.
  • the catalyst used in the process of the present invention comprises an amorphous-type catalyst.
  • the catalyst predominantly is an amorphous-type catalyst.
  • the catalyst consists of an amorphous-type catalyst.
  • the catalyst additionally comprises a further catalyst, in particular a zeolite-type catalyst.
  • amorphous-type catalyst is to be understood as an amorphous solid, such as an amorphous powder.
  • amorphous solids are known to the skilled person.
  • Amorphous solids lack crystallinity, namely the long-range order characteristic of a crystal. This feature may be observed via X-ray diffraction analysis by the lack of sharp Bragg reflexes.
  • an amorphous-type catalyst may comprise a certain amount of crystalline solids.
  • the amorphous-type catalyst comprises less than 50% by weight, more preferably less than 25% by weight, even more preferably less than 10% by weight, such as less than 5% by weight or less than 2% or even less than 1% by weight of crystalline solids, each based on the total weight of the catalyst.
  • the term “predominantly” defines a catalyst which is a mixture of an amorphous-type catalyst and a non-amorphous-type catalyst, such as a zeolite-type catalyst, but wherein the catalyst comprises more than 50% by weight of the amorphous-type catalyst based on the total weight of the catalyst.
  • the catalyst comprises more than 60%, more preferably more than 70%, even more preferably more than 80% and most preferably more than 90% of the amorphous-type catalyst.
  • the catalyst can comprise a single amorphous-type catalyst or a mixture of two or more amorphous-type catalysts.
  • FCC catalysts are well known to the person skilled in the art.
  • the amorphous-type catalyst may comprise silica, alumina, kaolin, or a mixture thereof.
  • Silica in particular in the form of sand, is well known for FCC catalytic applications.
  • Preferred amorphous-type catalysts comprise at least 60% by weight, preferably at least 70% by weight and even more preferably at least 80% by weight of silica-equivalent of an oxidic compound based on silicon like silica (Si 0 2 ), kaolin, etc.
  • the catalyst additionally comprises a zeolite-type catalyst, this may be selected from crystalline microporous zeolites which are known to the person skilled in the art and which are commercially available. Preferred examples for zeolite-type catalysts are described in WO 2010/135273, the content of which is incorporated herein by reference.
  • zeolite-type catalysts include but are not limited to ZSM-5, ZSM-11, ZSM-22, ZSM-23, ZSM-35, ZSM-48, ZSM-50, TS-1, TS-2, SSZ-46, MCM-22, MCM-49, FU-9, PSH-3, ITQ-1, EU-1, NU-10, silicalite-1, silicalite-2, boralite-C, boralite-D, BCA, and mixtures thereof.
  • the catalyst can be fresh catalyst, equilibrated catalyst (such as spent catalyst), or a mixture thereof.
  • the mixed waste plastic and the catalyst comprising the amorphous-type catalyst can be introduced within the reactor simultaneously or subsequently. Furthermore, the mixed waste plastic and the catalyst comprising the amorphous-type catalyst can be introduced within the reactor batchwise or continuously.
  • the rotary kiln is a cylindrical vessel, inclined slightly to the horizontal, which is rotated slowly about its axis. The material to be processed is fed into the upper end of the cylinder. As the kiln rotates, material gradually moves down towards the lower end, and may undergo a certain amount of stirring and mixing.
  • a fluid gas or liquid
  • a circulating fluidized bed also called transport reactor
  • the catalyst and the fluid flow co-currently at high speed.
  • a cyclone system is used to separate the fluid, which can undergo downstream processing, from the solid, which is recirculated to the reactor.
  • the whole process is conducted continuously.
  • the reactor in presence of the catalyst, at least a portion of the mixed waste plastic is converted to liquid fuels.
  • This conversion preferably takes place at an elevated temperature of for example above 350° C., preferably above 400° C., more preferably above 410° C.
  • the conversion tales place at a temperature in the range of above 410° C. to 500° C., more preferably in the range of from 420° C. to 470° C., such as about 450° C.
  • FIG. 1 the evolution with time of the overall cumulative conversion for different polystyrene loadings
  • FIG. 2 the evolution with time of corrected HDPE cumulative conversion for different polystyrene loadings.
  • FIG. 3 the relative values of kinetic rate constant for different polystyrene loadings
  • FIG. 4 the effect of polystyrene loading on selectivity
  • FIG. 5 the effect of polystyrene loading on the quality of the gasoline fraction
  • FIG. 6 the effect of polystyrene loading on the quality of the diesel fraction.
  • the temperature was increased to the reaction temperature at a heating rate of 10° C./min, and the collection of gases and nitrogen in the corresponding gas sampling bag was started.
  • the circulation of the gaseous products was commuted to another pair of glass traps and corresponding gas sampling bag. This was considered as the zero reaction time.
  • liquid and gaseous products were collected in a pair of glass traps and their associated gas sampling bag, respectively.
  • the reactor was cooled to room temperature. During this cooling step, liquids and gases were also collected.
  • reaction products were classified into 3 groups: i) gases, ii) liquid hydrocarbons and iii) residue (waxy compounds, ashes and coke accumulated on the catalyst). Quantification of the gases was done by gas chromatography (GC) using nitrogen as the internal standard, while quantification of liquids and residue was done by weight.
  • the simulated distillation (SIM-DIS) GC method allowed the determination of the different fractions in the liquid samples (according to the selected cuts); the detailed hydrocarbon analysis (DHA) GC method allowed the determination of the PIONA (paraffins, iso-paraffins, olefins, naphthenes, aromatics) components in the gasoline fraction of the last withdrawn sample (C5-C11: Boiling point ⁇ 216.1° C.; what includes C5-C6 in the gas sample and C5-C11 in the liquid samples), and GC ⁇ GC allowed the determination of saturates (everything that is not aromatic), mono-, di- and tri-aromatics in the diesel fraction of the last withdrawn liquid samples (C12-C21; 216.1 ⁇ BP ⁇ 359° C.).
  • the experiment was carried out following the general procedure described above.
  • the raw material was pure HDPE (labelled 0% PS).
  • Reaction temperature was set at 450° C.
  • 20 g of silica were used.
  • Catalyst to plastic weight ratio was equal to 20/30.
  • the raw material is a mixture containing 95 wt. % HDPE and 5 wt. % PS (labelled 5% PS).
  • Reaction temperature was set at 450° C.
  • 20 g of silica have been used.
  • Catalyst to plastic weight ratio was equal to 20/30.
  • the raw material was a mixture containing 90 wt. % HDPE and 10 wt. % PS (labelled 10% PS).
  • Reaction temperature was set at 450° C.
  • 20 g of silica were used.
  • Catalyst to plastic weight ratio was equal to 20/30.
  • the raw material was a mixture containing 80 wt. % HDPE and 20 wt. % PS (labelled 20% PS).
  • Reaction temperature was set at 450° C.
  • 20 g of silica were used.
  • Catalyst to plastic weight ratio was equal to 20/30.
  • the raw material was a mixture containing 50 wt. % HDPE and 50 wt. % PS (labelled 50% PS).
  • Reaction temperature was set at 450° C.
  • 20 g of silica were used.
  • Catalyst to plastic weight ratio was equal to 20/30.
  • the experiment was carried out following the general procedure described above.
  • the raw material was pure PS (labelled 100% PS).
  • Reaction temperature was set at 450° C.
  • 20 g of silica were used.
  • Catalyst to plastic weight ratio was equal to 20/30.
  • FIG. 1 The evolution of the overall cumulative conversion for the different polystyrene loadings over time is shown in FIG. 1 .
  • the PS conversion was then subtracted from the overall conversion thus obtaining the HDPE cumulative conversion for different polystyrene loadings shown in FIG. 2 .
  • the relative values of kinetic rate constant for different polystyrene loadings in HDPE pyrolysis were calculated.
  • FIG. 3 It is evident that the kinetic rate constant for the polyolefin conversion has a maximum at about 20% by weight of polystyrene present in the mixed waste plastic.
  • FIG. 5 shows the effect of the polystyrene loading on the quality of the gasoline fraction (P: paraffins, I: iso-paraffins, O: olefins, N: naphthenes, A: aromatics, U: unidentified).
  • FIG. 5 additionally shows the RON and MON of the gasoline fractions obtained with different polystyrene loadings. Surprisingly, both RON and MON increase if the amount of polystyrene in the mixed waste plastic is increased from 0% to 20%.
  • FIG. 6 shows the effect of the polystyrene loading on the quality of the diesel fraction (S: saturated, MA: monoaromatic, DA: diaromatic, TA: triaromatic, PA: polyaromatic). It is evident that the overall amount of aromatic compounds in the diesel fraction remains low even if the polystyrene content in the mixed waste plastic is increased up to 50% by weight. Only when the polystyrene content is increased to 100% (which is not according to the invention), the amount of aromatic compounds in the diesel fraction significantly increases.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
US16/062,702 2015-12-18 2016-12-15 Process for converting mixed waste plastic into liquid fuels by catalytic cracking Abandoned US20190002765A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP15201124.3 2015-12-18
EP15201124 2015-12-18
PCT/EP2016/081304 WO2017103015A1 (fr) 2015-12-18 2016-12-15 Procédé de transformation de déchets plastiques mélangés en combustibles liquides par craquage catalytique

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EP (1) EP3390574A1 (fr)
CN (1) CN107922850A (fr)
WO (1) WO2017103015A1 (fr)

Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN114133951A (zh) * 2021-12-14 2022-03-04 青海天创新能源科技有限公司 一种利用催化剂进行废弃塑料解聚制备燃油的方法
JP2024509805A (ja) * 2021-03-10 2024-03-05 エコラボ ユーエスエー インコーポレイティド プラスチック由来の合成原料のための安定添加剤

Family Cites Families (5)

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CN1150968A (zh) * 1995-11-23 1997-06-04 杨亚力 废塑料烃处理的方法和设备
CN102744101B (zh) * 2012-08-02 2014-07-09 新疆大学 用于废旧塑料裂解制汽油的催化剂及制备方法和使用方法
WO2014040634A1 (fr) * 2012-09-14 2014-03-20 Outotec Oyj Procédé et appareil de recyclage des déchets plastiques
ES2673596T3 (es) * 2014-02-25 2018-06-25 Saudi Basic Industries Corporation Proceso para convertir residuo plástico mezclado (MWP) en productos petroquímicos valiosos
CN104479721B (zh) * 2014-12-29 2017-12-12 金妙英 一种利用废弃塑料制取燃料油的制备工艺

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2024509805A (ja) * 2021-03-10 2024-03-05 エコラボ ユーエスエー インコーポレイティド プラスチック由来の合成原料のための安定添加剤
CN114133951A (zh) * 2021-12-14 2022-03-04 青海天创新能源科技有限公司 一种利用催化剂进行废弃塑料解聚制备燃油的方法

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WO2017103015A1 (fr) 2017-06-22
EP3390574A1 (fr) 2018-10-24

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