CN1462790A - Catalyst for cracking waste plastics to generate fuel - Google Patents
Catalyst for cracking waste plastics to generate fuel Download PDFInfo
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- CN1462790A CN1462790A CN 03117935 CN03117935A CN1462790A CN 1462790 A CN1462790 A CN 1462790A CN 03117935 CN03117935 CN 03117935 CN 03117935 A CN03117935 A CN 03117935A CN 1462790 A CN1462790 A CN 1462790A
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Abstract
A catalyst for cracking the waste plastics to produce fuel oil (gasoline or diesel oil) may be the DeLaZSM-5 prepared by modifying zeolite molecular sieve ZSM-5 or the composite cracking catalyst containing at least two carried metallic oxides as active components. Its advantages are low cracking temp and high output rate and quality of fuel oil.
Description
One, technical field
The invention belongs to catalyst technical field, be specifically related to a kind of cracking waste plastics that is used for to produce the catalyzer of fuel oil.
Two, background technology
The needs of environment protection are not only in the processing of waste or used plastics, also utilize for reasonable resources simultaneously again and have opened up an important channel.The processing of waste or used plastics at present roughly is divided into following four kinds of methods: landfill method, burning method, regeneration method and chemical cycle method.Wherein the chemical cycle method is to utilize light, heat, radiation, chemical reagent etc. to make the waste or used plastics polymer degradation become monomer or oligopolymer.Degraded product is that monomer can be used for synthetic new polymkeric substance, and degraded product is that oligopolymer can be used as oil product, and can not cause topsoil in the production process, so this kind technology is considered to the most promising waste plastics recovery method.
The main mode of chemical cycle method is to utilize heat energy that plastic waste is carried out cracking.Cracking process is divided into thermo-cracking and catalytic pyrolysis.Because the catalytic cracking reaction temperature is low, the added value of product height be the emphasis of studying both at home and abroad at present, and the effect of catalytic pyrolysis is owing to the catalyzer that depends primarily on use, so actual the concentrating on the catalyzer of emphasis of research.
At present, using in treatment of waste plastics has solid acid catalyst comparatively widely, and that wherein the most frequently used is amorphous aluminosilicate (SA) (H.Ohkita; R.Nishiyama; Y.Tochihara, et al.Ind.Eng.Chem.Res.1993,32:3112); Various types of molecular sieve zeolites, as HZSM-5, USY, REY and CaX (G.Manos, A.Garforth, J.Dwyer, Ind.Eng.Chem.Res.2000,39:1198); (Y.Uemichi such as Uemichi; Y.Kashiwaya; A.Ayame.et al.Chem.Lett.1984,41) gac that adopts.There is document to report some new catalysts successively in the recent period, as MCM-41, SAPO-37, KFS-16, (J.Aguada such as depleted catalyst for cracking in H-gallosilicate, cross-linked montmorillonite, using natural clinoptilolite and the oil factory, J.L.Sctelo, D.P.Serrano, et al.Energy.Fuels, 1997,11:1225; G.J.T.Femandes, V.J.Femandes, Jr.A.S.Araujo, Catalysis.Today, 2002,75:233; Y.Sakata; M.A.Uddin; A.Muto, et al.J.Anal.Appl.Pyrolysis.1997,43:15; Y.Uemichi, T.Suzuki.Chem.Lett.1999,1137-1138; G.Manos, I.Y.Yusof, N.H.Gangas, et al.Energy.Fuels.2002,16 (2): 485; J.R.Kim, Y.A.Kim, J.-H.Yoon, et al.Polym.Degrad.Stab.2002,75:287.S.C.Cardona, A.corma.Appl.Catal B Environ, 2000,25:151).In addition, (S.Nishio.Ind.Eng.Chem.Res.1995 34:4514), and takes by weighing certain catalytic pyrolysis effect for Z.Zhang, T.Hirose to also have bibliographical information to adopt solid base catalyst.
Though existing catalyzer is various in style, also obtained corresponding catalytic pyrolysis effect separately, however the use-testing result who carries out from the inventor, still there is following problem in above-mentioned catalyzer:
1, activity of such catalysts is lower, long reaction time, and the temperature of reaction height, and oil quality is not high, yield is low.
2, the function singleness of catalyzer only has the function of catalytic pyrolysis, when handling complicated component, when wherein containing the plastic waste of halogen, not only can emit hydrogen halide, etching apparatus in the cracking process; The oil product that cracking is generated contains more organic halogen material, does not reach the standard of fuel oil.
Three, summary of the invention
The objective of the invention is the deficiency at existing cracking waste plastics catalyzer, a kind of high lytic activity that has is provided, the reaction times is short, and temperature of reaction is low, can improve the catalyzer of the efficient and the quality product of cracking waste plastics system fuel oil.
Another object of the present invention provide a kind of have high lytic activity and dehalogenation function simultaneously be used for cracking waste plastics to produce the catalyzer of fuel oil.
Be used for cracking waste plastics to produce the catalyzer of fuel oil for what the last purpose of the present invention provided, it is characterized in that this catalyzer prepares by the following method, promptly in the ZSM-5 zeolite molecular sieve, add the Na of 0.1～2M by 1: 1～100 weight ratio
2CO
3Solution was in 40-120 ℃ of reaction 2～10 hours; Leave standstill after the reaction and incline and supernatant liquid, add the Na of 0.1～2M again by 1: 1～100 weight ratio again
2CO
3Solution in 40～120 ℃ of reactions 2～10 hours, filters, with 100～3000 parts of deionized water wash, and following dry 12 hours in 120 ℃; In the exsiccant solid, add 10～1000 parts of deionized waters then,, filter in 40～120 ℃ of reactions 2～10 hours, with 100～3000 parts of deionized water wash, and following dry 12 hours in 120 ℃; Dried solid again in 300～600 ℃ of activation 8～24 hours, is promptly made DeZSM-5; With the DeZSM-5 that makes 10-100 part 0.1～2M LaCl
3, down carried out ion-exchange 5～60 minutes in 40～120 ℃ with the 2450MHz microwave radiation, exchange is afterwards washed La to the washings with boiling water
3+Detection is zero, then in 120 ℃ dry 12 hours down, again in 300～600 ℃ down activation promptly made DeLaZSM-5 in 5～24 hours.
Wherein the ZSM-5 zeolite molecular sieve can be any in HZSM-5 zeolite molecular sieve or the NaZSM-5 zeolite molecular sieve.
Be used for cracking waste plastics to produce the catalyzer of fuel oil for what another purpose of the present invention provided, it is characterized in that this catalyzer is is that activeconstituents constitutes to be carried on the carrier by at least a metal oxide, with the catalyst weight is benchmark, and its content is 5～50%.
Wherein metal oxide is raw materials such as employing nitrate, in the preparation feedback process, generate, be specially zinc oxide, cupric oxide, ferric oxide, nickel oxide, magnesium oxide, oxidation Cobalt, manganese oxide, vanadium oxide, titanium oxide, calcium oxide, barium oxide, lanthanum trioxide, aluminum oxide, silicon-dioxide.Carrier is DeLaZSM-5, silicon-dioxide, activated carbon, aluminum oxide, silicon aluminium microsphere, CaX, NaY, USY, NaZSM-5, HZSM-5, MCM-41, SAPO-37, KFS-16, any in H-gallosilicate, using natural clinoptilolite, kaolin, polynite, the cross-linked montmorillonite.
The preparation method specifically can adopt any of coprecipitation method, pickling process, microwave solid reaction process, and these methods are
Prior art.
The present invention compared with prior art, its advantage is:
1, since cracking waste plastics catalyst provided by the invention active high, have an excellent catalytic pyrolysis function, thereby when being used for cracking waste plastics not only the reaction times short, only need 10～60 minutes, and cracking temperature is low, under 100～300 ℃, get final product, greatly reduce production cost.
2, contain the metal oxide catalyst for cracking except that having the catalytic pyrolysis function owing to provided by the invention, also has the dehalogenation function simultaneously, not only can make the organic halogen content of the oil product that obtains behind the cracking waste plastics is zero, and also can not emit hydrogen halide, etching apparatus in the cracking process.
3, use the comprehensive yield height of producing behind the cracking waste plastics catalyzer provided by the invention of fuel oil, all more than 80%, and color is pure, and is superior in quality, and gasoline can reach the national standard of 70～90# gasoline, and diesel oil can reach 0～-national standard of 35# diesel oil.
Four, embodiment
Provide embodiment below so that the present invention is carried out concrete description.Be necessary to be pointed out that at this following examples only are used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment to the present invention according to the invention described above content.
Embodiment one:
(1) preparation of catalyzer DeLaZSM-5: the Na that in 10 parts of HZSM-5 zeolite molecular sieves, adds 10 parts of 0.8M
2CO
3Solution was in 80 ℃ of reactions 4 hours; Leave standstill after the reaction and incline and supernatant liquid, add the Na of 10 parts of 0.8M more again
2CO
3Solution in 80 ℃ of reactions 4 hours, filters, with 100 parts of deionized water wash, and following dry 12 hours in 120 ℃; In the exsiccant solid, add 10 parts of deionized waters then,, filter in 80 ℃ of reactions 2 hours, with 100 parts of deionized water wash, in 120 ℃ dry 12 hours down, and activate 24 hours down in 360 ℃, promptly make DeZSM-5.With the DeZSM-5 that makes with 10 parts of 0.8M LaCl
3Carried out ion-exchange 30 minutes with the 2450MHz microwave radiation down in 100 ℃.Wash La to the washings with boiling water
3+Detection is zero, then in 120 ℃ dry 12 hours down, again in 600 ℃ down activation promptly made DeLaZSM-5 in 5 hours.
(2) cracking waste plastics oil-producing technique: plastic waste is cleaned, pulverizes, after the drying, presses plastic waste weight and add 5% above-mentioned catalyst for cracking, drop in the reactor, be warming up to 300 ℃ then and carry out scission reaction.The fuel oil that generates during reaction and carries out categorised collection by the boiling point of product to oil product outside pipe-line transportation goes out still.Wherein 160-180 ℃ product collection is a gasoline, and 350-380 ℃ product collection is a diesel oil.The cracking product adopts sodium hydroxide solution to carry out the alkali cleaning processing, the vitriol oil carries out cleanup acid treatment after condenser is cooled to 25 ℃ successively.Add weight ratio in the gasoline after processing and be 5% methylcarbonate and modulate boosting of octane rating.Add earlier weight ratio in the diesel oil after processing and be 0.1% cetane number improver, and then to add weight ratio be that 2 ‰ diesel pour inhibitor carries out pour point depression and handles.
Embodiment two:
(1) preparation of catalyzer DeLaZSM-5: the Na that in 10 parts of NaZSM-5 zeolite molecular sieves, adds 500 parts of 2M
2CO
3Solution was in 120 ℃ of reactions 2 hours.Leave standstill after the reaction and incline and supernatant liquid, add the Na of 500 parts of 2M more again
2CO
3Solution in 120 ℃ of reactions 2 hours, filters, with 1500 parts of deionized water wash, and following dry 12 hours in 120 ℃; In the exsiccant solid, add 500 parts of deionized waters then,, filter in 120 ℃ of reactions 2 hours, with 1500 parts of deionized water wash, in 120 ℃ dry 12 hours down, and activate 10 hours down in 450 ℃, promptly make DeZSM-5; With the DeZSM-5 that makes with 50 parts of 2M LaCl
3Down carried out ion-exchange 5 minutes with the 2450MHz microwave radiation in 80 ℃, exchange is afterwards washed La to the washings with boiling water
3+Detection is zero, then in 120 ℃ dry 12 hours down, again in 300 ℃ down activation promptly made DeLaZSM-5 in 24 hours.
(2) cracking waste plastics oil-producing technique: present embodiment cracking waste plastics oil-producing technique is except that the above-mentioned catalyst for cracking of pressing plastic waste weight adding 20%, and all the other are identical with embodiment one, do not state so omit.
Embodiment three:
(1) preparation of catalyzer DeLaZSM-5: the Na that in 10 parts of NaZSM-5 zeolite molecular sieves, adds 1000 parts of 0.1M
2CO
3Solution was in 40 ℃ of reactions 10 hours.Leave standstill after the reaction and incline and supernatant liquid, add the Na of 1000 parts of 0.1M more again
2CO
3Solution in 40 ℃ of reactions 10 hours, filters, with 3000 parts of deionized water wash, and under 120 ℃ in dry 12 hours; To in dry solid, adding 1000 parts of deionized waters,, filter then in 40 ℃ of reactions 10 hours, with 3000 parts of deionized water wash, in 120 ℃ dry 12 hours down, and activate 8 hours down in 550 ℃, promptly make DeZSM-5; With the DeZSM-5 that makes with 100 parts of 0.1MLaCl
3Down carried out ion-exchange 5 minutes with the 2450MHz microwave radiation in 120 ℃, exchange is afterwards washed La to the washings with boiling water
3+Detection is zero, then in 120 ℃ dry 12 hours down, again in 450 ℃ down activation promptly made DeLaZSM-5 in 15 hours.
(2) cracking waste plastics oil-producing technique: present embodiment cracking waste plastics oil-producing technique is except that the above-mentioned catalyst for cracking of pressing plastic waste weight adding 10%, and all the other are identical with embodiment one, do not state so omit.
Embodiment four:
(1) coprecipitation method prepares compound catalyst for cracking: take by weighing 50 parts of aluminum nitrates and 50 parts of zinc nitrates, with two kinds of nitrate mixed dissolutions in 200 parts of deionized waters; This solution splashed into slowly in the beaker that ammoniacal liquor is housed (amount of ammoniacal liquor with guarantee in precipitation process and afterwards ageing process in PH remain at more than 9 be advisable) make it precipitation, to precipitate then and 16 hours after-filtration of ageing of solution, taking precipitate was dried 72 hours down at 120 ℃, again 250 ℃ of following preheatings 16 hours, at last in 500 ℃ of activation 24 hours, promptly make the compound catalyst for cracking of aluminum oxide-zinc oxide, wherein metal oxide content is 50%, and carrier is 50%.
(2) cracking waste plastics oil-producing technique: present embodiment cracking waste plastics oil-producing technique is except that being the Halogen by the above-mentioned catalyst for cracking of plastic waste weight adding 15% and the plastic waste of processing, and all the other are identical with embodiment one, do not state so omit.
Embodiment five:
(1) coprecipitation method prepares compound catalyst for cracking: take by weighing 70 parts of aluminum nitrates and 30 parts of Xiao Suangus, with two kinds of nitrate mixed dissolutions in 500 parts of deionized waters; This solution splashed into slowly in the beaker that ammoniacal liquor is housed (amount of ammoniacal liquor with guarantee in precipitation process and afterwards ageing process in PH remain at more than 9 be advisable) make it precipitation, to precipitate then and 20 hours after-filtration of ageing of solution, taking precipitate was dried 24 hours down at 120 ℃, again 250 ℃ of following preheatings 10 hours, at last in 500 ℃ of activation 12 hours, promptly make the compound catalyst for cracking of aluminum oxide cobalt monoxide, wherein metal oxide content is 30%, and carrier is 70%.
(2) cracking waste plastics oil-producing technique: present embodiment cracking waste plastics oil-producing technique is except that being the Halogen by the above-mentioned catalyst for cracking of plastic waste weight adding 10% and the plastic waste of processing, and all the other are identical with embodiment one, do not state so omit.
Embodiment six:
(1) coprecipitation method prepares compound catalyst for cracking: take by weighing 60 parts of aluminum nitrates, 20 parts of cupric nitrates and 20 parts of nitrocalcite, to be dissolved in 200 parts of deionized waters after their mixing, this solution splashed into slowly in the beaker that ammoniacal liquor is housed (amount of ammoniacal liquor with guarantee in precipitation process and afterwards ageing process in PH remain at more than 9 be advisable) make it precipitation, to precipitate then and 20 hours after-filtration of ageing of solution, get and be deposited in 120 ℃ of following oven dry 24 hours, again 250 ℃ of following preheatings 10 hours, in 500 ℃ of activation 24 hours, promptly make aluminum oxide-cupric oxide-calcium oxide composite catalyst at last.Wherein metal oxide content is 40%, and carrier is 60%.
(2) cracking waste plastics oil-producing technique: present embodiment cracking waste plastics oil-producing technique is except that being the Halogen by the above-mentioned catalyst for cracking of plastic waste weight adding 15% and the plastic waste of processing, and all the other are identical with embodiment one, do not state so omit.
Embodiment seven:
(1) the compound catalyst for cracking of immersion process for preparing: take by weighing 30 parts of iron nitrates and 70 parts of silicon-dioxide, iron nitrate is dissolved in 500 parts of deionized waters, then with this solution impregnation to silicon-dioxide, product behind the dipping was dried 24 hours down at 120 ℃, 500 ℃ of activation 24 hours, promptly make the compound catalyst for cracking of ferric oxide-silicon-dioxide again.Wherein metal oxide content is 30%, and carrier is 70%.
(2) cracking waste plastics oil-producing technique: present embodiment cracking waste plastics oil-producing technique is except that being the Halogen by the above-mentioned catalyst for cracking of plastic waste weight adding 10% and the plastic waste of processing, and all the other are identical with embodiment one, do not state so omit.
Embodiment eight:
(1) the compound catalyst for cracking of immersion process for preparing: take by weighing 40 parts of cupric nitrates and 60 parts of DeLaZSM-5, cupric nitrate is dissolved in 500 parts of deionized waters, then with this solution impregnation to DeLaZSM-5, product behind the dipping was dried 24 hours down at 120 ℃, 500 ℃ of activation 48 hours, promptly make the compound catalyst for cracking of cupric oxide-DeLaZSM-5 again.Wherein metal oxide content is 40%, and carrier is 60%.
(2) cracking waste plastics oil-producing technique: present embodiment cracking waste plastics oil-producing technique is except that being the Halogen by the above-mentioned catalyst for cracking of plastic waste weight adding 3% and the plastic waste of processing, and all the other are identical with embodiment one, do not state so omit.
Embodiment nine:
(1) the microwave solid reaction process prepares compound catalyst for cracking: take by weighing 10 parts of magnesium oxide and 90 parts of polynites, mix under the microwave radiation that the back is 2450MHz in operating frequency and shone 30 minutes, promptly make magnesium oxide-montmorillonite Composite catalyst for cracking.Wherein metal oxide content is 10%, and carrier is 90%.
(2) cracking waste plastics oil-producing technique: present embodiment cracking waste plastics oil-producing technique is except that being the Halogen by the above-mentioned catalyst for cracking of plastic waste weight adding 10% and the plastic waste of processing, and all the other are identical with embodiment one, do not state so omit.
Embodiment ten:
(1) the microwave solid reaction process prepares compound catalyst for cracking: take by weighing 20 parts of calcium oxide and 80 parts of DeLaZSM-5, mixing the back is to shine 30 minutes under the 2450MHz microwave radiation in operating frequency, promptly makes the compound catalyst for cracking of calcium oxide-DeLaZSM-5.Wherein metal oxide content is 20%, and carrier is 80%.
(2) cracking waste plastics oil-producing technique: present embodiment cracking waste plastics oil-producing technique is except that being the Halogen by the above-mentioned catalyst for cracking of plastic waste weight adding 4% and the plastic waste of processing, and all the other are identical with embodiment one, do not state so omit.
Claims (4)
1, is used for cracking waste plastics to produce the catalyzer of fuel oil, it is characterized in that this catalyzer prepares by the following method, promptly in the ZSM-5 zeolite molecular sieve, add the Na of 0.1～2M by 1: 1～100 weight ratio
2CO
3Solution was in 40-120 ℃ of reaction 2～10 hours; Leave standstill after the reaction and incline and supernatant liquid, add the Na of 0.1～2M again by 1: 1～100 weight ratio again
2CO
3Solution in 40～120 ℃ of reactions 2～10 hours, filters, with 100～3000 parts of deionized water wash, and following dry 12 hours in 120 ℃; In the exsiccant solid, add 10～1000 parts of deionized waters then,, filter in 40～120 ℃ of reactions 2～10 hours, with 100～3000 parts of deionized water wash, and following dry 12 hours in 120 ℃; Dried solid again in 300～600 ℃ of activation 8～24 hours, is promptly made DeZSM-5; With the DeZSM-5 that makes 10-100 part 0.1～2M LaCl
3, down exchanging 5～60 minutes in 40～120 ℃ with 2450MHz microwave radiation ion, exchange is afterwards washed La to the washings with boiling water
3+Detection is zero, then in 120 ℃ dry 12 hours down, again in 300～600 ℃ down activation promptly made DeLaZSM-5 in 5～24 hours, or this catalyzer is to be that activeconstituents constitutes to be carried on the carrier by at least a metal oxide, with the catalyst weight is benchmark, and its content is 5～50%.
2, the cracking waste plastics that is used for according to claim 1 to be to produce the catalyzer of fuel oil, it is characterized in that ZSM-5 zeolite molecular sieve in this catalyzer is any in HZSM-5 zeolite molecular sieve or the NaZSM-5 zeolite molecular sieve.
3, the cracking waste plastics that is used for according to claim 1 is characterized in that to produce the catalyzer of fuel oil the metal oxide in this catalyzer is zinc oxide, cupric oxide, ferric oxide, nickel oxide, magnesium oxide, oxidation Cobalt, manganese oxide, vanadium oxide, titanium oxide, calcium oxide, barium oxide, lanthanum trioxide, aluminum oxide, silicon-dioxide.
4, according to claim 1 or the 3 described catalyzer that are used for cracking waste plastics with the production fuel oil, it is characterized in that the carrier in this catalyzer is DeLaZSM-5, silicon-dioxide, activated carbon, aluminum oxide, silicon aluminium microsphere, CaX, NaY, USY, NaZSM-5, HZSM-5, MCM-41, SAPO-37, KFS-16, any in H-gallosilicate, using natural clinoptilolite, kaolin, polynite, the cross-linked montmorillonite.
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| CN108273558B (en) * | 2018-02-11 | 2019-07-23 | 北京石油化工学院 | Catalytic cracking catalyst and its preparation method and application |
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