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CN105272801A - Method for transalkylation reaction - Google Patents

Method for transalkylation reaction Download PDF

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CN105272801A
CN105272801A CN201410353873.0A CN201410353873A CN105272801A CN 105272801 A CN105272801 A CN 105272801A CN 201410353873 A CN201410353873 A CN 201410353873A CN 105272801 A CN105272801 A CN 105272801A
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diisopropylnaphthalene
reaction
sio
grams
transalkylation reaction
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CN105272801B (en
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姚晖
高焕新
顾瑞芳
方华
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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Abstract

The present invention relates to a method for a transalkylation reaction. A purpose of the present invention is mainly to solve the problems of low 2,6-diisopropylnaphthalene selectivity, more heavy components and rapid catalyst deactivation in the prior art. According to the present invention, the used catalyst is organosilicon zeolite and has the following molar relationship composition (1/n)Al2O3:SiO2:(m/n)R, wherein n is 5-250, m is 0.01-50, R is at least one selected from alkyl, alkyl alkene and phenyl, the organosilicon zeolite-containing Si<29> NMR solid NMR map at least contains a Si<29> NMR resonance spectrum peak in -80 to +50 ppm, and the X-ray diffraction pattern of the organosilicon zeolite has the d- spacing maximal value at 12.4+/-0.2, 11.0+/-0.3, 9.3+/-0.3, 6.8+/-0.2, 6.1+/-0.2, 5.5+/-0.2, 4.4+/-0.2, 4.0+/-0.2 and 3.4+/-0.1 angstrom. The method of the present invention can be used for the 2,6-diisopropyl naphthalene preparation in the industrial production.

Description

For the method for transalkylation reaction
Technical field
The present invention relates to a kind of method for transalkylation reaction.
Background technology
Diisopropylnaphthalene is the low condensation point of a class colorless and odorless low toxicity, broad-spectrum important Organic Chemicals.2,6-DIPN is wherein the raw material manufacturing poly-2, the 6-naphthalene diethyl adipate (PEN) of high-performance polymer.PEN has the superior quality such as good thermotolerance, gas barrier, ultraviolet barrier property and chemical proofing, can manufacture hot canning beverage bottle, Recyclable beer bottle bottle, cosmetics of super quality bottle or high performance thin film, is new polyester material very powerful and exceedingly arrogant at present.Manufacture the technique of 2,6-DIPN except adopting naphthalene and propylene liquid-phase alkylation method, the by product that also alkylated reaction must be produced, as other isomers of isopropyl naphthalene and diisopropylnaphthalene, transformed by the method for transalkylation, to improving the yield of 2,6-DIPN.
The molecular sieve of MWW structure has half basket structure of ten-ring and twelve-ring duct and opening simultaneously, and has high thermal stability and stronger acidity, is widely used in the reactions such as the alkylation of benzene.Transalkylation reaction is also referred to as intermolecular and intramolecular isomerization reaction.Report MWW molecular sieve is seldom had to be applied to the serial reaction preparing 2,6-DIPN in document, just less for transalkylating reaction.
Document US4950824 refer to can be that raw material obtains a kind of containing mixture that is single, double and triisopropyl naphthalene with comprising isopropyl naphthalene and diisopropylnaphthalene, obtains the method for 2,6-DIPN after Component seperation.JP02088531 uses the solid acid catalyst of silicon-aluminum containing, after naphthalene and propylene are obtained by reacting list and diisopropylnaphthalene product, at relatively high temperatures product is carried out transalkylation reaction, improves the yield of 2,6-DIPN.
R.Brzozowski is in JournalofCatalysisA:General166 (1998): in 21-27 2,6-DIPN and 1,3-and 1,7-DIPN is used to isomerization reaction, obtains the mixture of multiple isomers under the effect of an acidic catalyst.But whole reaction has only carried out 6 hours.
All there is the problem that 2,6-DIPN selectivity is low, heavy constituent is many, catalyst deactivation is fast in above method.
Summary of the invention
Technical problem to be solved by this invention is the problem that prior art exists that 2,6-DIPN selectivity is low, heavy constituent is many, catalyst deactivation is fast, provides a kind of method for transalkylation reaction newly.It is good that the method has 2,6-DIPN selectivity, the feature that catalyst life is long.
For solving the problems of the technologies described above, the technical scheme that the present invention takes is as follows: a kind of method for transalkylation reaction, with the mixture of diisopropylnaphthalene or isopropyl naphthalene and diisopropylnaphthalene for raw material, be 150 ~ 300 DEG C in temperature of reaction, the weight space velocity of diisopropylnaphthalene is 0.1 ~ 10 hour -1, the weight ratio of isopropyl naphthalene and diisopropylnaphthalene is under the condition of 0 ~ 4, reaction raw materials and catalyst exposure, generates 2,6-DIPN; Described catalyst comprises following component:
A) the organosilicon zeolite of 50 ~ 80%;
B) binding agent of 20 ~ 50%;
Described organosilicon zeolite comprises the composition of following molar relationship: (1/n) Al 2o 3: SiO 2: (m/n) R, n=5 ~ 250 in formula, m=0.01 ~ 50, R is at least one in alkyl, alkane thiazolinyl or phenyl; The described Si containing organic silicone zeolite 29nMR solid state nmr collection of illustrative plates at least includes a Si between-80 ~+50ppm 29nuclear magnetic resonance spectrum peak; The X-ray diffracting spectrum of described organosilicon zeolite is 12.4 ± 0.2, and there is d-spacing maximum at 11.0 ± 0.3,9.3 ± 0.3,6.8 ± 0.2,6.1 ± 0.2,5.5 ± 0.2,4.4 ± 0.2,4.0 ± 0.2 and 3.4 ± 0.1 dust places.
In technique scheme, preferably, n=10 ~ 100, m=0.05 ~ 20.
In technique scheme, preferably, described alkyl to be carbonatoms be 1 ~ 8 alkyl, described alkane thiazolinyl to be carbonatoms be 2 ~ 10 alkane thiazolinyl.More preferably, described alkyl is methyl or ethyl, and described alkane thiazolinyl is vinyl.
In technique scheme, preferably, described binding agent is selected from least one in aluminum oxide, titanium oxide, zinc oxide or zirconium white.
In technique scheme, preferably, temperature of reaction is 150 ~ 270 DEG C.
In technique scheme, preferably, the weight space velocity of diisopropylnaphthalene is 0.1 ~ 2 hour -1.
In technique scheme, preferably, the weight ratio of isopropyl naphthalene and diisopropylnaphthalene is 0.5 ~ 3.
The synthetic method of the organosilicon zeolite in the inventive method is as follows:
A) by organosilicon source, inorganic silicon source, aluminium source, alkali, organic amine template and water mixing, with the SiO in inorganic silicon source 2for benchmark, reaction mixture with molar ratio computing is: SiO 2/ Al 2o 3=5 ~ 250, organosilicon source/SiO2=0.001 ~ 1, OH -/ SiO 2=0.01 ~ 5.0, H 2o/SiO 2=5 ~ 100, organic amine/SiO 2=0.01 ~ 2.0;
B) by above-mentioned reaction mixture under crystallization temperature is 90 ~ 200 DEG C of conditions, react after 1 ~ 100 hour and take out, through washing, dry obtained organosilicon zeolite.
In technique scheme, inorganic silicon source is be selected from least one in silicon sol, solid oxidation silicon, silica gel, silicon ester, diatomite or water glass.Organosilicon source is be selected from least one in halosilanes, silazane or organoalkoxysilane; Wherein halosilanes is be selected from least one in trimethylchlorosilane, dimethyldichlorosilane(DMCS), chlorotriethyl silane, diethyl dichlorosilane, dimethyl chloride bromo-silicane, dimethyl ethyl chlorosilane, dimethylbutyl chlorosilane, 3,5-dimethylphenyl chlorosilane, dimethylisopropyl chlorosilane, dimethyl tertiary butyl chlorosilane, dimethyl stearyl chlorosilane, methyl phenyl vinyl chlorosilane, vinyl trichloro silane or diphenyl dichlorosilane; Silazane is be selected from least one in hexamethyldisilazane, heptamethyldisilazane, tetramethyl-disilazane, divinyl tetramethyl-disilazane or diphenyltetramethyldisilazane; Organoalkoxysilane is be selected from least one in trimethylethoxysilane, dimethyldiethoxysilane, trimethylmethoxysilane, dimethyldimethoxysil,ne, trimethoxy-benzene base silane or diphenyl diethoxy silane.Aluminium source is be selected from least one in sodium aluminate, sodium metaaluminate, Tai-Ace S 150, aluminum nitrate, aluminum chloride, aluminium hydroxide, aluminum oxide, kaolin or polynite.Alkali is mineral alkali, for being selected from least one in lithium hydroxide, sodium hydroxide, potassium hydroxide, rubidium hydroxide or cesium hydroxide.Organic formwork agent is be selected from least one in quadrol, hexanediamine, hexahydroaniline, hexamethylene imine, heptamethylene imines, pyridine, hexahydropyridine, butylamine, hexylamine, octylame, decyl amine, amino dodecane, cetylamine or stearylamine.
Reaction mixture is with the SiO in inorganic silicon source 2for benchmark, with molar ratio computing preferable range be: SiO 2/ Al 2o 3=10 ~ 100, organosilicon source/SiO 2=0.005 ~ 0.5, OH -/ SiO 2=0.05 ~ 1.0, H 2o/SiO 2=10 ~ 80, organic formwork agent/SiO 2=0.05 ~ 1.0.Crystallization temperature preferable range is 100 ~ 180 DEG C, and crystallization time preferable range is 2 ~ 60 hours.During synthesis, preferred version is reaction mixture first ageing 2 ~ 100 hours under 10 ~ 80 DEG C of conditions before crystallization.
The preparation method of the catalyzer used in the inventive method is as follows:
Mixed with binding agent by the organosilicon zeolite of above-mentioned synthesis, zeolite content is 50 ~ 80 (weight) %.Then the dilute nitric acid solution adding 5 (weight) % is kneaded and formed, dry, and roasting to 480 in atmosphere ~ 600 DEG C, roasting time is obtain finished catalyst in 1 ~ 15 hour.
Owing to have employed, there is special diffraction peak and special Si in the present invention 29the organosilicon zeolites as catalysts active main body at nuclear magnetic resonance spectrum peak, during for transalkylation reaction, restrained effectively the side reactions such as dealkylation, thus the generation of the heavy constituents such as triisopropyl naphthalene is greatly reduced, and the selectivity of 2,6-DIPN is good.The present inventor finds that reaction is lower than under 270 DEG C of conditions, after 200 hours run, 2,6-diisopropylnaphthalene selectivity is more than 35%, and triisopropyl naphthalene content accounts for product molar ratio and is less than 11%, and catalyzer does not have the sign of inactivation, 2, the mol ratio of 6-diisopropylnaphthalene and 2,7-diisopropylnaphthalene is greater than 1.0, achieves good technique effect.
Below by embodiment, the invention will be further elaborated.
Embodiment
[embodiment 1]
By sodium aluminate (containing 42.0 % by weight Al 2o 3) 6.1 grams be dissolved in 288 grams of water, add 1.0 grams, sodium hydroxide and make it to dissolve.Then add hexahydropyridine 34.0 grams when stirring, then add solid oxidation silicon 60 grams, trimethylchlorosilane 5.5 grams, the material proportion (mol ratio) of reactant is:
SiO 2/Al 2O 3＝40
NaOH/SiO 2＝0.025
Trimethylchlorosilane/SiO 2=0.05
Hexahydropyridine/SiO 2=0.50
H 2O/SiO 2＝16
After question response mixture stirs, load in stainless steel cauldron, under agitation in 135 DEG C of crystallization 50 hours.Through filtration, washing, drying after taking-up.SiO is obtained through chemical analysis 2/ Al 2o 3mol ratio is 42.1.Its Si 29there is nuclear magnetic resonance spectrum peak at 15.1ppm in NMR solid core magnetic spectrum, its X-ray diffraction data are in table 1.
Table 1
Get the powdered samples of 50 grams of synthesis, 550 DEG C of roastings 5 hours, then exchange 3 times with the nitric acid of 1M, filter, drying.Afterwards, fully mix with 20 grams of aluminum oxide, the nitric acid adding 5 (weight) % is mediated, extruded moulding is the bar of Φ 1.6 × 2 millimeters, 120 DEG C of oven dry, and 550 DEG C of roastings 10 hours, are prepared into the catalyzer of needs.
The catalyst loading getting 10 grams of above-mentioned preparations, in fixed-bed reactor, then passes into raw material liq.Reaction conditions is: reaction raw materials is diisopropylnaphthalene, weight space velocity=2.0 hour -1, temperature of reaction 180 DEG C, reaction pressure 1.0MPa.
React after 200 hours, reaction result is: 2,6-DIPN selectivity 35.40%, and it is 10.85% that the above heavy constituent of triisopropyl naphthalene accounts for product molar ratio.The mol ratio of 2,6-DIPN and 2,7-diisopropylnaphthalene is 1.12.
[embodiment 2]
By sodium aluminate (containing 42.0 % by weight Al 2o 3) 8.0 grams be dissolved in 360 grams of water, add 4.0 grams, sodium hydroxide and make it to dissolve.Then add hexahydropyridine 34.0 grams when stirring, then add silicon sol 150 grams (containing 40 % by weight SiO 2), dimethyldichlorosilane(DMCS) 3.9 grams, the material proportion (mol ratio) of reactant is:
SiO 2/Al 2O 3＝30
NaOH/SiO 2＝0.05
Dimethyldichlorosilane(DMCS)/SiO 2=0.03
Hexahydropyridine/SiO 2=0.40
H 2O/SiO 2＝20
After question response mixture stirs, load in stainless steel cauldron, under agitation in 150 DEG C of crystallization 55 hours.Through filtration, washing, drying after taking-up.SiO is obtained through chemical analysis 2/ Al 2o 3mol ratio is 28.6.Its Si 29there is nuclear magnetic resonance spectrum peak at-5.7ppm and-16.4ppm in NMR solid core magnetic spectrum, its X-ray diffraction data are in table 2.
Table 2
Get the powdered sample of 50 grams of synthesis, the process of Kaolinite Preparation of Catalyst is with [embodiment 1].The catalyst loading getting 10 grams of above-mentioned preparations, in fixed-bed reactor, then passes into raw material liq.Reaction conditions is: raw material is the mixture of isopropyl naphthalene and diisopropylnaphthalene, and the weight ratio of isopropyl naphthalene and diisopropylnaphthalene is weight space velocity=1.6 hour of 0.5:1, diisopropylnaphthalene -1, temperature of reaction 230 DEG C, reaction pressure 1.0MPa.
React after 200 hours, reaction result is: 2,6-DIPN selectivity 40.82%, and it is 8.87% that the above heavy constituent of triisopropyl naphthalene accounts for product molar ratio.The mol ratio of 2,6-DIPN and 2,7-diisopropylnaphthalene is 1.05.
[embodiment 3]
3.0 grams, aluminum oxide is dissolved in 450 grams of water, adds 16.0 grams, sodium hydroxide and make it to dissolve.Then add hexamethylene imine 34.7 grams when stirring, then add solid oxidation silicon 60 grams, dimethyldiethoxysilane 5.9 grams, the material proportion (mol ratio) of reactant is:
SiO 2/Al 2O 3＝30
NaOH/SiO 2＝0.2
Dimethyldiethoxysilane/SiO 2=0.04
Hexamethylene imine/SiO 2=0.35
H 2O/SiO 2＝25
After question response mixture stirs, load in stainless steel cauldron, under agitation in 145 DEG C of crystallization 70 hours.Through filtration, washing, drying after taking-up.SiO is obtained through chemical analysis 2/ Al 2o 3mol ratio is 30.1.Its Si 29there is nuclear magnetic resonance spectrum peak at 5.8ppm and-15.9ppm in NMR solid core magnetic spectrum, its X-ray diffraction data are in table 3.
Table 3
Get the powdered sample of 50 grams of synthesis, the process of Kaolinite Preparation of Catalyst is with [embodiment 1].The catalyst loading getting 10 grams of above-mentioned preparations, in fixed-bed reactor, then passes into raw material liq.Reaction conditions is: raw material is the mixture of isopropyl naphthalene and diisopropylnaphthalene, and the weight ratio of isopropyl naphthalene and diisopropylnaphthalene is weight space velocity=1.0 hour of 1:1, diisopropylnaphthalene -1, temperature of reaction 240 DEG C, reaction pressure 1.0MPa.
React after 200 hours, reaction result is: 2,6-DIPN selectivity 41.46%, and it is 7.69% that the above heavy constituent of triisopropyl naphthalene accounts for product molar ratio.The mol ratio of 2,6-DIPN and 2,7-diisopropylnaphthalene is 1.08.
[embodiment 4]
By sodium aluminate (containing 42.0 % by weight Al 2o 3) 16.1 grams be dissolved in 540 grams of water, add 2.0 grams, sodium hydroxide and make it to dissolve.Then add hexamethylene imine 30 grams when stirring, then add solid oxidation silicon 60 grams, hexamethyldisilazane 3.2 grams, the material proportion (mol ratio) of reactant is:
SiO 2/Al 2O 3＝15
NaOH/SiO 2＝0.05
Hexamethyldisilazane/SiO 2=0.04
Hexamethylene imine/SiO 2=0.3
H 2O/SiO 2＝30
After question response mixture stirs, load in stainless steel cauldron, under agitation in 145 DEG C of crystallization 38 hours.Through filtration, washing, drying after taking-up.SiO is obtained through chemical analysis 2/ Al 2o 3mol ratio is 17.5.Its Si 29there is nuclear magnetic resonance spectrum peak at 14.8ppm in NMR solid core magnetic spectrum, its X-ray diffraction data are in table 4.
Table 4
Get the powdered sample of 50 grams of synthesis, the process of Kaolinite Preparation of Catalyst is with [embodiment 1].The catalyst loading getting 10 grams of above-mentioned preparations, in fixed-bed reactor, then passes into raw material liq.Reaction conditions is: raw material is the mixture of isopropyl naphthalene and diisopropylnaphthalene, and the weight ratio of isopropyl naphthalene and diisopropylnaphthalene is weight space velocity=0.5 hour of 1.5:1, diisopropylnaphthalene -1, temperature of reaction 220 DEG C, reaction pressure 1.0MPa.
React after 200 hours, reaction result is: 2,6-DIPN selectivity 41.35%, and it is 5.83% that the above heavy constituent of triisopropyl naphthalene accounts for product molar ratio.The mol ratio of 2,6-DIPN and 2,7-diisopropylnaphthalene is 1.10.
[embodiment 5]
By sodium aluminate (containing 42.0 % by weight Al 2o 3) 3.5 grams be dissolved in 540 grams of water, add 8.0 grams, sodium hydroxide and make it to dissolve.Then add hexamethylene imine 30 grams when stirring, then add solid oxidation silicon 60 grams, hexamethyldisilazane 8.0 grams, the material proportion (mol ratio) of reactant is:
SiO 2/Al 2O 3＝70
NaOH/SiO 2＝0.2
Hexamethyldisilazane/SiO 2=0.05
Hexamethylene imine/SiO 2=0.3
H 2O/SiO 2＝30
After question response mixture stirs, load in stainless steel cauldron, under agitation in 135 DEG C of crystallization 35 hours.Through filtration, washing, drying after taking-up.SiO is obtained through chemical analysis 2/ Al 2o 3mol ratio is 68.5.Its Si 29there is nuclear magnetic resonance spectrum peak at 16.8ppm in NMR solid core magnetic spectrum, its X-ray diffraction data are in table 5.
Table 5
Get the powdered sample of 50 grams of synthesis, the process of Kaolinite Preparation of Catalyst is with [embodiment 1].The catalyst loading getting 10 grams of above-mentioned preparations, in fixed-bed reactor, then passes into raw material liq.Reaction conditions is: raw material is the mixture of isopropyl naphthalene and diisopropylnaphthalene, and the weight ratio of isopropyl naphthalene and diisopropylnaphthalene is weight space velocity=0.5 hour of 2:1, diisopropylnaphthalene -1, temperature of reaction 250 DEG C, reaction pressure 1.0MPa.
React after 200 hours, reaction result is: 2,6-DIPN selectivity 41.32%, and it is 5.57% that the above heavy constituent of triisopropyl naphthalene accounts for product molar ratio.The mol ratio of 2,6-DIPN and 2,7-diisopropylnaphthalene is 1.00.
[embodiment 6]
By sodium aluminate (containing 42.0 % by weight Al 2o 3) 2.4 grams be dissolved in 900 grams of water, add 40 grams, sodium hydroxide and make it to dissolve.Then add hexamethylene imine 20 grams when stirring, then add solid oxidation silicon 60 grams, divinyldichlorosilane 48.5 grams, the material proportion (mol ratio) of reactant is:
SiO 2/Al 2O 3＝100
NaOH/SiO 2＝1.0
Divinyldichlorosilane/SiO 2=0.3
Hexamethylene imine/SiO 2=0.2
H 2O/SiO 2＝50
After question response mixture stirs, load in stainless steel cauldron, under agitation in 135 DEG C of crystallization 35 hours.Through filtration, washing, drying after taking-up.SiO is obtained through chemical analysis 2/ Al 2o 3mol ratio is 105.3.Its Si 29there is nuclear magnetic resonance spectrum peak at 4.2ppm and-17.5ppm in NMR solid core magnetic spectrum, its X-ray diffraction data are in table 6.
Table 6
Get the powdered sample of 50 grams of synthesis, the process of Kaolinite Preparation of Catalyst is with [embodiment 1].The catalyst loading getting 10 grams of above-mentioned preparations, in fixed-bed reactor, then passes into raw material liq.Reaction conditions is: raw material is the mixture of isopropyl naphthalene and diisopropylnaphthalene, and the weight ratio of isopropyl naphthalene and diisopropylnaphthalene is weight space velocity=0.5 hour of 0.75:1, diisopropylnaphthalene -1, temperature of reaction 230 DEG C, reaction pressure 1.0MPa.
React after 200 hours, reaction result is: 2,6-DIPN selectivity 42.39%, and it is 6.54% that the above heavy constituent of triisopropyl naphthalene accounts for product molar ratio.The mol ratio of 2,6-DIPN and 2,7-diisopropylnaphthalene is 1.03.
[embodiment 7]
By sodium aluminate (containing 42.0 % by weight Al 2o 3) 1.6 grams be dissolved in 720 grams of water, add 24 grams, sodium hydroxide and make it to dissolve.Then add hexamethylene imine 50 grams when stirring, then add solid oxidation silicon 60 grams, trimethoxy-benzene base silane 19.8 grams, the material proportion (mol ratio) of reactant is:
SiO 2/Al 2O 3＝150
NaOH/SiO 2＝0.6
Trimethoxy-benzene base silane/SiO 2=0.1
Hexamethylene imine/SiO 2=0.5
H 2O/SiO 2＝40
After question response mixture stirs, load in stainless steel cauldron, under agitation in 135 DEG C of crystallization 35 hours.Through filtration, washing, drying after taking-up.SiO is obtained through chemical analysis 2/ Al 2o 3mol ratio is 142.0.Its Si 29there is nuclear magnetic resonance spectrum peak at 17.1ppm in NMR solid core magnetic spectrum, its X-ray diffraction data are in table 7.
Table 7
Get the powdered sample of 50 grams of synthesis, the process of Kaolinite Preparation of Catalyst is with [embodiment 1].The catalyst loading getting 10 grams of above-mentioned preparations, in fixed-bed reactor, then passes into raw material liq.Reaction conditions is: raw material is the mixture of isopropyl naphthalene and diisopropylnaphthalene, and the weight ratio of isopropyl naphthalene and diisopropylnaphthalene is weight space velocity=0.5 hour of 1.5:1, diisopropylnaphthalene -1, temperature of reaction 220 DEG C, reaction pressure 1.0MPa.
React after 200 hours, reaction result is: 2,6-DIPN selectivity 40.86%, and it is 6.84% that the above heavy constituent of triisopropyl naphthalene accounts for product molar ratio.The mol ratio of 2,6-DIPN and 2,7-diisopropylnaphthalene is 1.07.

Claims (8)

1., for a method for transalkylation reaction, with the mixture of diisopropylnaphthalene or isopropyl naphthalene and diisopropylnaphthalene for raw material, be 150 ~ 300 DEG C in temperature of reaction, the weight space velocity of diisopropylnaphthalene is 0.1 ~ 10 hour -1, the weight ratio of isopropyl naphthalene and diisopropylnaphthalene is under the condition of 0 ~ 4, reaction raw materials and catalyst exposure, generates 2,6-DIPN; Described catalyst comprises following component:
A) the organosilicon zeolite of 50 ~ 80%;
B) binding agent of 20 ~ 50%;
Described organosilicon zeolite comprises the composition of following molar relationship: (1/n) Al 2o 3: SiO 2: (m/n) R, n=5 ~ 250 in formula, m=0.01 ~ 50, R is at least one in alkyl, alkane thiazolinyl or phenyl; The described Si containing organic silicone zeolite 29nMR solid state nmr collection of illustrative plates at least includes a Si between-80 ~+50ppm 29nuclear magnetic resonance spectrum peak; The X-ray diffracting spectrum of described organosilicon zeolite is 12.4 ± 0.2, and there is d-spacing maximum at 11.0 ± 0.3,9.3 ± 0.3,6.8 ± 0.2,6.1 ± 0.2,5.5 ± 0.2,4.4 ± 0.2,4.0 ± 0.2 and 3.4 ± 0.1 dust places.
2., according to claim 1 for the method for transalkylation reaction, it is characterized in that n=10 ~ 100, m=0.05 ~ 20.
3., according to claim 1 for the method for transalkylation reaction, it is characterized in that described alkyl to be carbonatoms be the alkyl of 1 ~ 8, described alkane thiazolinyl to be carbonatoms be 2 ~ 10 alkane thiazolinyl.
4., according to claim 3 for the method for transalkylation reaction, it is characterized in that described alkyl is methyl or ethyl, described alkane thiazolinyl is vinyl.
5., according to claim 1 for the method for transalkylation reaction, it is characterized in that described binding agent is selected from least one in aluminum oxide, titanium oxide, zinc oxide or zirconium white.
6., according to claim 1 for the method for transalkylation reaction, it is characterized in that temperature of reaction is 150 ~ 270 DEG C.
7., according to claim 1 for the method for transalkylation reaction, it is characterized in that the weight space velocity of diisopropylnaphthalene is 0.1 ~ 2 hour -1.
8., according to claim 1 for the method for transalkylation reaction, it is characterized in that the weight ratio of isopropyl naphthalene and diisopropylnaphthalene is 0.5 ~ 3.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04187648A (en) * 1990-11-20 1992-07-06 Nippon Steel Chem Co Ltd Production of 2,6-diethylnaphthalene
US6011190A (en) * 1997-07-02 2000-01-04 Kabushiki Kaisha Kobe Seiko Sho Process for preparing dialkylnaphthalene
CN101172254A (en) * 2006-11-02 2008-05-07 中国石油化工股份有限公司 Organosilicon micropore zeolite, synthesizing method and uses thereof
CN101239726A (en) * 2007-02-07 2008-08-13 中国石油化工股份有限公司 Organic silicon micro-pore zeolite and its synthetic method and application

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04187648A (en) * 1990-11-20 1992-07-06 Nippon Steel Chem Co Ltd Production of 2,6-diethylnaphthalene
US6011190A (en) * 1997-07-02 2000-01-04 Kabushiki Kaisha Kobe Seiko Sho Process for preparing dialkylnaphthalene
CN101172254A (en) * 2006-11-02 2008-05-07 中国石油化工股份有限公司 Organosilicon micropore zeolite, synthesizing method and uses thereof
CN101239726A (en) * 2007-02-07 2008-08-13 中国石油化工股份有限公司 Organic silicon micro-pore zeolite and its synthetic method and application

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