The method of obtaining 2,6-phenols dimethylsiloxane

 

(57) Abstract:

Usage: 2,6-DIMETHYLPROPANE phenols, obtaining catalytic methylation with methanol in orthopaedie. The inventive 2,6-dimethylsiloxane phenol receive a vapor-phase Automatisierung phenol, ortho -, meta - or paracresol methanol catalysts, which are molded with a binder or put on broad porous silica gel, and then activate at 200 - 400oWith the use of reductant type of hydrogen or methanol and calcined. Get the catalyst with an atomic ratio of iron:vanadium: manganese, equal(0,5 - 1) : (1 - 0,5) : (0,05 - 0,5), the content of the active component is more than 30 wt. %. The catalyst has large pores with a radius of more than 15 nm and a pore volume of 0.5 - 1.5 cm3/year table 2.

The invention relates to a process for the catalytic methylation of phenols having two hydrogen atoms in anthopology, with the formation of 2,6-dimethylpropionic phenols in the presence of zhelezovanadievyj oxide catalysts.

Methylpropane phenols are very valuable substances and have an extensive range of applications in organic and inorganic synthesis. They are used as antioxidants and stabiliseerumine nonionic surfactants, construction materials, plant protection products, pharmaceuticals, vitamin E, etc.

Currently, the main method of obtaining methylpropionic phenols is catalytic methylation of phenol in the liquid and the vapour phase [1] In the process of methylation is formed methyl ether and the various isomeric METHYLPHENOL. As catalysts are used for various acids, salts, individual oxides and oxide composition. It is shown that the conditions of alkylation and composition of the resulting products significantly depend on the used catalysts. From the published patent literature, the most effective in the reaction of methylation of phenols in anthopology are catalysts based on iron oxides and vanadium [2, 3] Proposed to metilirovanie phenols containing at least one hydrogen atom in anthopology, in the presence of oxide catalysts containing iron and vanadium, as well as additives of the third component [2] is Set intervals compositions of the catalysts and the reaction mixture, which is mainly methylation of benzene ring in orthopaedie. Selectivity for the amount of mono - and dimethylphenol on these catalysts is 97-otka more efficient way to obtain 2,6-dimethylpropionic phenols.

In the result, found that the selective methylation of phenol, o-, m - and p-cresol with the selectivity of the formation of 2,6-dimethylpropionic to 85-97% can be achieved zhelezovanadievyj oxide catalysts containing components within the atomic ratio Fe: V:Mn(0,5-1):(1-0,5):(0-0,5). The catalysts should be in the crystalline state and having, after calcination in the temperature range 500-800aboutWith large pores with a radius of more than 15 nm and 0.5-1.5 cm3/, in Addition, to reduce design time, typical catalysts of this type, and improving the selectivity of the catalysts before reaction it is necessary to activate the processing of substances-reducing agents, such as hydrogen, methanol, etc. at temperatures of 200-400aboutC.

To prepare zhelezovanadievyj oxide catalysts can be used any soluble salts of these elements, preferably nitrates of iron and manganese and vanadium oxalate. The catalysts obtained from a solution of salts of the starting components in the respective molar ratios one way: co-precipitation, followed by filtration and drying, spray drying of a solution with a binder, followed by granulation of pasta by extrusion through a die plate of a given shape and size, any of it to prepare tablets also certain size. The obtained granules or tablets of the catalyst is dried and calcined in the temperature range 500-800aboutC.

In addition to the massive in this process are encouraged to apply and catalysts on carriers. It is shown that the most effective - ness of the broad porous carrier is silica gel with pore 30-4000 nm and 0.5-1.0 cm3/, cook it For use Aerosil, which first plastificator, granularit, and then the granules are subjected to thermoprotei autoclave at a temperature of 250-350aboutC. the Catalyst is prepared by impregnation of silica gel for moisture capacity solution mixture of salts of the components are taken in a specific atomic ratio, followed by drying and calcination.

The reaction of methylation of phenols is carried out in a flow reactor with a fixed catalyst bed. In the reactor with an inner diameter of 1.8 cm was placed a portion of the catalyst from the top to fall asleep layer (4-5 cm) of crushed quartz with a particle size of 3-5 mm, serves as the evaporator of the reaction mixture. The catalyst was calcined in the reactor in a stream of nitrogen (1-15 l/s) at a temperature of 350-550aboutC for 1 h Then it is treated of vosstanovit, not stopping the flow of nitrogen into the reactor serves a mixture of phenol, methanol and water. The molar ratio between the components of the reaction mixture varies f: M: B 1:(1-10):(1-10). The reaction is carried out at a temperature of 300-400aboutC. the reaction Products are collected in a cooled trap and analyze method getaccountinfo chromatography. The contact time varies by changing the feeding speed of the reaction mixture and the amounts of catalyst.

According to the results of chromatographic analysis of phenolic parts and products of the reaction determine the degree of conversion of phenol and selectivity of methylation. The degree of transformation (X,) is defined as the ratio of the numbers of moles of unreacted phenol and missed, the selectivity of the formation of methylated phenol (S) is defined as the ratio of the number of moles formed methylated phenol and unreacted phenol.

P R I m e R 1. In a reactor equipped with a mixer, poured 1.2 l of distilled water and bring the temperature up to 70-90aboutWith, and then dissolved under stirring in her 300 g of oxalic acid. Then to this solution was added 100 g of V2O5after dissolving , the solution is cooled. To the resulting solution was added 444,2 g Fe(NOaboutWith, and binder is placed in a Z-shaped mixer and plastificator for 0.5 h, the resulting paste granularit by extrusion through a die plate with a diameter of 3 mm Cylindrical pellets of size 3 x 3 mm, dried, and then calcined at 650aboutC.

4 g of catalyst loaded into the reactor above the catalyst bed is put a layer of quartz (4-5 cm), is used as the evaporator of the reaction mixture. Before testing the activity of the catalyst was calcined in a reactor at 400aboutWith a stream of nitrogen, then reduce the temperature to 375aboutWith and without disrupting the flow of nitrogen into the reactor serves a liquid mixture of phenol (f), methanol (M), water (C) in a molar ratio of 1: 5:3. The volumetric feed rate of the nitrogen-steam mixtures 1410 h-1. The reaction products are collected in the trap and analyzed by gas chromatography.

Feature zhelezovanadievyj catalysts is their development during the first hours in the reaction medium. The content of 2,6-Xylenol in the reaction products after 30 min comp P R I m m e R 2. In a reactor equipped with a mixer, poured 2.6 liters of water, heated to 60aboutWith and dissolve in it 41.8 g NH4VO3. In another bowl, prepare a solution of salts of iron and manganese in 100 ml of distilled water dissolve 144,3 g Fe(NO3)39H2O and 14.7 g of Mn(NO3)26H2O. In the reactor with a solution of NH4VO3poured a solution of salts of iron and manganese, the resulting suspension is evaporated to a pasty condition and granularit pasta by extrusion, the granule size 3 x 3 mm Pellets, dried and calcined as in example 1. The atomic ratio of the components in the obtained catalyst Fe:V:Mn 1:1:0,14.

Test activity carried out analogously to example 1, the volumetric feed rate of the nitrogen-steam mixtures 1070 h-1.

P R I m e R 3. A solution of oxalate vanadyl, nitrate iron (III) and manganese nitrate (II) (Fe: V:Mn 1:1:0,1), prepared analogously to example 1, dispersed in the spray dryer. The resulting powder was tabletirujut, tablet size 3 x 3 mm Heat treatment of the catalyst is similar to example 1. Test activity analogously to example 1, the volumetric feed rate of the reaction mixture 1020 h-1.

P R I m e R 4. The catalyst is prepared analogously to example the ACI reaction mixture 1020 h-1, the molar ratio f:M:B 1:8:2.

P R I m e R 5. The catalyst is prepared analogously to example 3, the atomic ratio Fe: V:Mn 1:1:0,1. Test activity analogously to example 1, the volumetric feed rate of the nitrogen-steam mixtures 350 h-1, the molar ratio f:M:B 1:8: 2.

P R I m e R 6. The catalyst is prepared analogously to example 5. Test activity carried out analogously to example 1, the volumetric feed rate of 1060 h-1, the molar ratio f:M:B 1:5:4.

P R I m e R 7. The catalyst is prepared analogously to example 3, the atomic ratio Fe: V:Mn 1:1:0,3. Test activity carried out analogously to example 1, the volumetric feed rate of the nitrogen-steam mixtures 880 h-1.

P R I m e R 8. The catalyst is prepared analogously to example 3 without manganese atomic ratio Fe:V 1:1. Test activity carried out analogously to example 1, the volumetric feed rate of the nitrogen-steam mixtures 830 h-1.

P R I m e R 9. The catalyst is prepared analogously to example 8, the atomic ratio Fe:V to 0.8:1. Test activity carried out analogously to example 8.

P R I m e R 10. The catalyst is prepared analogously to example 8, the atomic ratio Fe:V to 1.2:1. Test activity carried out analogously to example 8.

P R I m e R 11. Catalyst d of example 1, the volumetric feed rate of the nitrogen-steam mixtures 580 h-1.

P R I m e R 12. The catalyst is prepared analogously to example 11, the atomic ratio of V:Mn 1:0,3. Test activity carried out analogously to example 11.

P R I m e p 13. The catalyst is prepared analogously to example 1, the atomic ratio Fe:V:Mn 1:0,7:0,3. The catalyst suspension is dried to a paste, and then granularit extrusion, the granule size 3 x 3 mm Heat treatment of the granules is similar to example 1, the volumetric feed rate of the nitrogen-steam mixtures 2210 h-1, the molar ratio f:M:B 1:8:3.

P R I m e R 14. The catalyst is prepared by impregnation of a broad porous silica gel with a solution of iron salts, vanadium and manganese, prepared analogously to example 1, with the atomic ratio Fe:V:Mn of 1.1:1:0,2. Silica gel is prepared by mixing 1 kg of Aerosil grades a-175, 2 liters of water and 30 g of ammonium acetate in Z-shaped blade mixer. The mass is stirred until the formation of plastic paste, then it granularit by extrusion through a die plate with a diameter of 3 mm Pellets of size 3 x 3 mm air-dried first at 20aboutAnd then at 110aboutC, and then autoclave water vapor at 350aboutC for 24 h Received the silica gel has a pore radius 30-4000 nm oil twice impregnated by capacity solution of iron salts, vanadium and manganese, prepared analogously to example 1, with intermediate drying of the pellets at 110aboutC. the Content of SiO2in the catalyst 73 wt. Heat treatment of the granules is similar to example 1. Test activity analogously to example 1, the volumetric rate of the nitrogen-steam mixtures 530 h-1.

P R I m e R 15. The catalyst is prepared analogously to example 14, the temperature of the autoclave silica gel 250aboutC. the ratio of the components in the impregnating solution Fe:V:Mn of 1.4:1.0 to:0,2. The content of SiO2in the catalyst 72 wt. Test activity carried out analogously to example 1, the volumetric feed rate of the nitrogen-steam mixtures 580 h-1.

P R I m e R 16. The catalyst is prepared analogously to example 1. Test activity carried out analogously to example 1. Before submitting the reaction mixture, the catalyst was activated: rinsed with hydrogen for 30 minutes at a temperature of 250aboutC, then the temperature was raised to 375aboutWith and carry out the reaction. The catalyst activity after 30 min approaches the stationary value: X3098.4% OF Sx75.4% of

P R I m e R 17. The catalyst is prepared analogously to example 1. Test activity carried out analogously to example 1. Activation of the catalyst is carried out in pairs of methanol in the course of the activity carried out analogously to example 1, instead of phenol used o-cresol (o-Cu), the ratio of the o-Cu:M:B 1:5:3. The volumetric feed rate of the nitrogen-steam mixtures 1250 h-1.

In table. 1 shows the stationary characteristics of the activity of the catalysts of examples 1-18.

P R I m e R 19. The catalyst is prepared analogously to example 1. Test activity carried out analogously to example 1, instead of phenol used m-cresol (m-Cu), the ratio of the components in the reaction mixture m-Cu:M:B 1:5:3, the volumetric feed rate of the nitrogen-steam mixtures 1330 h-1.

P R I m e R 20. The catalyst is prepared analogously to example 1. Test activity carried out analogously to example 19, the volumetric feed rate of the nitrogen-steam mixtures 1570 h-1.

P R I m e R 21. The catalyst is prepared analogously to example 1, the test activity carried out analogously to example 19, the ratio of the components in the reaction mixture m-Cu: M: B 1:8:3, the volumetric feed rate of the reaction mixture 1600 h-1.

The results of examples 19-21 are given in table. 2.

P R I m e R 22. The catalyst is prepared analogously to example 1. Test activity carried out analogously to example 1, instead of phenol used p-cresol (p-CR), the ratio of the components of the p-CR:M:B 1:5:3, the volumetric feed rate of the nitrogen-parthi carried out analogously to example 22, the volumetric feed rate of the nitrogen-steam mixtures 1660 h-1.

The results of examples 22 and 23 are given in table. 3.

As can be seen from the above results, the proposed method for the methylation of phenols with hydrogen atoms in anthopology, in the presence of macroporous zhelezovanadievyj catalyst increases the activity and selectivity for 2,6-methylpropionyl phenols in comparison with known methods. In addition, the proposed pre-activation of the catalysts in the presence of substances-reducing agents significantly reduces the period of development of such catalysts.

The METHOD of OBTAINING 2,6-DIMETHYLSILOXANE PHENOL vapor-phase Automatisierung phenols in the presence of the oxide zhelezovanadievyj catalysts, wherein the catalysts used pre-activated at 200 - 400oWith the environment reductant solid or deposited on a broad porous silica gel zhelezovanadievyj or zhelezomargantsevye catalysts with the active component at least 30 wt. %, the atomic ratio of the metals Fe and V is 0.5 - 1 : 1 - 0.5 or Fe : V : Mn 0,5 - 1 : 1 - 0,5 : 0,05 - 0,5, when this catalyst has large pores with a radius of b is

 

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