Method for preparing propylene oxide

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention proposes a method for preparing propylene oxide wherein (I) propene is subjected for conversion with hydrogen peroxide in the presence of methanol to propylene oxide to obtain a mixture (CI) containing propylene oxide, methanol, water and unreacted hydrogen peroxide; (II) from mixture (CI) mixture (CII) is removed that contains methanol, water and hydrogen peroxide to obtain mixture (Ca) containing propylene oxide; and (III) from mixture CII water is removed to obtain mixture (CIII) containing methanol and methyl formate. Invention provides enhancing yield of the end product and decreasing formation of by-side products.

EFFECT: improved preparing method.

9 cl, 1 ex

 

This invention concerns a method of producing propylene oxide from propene and hydrogen peroxide in the presence of methanol. In the framework of the method according to the invention after the interaction of propene with hydrogen peroxide mixture containing methanol, water and unreacted hydrogen peroxide is separated from the paged the reaction mixture and this mixture is subjected to a separation process, which yields the following mixture containing methanol and methylformate.

Methods for producing propylene oxide from propene known from the prior art. Typically, in these methods, a problem arises, namely, that during the reaction a certain amount of hydrogen peroxide is not converted and accumulated in subsequent separation of propylene oxide from the system paged reaction mass.

To resolve this problem were proposed, including conduct intermediate separation of hydrogen peroxide from the system paged the reaction mass of the first stage reaction and the second reaction stage again to put her transformation with the alkene. Such methods are described, for example, in PCT/EP 99/05740 and in the patent application Germany 100 15 246.5. At the second stage of the reaction it is possible to achieve almost complete conversion of the hydrogen peroxide. However, due to the second stage reaction required high cost of instrumentation.

Saddadinova of the invention was to develop a way in which the problem of accumulation of unreacted hydrogen peroxide would be solved with the lowest cost effectively and efficiently.

Accordingly, this invention concerns a method of producing propylene oxide, which

(I) propene is subjected to transformation with hydrogen peroxide in the presence of methanol in propylene oxide from a mixture (CI)containing propylene oxide, methanol, water and unreacted hydrogen peroxide,

(II) from a mixture (CI) separating the mixture (CII), containing methanol, water and hydrogen peroxide to obtain a mixture (CA), containing propylene oxide, and

(III) from a mixture (CII) separating water from the mixture (III)containing methanol and methylformate.

The solvent is particularly preferably used methanol. In addition to methanol, it is also possible to use one or more other solvents. As such additional solvents, in principle, it is possible to use all solvents which are suitable for the corresponding transformation. Are preferred, including, for example,

- water,

- alcohols, preferably lower alcohols, further preferred alcohols with less than 6 carbon atoms, such as, for example, ethanol, propanol, butanol, pentanol,

- diols or polyols, preferably less than 6 carbon atoms,

- ethers, such as, n is the sample, diethyl ether, tetrahydrofuran, dioxane, 1,2-diethoxyethane, 2-methoxyethanol,

- esters, such as, for example, methyl acetate or butyrolactone,

- amides, such as dimethylformamide, dimethylacetamide, N-organic,

- ketones, such as acetone,

- NITRILES, such as acetonitrile or

- a mixture of two or more of the above compounds.

The interaction of propene with hydrogen peroxide in the framework of the method according to the invention preferably occurs in the presence of a catalyst. As catalysts for the conversion of propylene to propylene oxide, in principle, possible, preferably all of heterogeneous catalysts suitable for the corresponding transformation.

Thus preferably used catalysts, which contain porous oxide substance, such as, for example, the zeolite. Preferably used catalysts, which as a porous oxide materials contain a titanium-, vanadium-, chromium-, niobium or zirconium bearing zeolite.

In particular, there are zeolites which contain no aluminum and silicate crystal lattice instead of Si(IV) is partially titanium as Ti(IV). Titanium zeolites, in particular, with the crystal structure of the MFI type, and the possibility of obtaining them are described, for example, in applications for European is their patents EP-A 0311983 or EP-A 0405978.

Titanium zeolites with MFI structure is known for the fact that they can be identified by a specific reference in the analysis of their images x-ray diffraction, and an additional band of skeletal vibrations in the infrared region (IR) at about 960 cm-1, and these differ from alkali metal titanates or crystalline and amorphous TiO2-phases.

Thus, in particular, suitable titanium-, vanadium-, chromium-, niobium-, circumistances zeolites with pentasil-zeolite structure, in particular, their types are attributed on the basis of x-ray to ABW-, ACO-, AEI-, AEL-, AEN, AET-, AFG-, AFI, AFN-, AFO-, AFR-, AFS, AFT, AFX-, AFY-, ANT-, ANA-, APC-, APD-AST-, ATN-ATO-, ATS-, ATT-, ATV, AWO-, AWW, BEA-, BIK-, FIFTH-, BPH-, BRE-, CAN-, CAS-, CFI, CGF-CGS-, SLEEP-, CHI-, CLO-, CON-, CZP-, DAC, DDR, DFO-, DFT, DOH-DON-TECHNOLOGICAL, EDI, EMT-, EPI-, ERI-, ESV-, EUO-, FAU-, FER-, GIS, GME-, GOO-, HEU-, IFR-, ISV, ITE, JBW-, KFI-, LAU-A, LEV-, LIO-, LOS, LOV-, LTA-, LT-, LTN-, MAZ-, MEI-, MEL-, MER-A, MER, MFI-, MFS-, MON-, MOR-, MSO-, MTF-, MTN-, MTT, MTW-, MWW-, NAT, NES, NON, OFF, OSI, PAR, PAU-, PHI-, RHO-, R-, RSN-, RTE, RTH-, RUT-, SAO, SAT, SBE-, SBS, SBT-, SFF, SGT, -, SOD-, STF-, STI, STT-, TER-, THO-, TON-, TSC-, VET, VFI-, VNI-, VSV-, WEI-, WEN-, YUG-, ZON-structure, and to mixed structures of two or more of the above structures. For use in the method according to the invention valid, in addition, titanium containing zeolites with structure UTD-1, CIT-1 or CIT-5. As other titanium containing zeolites include zeolites with structure of ZSM-48 or ZSM-12.

As the person is but a preferred method according to the invention should be considered Ti-zeolites with MFI-, MEL-structure or MFI/MEL-mixed structure. Further, as preferred, in particular, should be called titanium containing catalysts based on zeolite, which, in General, referred to as TS-1, TS-2, TS-3, as well as Ti-zeolites with structure of the skeleton, isomorphous beta zeolite.

In the method according to the invention is particularly preferably used heterogeneous catalyst which contains titanium containing silicalite TS-1.

Accordingly, the invention also concerns the method described above, which is characterized by the fact that to obtain propylene oxide is used zeolite catalyst, preferably titanosilicate catalyst and, in particular, titanosilicates the catalyst structure of TS-1.

The separation of water from the mixture (CII) in the method according to the invention is preferably carried out by distillation, and you can use one or more distillation columns. Preferably use one or two distillation columns. If there is no need to dispose of heat, preferably using one distillation column. Two or more distillation columns are preferably used, if in the process it is necessary to provide particularly good heat integration.

With regard to the physical parameters such as temperature or pressure, when distillation is the separation of water from the mixture (CII), there is no special limitation, while it is guaranteed that when the distillation is cleaved with hydrogen peroxide and it turns out the mixture (III)containing methylformate and methanol.

If in the method according to the invention for separating water from a mixture of (CII) use only one column, then this column should be preferably at least 5, preferably at least 20, and further preferably at least 30 theoretical plates. Preferably the distillation is carried out at a pressure in the range from 0.5 to 40 bar, preferably from 1.0 to 20 bar and particularly preferably from 2 to 15 bar.

If in the method according to the invention for separating water from a mixture of (CII) use two columns, the pressure is chosen so that the heat of condensation at the head of the columns, it was possible to heat the other threads in the process. This is achieved, for example, the fact that the capacitor, at least one of the column is cooled, for example water and the resulting cooling hot water or resulting from the cooling steam is used to heat one or more stages of the method according to the invention or even one or more other processes.

The first distillation column is preferably operated at a pressure in the range from 0.5 to 40 bar and preferably from 1 to 20 bar. In a possible form of realization of the first column of blocks is comfort at a higher pressure level, than the second column. In this case, the sump of the second column is heated by the vapour of the first column. In a preferred form of implementation of the first column operated at a lower pressure level than the second column. In this case, the first sump of the column is heated by the steam of the second column.

In a particularly preferred form of implementation of the first column operated at a pressure in the range from 4 to 9 bar, and further preferably in the range from 6 to 8 bar, and the second column is in the range from 11 to 16 bar and further preferably in the range from 12 to 14 bar. At the head of the first column is separated through the top of the column, in General, 20 to 80%, preferably 30 to 70% and particularly preferably 40 to 60% is contained in the mixture (CII) of methanol together with methylformate. The mixture, which is obtained from the first sump of the column, used as starting material for the second column. The head fraction of the second column contains the residual methanol and methylformate and Symphony product contains water. Head of the faction of the first and second columns are combined into a mixture (III).

As in the case of water separation in two columns, and in the case of water separation in the same column conditions offices are particularly preferably chosen so that the water content in the mixture (III), in General, was less than 3 wt.%, preferably less than 1 wt.% and particularly preferably Myung is above 0.3 wt.%. The conditions of the separation are preferably chosen so that the methanol content in distillate of the sump was less than 5 wt.%, preferably less than 1 wt.% and particularly preferably less than 0.2 wt.%.

Along with this, the distillate from the sump may contain as additional components, including, for example, methoxypropanol, propylene glycol, formic acid, simple onomatology broadcast dipropyleneglycol, formaldehyde.

Accordingly, the invention also concerns the method described above in which the water is separated by distillation according to (III), characterized in that

(IV) in the first distillation column from a mixture of (CII) is separated through the head of mixture (CIV), which contains mainly methanol and methylformate,

(V) the mixture resulting from the sump of the first distillation column, serves as the initial reaction mixture in a second distillation column,

(VI) from the second distillation column through the head part receiving the mixture (CVI), which contains mainly methanol and methylformate,

(VII) a mixture of (IV) and (VI) are combined with the mixture (III).

A mixture of (III), which is obtained after separation of the water, in the preferred form of the method according to the invention serves to the next stage of processing. Thus from a mixture of (III) separating the methane and methylformate.

In another preferred form of the method according to the invention the extracted thus methanol in return (I).

Therefore, this invention also concerns the method described above, which differs from the mixture of (III) separating the methanol and methylformate and the separated methanol is returned to (I).

This separation of methanol from the mixture (III)containing methylformate and methanol, in principle, can be produced according to all possible ways, if it is guaranteed that the purity of the separated methanol meet the set requirements.

Here among the other should be called chemical methods. For example, sometimes a mixture containing methanol and methylformate, to enter into contact with a suitable alkaline ion exchange resin, resulting in the formation of methanol and formate remains on the resin. This technique is described among others in U.S. patent 5107002.

Next, a mixture containing methanol and methylformate, can be treated with base, with methylformate hydrolyzed. And apply all the bases, with which you can achieve hydrolysis of methylformate. Preferably used strong bases. As a particularly preferred bases in the framework of this invention it should be called the salt of the acid which is weaker than that of formic acid. Predpochtitel is but it should be called, including hydroxides of alkali and alkaline earth metals or alkali metal salts of alcohols or phenols. Of course, you can also use a mixture of two or more of these grounds.

Hereinafter, preferred for the separation of methanol from a mixture containing methanol and methylformate are physical methods, such as, for example, the method of distillation.

Among them is possible, for example, methods of extractive distillation, known from the prior art and shown, for example, in the above-mentioned U.S. patent 5107002.

However, preferably used methods of distillation, the apparatus which is less costly than the above methods extractive distillation.

The preferred method is distillation, which uses one or more columns, more preferably one column. If you use one column, it must have at least 5, preferably at least 10 and, in particular, at least 20 theoretical plates.

The pressure, which preferably are, in General, lies in the range from 0.2 to 50 bar, preferably in the range from 1.5 to 30 bar, in particular, in the region of from 2.0 to 20 bar.

The temperature of the upper part of the column and the temperature of the sump is uniquely defined by the selected pressure. In a particularly preferred form of domestic these columns, which have approximately 20 theoretical plates and operated at a pressure in the range from 2.0 to 20 bar. As head of the faction get the mixture containing methylformate and a small amount of methanol contained in the original mixture. Preferably the content of methanol in the mixture is less than 80 wt.%, more preferably less than 50 wt.%, and especially preferably less than 20 wt.%.

Further, it is possible that the mixture (III)containing methanol and methylformate, along with methylformate optionally contains other components. The concept of "components" in this case refers to both pure compounds, and azeotropy, having a boiling point that is lower than the boiling point of methanol. As such components, in particular, should be called, for example, acetaldehyde, 1,1-dimethoxyethane, propionic aldehyde, 1,1-dimethoxypropane, acetone or 2,4-dimethyl-1,3-dioxolane. They can also be separated from the mixture during processing.

Thus, it is possible to separate these by-products from the mixture before separation of methanol from methylformate one or more of prihodnje physical or chemical methods. It is also possible first to separate from a mixture of methanol, and the result can form a mixture, which contains methanol and at least one impurity. In this case, to the separation of methanol from specimages to join one or several stages of separation, in which methanol is separated from at least one impurity. Similarly, the separation of methanol from the mixture can be formed mixture, which contains methylformate and one or more impurities. If necessary, you can also divide this mixture into its component parts using one or more suitable physical or chemical methods. In this case, the component parts can be separated or enter together in one or more subsequent processes as starting substances or disposed of by heat.

Depending on the chemical nature of the impurities, it is also possible to separate the methanol from the mixture so that as methylformate, and at least one impurity to be separated from the methanol for one stage of the process.

In this way it does not, above, are preferably used according to the invention, distillation get methanol fraction containing methylformate, in General, less than 500 ppm, preferably less than 100 ppm and particularly preferably less than 20 h/million

Depending on the requirements that apply to the purity of the methanol fractions, residues of other components, such as acetaldehyde, 1,1-dimethoxyethane, propionic aldehyde, 1,1-dimethoxypropane, acetone or 2,4-dimethyl-1,3-dioxolane, which after distillation processing OST who are in the methanol fraction, can be separated using one or more suitable procedures, such as one or more authonomy methanol.

In General, it is sufficient if the concentration of each side component in methanol below 1 wt.%, and the sum of all side components does not exceed 5 wt.%.

Methanol, separated thus from methylformate, can be re-used, and essentially should, if possible, to return the methanol in the process of obtaining propylene oxide or, if necessary, to submit methanol is another process in which methanol as a solvent, or as a starting material, or in its normal function. Of course, the flow of methanol, which is formed as a result of separation according to the invention may be divided into two or more threads, and each thread to serve in another process.

In a particularly preferred form of the method according to the invention the methanol, which was separated from methylformate and, if necessary, from one or more by-products or impurities, as described above, return in the process of obtaining propylene oxide. In addition, it is preferable to pump the methanol in the buffer tank and from it to enter into the process.

As for obtaining propylene oxide according to (I), it is even more preferred is sustained fashion is carried out in one stage. The concept of "one-stage"used in this application, means the carrying out of the process, with no separation of hydrogen peroxide. In the framework of this invention, along with ways in which the original products are subjected to interaction with each other in the reactor and paged the reaction mass is then treated, single-stage method comprises, in addition, also the ways in which

- at one stage the reaction of propene is subjected to interaction with hydrogen peroxide to obtain a product stream,

- the stream to produce at least one intermediate processing, and the result of this processing receive an additional stream of products, and

- additional product stream is served to the next stage reaction in which hydrogen peroxide is subjected to interaction with propene, and intermediate processing does not represent a branch of hydrogen peroxide.

Of course, there are also other stages of the reaction, and between the two stages may, but not necessarily, take place one intermediate processing. As an intermediate processing, in particular, possible additive grounds to the product flow, and particularly preferably it is possible to use alkaline compounds, which in the framework of the method according to the invention in the desired manner affect maintains deistvie hydrogen peroxide with propene. When heterogeneous catalysts are used, for example, zeolites, preferably using alkaline compounds that reduce the acidity of these zeolites. Such grounds are described, for example, in the patent application Germany 100 15 246.5 that in the part that refers to this in full included in the context of this application by reference.

For example, the location and type of reactors that use in (I), there are also valid all suitable reactors. In particular, it is possible, for example, be used in one or more of the above-mentioned reaction stages two or more parallel-connected reactor. Relative to this reference should be made to patent application Germany 100 15 246.5 that due to possible locations of the reactors were fully integrated in the context of this application by reference.

Therefore, this invention concerns a method described above, which is characterized by the fact that the interaction according to (I) is carried out in one stage.

Further, during the process of obtaining propylene oxide from propene and hydrogen peroxide, you can change the temperature and pressure of the reaction medium. You can also change the pH and temperature of the reaction medium. It is also possible in addition to the pH and the temperature of the reaction medium, to vary the pressure at which the reaction occurs. Regarding this, it is necessary to send the I to the patent application Germany 199 36 547.4, which link related to this, in full included in the context of this application.

Especially, it is preferable to make propylene oxide according to (I) so that the conversion of hydrogen peroxide were, in General, in the range from 85 to 99.99%, preferably in the range from 90 to 99.9% and especially preferably in the range from 95 to 99.5%.

Therefore, this invention also concerns the method described above, which is characterized by the fact that the conversion of hydrogen peroxide in (I) is the area from 85 to 99.99%.

According to the invention from a mixture of (CI) separating the mixture (CII), containing methanol, water and hydrogen peroxide, to obtain a mixture (CA), containing propylene oxide. This separation can be accomplished, in General, all suitable methods. Preferably the separation is performed by distillation.

Preferably used the method of distillation, which uses one or more columns, more preferably share the same column. If you use one column, it must have at least 5, preferably at least 10, in particular at least 15 theoretical plates. The pressure, which preferably are, in General, lies in the range from 0.5 to 10 bar, preferably in the range from 0.8 to 3 bar, in particular, in the area of ambient pressure.

Temperature head frequent the columns and sump are uniquely determined by the selected pressure. In an even more preferred form of implementation of this column, which has approximately 15 theoretical stages of separation, operate at ambient pressure. When the head temperature of the column in the area around 35°as head of the faction receive a mixture (CA), containing propylene oxide. As sumptuoso product at a temperature sump approximately 68°get the formula (CII), containing methanol, water and unreacted hydrogen peroxide.

The mixture (CII), in addition to methanol, water and hydrogen peroxide, may contain one or more other compounds, which may be, for example, by-products of the reaction according to (I), or compounds, which are formed in the separation according to (II), or connections that have been made in the form of impurities of the original substances (I), or solvents, which were, for example, used in addition to the solvent, methanol, or compounds that were used for the distillation separation according to (II), or compounds which for example, were added within the above-described intermediate processing. Upon receipt of propylene oxide from propene according to (I) a mixture of (CII) may contain, including 1,1-dimethoxyethane, acetone, acetaldehyde, 1,1-dimethoxypropane, propionic aldehyde, methylformate or/and 2,4-dimethy who -1,3-dioxolane.

The mixture (CA) can also in addition to propylene oxide to contain one or more other compounds, which again can be, for example, by-products of the reaction according to (I), or compounds, which are formed in the separation according to (II), or connections that have been made in the form of impurities of the original substances (I), or methanol or solvents, which were, for example, used in addition to the solvent, methanol, or compounds that were used for the distillation separation according to (II), or compounds that, for example, were added in the framework of the above-described intermediate processing.

Depending on the mode of the process, in the framework of the method according to the invention allow the mixture (CA), which is obtained from the system paged reaction mixture according to (I), in addition to propylene oxide contained methanol. Preferred is methanol content in the range from 10 to 90 wt.%, particularly preferably in the range from 25 to 75 wt.% and even more preferably in the range from 40 to 60 wt.%.

In particular, in one preferred form of implementation of the methanol, which is contained in (Sa)is separated from (Sa) and add to the mixture (CII). The expression "to add to the mixture (CII)in the framework of this proposal includes both forms of the method according to the invention, which is separated from (Sa methanol first serves in (CII) and the resulting mixture is sent to the stage of the process (III), and forms of implementation, which is separated from (Sa) methanol and separated by formula (CII) is directed to process stage (III), and only where they come in contact.

In addition, methanol can also be added to the mixture (III).

Therefore, this invention also concerns the method described above, and the mixture (CA), in addition to propylene oxide, contains methanol, wherein the methanol is separated from (Sa) and add to the mixture (CII) or to a mixture of (III) or mixtures (CII) and (CIII).

The separation of methanol from the mixture (CA)containing methanol and propylene oxide, preferably occurs through a process of distillation, and the number of columns, basically any. Preferably use one column. Moreover, this column preferably has at least 20, preferably at least 40, and further preferably at least 60 theoretical plates.

The distillation in the column is preferably carried out at a pressure in the range from 0.3 to 10 bar, preferably from 0.4 to 2 bar and particularly preferably from 0.6 to 1.2 bar.

Therefore, this invention also concerns the way in which from (Sa) separating methanol, and as described above, which is characterized by the fact that the separation of methanol takes place in the column, at least 20 theoretical plates at a pressure in the range from 0.3 to 10 bar.

Paged from (I) the reaction is second mass may contain (I) unreacted propene. Preferably it is separated from the system paged mass.

In one preferred form of the method according to the invention the separation of non-reacted propene takes place in the framework of the separation of mixtures (CII) at the stage (II) of the process. In another preferred form of implementation of the distillation separation according to (II) is conducted in such a way that, for example, formula (CII) is separated from the sump, a mixture (CA) is separated through the side outlet of distillation columns, and unreacted propene is separated through the head of the column.

In the preferred form of the method according to the invention the separation according to (II) is conducted in such a way that, for example, a mixture (CA), which is obtained from (II), in addition to propylene oxide and, under certain conditions - to the methanol contains (I) unreacted propene. In the subsequent process, the propene preferably separated from (Sa).

Therefore, this invention also concerns the method described above, wherein the mixture (CA) along with propylene oxide and, under certain conditions with methanol, further comprises (I) unreacted propene, characterized in that the produce propene from the mixture (CA).

The Department of non-reacted propene (Sa) is preferably carried out by distillation. The number of used columns, basically, Liu is passed. Preferably use one column. This column has, in General, at least 5, preferably at least 10, and further preferably at least 15 theoretical plates. The distillation in the column is preferably carried out at a pressure in the range from 0.5 to 25 bar, more preferably from 0.7 to 5 bar and particularly preferably in the range from 0.9 to 1.5 bar.

The Department of non-reacted propene under certain conditions the problem occurs, namely, that the separation of propene in the form of a low-boiling fraction, as described above, this fraction can accumulate oxygen in a concentration that makes the low-boiling fraction in able to ignite the mixture. As a consequence, there may be a serious security risk if propene again be separated from low-boiling fractions by distillation, so that in this case becomes the preferred option in which the propene to be returned in (I).

This problem can be solved, for example, in such a way that the propene is removed by distillation of low-boiling mixture and in the upper part is used for this separation devices add an inert substance with a boiling point that is lower than that of propene, preferably methane, in an amount such that the oxygen was diluted to a concentration at which the mixture is no longer I who is ignited. This method is described, for example, in the application for the European patent EP-0719768. However, it is preferable solve the problem due to the fact that the applied method for processing a mixture containing propene and oxygen in which the oxygen is removed from the mixture by distillation to obtain another mixture, and separating propene from another mixture by distillation.

This method is described in the patent application Germany 10001401.1, which, in this respect, fully integrated in the context of this application through the link.

In a particularly preferred form of the method according to the invention separated propene again return as the starting material in (I).

In another particularly preferred form of implementation of all the above mentioned stages of the method take place continuously. Of course, it is also possible to carry out one or more stages in periodic mode.

1. The method of producing propylene oxide, which

(I) propene is subjected to transformation with hydrogen peroxide in the presence of methanol in propylene oxide from a mixture (CI)containing propylene oxide, methanol, water and unreacted hydrogen peroxide,

(II) from a mixture (CI) separating the mixture (CII), containing methanol, water and hydrogen peroxide, to obtain a mixture (CA), containing propylene oxide, and (III) from a mixture (CII) separating water from the mixture (III)containing methanol and metalf RMIT.

2. The method according to claim 1, characterized in that for obtaining propylene oxide is used zeolite catalyst, preferably titanosilicate catalyst and, in particular, titanosilicates the catalyst structure of TS-1.

3. The method according to claim 1 or 2, in which the water is separated by distillation according to (III), wherein (IV) from a mixture (CII) in the first distillation column is separated through the head of mixture (CIV), which mainly contains methanol and methylformate, (V) the mixture resulting from the sump of the first distillation column is sent as feedstock to the second distillation column,

(VI) from the second distillation column through the head part receiving the mixture (CVI), which contains mainly methanol and methylformate, and

(VII) a mixture of (IV) and (VI) are combined with the mixture (III).

4. The method according to one of claims 1 to 3, characterized in that the mixture of (III) the methanol is separated from methylformate and the separated methanol is returned to(I).

5. The method according to one of claims 1 to 4, characterized in that the transformation according to (I) is carried out in one stage.

6. The method according to claim 5, characterized in that the conversion of hydrogen peroxide in (I) is in the range from 85 to 99.99%.

7. The method according to one of claims 1 to 6, and the mixture (CA) in addition to propylene oxide contains methanol, wherein the methanol is separated from (Sa) and add to the art (CII), or to a mixture of (III), or formula (CII) and (CIII).

8. The method according to claim 7, characterized in that the separation of methanol takes place in the column, at least 20 theoretical plates at a pressure in the range from 0.3 to 10 bar.

9. The method according to one of claims 1 to 8, and the mixture (CA) along with propylene oxide and under certain conditions the methanol further comprises (I) unreacted propene, wherein the propene is separated from the mixture (CA).



 

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FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention describes a method for preparing oxirane in reactor comprising a liquid reaction medium. Method involves carrying out reaction between olefin and peroxide compound in liquid reaction medium in the presence of a solid catalyst and a solvent. Solid catalyst comprises zeolite as an active component and it is used in form of particles wherein at least part of particles present in reactor in the fluidized state. Invention provides increasing rate of the process that results to the enhanced output.

EFFECT: improved preparing method.

1 ex

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

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

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