Method of producing propylene and butene-1

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing propylene and butene-1 from ethylene at high temperature in a continuous or periodic mode in the presence of a catalyst deposited on a support. The method is characterised by that the process is carried out at temperature 75-110°C in the presence of a catalyst containing the following in wt %: Re - 5-15, B2O3 - 3-10, γ-Al2O3 - the balance.

EFFECT: use of the present method simplifies the process and increases selectivity thereof during formation of propylene, and also enables to obtain a mixture of propylene and butene-1 as the end product.

2 cl, 6 ex, 2 tbl

 

The present invention relates to the field of organic chemistry, in particular to the process of conversion of ethylene, namely a previously unknown method for producing propylene and butene-1 directly from ethylene registersystem heterogeneous catalyst.

Propylene is an important petrochemical product, in particular, to obtain polypropylene, Acrylonitrile and propylene oxide. In the chemical industry propylene, together with ethylene, get, mainly in oil cracking. In the future propylene will be more popular than ethylene, because of its use for the preparation of polypropylene and propylene oxide. Propylene usually get or cracking of crude oil (69%) or catalytic cracking gasoline. Only 2-3% of the total amount of propylene falls on the reaction of dehydrogenation of propane. This method of production of propylene is associated with certain difficulties. The first source of propane must be located near the region's consumption of propylene. The second reason is economic. Propane is often more expensive than propylene. In addition, the process itself is costly, in particular, energy. Currently propylene is also produced by metathesis reaction, for which required, in addition to ethylene, butene-2, the latter has preliminarily who must be obtained by the reaction of ethylene with subsequent isomerization of butene-1 to butene-2 [M.Taoufic, E.Le Roux, J.Thivolle-Cazat, J.-M.Basset. Angewandte Chemie. 2007, 119, 7340 tel. Direct transformation of ethylene into propylene catalyzed by a tungsten hydride supported on alumina: trifunctional single-site catalysis].

Butene-1 is the raw material for the production of polybutene-1, ethylene-butenova plastics (including low density polyethylene), methyl ethyl ketone, acetic acid and other products. To obtain a propylene-butenova plastics (plastics) as a valuable product with good strength characteristics is used a mixture of propylene and butene-1. Usually butene-1 is produced by catalytic dimerization of ethylene. The process is carried out at elevated pressures (15-20 ATM) and a temperature of 50-60°C using a homogeneous Ti-containing catalyst, requiring special conditions for preparing and using in the process of producing butene-1. In addition to butene-1 as side products are formed which are difficult to separate oligomers, resulting in the obliteration of the polyethylene walls of the reactor and feed ethylene [Institute of problems of chemical physics RAS, Chernogolovka. Exhibition: the Forum and the presentation of new scientific and industrial technologies "Archimedes", "High technologies of XXI century". the 15th international exhibition "Chemistry 2009". The exhibition "Innovation Sciences 2010"].

From literature is known just a few examples of the conversion of ethylene to propylene. Thus, the described prevremeni the ethylene to propylene using a catalyst Mo(CO) 6deposited on Al2O3without details of a process [P.P.O''neill, J.J.Rooney. J. Am. Chem. Soc., 1972, 94, 4383. Direct transformation of ethylene to propylene on an propylene metathesis catalyst].

The conversion of ethylene to propylene was described in the presence of a catalyst containing 2.8 wt.% Mo/SiO2[T.Katsumi, T.Kenichi. J. Chem. Soc., Faraday Trans.1 1987, 83(6), 1859. Reactive intermediate for the ethylene homologation reaction on molybdena-silica catalysts]. However, the basic process indicators (conversion, selectivity) were low.

The closest solution of the problem is the method of obtaining propylene from ethylene in a continuous or periodic modes in the presence of a tungsten catalyst supported on alumina [US Pat no. 7638672, 2009]. The process is conducted at a temperature of 150°C. the Main byproducts are butenes (butene-1, butene-2, isobutene) and hexene.

The disadvantages of this process is not sufficiently high selectivity in the formation of propylene (maximum selectivity for propylene is 93 wt.% when the conversion 6-10 wt.%) and a higher reaction temperature (150°C). However, the main disadvantage of the proposed process is the use of freshly prepared catalyst in situ in a special unit (the box) with the use of harmful ORGANOMETALLIC compounds in the environment of hydrogen without traces of air. Inadmissibility of getting air in the cooking process, and the use of the catalyst. In the presence of even traces of air, the conversion of ethylene to propylene is not happening. All this complicates the process.

The present invention is to simplify the process and increase its selectivity in the formation of propylene, as well as the possibility of obtaining a mixture of propylene and butene-1 as the target product.

This object is achieved by the proposed method of obtaining propylene and butene-1 ethylene in a continuous or batch mode at a temperature of 75-110°C in the presence of a catalyst containing, wt.%: Re - 5-15, In2About3- 3-10, γ-Al2O3- the rest.

The process according to the invention is carried out at a relatively low temperature 75-110°C.

For preferential receipt of propylene, the process is conducted in a continuous mode at a flow rate of the feed 75-100 h-1. The selectivity for propylene reaches 96,7 wt.%, and conversion of 47.9 wt.%.

The carrier of γ-Al2O3has a specific surface area of 196 m2/g, granule size of 0.1 to 1.5 mm, preferably 0.3 to 0.6 mm

The catalyst is prepared by impregnation of γ-Al2O3a solution of N3IN3in distilled water, followed by drying for 1 h in air, then 1.5 h at 150°C. Next, the resulting solid mass is impregnated with the aqueous solution of NH4ReO4, allowed to stand for 1 hour in air, and then 1.5 hours at 150°C, place the t in the reactor and calcined in a stream of dry air at a temperature of 450-600°C for 1 hour.

In contrast to the catalyst of the prototype of the proposed catalyst calcined in a stream of dry air at a temperature of 450-600°C., preferably 480-550°C. the Catalyst can be repeatedly regenerated in the above conditions. The process of conversion of ethylene is carried out in an air environment.

The process according to the invention can be performed periodically in a static reactor. This method is preferred for preferential receipt of butene-1. In this way, the butene-1 obtained for the first time, as the product formed from propylene. However, for selective receipt of propylene, the process is preferably carried out in flowing conditions, when ethylene is introduced continuously. Compared with the prototype process is carried out at lower temperatures and with higher selectivity. In contrast to the prototype of propylene according to the invention is produced directly from ethylene without intermediate stages.

The technical result of the proposed method is a simplification of the process by holding it in an atmosphere of air, increasing the selectivity of obtaining propylene to 96.7 wt.%, obtaining butene-1 with access to 83,8 wt.%, as well as the mixture of propylene and butene-1 which can later be used without separation to obtain a propylene-butenova plastics.

The invention soo which corresponds to the criterion "novelty", as known in the scientific-technical and patent literature does not include a full set of features characterizing the present invention. The invention also meets the criterion of "inventive step"as the process in the presence of a catalyst to Re-In2About3/Al2O3to obtain propylene and butene-1 was not obvious, since according to literature data [K.I.Ivin, J.C.Mol. Olefins metathesis and metathesis polymerization, Academic Press, 1997, 93] Re/Al2O3the catalyst is not active in the conversion of ethylene and at Re/In2O3this process was not conducted.

The following examples illustrate the present invention but do not limit its scope.

Example No. 1. The method of preparation of the catalyst.

For the preparation of the catalyst charge of 1.46 g of N3IN3, dissolved in 21 ml of distilled water and impregnated with the obtained solution of 16.4 g of γ-Al2O3(S beats. 196 m2/g granules of 0.3-0.6 mm). Dried 1 h in air, then 1.5 h at 150°C. Next of 8.25 g of the obtained solid mass is impregnated with the aqueous solution of NH4ReO4(10 ml of N2Oh and 0.71 g NH4ReO4). Allowed to stand for 1 hour in air, and then 1.5 hours at 150°C, are placed in a reactor and calcined in a stream of dry air (6 l/h) at 530°C for 1 hour. The resulting catalyst has a composition, wt.%: 6 Re, 5 V2O3, 89 γ-Al2O3./p>

Similarly receive catalysts with different content components, the compositions of which are given in tables 1 and 2.

Example No. 2. Catalytic conversion of ethylene in a static reactor.

0.71 g of the catalyst prepared according to example No. 1 of the composition, wt.%: 6 Re, 5 V2O3, 89 γ-Al2O3placed in a glass flask of 50 ml volume filled with air, and then poured into the flask and 1.4 ml of n-octane and miss ethylene to establish a pressure of ethylene 80-90 kPa and heated the mixture at 8-10°C/min to a temperature of 91°C at a rotation speed of the stirrer approximately 100 rpm Over 1.7 hours the yield of propylene 33.2 wt.%, as butene-1 - 58,7 wt.% the total conversion of ethylene 91,9 wt.%.

Table 1 shows the results for various combinations of catalyst and process conditions in periodic mode.

Table 1.
# examplethe composition of the catalyst, wt. %temperature op.,0time slave., hyield, wt.%conversion, wt.%
ReB2O3 Al2O3propylenebutene-1
3.71083910,6321,860,882,6
2,0of 37.9of 60.598,4
4.9586902,018,976,795,6
2,511,7is 83.895,5
5.123852,532,665,598,1

As can be seen from table No. 1, the proposed method allows to obtain butene-1 with a sufficiently high yield, reaching 83,8 wt.%, at high conversion of ethylene.

Example No. 6. Catalytic conversion of ethylene to propylene and butene-1 in a flow reactor.

of 1.75 g of the catalyst prepared as in example No. 1, composition, wt.%: 12 Re, 5 V2O3, 83 γ-Al2O3loaded into a quartz glass reactor, preheated in air to a temperature of 100°C, then let ethylene with a bulk velocity 80 h-1. Through 0,62 hours, the conversion of ethylene is 23.9 wt.% when the selectivity to propylene and butene-1 94 and 6 wt.% respectively.

Table 2 shows the results for various combinations of catalyst and process conditions in a continuous mode.

tr>
Table 2.
No. when
measure
the catalyst composition, wt.%Top.,0Vabout.,h-1time slave., h conversion, wt. %selectivity, wt. %
propylenebutene-1
ReIn2O3Al2O3
7.12583100800,520,295,54,5
0,818,4964,0
8.958693900,520,793,76,3
0,6324,3955,0
0,813,2a 94.25,8
9.71083110900,7519,393,56,5
0,8822,393,56,5
1,018,7946,0
10.958687750,71694,45,6
0,8318,2955,0
1,018,9for 95.24,8
11.6589110800,828,55545
0,947,96733
1,0437723
12.559087911,521,496,73,3
1,7529,393,76,3
2,027,494,3the 5.7
the 2,5of 21.2946
13.15580951000,819,7for 93.46,6
1,019,494,55,5

As can be seen from table No. 2, the proposed method is superior in selectivity in the formation of propylene prototype, and at higher conversions. In addition, according to example No. 11 in certain conditions it is possible to obtain almost the equilibrium mixture of propylene and butene-1.

1. The method of obtaining propylene and butene-1 ethylene at elevated temperature in a continuous or periodic mode in the presence of a catalyst supported on a carrier, distinguishing the I, the process is conducted at a temperature of 75-110°C in the presence of a catalyst containing, wt.%:

Re5-15
In2About33-10
γ-Al2O3rest

2. The method according to claim 1, characterized in that the preferential receipt of propylene, the process is conducted in a continuous mode at a flow rate of the feed 75-100 h-1.



 

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