Method for preparing oxirane involving isolation of oxirane from reaction mixture

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for preparing oxirane. Method involves interaction of olefin and peroxide compound in the presence of catalyst and solvent in at least two in-line fitted reactors and each reactor comprises part of catalyst. Method is carried out for two successive epoxidation reactions with intermediate distillation. Method provides reducing formation of by-side substances.

EFFECT: improved preparing method.

10 cl, 1 dwg, 2 ex

 

The present invention relates to a method of obtaining oxirane interaction of the olefin with a peroxide compound in the presence of a catalyst and solvent. The invention in particular relates to the production of propylene oxide or epichlorohydrin) by epoxidation of propylene (or allyl chloride) with hydrogen peroxide in the presence of a catalyst containing TS-1.

A known method of producing propylene oxide by reacting propylene with a peroxide compound in the presence of TS-1. For example, in U.S. patent 5849937 similar process is carried out in several reactors arranged in series.

The applicant found that this method has the disadvantage in the formation of by-products, if, for example, peroxide compounds using aqueous hydrogen peroxide solution, and the solvent used methanol. Indeed, if these conditions are propylene oxide, by-products are formed by reaction between propylene oxide and water or methanol, in particular formed propylene glycol and methoxypropanol formula CH3-SNON-CH2-Och3and CH3-CH(och3)-CH2HE. If you get the epichlorohydrin, the by-products formed by the reaction between epichlorohydrin and water or methanol, is when by-products are in particular, 1-chloropropanediol and chloromethoxypropyl formula ClCH2-CHOH-CH2-OCH3and Cl-CH2-CH(OCH3)-CH2OH. The formation of these by-products reduces the selectivity of the method, and hence the yield of the target product.

The aim of the present invention is to eliminate this drawback by using a new method of obtaining oxirane, which is characterized by a high selectivity and keeps it's performance (or speed of reaction).

Thus, the invention relates to a method of obtaining oxirane by reacting the olefin with a peroxide compound in the presence of a catalyst and a solvent is provided, in at least two reactors arranged in series, each of which contains a portion of the catalyst in the first reactor is served the first part of the olefin, the solvent and the peroxide compound, conduct epoxidation first part of the olefin with the formation of the first part of oxirane, derive from this reactor reaction medium consisting of a first part received oxirane, solvent, unreacted olefin and possibly unreacted peroxide compounds, introducing the resulting mixture to a distillation column, in the head part which is going to bómost received the ACS is wound and unreacted olefin, and columns in the cube is going mixture depleted in oxiranes and may contain unreacted peroxide compound is introduced into the next reactor mixture depleted in oxiranes, and another part of the olefin and, if necessary, another part of peroxide compounds, conduct epoxidation another part of the olefin with the formation of another part of oxirane and get another part thus obtained of oxirane.

One of the distinguishing characteristics of the present invention is the fact that you are doing the intermediate distillation in the interval between the two reactions epoxidation. This allows you to minimize the formation of by-products.

The purpose of distillation is to as quickly as possible to remove oxiran from the reaction mixture, since its formation, in order to avoid contact of oxirane with other components of the reaction mixture and to avoid the formation of side products. This selection is carried out in a separate distillation column, different from the epoxidation reactor. As the catalyst is not separated from the epoxidation reactor, the distillation is carried out in the absence of catalyst for epoxidation to avoid contacting the obtained oxirane and epoxidation catalyst, because it promotes the formation of by-products.

Distillation call is employed to allocate the major part of the resulting oxirane from the reaction mixture when epoxydecane. This part is usually greater than or equal to 80% of the number of oxirane obtained in the first reactor. Most often it is equal to or exceeds 90%. Usually it is less than or equal to 99%. In particular, it is less than or equal to 95%.

The conditions under which conduct the distillation depends on the nature of oxirane (in particular, from its boiling point), its concentration in the mixture introduced into the distillation column, from the nature of other components of the mixture (unreacted olefin and solvent), from the temperature of boiling and the desired output of distillation.

Typically, the distillation is carried out at a temperature equal to or greater than 10°With, mainly at temperatures above 35°recommended values are greater than or equal to 45°C. Usually the temperature is below or equal to 125°With, often lower than or equal to 100°C, preferably lower than or equal to 90°C.

Typically, the distillation is carried out at a pressure higher than or equal to 0.1 bar, preferably higher than or equal to 0.5 bar, the most commonly used pressure is higher than or equal to 1 bar. Usually the pressure is below or equal to 10 bar, in particular less than or equal to 5 bar, most recommended pressure lower than or equal to 2 bar. In the present description, any reference to a pressure distillation corresponds to the absolute pressure measured at the head of the distillation column.

The column used in the method according from what retenu, is known. For example, you can use normal dish-shaped column or disc column type "dual stream", as well as the Packed column Packed type or a structured Packed column.

Usually the number of theoretical plates of the distillation column is greater than or equal to 20, mainly greater than or equal to 30. Good results were obtained on a column with number plates, less than or equal to 80. The recommended number of theoretical plates is less than or equal to 60.

Usually the molar reflux number (which corresponds to a molar flow rate of the fluid returned to the head of the column, relative to the total amount of the distillate coming from the head of the column, and represents the liquid plus vapor phase) distillation column above or equal to 0.5, tend to be higher than or equal to 0.8. This is usually reflux the number below or equal to 5, most often it is less than or equal to 2.5.

In the method according to the invention using the installation including at least two of the epoxidation reactor arranged in series and connected to each other. In each reactor an olefin. The peroxide compound and the solvent are placed in the first reactor. Part of a fresh quantity of peroxide compounds may be placed in one or more subsequent reactors. Each the reactor contains a portion of the catalyst, which do not emit from the specified reactor. Since the catalyst is present in the form of a fixed layer, usually precautions to maintain the catalyst in the reactor do not accept. Alternatively, the catalyst may be present in the form of particles, at least part of which is in a fluid state under the action of fluid flow, or by mechanical mixing, or under the influence of the gas flow. If you use the liquid stream, it is expedient to provide for the allotment area above the liquid layer, so as to stop the moving catalyst particles, and/or to provide a filter at the reactor exit.

The installation may include more than two reactors arranged in series. In this case, in the first of the successive reactors serves olefin, a peroxide compound, a solvent and, if necessary, the fraction of the mixture obtained in Cuba distillation columns, which corresponds to a given reactor), and in each subsequent reactor an olefin, the remainder of the mixture coming from the preceding reactor, and, if necessary, a fresh portion of peroxide compounds. Mainly use three consecutive reactor.

In the method according to the invention mainly use reactors of the same size. This allows che is adovate the operation of the reactors at that time, when is the replacement of spent catalyst in any reactor in the fresh or regenerated catalyst, it is not contrary to the operation of the plant (this principle is called "circular line").

In accordance with the first embodiment of the invention, not only the first reactor installed in series reactors, but also for each subsequent reactor is located directly distillation column, which is called the "subsequent distillation. Specified subsequent distillation and intermediate distillation, which is carried out in the interval between the two reactions epoxidation, have the same function. Conditions for subsequent distillations are similar to conditions described above for intermediate distillation. In the specified embodiment of the invention, the reaction medium exiting each subsequent reactor and containing the other part of oxirane, solvent, unreacted olefin and possibly unreacted peroxide connection, enter the following distillation column, at the head of which is going the other part of oxirane and unreacted olefin, and columns in the cube remains solvent and possibly unreacted peroxide compound. In the continuous method, you may be in recyclenow the th environment, produced in Cuba last distillation column (which contains the solvent and possibly unreacted peroxide compound)in the first reactor. For example, if the method is carried out in two successive reactors, collected at the base of the second distillation column, the mixture can be re-used in the first reactor.

In accordance with the second embodiment of the invention the mixture of oxirane and unreacted olefin allocated at the head of the distillation column (first and/or subsequent), placed in a container, in which oxiran separated from the unreacted olefin. Specified unreacted olefin can then be reused in one of the reactors, mainly in the first reactor. The capacity can be equipped with fridge, or contain liquid or solid absorbent or selectively permeable membrane. It is more convenient to use the fridge.

In accordance with a third embodiment of the invention using the catalyst in the form of particles, at least part of which is in a fluid state, as described by the applicant in the patent application filed on the same day as the present application, and entitled "Method of obtaining oxirane in the presence of a catalyst in the form of particles (the content of which is contained is here as a reference). In this case, it is recommended to provide a filter through which passes the mixture leaving the reactor (first and/or subsequent) before you send it to a distillation column (first and/or subsequent). This method of carrying out the invention allows to obtain a homogeneous dispersion of the catalyst in the reaction medium epoxidation, to provide good heat transfer and, thus, to perform easy control of the reaction temperature.

In accordance with the fourth embodiment of the invention, the mixture flowing in the distillation column (first and/or subsequent), before you send it in this distillation column is subjected to throttling. This option is particularly useful when the epoxidation perform under pressure and in the presence of gaseous compounds. As specified gaseous compounds may act olefin (e.g. propylene) or inert gas, which is served in the reaction mixture when epoxydecane in order to remove oxiran with the gas stream from the reactor, as described by the applicant in the patent application WO 99/48883.

In accordance with the fifth embodiment of the invention all the amount of peroxide compounds are placed in the first reactor, as described by the applicant in the patent application filed on the same day that this bid, medium, small is, and having the title "Method of obtaining oxirane using peroxide compounds" (the contents of which are cited as references). In this case, in one or more reactors are not served fresh peroxide compound, and use of peroxide compound, which is present in the mixture emerging from the previous reactor, and which have not entered into reaction in the previous reactor. Usually in the first reactor also serves water with a peroxide compound. The fact that part of the peroxide compounds are not added in future(s) of the reactor(s), allows you to use 100% of the total amount of peroxide compounds, and the reaction rate decreases significantly from the manner in which you use the same total amount of peroxide compounds, but in which in each reactor add a fresh portion of peroxide compounds.

The preferred method of carrying out the invention is schematically represented in the drawing. In the specified preferred method, the first reactor 1 contains a portion of the catalyst, mainly in the form of a liquid layer 2. In the reactor 1 via line 3 and then the pipe 4 serves the first part of the olefin; pipeline 5, and then the pipe 4 serves peroxide compound; and a solvent serves to line 4, from another part of the installation, which will be described later. The first is auctore the first part of the olefin interacts with a peroxide compound in the presence of a catalyst with the formation of the first part of oxirane. The mixture emerging from the reactor 1 via line 6 contains a solvent, the first part of oxirane, unreacted peroxide compound and unreacted olefin. This mixture passes through the filter 7 and flows through the pipe 8 into the tank 9, where it drossellied. The mixture is then fed through line 10 to distillation column 11. From the head part of this distillation column 11 remove mixture of oxirane and unreacted olefin. This mixture flows through the pipe 12 into the refrigerator 13, which separates oxiran from unreacted olefin. Unreacted olefin is returned to the reactor 1 through the piping 14, 3, and 4. The first part of oxirane selected as a final product through the pipeline 15. In Cuba distillation columns 11 are selected mixture solvent containing peroxy compound, unreacted in the reactor 1, and possibly part of the unreacted olefin. The specified mix, part of which may be, if necessary, returned to the reactor 1 through the pipe 30, flows through the pipe 16 into the second reactor 17, containing another portion of the catalyst, preferably in the form of a liquid layer 18. In the second reactor 17 through line 19 serves the second part of the olefin. In the second reactor 17 the second part of the olefin interacts in the presence of the catalyst 18 is not came the Evesham in the reaction of the peroxide compound, received from the first reactor, with the formation of the second part of oxirane. Conditions in the second reactor 17 are chosen primarily so that all of peroxide compound, coming from the first reactor was used in the reaction. The mixture leaving the reactor 17 through the pipe 20 contains, therefore, the solvent, the second part of oxirane and unreacted olefin. This mixture passes through the filter 21, flows through the pipe 22 into the tank 23, where it drossellied. Then the mixture flows through the pipe 24 into the second distillation column 25. From the head part of this distillation column 25 remove the second part of oxirane and unreacted olefin. This mixture flows through the pipe 26 into the refrigerator 27, in which oxiran separated from the unreacted olefin. Unreacted olefin return to the reactor 1 through the piping 28, 14, 3, and 4. The second part of oxirane selected as the final product pipeline 29. In Cuba distillation columns 25 are selected solvent, which return to line 4 in the first reactor 1, and the liquid effluent, which is brought out through the pipe 31.

Used in the method according to the invention, the catalyst usually contains zeolite as the active element, preferably titanium containing zeolite. Under the titanium containing zeolite firmly understood the matter, containing silicon dioxide and having a microporous crystalline structure type zeolite, in which some of the silicon atoms are replaced by titanium atoms. Titanium containing zeolite is mainly crystalline structure of ZSM-5, ZSM-11, ZSM-12, MCM-41, ZSM-48. He also may have a crystalline structure type beta zeolite, preferably not containing aluminum. Suitable zeolites having an absorption band in the infrared region of the spectrum in the range of about 950-960 cm-1. Preferred titanium containing zeolites of type silicalite. Effective such zeolites which correspond to the formula xTiO2(1-x)SiO2in which x has a value of from 0.0001 to 0.5, preferably from 0.001 to 0.05. Compounds of this type, known under the name of TS-1 are microporous crystalline zeolite a structure similar to the structure of zeolite ZSM-5.

The catalyst used in the method according to the invention, is present predominantly in the form of particles obtained by extrusion, as described by the applicant in the patent application WO 99/28029, or spraying, as described by the applicant in the patent application WO 99/24164. The contents of both of these patent applications cited in the present description by reference.

The solvent used in the method according to the invention may be selected from saturated aliphatic alcohol is in, linear or branched. Usually, the alcohol solvent contains up to 10 carbon atoms, preferably from 1 to 6 carbon atoms. As examples are methanol and ethanol. Preferred is methanol.

Usually the amount of solvent used in the first reactor is at least 25% of the weight. from the composition of the liquid reaction mass located in the first reactor, in particular at least 40 wt%, for example, at least 50% weight. Typically, the specified number is not greater than 99 wt%, in particular, 95% of the weight.

Typically, the molar ratio between the amount of the olefin and the number of entered peroxide compounds is at least of 0.1, in particular at least 0.2 and preferably at least 0.5 in. Often specified molar ratio is not more than 100, in particular not more than 50, preferably not more than 25.

The method according to the invention is carried out in a continuous mode or intermittent.

In the method according to the invention, when it is carried out in continuous mode, the peroxide compound is usually served in the first reactor in the amount at least of 0.005 mole per hour per gram of catalyst placed in the first reactor, in particular at least 0.01 mole per hour. Typically, the amount of peroxide compounds is less than or equal to 25 moles and frequent the spine, less than or equal to 10 moles. Preferably the amount of peroxide compounds is greater than or equal to 0.03 to moles and less than or equal to 2.5 moles.

In the method according to the invention mainly use peroxide compound in the form of an aqueous solution. Typically, the aqueous solution contains at least 2 wt%. peroxide compounds, in particular at least 5 wt%. Often it contains a maximum of 90% of the weight. peroxide compounds, in particular 70% weight.

The temperature of the reaction between the olefin and the peroxide compound can vary from 10°C to 125°C. as the preferred option by the applicant in the Patent application EP 99/08703 temperature is above 35°With avoid increasing deactivation of the catalyst. The temperature may be higher or equal to 40°and, mainly, above or equal to 45°C. particularly preferred is a temperature above or equal to 50°C. the reaction Temperature is preferably less than 100°C.

In the method according to the invention the reaction between the olefin and the peroxide compound may occur at atmospheric pressure. It can also take place under pressure. Usually this pressure does not exceed 40 bar. In practice, it is convenient to apply a pressure of 20 bar.

Peroxide compounds which may be used in the method according invented the Yu, are peroxide compounds containing one or more peroxy groups (-UN), which can release active oxygen and capable of epoxidation. Suitable hydrogen peroxide and peroxide compounds that can release hydrogen peroxide under the reaction conditions of the epoxidation. Preferred is hydrogen peroxide.

If you use hydrogen peroxide, it is advisable to use in the method according to the invention an aqueous solution of hydrogen peroxide in the raw, i.e. in crude form. For example, you can use the solution obtained by conventional extraction purified to a high degree of water from the mixture obtained by oxidation of at least one alkylanthraquinones (method named "method JSC auto-oxidation") without subsequent washing and/or cleaning. These crude solutions of hydrogen peroxide usually contain from 0.001 to 10 g/l of organic impurities, the number of which is expressed by the value M (total organic carbon). These solutions usually contain cations of metals such as alkali or alkaline earth metals, for example sodium) and anions (such as phosphates, nitrates) in quantities from 0.01 to 10 g/L.

As an alternative, you can use the hydrogen peroxide solution obtained by direct synthesis from oxygen in Dorada in the presence of methanol.

Oxiran, which can be obtained by the method according to the invention, is an organic compound that contains a group of General formula

Usually oxiran contains from 2 to 10 carbon atoms, preferably from 3 to 6 carbon atoms. Oxirane, which can be obtained mainly by the method according to the invention are 1,2-epoxypropane and 1,2-epoxy-3-chloropropane. The preferred oxirane is 1,2-epoxypropane.

In the method according to the invention most suitable olefins generally containing from 2 to 10 carbon atoms and preferably from 3 to 6 carbon atoms. Suitable propylene, butylene and allyl chloride. Preferred are propylene and allyl chloride. In particular, preferred is propylene.

In the method according to the invention it is advisable to monitor the pH of the liquid phase. For example, it is advisable to maintain the pH of the liquid phase during the reaction between the olefin and the peroxide compound at a level of from 4.8 to 6.5, for example, by adding a base (sodium hydroxide) in a mixture of epoxidation, as recommended by the applicant in the patent application W 99/48882 (the content of which is contained in the present patent application by reference). The specified radix, you can enter in one reactor (e.g., first) or in som is to reactors. Mostly it is introduced into each reactor.

The reaction between the olefin and the peroxide compound may occur in the presence of salts such as sodium chloride, as described by the applicant in the patent application WO EP 99/08703 (the content of which is contained in the present patent application by reference). The specified salt can be entered in one reactor (e.g., first) or in multiple reactors. Preferably it is introduced into each reactor.

It is expedient to introduce the olefin in diluted form in one or more alkanes. For example, in the epoxidation reactor is possible to introduce a liquid product containing olefin, and at least 10% vol. (in particular, 20% vol., for example, at least 30% vol.) one or more alkanes. For example, if they use propylene, it is mixed, at least 10% vol. propane, if the reactor is injected recycled unreacted propylene. You can also use propylene, which is completely cleared of propane.

Below are examples intended to illustrate the invention but do not restrict it.

Examples 1 and 2 were calculated using the software product ASPEN PLUS company ASPEN TECHNOLOGY INC. using the kinetic parameters of the reaction, obtained on the basis of experimental data and equilibria in the system liquid - vapor available in the literature.

Comparative example 1

In this example, the synthesis of propylene oxide is carried out in two reactors arranged in series without intermediate allocation of propylene oxide obtained in the first reactor.

326,5 KMOL/h of hydrogen peroxide and 1100 KMOL/h of water are mixed with 1500 KMOL/h of methanol and 250 KMOL/h of propylene under pressure sufficient to dissolve all the amount of propylene at the chosen reaction temperature. The reaction mixture is continuously served at 70°in technological reactor containing 600 kg of catalyst.

Coming out of the reactor stream is mixed with 200 KMOL/h of propylene at a pressure sufficient to dissolve all the amount of propylene at the chosen reaction temperature, and continuously directed at 70°With the second technological reactor containing 600 kg of catalyst.

Leaving the second reactor, the stream contains 2.3 KMOL/h of unreacted hydrogen peroxide, 243,9 KMOL/h of propylene oxide and 77.4 KMOL/h-products (mainly methoxypropanol and propandiol); the yield of the target product, containing three carbon atoms, reaches 74.7% when the degree of conversion of hydrogen peroxide equal to 99.3 percent.

Example 2 (according to the invention)

In this example, the synthesis of propylene oxide is carried out in two reactors arranged in series with intermediate selection is of propylene oxide, obtained in the first reactor.

326,5 KMOL/h of hydrogen peroxide and 1100 KMOL/h of water are mixed with 1500 KMOL/h of methanol and 250 KMOL/h of propylene under pressure sufficient to dissolve all the amount of propylene at the chosen reaction temperature. The reaction mixture is continuously served at 70°in technological reactor containing 600 kg of catalyst.

Coming out of the reactor stream is sent to a distillation column having 50 theoretical plates (equipped with refrigerator and evaporator); feed mixture occurs on the tenth level of theoretical plates (counting starts with fridge); column operates under an absolute pressure of 1.1 bar (the pressure in the head part of the column); the temperature at the head of the column support at a temperature of 40° (distillate partially evaporates); reflux number is set to 1; the flow of distillate are selected so as to obtain from the head of the column 95% of propylene oxide, available supplied in the download column.

The mixture is taken from the cube columns depleted propylene oxide, mixed with 200 KMOL/h of propylene under pressure sufficient to dissolve all the amount of propylene at the chosen reaction temperature, and served continuously at 70°With the second technological reactor containing 600 kg of catalyst.

P is the current from the second reactor contains 0.5 KMOL/h of unreacted hydrogen peroxide, 85,9 KMOL/h of propylene oxide and 68.5 KMOL/h-products (mainly methoxypropanol and propandiol); the distillate of the column contains 168, 8mm KMOL/h of propylene oxide; the yield of the target product, containing three carbon atoms, reaches 78,0% when the degree of conversion of hydrogen peroxide equal to 99.9%.

1. The method of receiving oxirane interaction between the olefin and the peroxide compound in the presence of a catalyst and solvent in at least two reactors arranged in series, each of which contains a portion of the catalyst, according to which the first reactor is injected first portion of the olefin, the solvent and the peroxide compound and carry it to the epoxidation reaction the first part of the olefin with the formation of the first part of oxirane, remove from the reactor mixture containing the first portion of oxirane, solvent, unreacted olefin and, optionally, unreacted peroxide compound, introducing the mixture into the distillation column and collect in the head of column bóthe greater part of the obtained oxirane and unreacted olefin, and in Cuba columns receive the mixture, depleted oxiranes, and possibly unreacted peroxide compound is introduced into the next reactor mixture depleted in oxiranes, and another part of the olefin and possibly another part of the peroxide is to be placed, spend the reaction of epoxidation another part of the olefin with the formation of another part of oxirane and get another part thus obtained of oxirane.

2. The method according to claim 1, in which the mixture emerging from the subsequent reactor and containing the other part of oxirane, solvent, unreacted olefin and possibly unreacted peroxide compound is introduced into a subsequent distillation column, select at the head of the specified column bómost of the other parts of oxirane and unreacted olefin, and in Cuba the specified column selected solvent and possibly unreacted peroxide connection.

3. The method according to claim 2, in which the method is carried out in two reactors arranged in series, and in which is received by the cube of the second distillation column a mixture of recycle in the first reactor.

4. The method according to any one of claims 1 to 3, in which the mixture of oxirane and unreacted olefin, obtained at the head of the distillation column (first and/or subsequent), enter in the refrigerator, in which oxiran separated from the unreacted olefin, which is then recycle in one of the reactors.

5. The method according to any one of claims 1 to 4, in which all reactors have the same size.

6. The method according to any one of claims 1 to 5, in which the catalyst is contained in each reactor in the form of particles at least part of which is in a fluid state.

7. The method according to claim 6, in which the mixture leaving the reactor (first and/or subsequent), passes through the filter before it is entered into the distillation column (first and/or subsequent).

8. The method according to any one of claims 1 to 7, in which the mixture is supplied to a distillation column (first and/or subsequent), before its introduction into the specified distillation column is subjected to throttling.

9. The method according to any one of claims 1 to 8, in which the entire quantity of peroxide compound is introduced into the first reactor.

10. The method according to any one of claims 1 to 9, in which oxiran is propylene oxide or epichlorohydrin, the olefin is propylene or allyl chloride, peroxide compound is hydrogen peroxide, the solvent is methanol and the catalyst contains TS-1.



 

Same patents:

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for preparing oxyrane. Method involves reaction of olefin with peroxide compound in the presence of catalyst and a solvent in at least two reactors arranged in series and each reactor contains part of catalyst. Peroxide compound is added to the first reactor only and the next or the following reactors are fed with peroxide compound presenting in medium preparing from the preceding reactor but not with fresh peroxide compound or used in this preceding reactor. Method provides enhancing output and reducing formation of by-side products.

EFFECT: improved method for preparing.

10 cl, 1 dwg, 2 ex

The invention relates to a method of improving the quality of propylene oxide contaminated with poly(propylene oxide), which includes the following stages: (a) interaction of liquid propylene oxide powder of the adsorbent in an amount of from 0.05 to 15 wt.% in relation to the mass of liquid propylene oxide consisting of a silicate of magnesium and/or calcium silicate, with taking the suspension, where the average particle size of the specified powder is from 1 to 100 μm, or deletion of contaminated propylene oxide over at least one layer of the extrudates of the same adsorbent, and (b) isolation of the pure product of propylene oxide

The invention relates to a method for selection of the ethylene oxide absorption from the gas mixture obtained in the oxidation of ethylene with oxygen in the presence of silver-containing catalyst, and can be used in the production of ethylene oxide

The invention relates to a method for selection of the ethylene oxide absorption from the gas mixture obtained in the oxidation of ethylene with molecular oxygen in the presence of silver-containing catalyst, and can be used in the production of ethylene oxide

The invention relates to the technology of production of ethylene oxide, in particular to a method for separation of ethylene oxide from a mixture containing ethylene oxide

The invention relates to petrochemistry, in particular to a method of allocation of ethylene oxide

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for preparing oxyrane. Method involves reaction of olefin with peroxide compound in the presence of catalyst and a solvent in at least two reactors arranged in series and each reactor contains part of catalyst. Peroxide compound is added to the first reactor only and the next or the following reactors are fed with peroxide compound presenting in medium preparing from the preceding reactor but not with fresh peroxide compound or used in this preceding reactor. Method provides enhancing output and reducing formation of by-side products.

EFFECT: improved method for preparing.

10 cl, 1 dwg, 2 ex

FIELD: petrochemical industry; production of zeolite.

SUBSTANCE: the invention offers the method of production of titanium-containing zeolite by: (a) combining a capable to be hydrolyzed silicon compound and a capable to be hydrolyzed titanium compound; (b) adding a basic quaternary ammonium compound in a water medium into the mixture from a stage (a) and a hydrolysis of a reaction mixture at the temperature within the interval from 0 up to 100°C with production of a synthesis sol; and then (c) the synthesis sol aging at the temperature within the interval from 150 up to 190°C and (d) crystallizations of the synthesis sol at this temperature, differing by the fact, that aging duration at the increased temperature at the stage of (c) makes less than 240 minutes. The method ensures production of zeolite with a catalytic activity in reactions of epoxidation of olefins by hydrogen peroxide.

EFFECT: the invention ensures production of zeolite with a catalytic activity in reactions of epoxidation of olefins by hydrogen peroxide.

8 cl, 1 tbl

FIELD: chemical industry; production of a catalyst carrier material and the catalyst.

SUBSTANCE: the invention is dealt with the field of chemical industry. The method of production of a catalyst carrier material includes the following stages: (a) treatment of the utilized catalyst of titanium dioxide-on-silicon dioxide to clear from coke; (Ь) washing of the catalyst cleared from the coke by a flushing fluid chosen from a water solution of an inorganic acid, a water solution of an ammonium salt and their combinations; (c) drying and calcination of the catalyst washed out and cleared from the coke with production of the catalyst carrier material. The technical effect - the material produced this way is fit for use as the carrying agent material for titanium dioxide in a heterogeneous catalyst for epoxidation of olefines in alkylene oxide.

EFFECT: the invention ensures production of the material fit for use as the carrying agent material for titanium dioxide in a heterogeneous catalyst for epoxidation of olefines in alkylene oxide.

12 cl, 4 ex, 1 tbl

FIELD: chemical industry; production of hydrogen peroxide and oxiranes.

SUBSTANCE: the invention is dealt with a method of production of hydrogen peroxides and oxiranes. The invention provides for conductance of reaction of olefin with hydrogen peroxide at the presence of a catalyst and organic thinner. At that hydrogen peroxide is present as a water solution of hydrogen peroxide extracted mainly with the help of purified water out of a mixture produced as a result of oxidation at least of one alkylanthrahydroquinone without aftertreatment with a cleansing water and-or purification. The technical result is an increase of an output and selectivity of oxirane.

EFFECT: the invention ensures increased output and selectivity of oxirane.

17 cl, 5 tbl, 10 ex

The invention relates to a method for epoxidation prehiring of olefin, which includes the interaction prehiring of the olefin with oxygen source in the presence of salt catalyst

FIELD: chemical industry; production of hydrogen peroxide and oxiranes.

SUBSTANCE: the invention is dealt with a method of production of hydrogen peroxides and oxiranes. The invention provides for conductance of reaction of olefin with hydrogen peroxide at the presence of a catalyst and organic thinner. At that hydrogen peroxide is present as a water solution of hydrogen peroxide extracted mainly with the help of purified water out of a mixture produced as a result of oxidation at least of one alkylanthrahydroquinone without aftertreatment with a cleansing water and-or purification. The technical result is an increase of an output and selectivity of oxirane.

EFFECT: the invention ensures increased output and selectivity of oxirane.

17 cl, 5 tbl, 10 ex

FIELD: chemical industry; production of a catalyst carrier material and the catalyst.

SUBSTANCE: the invention is dealt with the field of chemical industry. The method of production of a catalyst carrier material includes the following stages: (a) treatment of the utilized catalyst of titanium dioxide-on-silicon dioxide to clear from coke; (Ь) washing of the catalyst cleared from the coke by a flushing fluid chosen from a water solution of an inorganic acid, a water solution of an ammonium salt and their combinations; (c) drying and calcination of the catalyst washed out and cleared from the coke with production of the catalyst carrier material. The technical effect - the material produced this way is fit for use as the carrying agent material for titanium dioxide in a heterogeneous catalyst for epoxidation of olefines in alkylene oxide.

EFFECT: the invention ensures production of the material fit for use as the carrying agent material for titanium dioxide in a heterogeneous catalyst for epoxidation of olefines in alkylene oxide.

12 cl, 4 ex, 1 tbl

FIELD: petrochemical industry; production of zeolite.

SUBSTANCE: the invention offers the method of production of titanium-containing zeolite by: (a) combining a capable to be hydrolyzed silicon compound and a capable to be hydrolyzed titanium compound; (b) adding a basic quaternary ammonium compound in a water medium into the mixture from a stage (a) and a hydrolysis of a reaction mixture at the temperature within the interval from 0 up to 100°C with production of a synthesis sol; and then (c) the synthesis sol aging at the temperature within the interval from 150 up to 190°C and (d) crystallizations of the synthesis sol at this temperature, differing by the fact, that aging duration at the increased temperature at the stage of (c) makes less than 240 minutes. The method ensures production of zeolite with a catalytic activity in reactions of epoxidation of olefins by hydrogen peroxide.

EFFECT: the invention ensures production of zeolite with a catalytic activity in reactions of epoxidation of olefins by hydrogen peroxide.

8 cl, 1 tbl

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for preparing oxyrane. Method involves reaction of olefin with peroxide compound in the presence of catalyst and a solvent in at least two reactors arranged in series and each reactor contains part of catalyst. Peroxide compound is added to the first reactor only and the next or the following reactors are fed with peroxide compound presenting in medium preparing from the preceding reactor but not with fresh peroxide compound or used in this preceding reactor. Method provides enhancing output and reducing formation of by-side products.

EFFECT: improved method for preparing.

10 cl, 1 dwg, 2 ex

Up!