CN102872857B - Production method of butene disproportionation catalyst - Google Patents

Production method of butene disproportionation catalyst Download PDF

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CN102872857B
CN102872857B CN201110193498.4A CN201110193498A CN102872857B CN 102872857 B CN102872857 B CN 102872857B CN 201110193498 A CN201110193498 A CN 201110193498A CN 102872857 B CN102872857 B CN 102872857B
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roasting
silica gel
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CN102872857A (en
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王仰东
宣东
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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 invention discloses a production method of a butene disproportionation catalyst, mainly solving the problems of difficulty in band extrusion and easiness in fracture in the catalyst production in the prior art. The method disclosed herein comprises the following steps: a) roasting silica gel at atmospheric condition for 2-12 h at 300-600 DEG C; b) uniformly mixing the silica gel obtained by the step a) with sesbania powder in proportion to obtain a mixture I; c) preparing needed active components into a solution to obtain a solution II; and d) adding the solution II and needed cellulose to the mixture I, then conducting band extrusion, drying, and roasting to obtain a finished product of the catalyst. The method disclosed herein well solves the problem and can be used in the industrial production of hexene by butene disproportionation.

Description

The production method of butylene disproportionation catalyst
Technical field
The present invention relates to a kind of production method of butylene disproportionation catalyst.
Background technology
In recent years, along with economic development, market will constantly increase the demand of light olefin (comprising ethene, propylene etc.).Propylene is scale inferior to one of most important basic organic of ethene, and its maximum purposes is to produce polypropylene (account for its total amount half), is secondly to produce acrylonitrile, expoxy propane, isopropyl alcohol, isopropylbenzene, oxo-alcohols, acrylic acid, oligomerization of propene thing.
Traditional ethene coproduction and refinery's Propylene recovery method are obviously difficult to meet growing propylene demand, adopt olefin(e) disproportionation technology can digest C when not reducing naphtha pyrolysis severity 4cut, and can propylene enhancing, thereby the research and development of preparing propylene through olefin disproportionation technology is not only to improving the output of propylene, simultaneously to promoting low value-added C 4the comprehensive utilization of cut all has great significance, and wherein producing propene from butylene by disproportion involved in the present invention is a kind of up-and-coming technique.
Olefin(e) disproportionation (Olefin metathesis) is a kind of conversion of olefines process.Under the effect at transition-metal catalyst (as W, Mo, Re etc.), the fracture of the two keys of C=C and formation again in alkene, thus can obtain new olefin product.We can represent simply from following reaction equation the dismutation of alkene:
R in reaction equation 1, R 2, R 3, R 4represent respectively different alkyl or hydrogen atom.If wherein the disproportionated reaction of same alkene (suc as formula 1) is called self disproportionation (self-metathesis); Disproportionated reaction between different alkene (formula 2) is called cross disproportionation (cross-metathesis).
US5300718 has reported the route of being produced propylene by the butene-2 raw material that contains butene-1 and oxygenatedchemicals.This technique comprises: first raw material is passed through to alumina removal oxygenatedchemicals; Under the effect that in raw material, butylene is urged at magnesia, isomery turns to butene-2; Butene-2 and ethene disproportionation generate third rare three steps.The catalyst that wherein butene-2 and ethene disproportionation are used is MgO and WO 3/ SiO 2mixed bed.
WO00014038 has introduced a kind of method of preparing propylene by butene disproportionation.Raw material butylene is butene-1, butene-2 or its mixture, and catalyst is WO 3/ SiO 2, common reaction temperature is 500-550 ℃, reaction pressure is 1atm.
US513891 has reported the preparation method of olefin disproportionation catalyst, and its catalyst consists of B 2o 3-Re 2o 7/ Al 2o 3/ SiO 2, using amorphous aluminum silicide as catalyst carrier, the activity of olefin dismutation reaction improves greatly.
When the production for butylene disproportionation catalyst, all there is catalyst extrusion difficulty, the problem of frangibility in the method in above document.
Summary of the invention
Technical problem to be solved by this invention is extrusion difficulty in the production process existing in prior art, and the problem of frangibility provides a kind of production method of new butylene disproportionation catalyst.When the method is used for the industrial production of butylene disproportionation catalyst, have easy extrusion, catalyst is frangibility and active good advantage not.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of production method of butylene disproportionation catalyst, comprises the following steps: by specific area, be a) 150～350 meters 2/ gram silica gel roasting under air atmosphere, sintering temperature is 300～600 ℃, roasting time is 2～12 hours; B) silica gel step a being obtained and sesbania powder obtain mixture I after evenly mixing in required ratio; C) will after aequum active component wiring solution-forming, obtain solution II; D) to the cellulose that adds solution II and aequum in mixture I, obtain finished catalyst after by extrusion, oven dry, roasting.Wherein in preparation process, the part by weight of contained component is as follows, silica gel: sesbania powder: Ludox: active component: cellulose ratio is 1: (0.01～0.1): (0.4～1.2): (0.08～0.22): (0.02～0.20).
In technique scheme, the preferred version of silica gel is 400～1000 orders, and specific area is 200～300 meters 2/ gram, sesbania powder: Ludox: active component: the preferred proportion of cellulose is 1: (0.02～0.06): (0.6～0.8): (0.10～0.18): (0.07～0.15); The preferred version of active component is ammonium metatungstate; Cellulosic preferred version is hydroxypropyl methylcellulose; The preferred version that catalyst is dried is 80～100 ℃ of bake out temperatures, and drying time is 4～24 hours; The preferred version of catalyst roasting is 520～560 ℃ of sintering temperatures, and roasting time is 6～48 hours.
Catalyst prepared by technique scheme is for olefin dismutation reaction, and the embodiment of the present invention is 1-preparing hexane by disproportionating butylene.Reaction condition is as follows: in fixed bed reactors, and the 1-butylene that reaction raw materials is 99.9%, reaction temperature is 400 ℃, and reaction pressure is 0.5MPa, and the mass space velocity of 1-butylene is 10 hours -1.
The present invention by having added a certain amount of cellulose in the preparation process of disproportionation catalyst, cellulose has thickening capabilities, water-retaining property and caking property, humidity and the viscosity that in extrusion and shear history, can keep catalyst, guarantee the continuous production of catalyst strip in extrusion process, the difficult extrusion that prevents fracture or overdrying and cause and the generation of the low situation of shear efficiency, cellulose can be completely removed in roasting process, do not affect physical property and the reactivity worth of catalyst, the duct that cellulosic introducing simultaneously produces catalyst in roasting process is more, specific surface increases, thereby reactivity improves.In reaction temperature, be 400 ℃, reaction pressure is 0.5MPa, and the weight space velocity of 1-butylene is 10 hours -1under condition, by catalyst and 1-butylene haptoreaction, the conversion ratio of its 1-butylene can reach 65%, the weight yield of hexene can reach 28%, compare conversion ratio and weight yield and improve respectively 3% and 5%, cellulosic interpolation simultaneously makes easy extrusion in production process, and frangibility, has not obtained good technique effect.
Below by embodiment, the present invention is further elaborated.
The specific embodiment
[embodiment 1]
By specific area, it is 250 meters 2/ gram silica gel roasting under air atmosphere, sintering temperature is 550 ℃, roasting time is 6 hours; After getting 40 kilograms and the 1.6 kilograms sesbania powder mixing of silica gel after roasting, add in mixer, uniform stirring obtains mixture I after 20 minutes; 7.2 kilograms of ammonium metatungstates are dissolved in 50 kilograms of deionized waters, fully dissolve 30 kilograms of Ludox of heel and be mixed to get solution II; Solution II is added in mixture I, stir 1 hour after adding 4.3 kilograms of hydroxypropyl methylcelluloses simultaneously, extrusion, shears, and under 100 ℃ of air atmosphere, processes 10 hours, and after oven dry, under 550 ℃ of conditions, roasting obtained finished catalyst after 24 hours.The evaluation of catalyst is carried out on olefin(e) disproportionation evaluating apparatus, the 1-butylene that reaction raw materials is 99.9%, and reaction temperature is 400 ℃, and reaction pressure is 0.5MPa, and the mass space velocity of 1-butylene is 10 hours -1.Evaluation result and the condition of production of catalyst are as shown in table 1.
[embodiment 2]
By specific area, it is 300 meters 2/ gram silica gel (400～600 order) roasting under air atmosphere, sintering temperature is 500 ℃, roasting time is 10 hours; After getting 40 kilograms and the 0.4 kilogram sesbania powder mixing of silica gel after roasting, add in mixer, uniform stirring obtains mixture I after 30 minutes; 8.8 kilograms of ammonium metatungstates are dissolved in 48 kilograms of deionized waters, fully dissolve 16 kilograms of Ludox of heel and be mixed to get solution II; Solution II is added in mixture I, stir 1.5 hour after adding 8 kilograms of hydroxypropyl methylcelluloses simultaneously, extrusion, shears, and under 90 ℃ of air atmosphere, processes 16 hours, and after oven dry, under 520 ℃ of conditions, roasting obtained finished catalyst after 30 hours.The evaluation of catalyst is carried out on olefin(e) disproportionation evaluating apparatus, the 1-butylene that reaction raw materials is 99.9%, and reaction temperature is 400 ℃, and reaction pressure is 0.5MPa, and the mass space velocity of 1-butylene is 10 hours -1.Evaluation result and the condition of production of catalyst are as shown in table 1.
[embodiment 3]
By specific area, it is 350 meters 2/ gram silica gel (600～800 order) roasting under air atmosphere, sintering temperature is 600 ℃, roasting time is 4 hours; After getting 40 kilograms and the 4 kilograms sesbania powder mixing of silica gel after roasting, add in mixer, uniform stirring obtains mixture I after 25 minutes; 3.2 kilograms of ammonium metatungstates are dissolved in 40 kilograms of deionized waters, fully dissolve 48 kilograms of Ludox of heel and be mixed to get solution II; Solution II is added in mixture I, stir 2 hour after adding 0.8 kilogram of hydroxypropyl methylcellulose simultaneously, extrusion, shears, and under 80 ℃ of air atmosphere, processes 24 hours, and after oven dry, under 500 ℃ of conditions, roasting obtained finished catalyst after 48 hours.The evaluation of catalyst is carried out on olefin(e) disproportionation evaluating apparatus, the 1-butylene that reaction raw materials is 99.9%, and reaction temperature is 400 ℃, and reaction pressure is 0.5MPa, and the mass space velocity of 1-butylene is 10 hours -1.Evaluation result and the condition of production of catalyst are as shown in table 1.
[embodiment 4]
By specific area, it is 200 meters 2/ gram silica gel (800～1000 order) roasting under air atmosphere, sintering temperature is 400 ℃, roasting time is 12 hours; After getting 40 kilograms and the 2 kilograms sesbania powder mixing of silica gel after roasting, add in mixer, uniform stirring obtains mixture I after 45 minutes; 6 kilograms of ammonium metatungstates are dissolved in 65 kilograms of deionized waters, fully dissolve 25 kilograms of Ludox of heel and be mixed to get solution II; Solution II is added in mixture I, stir 1 hour after adding 3.2 kilograms of hydroxypropyl methylcelluloses simultaneously, extrusion, shears, and under 100 ℃ of air atmosphere, processes 4 hours, and after oven dry, under 560 ℃ of conditions, roasting obtained finished catalyst after 8 hours.The evaluation of catalyst is carried out on olefin(e) disproportionation evaluating apparatus, the 1-butylene that reaction raw materials is 99.9%, and reaction temperature is 400 ℃, and reaction pressure is 0.5MPa, and the mass space velocity of 1-butylene is 10 hours -1.Evaluation result and the condition of production of catalyst are as shown in table 1.
[embodiment 5]
By specific area, it is 160 meters 2/ gram silica gel (600～1000 order) roasting under air atmosphere, sintering temperature is 300 ℃, roasting time is 12 hours; After getting 40 kilograms and the 2.4 kilograms sesbania powder mixing of silica gel after roasting, add in mixer, uniform stirring obtains mixture I after 60 minutes; 7.2 kilograms of ammonium metatungstates are dissolved in 30 kilograms of deionized waters, fully dissolve 32 kilograms of Ludox of heel and be mixed to get solution II; Solution II is added in mixture I, stir 1 hour after adding 2.8 kilograms of hydroxypropyl methylcelluloses simultaneously, extrusion, shears, and under 85 ℃ of air atmosphere, processes 20 hours, and after oven dry, under 550 ℃ of conditions, roasting obtained finished catalyst after 25 hours.The evaluation of catalyst is carried out on olefin(e) disproportionation evaluating apparatus, the 1-butylene that reaction raw materials is 99.9%, and reaction temperature is 400 ℃, and reaction pressure is 0.5MPa, and the mass space velocity of 1-butylene is 10 hours -1.Evaluation result and the condition of production of catalyst are as shown in table 1.
[embodiment 6]
By specific area, it is 220 meters 2/ gram silica gel (400～800 order) roasting under air atmosphere, sintering temperature is 550 ℃, roasting time is 8 hours; After getting 40 kilograms and the 0.8 kilogram sesbania powder mixing of silica gel after roasting, add in mixer, uniform stirring obtains mixture I after 15 minutes; 4 kilograms of ammonium metatungstates are dissolved in 100 kilograms of deionized waters, fully dissolve 24 kilograms of Ludox of heel and be mixed to get solution II; Solution II is added in mixture I, stir 1 hour after adding 6 kilograms of hydroxypropyl methylcelluloses simultaneously, extrusion, shears, and under 95 ℃ of air atmosphere, processes 5 hours, and after oven dry, under 550 ℃ of conditions, roasting obtained finished catalyst after 10 hours.The evaluation of catalyst is carried out on olefin(e) disproportionation evaluating apparatus, the 1-butylene that reaction raw materials is 99.9%, and reaction temperature is 400 ℃, and reaction pressure is 0.5MPa, and the mass space velocity of 1-butylene is 10 hours -1.Evaluation result and the condition of production of catalyst are as shown in table 1.
[comparative example 1]
Take 7.2 grams of ammonium metatungstates and put into beaker, add 20 grams of deionized waters, after dissolving, pour equably evaporating dish into, with glass rod, stir and make tungsten ion be uniformly impregnated within 49 grams of chromatographic silica gel surfaces, dry after roasting catalyst compressing tablet, fragmentation, be sized to 20～40 object catalyst finished products, the content 12% of tungsten oxide.The evaluation of catalyst is carried out on olefin(e) disproportionation evaluating apparatus, the 1-butylene that reaction raw materials is 99.9%, and reaction temperature is 400 ℃, and reaction pressure is 0.5MPa, and the mass space velocity of 1-butylene is 10 hours -1.Evaluation result and the condition of production of catalyst are as shown in table 2.
[comparative example 2]
Take 8.8 grams of ammonium metatungstates and put into beaker, add 20 grams of deionized waters, after dissolving, pour equably evaporating dish into, with glass rod, stir and make tungsten ion be uniformly impregnated within 45 grams of chromatographic silica gel surfaces, dry after roasting catalyst compressing tablet, fragmentation, be sized to 20～40 object catalyst finished products, the content 16% of tungsten oxide.The evaluation of catalyst is carried out on olefin(e) disproportionation evaluating apparatus, the 1-butylene that reaction raw materials is 99.9%, and reaction temperature is 400 ℃, and reaction pressure is 0.5MPa, and the mass space velocity of 1-butylene is 10 hours -1.Evaluation result and the condition of production of catalyst are as shown in table 2.
[comparative example 3]
Take 3.2 grams of ammonium metatungstates and put into beaker, add 20 grams of deionized waters, after dissolving, pour equably evaporating dish into, with glass rod, stir and make tungsten ion be uniformly impregnated within 54 grams of chromatographic silica gel surfaces, dry after roasting catalyst compressing tablet, fragmentation, be sized to 20～40 object catalyst finished products, the content 5% of tungsten oxide.The evaluation of catalyst is carried out on olefin(e) disproportionation evaluating apparatus, the 1-butylene that reaction raw materials is 99.9%, and reaction temperature is 400 ℃, and reaction pressure is 0.5MPa, and the mass space velocity of 1-butylene is 10 hours -1.Evaluation result and the condition of production of catalyst are as shown in table 2.
The evaluation result of table 1 Different Preparation catalyst
The specific activity of table 2 example and comparative example

Claims (6)

1. a production method for butylene disproportionation catalyst, comprises the following steps:
A) by specific area, it is 150～350 meters 2/ gram silica gel roasting under air atmosphere, sintering temperature is 300～600 ℃, roasting time is 2～12 hours;
B) silica gel step a being obtained and sesbania powder obtain mixture I after evenly mixing in required ratio;
C) will after aequum active component wiring solution-forming, obtain solution II;
D) to the cellulose that adds solution II and aequum in mixture I, obtain finished catalyst after by extrusion, oven dry, roasting, wherein in preparation process, the part by weight of contained component is as follows, silica gel: sesbania powder: Ludox: active component: cellulose ratio is 1:(0.02～0.06): (0.6～0.8): (0.10～0.18): (0.07～0.15).
2. the production method of a kind of butylene disproportionation catalyst according to claim 1, the specification that it is characterized in that silica gel is 400～1000 orders, specific area is 200～300 meters 2/ gram.
3. the production method of a kind of butylene disproportionation catalyst according to claim 1, is characterized in that active component is ammonium metatungstate.
4. the production method of a kind of butylene disproportionation catalyst according to claim 1, is characterized in that cellulose used is hydroxypropyl methylcellulose.
5. the production method of a kind of butylene disproportionation catalyst according to claim 1, is characterized in that bake out temperature is 80～100 ℃, and drying time is 4～24 hours.
6. the production method of a kind of butylene disproportionation catalyst according to claim 1, is characterized in that steps d) in roasting condition be: the sintering temperature under air atmosphere is 520～560 ℃, and roasting time is 6～48 hours.
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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4559320A (en) * 1984-05-04 1985-12-17 Phillips Petroleum Company Catalysts for olefin conversions
CN1253855A (en) * 1998-11-18 2000-05-24 中国石油化工集团公司 Alkyl aromatics dehydrogenation catalyst
CN1490289A (en) * 2002-10-16 2004-04-21 中国石油化工股份有限公司 Method for preparing propylene by butene disproportionation
CN1490081A (en) * 2002-10-16 2004-04-21 中国石油化工股份有限公司 Fixed bed catalyst for producing propene from butylene by disproportion
CN101045214A (en) * 2006-03-27 2007-10-03 中国石油化工股份有限公司 Method for preparing propylene epoxidation catalyst
CN101428215A (en) * 2008-12-18 2009-05-13 哈尔滨工业大学 Process for producing flue gas denitration catalyst and flue gas denitration catalyst produced with the process
CN101444727A (en) * 2008-12-17 2009-06-03 中材高新材料股份有限公司 Integral honeycombed catalyst for SCR flue-gas denitration and preparation method therefor
CN102040454A (en) * 2009-10-13 2011-05-04 中国石油化工股份有限公司 Method for preparing hexane by disproportionating butylene

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4559320A (en) * 1984-05-04 1985-12-17 Phillips Petroleum Company Catalysts for olefin conversions
CN1253855A (en) * 1998-11-18 2000-05-24 中国石油化工集团公司 Alkyl aromatics dehydrogenation catalyst
CN1490289A (en) * 2002-10-16 2004-04-21 中国石油化工股份有限公司 Method for preparing propylene by butene disproportionation
CN1490081A (en) * 2002-10-16 2004-04-21 中国石油化工股份有限公司 Fixed bed catalyst for producing propene from butylene by disproportion
CN101045214A (en) * 2006-03-27 2007-10-03 中国石油化工股份有限公司 Method for preparing propylene epoxidation catalyst
CN101444727A (en) * 2008-12-17 2009-06-03 中材高新材料股份有限公司 Integral honeycombed catalyst for SCR flue-gas denitration and preparation method therefor
CN101428215A (en) * 2008-12-18 2009-05-13 哈尔滨工业大学 Process for producing flue gas denitration catalyst and flue gas denitration catalyst produced with the process
CN102040454A (en) * 2009-10-13 2011-05-04 中国石油化工股份有限公司 Method for preparing hexane by disproportionating butylene

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