The method of producing allylchloride and reactor for its implementation

 

(57) Abstract:

The invention relates to a method of producing allylchloride to the reactor for its implementation. The reaction is carried out at a molar ratio of propylene and molecular halogen with at least a 2.5: 1 at a temperature of from 400 to 525°C. the Reaction is carried out in the area, representing the reactor continuous mixing (LDCs), with the subsequent flow of the reaction mixture in the area, representing the ideal reactor displacement, where the reaction is continued until complete reaction of the molecular halogen. The reactor includes a housing with walls forming a chamber, which includes a zone representing the reactor LDCs connected to the area of the cylindrical reactor. The ratio of the volume zone LDCs to the total area of the LDCs and the cylindrical zone of the reactor is from about 0.1: 1 to about 0.9:1. The technical result is an increase in the yield of the target product by reducing the decomposition of allylchloride, which is achieved by improving the mixing of reagents. 2 S. and 9 C.p. f-crystals, 1 tab., 2 Il.

The present invention concerns a gas-phase reactions of halogenation and reactors used in these reactions.

It is well known that propylene and chlorine to reagire allylchloride. See, for example, Samples et al., U.S. patent 3054831 (18 September 1962). In such reactions propylene and chlorine react at a temperature of from 400 to 500oC. the Molar ratio of propylene to chlorine in the reactor is typically between 3:1 and 5:1. The conversion of chlorine is usually around 100% and the conversion of propylene is usually in the range from 20 to 35%.

After separation of propylene from the reaction mixture the reaction product typically contains from 70 to 80 wt.% allylchloride, and other products mainly are a mixture of a large number of different chlorinated alkanes and alkenes. The reaction also produces small amounts of soot (carbon). Soot is deposited in the reactor during the whole time of his work up until the reactor is stopped for cleaning.

The product composition depends on the temperature. Temperature below approximately 400oC favour the formation of excessive dehalogenating by-products, while temperatures above approximately 500oC favor the decomposition of allylchloride with the formation of increased amounts of carbon black and other products. See, for example. Samples et al., (see above) column 1, lines 15-25; and the United Kingdom patent 761831 (published November 21, 1956), column 1, lines 28-40. what to temperature control is difficult, because the reaction is highly exothermic. The reagent should be introduced into the reactor at a temperature substantially lower than the desired reaction temperature, or the heat of reaction can raise the temperature in the reactor to an unreasonably high level. Even in such a case, the reactor can be hot and cold areas, because of the presence of which the formation of undesirable large amounts of side reaction products.

Been suggested several ways to improve mixing in the reactor, in order to minimize temperature differences in different parts of the reactor.

(1) Vandijk, U.S. patent 2763699 (published 18 September 1956), the United Kingdom patent 761831 (published November 21, 1956) and the United Kingdom patent 765764 (published 9 January 1957) describe the various spherical, ovoid, oval, etc. reactors that can be used to obtain allylchloride. These spherical reactors still have a tendency to soot pollution. In the United Kingdom patent 761831 shown that high outputs allylchloride obtained by using the row of three connected in series spherical reactors. A row of three connected in series spherical reactor is effectif from one reactor to another. This system is also particularly sensitive to contamination with soot, because the soot formed in the first reactor, must pass through a narrow injectors and piping subsequent reactors.

(2) Samples et al., U.S. patent 3054831 describes a complex system of injection to maintain turbulence and mixing within the reactor.

(3) Yamamoto et al., published Japan's bid 48-26732 (published 15 August 1973) describes a circular tube reactor with the guide walls near the injector to enter reagents to improve the mixing.

(4) Spadio et al., patent Poland 136334 (published 20 February 1987) offers a preliminary mixing of reagents at low temperature before putting them into the reactor.

All of these reactors have a tendency to form soot. They must be periodically shut down for cleaning. If sooting is reduced, the reactor is able to work longer between stops. The required reactor and/or process that has a high selectivity for allylchloride and which produces very little soot, and no need for constant heating and cooling of the reaction products.

One aspect of the present invention is a method of obtaining allylchloride reaction from 400 to 525oC, characterized in that:

(1) propylene and molecular halogen partially react in the zone, representing a continuously operating reactor mixing" (LDCs) ("continiously stirred tank reactor", CSTR) at a temperature of from 400 to 525oC; and

(2) the reaction mixture from stage (1) is fed into the zone, representing the ideal reactor displacement (plug-flow reactor, where the reaction proceeds at a temperature of from 400 to 525oC up until almost all chlorine is not used.

(For practical purposes, the term "continuously operating reactor mixing" (LDCs) do not necessarily imply or exclude the presence of agitators or other mechanism for mixing. "LDC" means that the reaction zone is of such a construction, which is designed to create turbulence, which minimizes temperature gradients and concentration of reagents in the zone LDCs).

The second aspect of the present invention is a reaction vessel containing:

(1) approximately spherical, ovoid or oval zone of the reactor;

(2) the tubular reactor attached to spherical, ovoid or oval area of the reactor;

(3) one or more inlets for entry of the gaseous reagents in a spherical, oval-shaped product.

LDC provides exceptionally good mixing, in order to quickly bring the reactants to the desired temperature with minimal thermal gradients. On the other hand, we found that the reactors LDCs, as, for example, spherical reactors, have a tendency to excessive back mixing, when they are the only reactor used for the reaction. Excessive back mixing increases the sooting and further chlorination of allylchloride education dichlorsilane by-products, as part of the product remains in the reactor for too long.

In the present invention the reaction starts in the area of ongoing reactor mixing to ensure good mixing, but the reaction mixture is then transported into the reactor ideal displacement before the completion of the reaction, in order to minimize the formation of by-products. The method of the present invention is used to obtain allylchloride high purity with little formation of by-products. The reactor of the present invention can be used in this way or in other ways, which include reaction in the vapor phase.

In Fig. 1 shows a side view of the reactor,inogo displacement (2); the inlet to the input of the first reagent (3); input entry opening of the second reagent (4); and an outlet for exhaust products from the reactor (5).

Fig. 2 shows a top view of the spherical zone of an ongoing reactor mixing (1), which is part of the reactor of Fig. 1. It contains an area of spherical LDCs (1); the inlet to the input of the first reagent (3); input entry opening of the second reagent (4); and output (6) to flow partially reacted mixture in the reactor of ideal displacement. This illustration shows that the inputs (3) is not aimed directly at the center of the sphere, but that the entrance to the reactor is directed at an angle to the direction of the center.

In many respects, the method of the present invention is carried out under normal conditions, the vapor halogenation of propylene with the aim of obtaining allergological. Propylene and halogen react with each other at elevated temperature. Halogen preferably represents chlorine or bromine, and most preferably chlorine. The molar ratio of propylene to the halogen in the feed to the reactor is at least a 2.5:1 and preferably at least 3:1. The molar ratio of propylene to the halogen in the feed to the reactor predpochtitelnei 400oC, preferably at least about 425oC, more preferably at least about 450oC and most preferably at least about 460oC. the Temperature in the reactor is not more than about 525oC, preferably not more than about 500oC and more preferably not more than about 480oC.

In most cases, it is desirable to pre-heat the propylene before it is fed into the reactor, especially when the ratio of propylene to chlorine is high. The optimal degree of pre-heating depends on the reactor and the reaction conditions, and it can easily identify experts in this field experimentally. Preheating should be sufficient to maintain the temperature in the reactor at the desired level. If the reagents to warm up too much, the temperature in the reactor may rise too high, which will lead to side reactions and sazheobrazovanie. Preferably propylene prior to feeding into the reactor heated to a temperature of from 150 to 350oC. For this step is preferably used as the heat taken from the mixture leaving the reactor.

The halogenation reaction proceeds in two different zones. On the lane which can be any reactor, which is continuous turbulence or agitation in order to quickly bring the reactants to the reaction temperature and to minimize temperature gradients and concentration within the zone of the LDCs. Examples of reactors LDCs are described in the following publications: Vandijk et al., U.S. patent 2763699 (September 18, 1956 ) and G. Froment and K. Bischoff, Chemical reactor Analisys and Design, pages 420 and beyond (J. Wiley and Sons, 1979). The reactor LDCs is preferably approximately spherical, ovoid or oval, and more preferably approximately spherical. It preferably has a smooth inside surface except input of the reactants and preferably does not contain any protruding from the walls of the devices, reflective walls or agitators.

Propylene and halogen can be mixed in the area of LDCs or before they will be introduced in the area of the LDCs, as they are well micromachined with each other immediately after their introduction in the area of the LDCs. Good micromachine can be obtained by using intersecting streams of propylene and halogen, which have a high value of shear moment relative to each other as in the area of the LDCs, and the pipe leading to the zone of the LDCs. For example, when propylene and halogen are introduced separately, etc the ez inlet. If the reactor does not provide adequate micromachine, then formed a very large amount of soot.

The inlet zone LDCs preferably not direct the flow of the reagent toward the exit of the reactor, which leads to a zone of the reactor of ideal displacement. The angle between the flow direction, in which the reagents are introduced into a zone of LDCs, and the direction of flow, in which the reaction mixture leaves the zone LDCs (or the direction of the flow entering the reactor ideal displacement), is preferably not more than approximately 90o.

In addition, it may be desirable to enter into a zone of LDCs small amount of diluent in order to maintain the desired reaction temperature. The diluent preferably is either galoidovodorodov or gas which is inert to the reactants and to the reaction vessel in the reaction conditions. Examples of suitable inert diluents are nitrogen, helium and other noble gases. The molar ratio of solvent to reactants in the feed to the reactor flows preferably less than 3:1, more preferably less than 2:1 and most preferably less than 1:1. The molar ratio of diluent to the reagents may be the e preferably at least the 0.05:1 and most preferably at least 0,1:1.

The average time of stay in the zone LDCs preferably chosen so that the halogenation reaction took place not more than a depth of 90% (measured by the flow rate of chlorine, which can approximately be determined by measuring the temperature increase in the area of the LDCs. The halogenation reaction preferably takes place at least to a depth of about 50% in the area of LDCs and more preferably at least to a depth of approximately 75% in the area of the LDCs. The concentration of unreacted halogen in the mix, out of the zone LDCs, is preferably at least 10% of the concentration of chlorine in the reagents supplied in the area of the LDCs. The concentration of unreacted halogen, more preferably is not more than about 50% of the concentration in the source reagents and most preferably no more than about 25% of the concentration in the original reagents.

The reaction mixture from the zone of LDCs is in the area of reactor ideal displacement. Zone of the reactor of ideal displacement preferably is a simple tubular reactor. Temperature in the reactor of ideal displacement is in the same range and has toctitle is sufficient to to all chlorine reacted, still remaining in the reaction mixture.

The ratio of the volume zone LDCs to the total area of the LDCs and the core ideal of displacement is preferably from 0.1:1 to 0.9:1 and more preferably from 0.4:1 to 0.85:1. In the case when the area of the LDCs is approximately spherical, and the area of the reactor ideal displacement is a tubular reactor, the ratio of the inner diameter of the spherical portion to the inner diameter of the tubular portion of the reactor is preferably from 1.4:1 to 5:1. The reaction mixture from zone LDCs preferably passes directly into the reactor ideal displacement, without passing through any other pipe or transporting the environment, in order to minimize the need for cooling and subsequent heating of the reagent.

The total residence time of the reactants in the reactor is preferably on average from 0.3 seconds to 7 seconds. The optimal duration of the reaction varies depending on the reaction conditions and can be easily determined by the expert in this field.

In the above schemes propylene is fed in approximately spherical part of the reactor (1) pipeline (3). Propylene m is positive between these two extreme directions, as shown in Fig. 2. Chlorine is introduced into approximately spherical part (1) pipeline (4). Streams of propylene and chlorine intersect each other inside a spherical part (1) almost immediately after entering the reactor. The streams are mixed and partially react in a spherical part (1) of the reactor. The reaction mixture emerging from the spherical part of the reactor, flows into the tubular part (2). This mixture still contains a significant concentration of molecular chlorine. She has a temperature of about 450oC. Chlorine reacts in the tubular part (2) of the reactor as long as the concentration of molecular chlorine becomes approximately equal to zero at the end of the tubular reactor. Product flow is discharged through the outlets (5).

Of course, the reactor must be made of materials that do not affect the reaction and does not decompose under the reaction conditions. Examples of suitable materials are glass and Nickel alloys such as Nickel-chromium alloy INCONEL (manufactured by the International Nickel Co."). The reactor is preferably made of INCONEL.

After removal of unreacted propylene, galoidovodorodov and inert diluent, the product stream preferably contains at least about 80% of allylchloride, more inflorida and most preferably at least about 86% of allylchloride. The product stream preferably contains less than 2% of dichloropropane and more preferably less than 1% of dichloropropane. The product stream preferably contains almost no molecular chlorine. The concentration of unreacted molecular chlorine is preferably not more than about 1 wt.%, more preferably no more than about 0.5 wt.% and most preferably not more than about 0.1 wt.%.

This invention is more specifically illustrated by the following examples.

The following examples are only for illustration purposes, and should not assume that they limit the scope of the description or claims. Unless otherwise noted, all parts and percentages are molar.

Examples 1-4

Were made of two glass reactor having approximately spherical zone LDCs and zone tubular reactor of ideal displacement with dimensions shown in the table. Spherical zone LDCs in each reactor had a nozzle diameter of 0.5 mm for the introduction of propylene and a nozzle diameter of 0.5 mm for the introduction of chlorine located in such a way that the streams of reactants are faced with each other immediately after their entry into the reactor. The number of pairs of nozzles to enter the reagents PRIOME in the table. Helium was introduced through the hole to enter the chlorine simultaneously with chlorine. Propylene was pre-heated to the temperature shown in the table. The reactor was heated and insulated to maintain the desired reaction temperature. The residence time in the reactor and the temperature of the reactor shown in the table. The products were isolated and analyzed by gas chromatography (GC) analysis on the chromatograph Hewlett Packard 5890 with column I and W Scientific DB-1. The product composition is shown in table.

1. The method of producing allylchloride by the reaction of propylene with molecular halogen at a molar ratio of at least 2.5 to 1, at a temperature of from 400 to 525oC, wherein propylene and molecular halogen react in the zone representing the reactor continuous mixing (LDCs) with partial conversion of propylene and halogen in allergological with the subsequent flow of the reaction mixture in the area, representing the ideal reactor displacement, where the reaction proceeds at a temperature of 400 to 525oC to practically complete reaction of molecular halogen.

2. The method according to p. 1, wherein the molecular halogen is a chlorine.

3. The method according to any the perfect actor displacement is cylindrical.

4. The method according to p. 1, characterized in that the molar ratio of propylene to the halogen fed to the reactor is not more than 5 : 1.

5. The method according to any of the preceding paragraphs, characterized in that the temperature in the zone of LDCs is from 425 to 500oC.

6. The method according to any of the preceding paragraphs, characterized in that the ratio of the volume zone LDCs to the total area of the LDCs and the core ideal of displacement is from 0.4 : 1 to 0.85 : 1.

7. The method according to any of the preceding paragraphs, characterized in that the range of concentrations of unreacted chlorine in the reaction mixture, leaving areas of LDCs, is from 10 to 50% of the concentration in the original reagents.

8. The method according to any of the preceding paragraphs, characterized in that the total residence time of the reactants in the reactor ranged from 0.3 to 7 C.

9. The reactor for the production of allylchloride, comprising a housing with walls forming a chamber, which includes a zone representing the reactor continuous mixing (LDCs), connected to the area of the cylindrical reactor, one or more inputs to the reactor to enter the gaseous reagents in the area of LDCs, means for passing a gas stream from the zone of LDCs in the area of cilin is Toda gaseous product from the zone of the cylindrical reactor, moreover, these areas of LDCs and cylindrical reactor are specified amount, wherein the ratio of the volume zone LDCs to the total area of the LDCs and the cylindrical zone of the reactor is from about 0.1 : 1 to about 0.9 : 1.

10. The reactor under item 9, characterized in that the ratio of the volume zone LDCs to the total area of the LDCs and the cylindrical zone of the reactor, which represents the ideal reactor displacement is from 0.4 : 1 to 0.85 : 1.

11. The reactor under item 9, characterized in that the area of the LDCs is spherical, ovoid or oval.

 

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