Method for preparing epsilon-caprolactam

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to technology for preparing caprolactam by the cyclization reaction of derivatives of aminocaproic acid. Method is carried out by cyclizing hydrolysis of compound chosen from the group comprising aminocaproic acid esters or amides, or their mixtures. The process is carried out in the presence of water, in vapor phase at temperature 200-450°C in the presence of a solid catalyst comprising of aluminum oxide that comprises at least one macroporosity with pores volume corresponding to pores with diameter above 500 Å taken in the concentration 5 ml/100 g of above. Preferably, the specific square of catalyst particles is above 10 m2/g and the total volume of pores is 10 ml/100 g or above wherein pores volume corresponds to pores with diameter above 500 Å is 10 ml/100 g or above. Invention provides improving the process indices due to the improved properties of the solid catalyst.

EFFECT: improved preparing method.

5 cl, 2 ex

 

The present invention relates to the preparation of the lactam cyclization of esters and amides of 6-aminocaproic acid.

Aliphatic lactams, such as, in particular, Epsilon-caprolactam, are the starting compounds for obtaining polyamides (polyamide-6 from caprolactam).

One known way of obtaining the above lactams is to implement ciclismo hydrolysis of the corresponding aminonitriles, more specifically, unbranched aliphatic aminonitriles, passing in the vapor phase with water over a solid catalyst.

So, in the American patent US 2357484 described a method of producing lactam in the vapor phase, which consists in passing a mixture of water and aminonitriles over a catalyst such as activated alumina, silica gel or Biofactory acid.

In the American patent US 4628085 method for obtaining lactam in the vapor phase, which consists in bringing into contact aliphatic or aromatic aminonitriles and water with a catalyst based on silica in the form of spherical particles having a specific surface area according to BET more than 250 m2/g and an average pore diameter of less than 20 nm, and typically in the presence of hydrogen and ammonia.

Another possible way of access to the caprolactam is the reaction of cyclization of compounds such as 6-aminaka Renova acid, esters of 6-aminocaproic acid, 6-aminocaproate or mixtures thereof.

So, in documents WO 98/37063 and EP 1028109 describes how cyclization of these compounds in the presence of superheated steam. In the American patent US 5973143 describes the cyclization of these compounds in a liquid medium using alcohol as a solvent.

The mentioned methods is carried out in the absence of catalyst for cyclization.

One of the purposes of the present invention is a proposal to carry out the cyclization of these compounds in the presence of a catalyst.

More precisely, the invention consists in the method of producing the lactam cyclization in the vapour phase compounds selected from the group containing esters, or amides of 6-aminocaproic acid, or mixtures thereof, characterized in that the reaction is carried out in the presence of a solid catalyst.

In a preferred embodiment of the invention the reaction is carried out in the presence of water in the form of steam. Mentioned water allows you to limit the formation of by-products and promotes the recovery of caprolactam.

According to one feature of the invention, the catalyst according to the invention selected from the group containing metal oxides, such as oxides of aluminum, for example, zeolites, clays, phosphates of metals.

So, clay, suitable for the invention are particularly the, in particular, phyllosilicate, which are classified into groups in accordance with their nature and their physico-chemical properties, such as kaolins, serpentines, smectites or montmorillonite, illite or mica, glauconite, chlorites or vermiculite, attapulgite or sepiolites, zesannelaynep clay, allophane or imogolite and clay with a high content of aluminum oxide.

Some clays have a layered structure with expanding lattice. They have the ability to absorb various solvents, in particular water, between planes, which they are, which causes swelling of the solids due to the weakening of the electrostatic linkages between planes. Mentioned clay belong mainly to the group of smectites (or in addition to the montmorillonite group) and some of them to the group of vermiculite.

Their structure is composed of "elementary" planes, with three layers: two simple layer of tetrahedra SiO4in which part of the silicon can be replaced by other cations in the tetrahedral position, such as Al3+or, in some cases, Fe3+and between these two layers of tetrahedra layer of the oxygen octahedra, which are cations of metals such as Al3+, Fe3+, Mg2+. This octahedral layer consists of a dense packing the Cai from oxygen atoms, happening of any of the vertices of the previous tetrahedra any of the hydroxyl groups. Dense hexagonal lattice mentioned oxygen atoms contains 6 octahedral cavities.

When the metal cations occupy 4 of the mentioned cavities (2 cavity 3, as in the case of aluminum, for example, a layer called dioctahedral; when they occupy the entire cavity 3 cavity 3, as in the case of magnesium, for example, a layer called trioctadecyl.

Elementary plane above clays are carriers of negative charge that is compensated by the presence of exchangeable cations, alkaline metals such as Li+, Na+, K+, alkaline earth metals such as Mg2+Ca2+and in some cases oxonium ion H3O+. Smectites have a charge density on the surfaces that are lower than the corresponding charge densities of the clay type of vermiculite: approximately 0.66 elementary charges on the cell against 1-1,4 charges on unit cell for vermiculite.

Compensating cations are mainly cations of sodium and calcium in the smectites, the cations of magnesium and calcium in vermiculite. From the point of view of the density of charges, smectites and vermiculite are intermediate between talc and pyrophyllite, on the one hand, the plane of which are neutral, and mica and, on the other hand, is characterized by a significant charge density on the surfaces (approximately 2 per unit cell), usually compensated by ions To+.

The interlayer cations in smectites and vermiculites can be fairly easily replaced by means of ion exchange with other cations such as ammonium ions or ions of alkaline-earth metals or rare earth metals. Swelling properties of clays depend on various factors, including the density of the charge and the nature of the compensating cation.

Thus, the smectites, the charge density which is lower than the charge density of vermiculite, have characteristics of swelling, clearly better than the swelling properties of these latter and, consequently, form a very interesting class of solids. A recurring interval, or basal distance represents the shortest distance separating two crystallographically identical elementary cells arranged in two adjacent planes.

The basal distance in smectites can, thus, be achieved by the swelling values varying in the range from 1 nm to approximately more than 2 nm.

Among the "swelling" filitosa silicates type of smectites include solid natural substances of General formula

(M1n+)x/n(M2)2VI(M3)4IVO10(OH)2

where M1denotes the interlayer cation,

M2refers to the metal in octahedral position,

M3refers to the metal in the tetrahedral position,

x denotes the number of charges incurred by the cation M1.

Dioctahedral smectites:
montmorillonite

beidellite

ControlIT
(H, Na, Ca1/2)x(MgxAl2-x)VISi4IVO10(OH)2;

(H, Na, Ca1/2)xAl2VI(AlxSi4-x)IVO10(OH)2;

(H, Na, Ca1/2...)x(FeAl)2VI(AlxSi4-x)IVO10(OH)2
Trioctadecyl smectites:
hectoriteNax(LixMg3-x)VISi4IVO10(OH)2;
saponiteNaxMg3VI(AlxSi4-x)IVO10(OH)2;
stevensiteNa2xMg3-xVISi4IVO10(OH)2.

In the smectite after adsorption to saturation of water or polar organic solvent interplanar distance (between the two plosko the s) is maximum. It can reach values close to 1 nm.

Data solids are therefore potentially interesting for catalysis because of their possible specific surface area and their potential acidity is high.

According to a preferred variant of the invention the clay, which is a catalyst for the cyclization of esters or amides of 6-aminocaproic acid lactam, is a smectite. More preferably, the clay is a montmorillonite.

Unfortunately, some clays have the disadvantage that they lose their expanding nature when heated at 100°and therefore do not retain the increase in specific surface area, resulting from their expansion. So, in particular, for smectites.

In the prior art have been described various ways of introducing between the planes of smectites jumper or bridge ties, in order to get the bridge smectites, which retain a large interplanar distance after they have been heat treated.

The method, which consists in the introduction of bridging bonds formed by oligomers of the hydroxide of the metal, in particular aluminum hydroxide was described in the article LAHAV, SHAMI, SHABTAI, Clays and Clays Mineral, vol.26 (n°2), p. 107-115 (1978) and in the French patent 2394324. The formation of bridging ties, about asavanich the oligomers of mixed hydroxides of silicon and boron, described in the American patent US 4248739. Method cross-linkage of smectites by dialysis, using hydroxides of aluminum, chromium, zirconium and titanium, etc. stated in the European patent EP 0073718.

In principle, these methods consist in bringing the clay into contact with a solution containing more or less oligomerization ion particles, type hydroxylamine (in the case of aluminium). This operation is carried out usually in slabokontsentrirovannye solution at a temperature below 80°and, if possible, in the absence of turbidity caused by the beginning of the deposition of the metal hydroxide. Metal ion concentration and clay must be optimized in order was the formation of a sufficient number of strong cross-linking, and that the porosity of the clay would not be greatly reduced by the introduction of too many metal oxide.

When the interlayer ions of alkali or alkaline earth metals are replaced by protons, either directly, using a very dilute solution, or, preferably, by exchange with ammonium salt and subsequent annealing in the range from 300 to 700°, bridge smectites acquire a strong acidity, although smaller in General than the normal acidity of the zeolite type Y or mordenite, for example.

According to a preferred variant implementation of izopet the deposits of clay, used as catalyst for the cyclization of esters or amides of 6-aminocaproic acid lactam, is the bridge.

According to a special variant of the invention the catalyst may contain in addition to the clay one or more other metal compounds, often referred to as alloying additives, such as, for example, compounds of chromium, titanium, molybdenum, tungsten, iron, zinc. Among the above-mentioned alloying additives compounds of chromium and/or iron and/or titanium is considered as the most interesting. Data alloying additives are usually in wt.% in relation to the mass of clay from 0% to 10% and preferably from 0% to 5%.

Under the connection metal imply as elemental metal, metal ion, or any combination containing the metal element.

Another preferred class of catalysts according to the invention is composed of particles of the catalysts obtained by forming at least one simple or mixed inorganic oxide is at least one element selected from the group consisting of silicon, aluminum, titanium, zirconium, vanadium, niobium, tantalum, tungsten, molybdenum, iron, rare earth elements.

According to the invention consisting of particles of the catalyst has at least one macroporosity characterized by a pore volume, according to stoysin pores with a diameter greater than 500 Å greater than or equal to 5 ml/100 g

Mentioned macroporosity form mainly during the molding process of the particles by the methods described below, or such as, for example, adding poroporo.

The catalyst may be used in various forms, such as beads, milled product, the extrudates in the form of cylindrical pellets, full or solid, honeycombs, plates, and forming, if necessary, can be carried out with the aid of a binder.

First, you can touch the balls of inorganic oxides obtained by the molding method of the oil drops (or coagulation of drops). This type of beads may be, for example, obtained by the method similar to that described for the formation of balls of aluminum oxide in the patents EP-A-0015801 or EP-A-0097539. Regulation of porosity can be carried out, in particular, according to the method described in the patent EP-A-0097539, coagulation drops in suspension water dispersion of inorganic oxide.

The balls can also be obtained by sintering in a box of chocolates or a rotating drum.

You can also touch the extrudates of inorganic oxides. Mentioned extrudates can be obtained by stirring and then extrusion product based on an inorganic oxide. Regulation of porosity data of the extrudates may be the implementation of the Leno choice oxide used and the conditions for obtaining the above-mentioned oxide or mixing conditions of this oxide before extrusion. The inorganic oxide may be mixed while stirring with performi. As an example, the extrudates can be obtained by the method described in the American patent US 3856708.

Similarly beads with controlled porosity can be obtained by adding poroporo and agglomeration in the rotary drum or box of chocolates, or a method of "oil drops".

According to another characteristic of the invention, the catalyst particles have a specific surface area greater than 10 m2/g and a pore volume greater than or equal to 10 ml/100 g, while the pore volume corresponding to pores with a diameter greater than 500 Å, greater than or equal to 10 ml/100 g

According to another characteristic of the invention, the catalyst particles have a specific surface area greater than 50 m2/year

Preferably they have a total pore volume greater than or equal to 15 ml/100 g with a pore volume corresponding to pores with a diameter greater than 200 Å, greater than or equal to 15 ml/100 g, preferably greater than or equal to 20 ml/100 g

The data, consisting of particles, the catalysts may also contain at least one element selected from silicon, titanium, zirconium, vanadium, niobium, tantalum, tungsten, molybdenum, iron, rare earth elements, or can be obtained by precipitation and/or adsorption of at least one oxygen-containing compounds, at IU is e, one element selected from the group consisting of elements belonging to 1-16 groups universal classification of the elements (new classification), this list also includes the rare earth elements. These elements or compounds precipitated or adsorbed on consisting of particles of the catalyst.

In the operating method containing porous consisting of particles of the catalyst carrying oxygen-containing compounds of the elements mentioned elements are preferably selected from silicon, titanium, zirconium, vanadium, niobium, tantala, tungsten, molybdenum, phosphorus, boron, iron, alkali metals, alkaline earth metals, rare earth metals. Oxygen-containing compound is a mostly simple or mixed oxide of one or more of the elements listed above.

In this way the implementation of the porous catalyst is a preferably aluminum oxide. Preferably the above-mentioned aluminum oxide has the characteristics of specific surface area and distribution of pores defined before this.

Mass concentration of oxygen-containing compounds deposited on the porous carrier is preferably in the range from 1000 ppm to 30%, based on the weight of the element oxygen-containing compounds, relative to the weight of the catalyst. More preferably, this concentration is in the range from 0.5 to 15 wt.%.

When the porous media meet the oxides of aluminum according to the invention, usually get them by dehydration of gibbsite, bayerite, nordstrandite or their mixtures. Different ways of obtaining alumina described in the encyclopedia KIRK-OTHMER, volume 2, pages 291-297.

You can get aluminum oxide used in the present method, the contacting of hydrated aluminum oxide in finely ground form with a stream of hot gas at a temperature in the range from 400 to 1000°With, then maintaining contact between the hydrate and gas during the time period varying from fractions of a second to 10 seconds, and finally, separation of the partially digidratirovannogo of aluminum oxide and hot gases. It is possible, in particular, to refer to the method described in the American patent US 2915365.

You can also autoclaving agglomerates of alumina, obtained earlier in the aquatic environment, if necessary, in the presence of acids at temperatures above 100°and preferably in the range from 150 to 250°With, in the course of time, preferably comprising from 1 hour to 20 hours, with subsequent drying and firing.

The firing temperature regulate so that you receive the specific surface area and the volume of what we long in the areas of values specified.

Preferably the catalysts according to the invention have a specific surface area greater than 50 m2/year

In addition, they preferably have pores with a diameter larger than 0.1 μm, while the pore volume generated data pores greater than or equal to 5 ml/100 g, preferably greater than or equal to 10 ml/100 g

In a preferred embodiment of the invention, these catalysts also contain pores with a diameter equal to or greater than 0.5 μm, while the corresponding pore volume equal to or greater than 5 ml/100 g, preferably greater than or equal to 10 ml/100 g

This pore volume created by pores with a diameter greater than 500 Åpreferably larger than 0.1 μm and more preferably 0.5 microns, allows to obtain catalysts with long cycle as a catalyst for the reaction of cyclization of esters or amides of 6-aminocaproic acid lactam. Thus, these catalysts can be used in industrial methods of production of lactams.

According to the invention catalysts containing oxygen-containing compounds, which are deposited on a porous catalyst, usually get impregnated catalyst, in particular of aluminum oxide with a solution of salts or compounds of the elements mentioned above, and then drying and firing at a temperature of, avnoj or more 400° With, in order to transform, if necessary, and preferably above compounds or salts in oxygen-containing compounds, preferably oxides.

Oxides deposited on the surface of the pores of the porous catalyst.

In another embodiment, the connection elements can be added to the material forming the porous catalyst prior to its formation or during the molding process.

Firing the impregnated catalysts is preferably carried out in an oxidizing atmosphere such as air.

According to another another variant embodiment of the invention the catalyst may be a metal phosphate of the General formula:

(PO4)nHhM,(Imp)p

in which:

M denotes a divalent, trivalent, tetravalent or pentavalent element selected from groups 2A, 3b, 4b, 5b, 6b, 7b, 8, 2b, 3A, 4A and 5A of the Periodic system of elements, or a mixture of several of these elements, or M=0,

- Imp denotes a sealing connection of the main character, which represents an alkaline or alkaline-earth metal or a mixture of several of these metals, associated with protivoiona to ensure electroneutrality,

n denotes 1, 2 or 3,

- h represents 0, 1 or 2,

p denotes a number in the interval from 0 to 1/3, and corresponds to a mole is th ratio between the impregnating substance Imp and impregnated (PO 4)nHhM.

Among the metals of groups 2A, 3b, 4b, 5b, 6b, 7b, 8, 2b, 3A, 4A and 5A of the Periodic system of elements can be called, in particular, beryllium, magnesium, calcium, strontium, barium, aluminum, boron, gallium, indium, yttrium, lanthanides, such as lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutetium, zirconium, titanium, vanadium, niobium, iron, germanium, tin, bismuth.

Among the lanthanide phosphates can distinguish the first family, which combines the orthophosphate light rare earth elements, also called cerium rare earth elements including lanthanum, cerium, praseodymium, neodymium, samarium and europium. These orthophosphate are dimorphic. They have a hexagonal structure and turn into monoclinically structure when heated to a temperature in the range from 600 to 800°C.

The second family of lanthanide phosphates combines orthophosphate gadolinium, terbium and dysprosium. These orthophosphate have the same structure as that of the cerium orthophosphate rare earth elements, but have, in addition, a third crystalline phase quadratic structure at high temperature (near 170°).

The third family of lanthanide phosphates combines orthophosphate heavy rare earth elements, also called yttrium is redkozemelnye elements, includes yttrium, holmium, erbium, thulium, ytterbium and lutetium. These compounds crystallize only in quadratic form.

From the above-mentioned various families orthophosphate rare earth elements is preferable to use cerium orthophosphate rare earth elements.

You can use the phosphates of metals of the previous formula, which is a mixture of phosphates of several metals mentioned before, or mixed phosphates of several metals mentioned before, or mixed phosphates containing one or more of the metals mentioned before, and one or more other metals, such as alkaline or alkaline-earth metals.

Protivoanemi included in the formula impregnating compounds Imp, are basic. In particular, you can use the following ions: hydroxyl, phosphate, hydrogen phosphate, dihydrophosphate, chloride, fluoride, nitrate, benzoate, oxalate, except that these links would be restrictive.

The molar ratio R is preferably in the range from 0.02 to 0.2.

If we turn to the usual methods of obtaining phosphates (such as described in particular in "PASCAL P. Nouveau traité' de chimie minerale" tome X (1956), pages 821-823 and in "GMELINS Handbuch der anorganischen Chemie" (8emeedition), volume 16(C), pages 202-206 (1965), one can distinguish two basic ways of access to the phosphates. With one of the second side, the precipitation of the soluble metal salt (chloride, nitrate) ammonium phosphate or phosphoric acid. On the other hand, dissolution of the oxide or metal carbonate (insoluble) with phosphoric acid, usually by heating, and subsequent precipitation.

Precipitated phosphates obtained according to one of the specified paths, can be dried, treated with an organic base (such as ammonium hydroxide) or inorganic base (such as a hydroxide of an alkali metal) and subjected to firing, with three of the above operations can be performed in the order shown or in a different order.

Phosphates of metals of the previous formula, for which the index p is greater than 0, can be obtained by impregnating compounds (PO4)nHnM, prepared according to one of the methods described before, with a solution or suspension Imp in a volatile solvent, such as preferably water.

Results the better, the more soluble is the Imp and the more freshly prepared is the compound (PO4)nHhM.

Thus, the preferred method of obtaining the above-mentioned phosphates is:

(a) the implementation of the synthesis of compounds (PO4)nHhM ; subsequent, preferably without isolation (PO4)nHhM of the reaction medium,

b) the introduction of PR is mityayevo substances Imp in the reaction medium,

(C) the Department, if necessary, residual liquid from the solid reaction product, and

d) drying and, if necessary, firing.

The characteristics of these catalysts and, in particular, their resistance to deactivation can also be improved by burning. The firing temperature will preferably be in the range from 300 to 1000°and preferably from 400 to 900°C. the duration of the calcination may vary within wide limits. For information, it is usually in the range of from 1 hour to 24 hours.

Among the catalysts of formula (II), preferable in the method according to the invention, can be called, more specifically, lanthanum phosphate, calcined phosphate of lanthanum, the lanthanum phosphate associated with the derived caesium, rubidium or potassium, consisting of calcined cerium phosphate, cerium phosphate, associated with the connection of cesium, rubidium or potassium, samarium phosphate associated with the connection of cesium, rubidium or potassium, aluminum phosphate, aluminum phosphate, associated with the connection of cesium, rubidium or potassium hydroxide, calcined phosphate, niobium, phosphate, niobium, coupled with a compound of cesium, rubidium or potassium hydroxide, calcined phosphate, zirconium, zirconium phosphate, coupled with a compound of cesium, rubidium or potassium.

The cyclization reaction requires the presence of water, preferably, in order to limit the formation of obecnych products. The molar ratio between water and participating in the reaction zillisheim connection is usually in the range from 0.5 to 50, preferably from 1 to 20.

Ciclismo compound and water can be introduced into the reactor in the form of their mixtures in the vapor state, or may be introduced into the reactor separately. You can pre-evaporation of the reagents, which then circulate in the mixing chamber.

Without inconvenience, as a carrier you can use any inert gas, such as nitrogen, helium or argon.

The temperature at which carry out the method according to the invention, should be sufficient to ensure that the reagents would be in the form of vapour. Usually, it is between 200 and 450°and preferably between 250 and 400°C.

The contact time between zillisheim compound and the catalyst is not critical. It may change, in particular in accordance with your installation. Mentioned contact time is preferably in the range from 0.5 to 200 seconds, and more preferably from 1 to 100 seconds.

Pressure is not a critical parameter of the process. Thus, it is possible to operate at pressures from 10-3bar up to 200 bar. Preferably the method will be carried out at a pressure of from 0.1 to 20 bar.

It is not excluded to use a solvent inert in the reaction conditions, the th as for example, alkane, cycloalkane, aromatic hydrocarbon or one of the listed previous halogenated hydrocarbons in the form, and, thus, to be in the reaction stream in the liquid phase.

Tests were carried out according to the operating method described below.

The medium containing methylaminopropyl in solution in water or in methanol, is injected by moving the syringe with the speed of 4.3 l/h in a tube made of Pyrex, located vertically in the furnace, the temperature of which is equal to 300°and which is blown by a stream of nitrogen 5.3 l/h of the Catalyst in the amount of 2 g (macroporous alumina supplied to the sale by the company PROCATALYSE under the name of SCM 139 XL, placed between two layers of glass powder with a volume of 5 ml. injection box is directly above the upper glass layer, the flow of nitrogen carries products through the catalyst bed. At the exit from the furnace gases condense in the tube placed in an ice bath, and then analyzed by gas chromatography.

Example 1:

The environment contains 60 wt.% methylaminopropane.

Conversion of methylaminopropane is full, the selectivity of conversion to caprolactam is 26 %.

Example 2:

The environment contains 40 wt.% methylaminopropane.

Conversion of methylaminopropane is full, the selectivity of conversion to caprolactam is avna 68 %.

1. A method for production of Epsilon-caprolactam collisuem hydrolysis of compounds selected from the group consisting of esters or amides of 6-aminocaproic acid, or mixtures thereof in the presence of water, wherein the interaction is carried out in the vapor phase and in the presence of a solid catalyst consisting of aluminum oxide containing at least one macroporosity characterized by a pore volume corresponding to pores with a diameter greater than 500 Å, greater than or equal to 5 ml/100 g

2. The method according to claim 1, characterized in that it consists of particles of the catalyst has a specific surface area greater than 10 m2/g and a total pore volume greater than or equal to 10 ml/100 g, while the pore volume corresponding to pores with a diameter greater than 500 Å, greater than or equal to 10 ml/100 g

3. The method according to claim 1, characterized in that the catalyst has a specific surface area greater than 50 m2/year

4. The method according to claim 1, characterized in that the catalyst has a total pore volume greater than or equal to 20 ml/100 g, while the pore volume corresponding to pores with a diameter of more than 70 Å, greater than or equal to 20 ml/100 g

5. The method according to claim 1, characterized in that the temperature at which it is carried out, is in the range from 200 to 450°and preferably from 250 to 400°C.



 

Same patents:

FIELD: chemistry of lactams' derivatives.

SUBSTANCE: the present innovation deals with obtaining N-(2-chloroalkyl)- and N-alkyl-aromatic derivatives of lactams of the following general formula: , where R=H, Cl, R'=(CH2)3, (CH2)5 which could be modifiers of unsaturated carbon-chain caoutchoucs and rubber mixtures based upon them. The suggested method for obtaining the mentioned N-substituted lactams deals with combining N-chlorolactams and allyl benzene, moreover, as N-lactams one should apply either N-chlorobutyrolactam or N-chlorocaprolactam. The process should be carried out at molar ratio of N-chlorolactam to allyl benzene being equal to 1-1.15:1, at availability of a catalyzer as mono-tertiary-butylperoxy-α-methylmethoxyethoxyethyl ether of ethylene glycol taken at the quantity of 0.4-4.0% weight, in the medium of inert solvent, for example, chlorobenzene at 100-125° C for about 15-20 min. The innovation enables to shorten terms of reaction by 20-30 times, simplify the way for obtaining target products and widen the assortment of the obtained compounds, as well.

EFFECT: higher efficiency.

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FIELD: catalyst preparation.

SUBSTANCE: invention relates to supported catalysts and provides a method for preparing catalyst-containing solid product comprising step, wherein ceramic carrier is applied onto metallic surface, and depositing catalytically active material onto ceramic carrier, which was preliminarily coated with supporting porous metallic material, ceramic carrier being applied onto and/or into supporting porous metallic material. Invention also describes device used in preparation of catalyst-containing solid product for applying supporting porous material onto inside or outside metallic surfaces of the hollow body.

EFFECT: increased stability of catalyst.

7 cl, 2 dwg

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