Catalyst and method of obtaining methanoic acid

FIELD: chemistry.

SUBSTANCE: present invention relates to vanadium-titanium oxide catalysts, used in production of methonoic acid through gas-phase oxidation of formaldehyde with oxygen and methods of obtaining methanoic acid using these catalysts. Described is a catalyst based on vanadium and titanium oxides, containing 7.0-50.0 wt % vanadium oxide and in form of granules with one or several through-holes and equivalent diametre of the granules defined by the ratio 6V/S, where V is the volume of the catalyst granule and S is the outer surface area of the catalyst granule. The equivalent diametre lies between 2.0 and 3.9 mm and mainly between 2.4 and 3.5 mm. Described also is a method of obtaining methanoic acid through oxidation of formaldehyde with oxygen in one or several serial pipe reactors in the presence of the above described catalyst.

EFFECT: increased catalyst activity and increased output of methanoic acid.

7 cl, 10 ex, 1 tbl

 

The invention relates to vanadium oxide-titanium catalysts used for formic acid by gas-phase oxidation of formaldehyde oxygen and the methods of obtaining the formic acid with the use of these catalysts.

Known catalyst for the synthesis of formic acid (U.S. Pat. Of the Russian Federation No. 2235586, B01J 23/22, 10.09.2004)containing, wt.%: the vanadium oxide 10-25, the oxide of the alkali earth metal 0,5-10 and titanium oxide - rest. The catalyst is a cylindrical pellet size 4×4 mm and has a value of specific surface area 153-190 m2/, At a temperature of 110-120°C and contact time is 4-6,and 7 seconds (sec·g/ml) degree of conversion of formaldehyde (X, %) is 75,8-to 81.7% and the selectivity (S, %) 76,5-93,5%. The yield of formic acid (X × S, %) even for the best sample does not exceed 76%.

The disadvantage of the catalyst is low activity, as evidenced by insufficiently high conversion of formaldehyde with significant contact times and low yield of formic acid.

When the reaction of oxidation of formaldehyde to formic acid is allocated a large amount of heat, which may result in heating of the catalyst. At the same time, from kinetic considerations, the reaction should be carried out in the temperature range of 110-130°C. To keep the reaction in this temperature range, you must ensure the ecity the heat of reaction. In practice, this is implemented by placing the pelletized catalyst inside the tubes of the tubular reactor. In the annular space of the reactor is the heat-transfer fluid - boiling liquid, such as water or circulating fluid. Reaction heat is removed from the catalyst layer to the carrier due to the radial heat conduction layer and the heat transfer through the wall. The intensity of heat transfer depends on the shape and size of the granules of the catalyst. The shape and size of the granules of the catalyst is essential for the pressure drop in the layer and use the internal surface of the catalyst. From a practical point of view, acceptable pressure drop are realized when the hydraulic size of the granules of the catalyst is not less than 3 mm At the same time increasing the size of the granules leads to difficulty of diffusion of the reactants to the inner surface of the catalyst, that is, to interdiffuse inhibition. The result interdiffuse inhibition is the reduction of the observed activity and selectivity of the catalyst.

The invention solves the problem of increasing the activity and selectivity of the catalyst, that is, to increase the yield of formic acid.

The problem is solved as suggested by the catalyst.

Proposed a catalyst based on oxides of vanadium and titanium for formic acid by g is softgogo oxidation of formaldehyde by oxygen, containing 7,0-to 50.0 wt.% vanadium oxide granules which have one or more through holes, and the equivalent diameter of the granules, defined as 6V/S, where V is the volume of the catalyst pellet, S - area of the outer surface of the catalyst pellet is in the range of 2.0-3.9 mm, mostly in the range of 2.4-3.5 mm using a catalyst with such characteristics allows to minimize negative effects from interdiffuse braking and thereby increase its activity and selectivity. The granules may be in the form of Raschig rings, or trilistniku with holes, or chetyrehlistnik with holes, or spoked wheels or cylinders with a few holes. The use of the catalyst of this form allows you to increase the hydraulic diameter (reducing the hydraulic resistance of the catalyst layer), retaining its activity and selectivity.

The surface of the catalyst is not less than 40 m2/year

The task is also solved by a method of obtaining formic acid by oxidation of formaldehyde oxygen in one or several tubular reactors in the presence of the above catalyst. The process can be carried out in the presence of water vapor. For formic acid is used formaldehydefree gas mixture, the resulting oxidized who eat methanol or obtained in any other way. Formaldehyde containing gas mixture can be obtained by passing a gas mixture containing methanol and oxygen, sequentially through the tubular reactor zhelezorudnom catalyst and through the adiabatic layer of the catalyst.

The catalytic activity of the samples in the oxidation of formaldehyde determined in a flow-circulation installed in the temperature range of 105-135°C. when the content in the original reaction mixture of formaldehyde from 3.5 to 10 vol.%, oxygen 5-20%, water vapor 0-40%, the rest is nitrogen at different contact times. The main products of the oxidation reaction of formaldehyde (CH2O) are formic acid (CH2About2), carbon oxides (CO, CO2and methylformate (SOON3).

In this invention the catalytic activity is characterized by a reaction rate constant of the first order (K, ml/g·sec), the selectivity for the reaction products (S, %), degree of conversion of formaldehyde (X, %) and the yield of formic acid (Y, %). Contact time is defined as the ratio of the weight of catalyst in grams to the flow of the original reaction mixture in ml/sec.

The specific surface of the catalyst (Sbeatsm2/g) determined by the BET method by thermal desorption of argon.

For the preparation of vanadium-titanium catalysts as a source of vanadium compounds COI is lsout solution of oxalate vanadyl, which is prepared by dissolving vanadium pentoxide in oxalic acid as a starting compound of titanium - titanium oxide, a hydrogel or a xerogel of titanium dioxide amorphous or crystalline structure of anatase. As starting compounds of the promoters use soluble salts, hydroxides or oxides of the respective metals.

The catalysts can be prepared in various ways, for example through the following stages:

1 - preparation of the solution of salt of vanadium;

2 - preparation of a suspension of titanium dioxide in a solution of salt;

3 - drying the catalyst slurry;

4 - mix the powder with forming additives;

5 - granulation of the catalyst;

6 - the crop has wilted catalyst in air;

8 - heat treatment of the catalyst at a temperature of 400-550°C.

The following examples illustrate the essence of the invention.

Example 1.

Charged to the reactor oxide vanadium-titanium catalyst composition, wt.%: 20 vanadium oxide and 80 titanium oxide with a surface of 120 m2/g, made in the form of rings 4×2.4 mm×4 mm (external diameter × inner diameter × height). The equivalent diameter of the catalyst pellet is 2.0 mm, the Volume and the surface of the catalyst pellet is shown in the Table. The original reaction mixture, vol.%: 5 formaldehyde, 15 oxygen, 10 water vapor, Stalin the e - the nitrogen is directed into the reactor, the conditional contact time 4.9 sec·g/ml, the temperature in the reactor to 120°C. the Conversion of formaldehyde 90.2%, the selectivity for formic acid 89.5%, the selectivity for products of deep oxidation 10.5%methylformate <0.05%. The yield of formic acid is 80.8%.

Example 2.

Charged to the reactor oxide vanadium-titanium catalyst composition, wt.%: 20 vanadium oxide and 80 titanium oxide with a surface of 120 m2/g, made in the form of rings 5×3×5 mm Equivalent diameter of the catalyst pellet is 2.5 mm, the Volume and the surface of the catalyst pellet is shown in the Table. The original reaction mixture, vol.%: 5 formaldehyde, 15 oxygen, 10 water vapor, the rest is nitrogen, is directed into the reactor, the conditional contact time 4.9 sec·g/ml, the temperature in the reactor to 120°C. the Conversion of formaldehyde 89.3%, the selectivity for formic acid 90.3%, the selectivity for products of deep oxidation 9.7%methylformate <0.05%. The yield of formic acid is 80.6%.

Example 3.

Charged to the reactor oxide vanadium-titanium catalyst composition, wt.%: 20 vanadium oxide and 80 oxide surface 120 m2/g, made in the form of rings 5×2×5 mm Equivalent diameter of the catalyst pellet is 3.5 mm, the Volume and the surface of the catalyst pellet is shown in the Table. The initial reaction mixture contains, vol.%: 5 formaldehyde, 15 oxygen, 10 water vapor, the rest is nitrogen, is directed into the reactor, the conditional contact time 4.9 sec·g/ml, the temperature in the reactor to 120°C. the Conversion of formaldehyde 87.1%, the selectivity for formic acid 91.0%, the selectivity for products of deep oxidation 9.0%methylformate <0.05%. The yield of formic acid is 79.3%.

Example 4.

Charged to the reactor oxide vanadium-titanium catalyst composition, wt.%: 20 V2O5and 80 TiO2with the surface to 120 m2/g, made in the form of rings 6×2.7×6.1 mm Equivalent diameter of the catalyst pellet is 3.9 mm, the Volume and the surface of the catalyst pellet is shown in the Table. The original reaction mixture, vol.%: 5 formaldehyde, 15 oxygen, 10 water vapor, the rest is nitrogen, is directed into the reactor, the conditional contact time 4.9 sec·g/ml, the temperature in the reactor to 120°C. the Conversion of formaldehyde 86.0%, the selectivity for formic acid 90.0%, the selectivity for products of deep oxidation 10.0%methylformate <0.05%. The yield of formic acid is 77.4%.

Example 5.

Charged to the reactor oxide vanadium-titanium catalyst composition, wt.%: 7 vanadium oxide and 93 of titanium oxide with a surface of 40 m2/g, made in the form of rings 5×3×5 mm Equivalent diameter of the catalyst pellet is 2.5 mm, the Volume and surface gra the ula catalyst shown in the Table. The original reaction mixture, vol.%: 5 formaldehyde, 10 oxygen, 10 water vapor, the rest is nitrogen, is directed into the reactor, the conditional contact time 4.5 sec·g/ml, the temperature in the reactor at 135°C. the Conversion of formaldehyde 83%, the selectivity for formic acid 93.0%, the selectivity for products of deep oxidation 7.0%methylformate <0.05%. The yield of formic acid 77.2%.

Example 6.

Charged to the reactor oxide vanadium-titanium catalyst composition, wt.%: 50 vanadium oxide and 50 titanium oxide with a surface of 250 m2/g, made in the form of rings 5×3×5 mm Equivalent diameter of the catalyst pellet is 2.5 mm, the Volume and the surface of the catalyst pellet is shown in the Table. The original reaction mixture, vol.%: 5 formaldehyde, 10 oxygen, 10 water vapor, the rest is nitrogen, is directed into the reactor, the conditional contact time of 5.0 sec·g/ml, the temperature in the reactor 105°C. the Conversion of formaldehyde to 90%, the selectivity for formic acid 92.0%, the selectivity for products of deep oxidation 8.0%methylformate <0.05%. The yield of formic acid 82.8%.

Example 7 (comparative).

Charged to the reactor oxide vanadium-titanium catalyst composition, wt.%: 20 vanadium oxide and 80 titanium oxide with a surface of 120 m2/g, made in the form of cylinders 6×6 mm (external diameter × height). The equivalent diameter of g is analy catalyst is 6.0 mm The volume and the surface of the catalyst pellet is shown in the Table. The original reaction mixture, vol.%: 5 formaldehyde, 15 oxygen, 10 water vapor, the rest is nitrogen, is directed into the reactor, the conditional contact time 4.9 sec·g/ml, the temperature in the reactor to 120°C. the Conversion of formaldehyde 80.7%, the selectivity for formic acid 82.0%, the selectivity for products of deep oxidation 18.0%methylformate <0.05%. The yield of formic acid is 66.2%.

Example 8 (prototype).

The catalyst composition, wt.%: 20 V2O5, 74 TiO2and 6 Cao surface 190 m2/g, made in the form of cylinders 4×4 mm Equivalent diameter of the catalyst pellet is 4.0 mm, the Volume and the surface of the catalyst pellet is shown in the Table. The initial reaction mixture containing 7 vol.% formaldehyde, oxidizes when the conditional contact time 4.5 sec·g/ml, the temperature in the reactor 110°C. the Conversion of formaldehyde 81.7%, the selectivity for formic acid 87.7%. The yield of formic acid is 71.6%.

Example 9 (method implementation).

In the evaporator serves 247 g/hour of methanol and 2.7 m3/h of air. Received metrologichna gas mixture is fed to the tube with zhelezorudnom catalyst, placed in a fluidized sand layer with a temperature of 270°C. Fluidized bed acts as a thermostat for the heat of reaction. The tube has the t internal diameter of 24 mm, the contact time of the gas in the tube is 0.5 C. Coming out of the tube, the reaction mixture with a temperature of 300°C is served in the adiabatic layer zhelezorudnogo catalyst and exits with a temperature of 345°C. the contact Time in the adiabatic layer is 0.15 C. At the outlet of the adiabatic layer, the degree of conversion of methanol is 99.7%, the selectivity of the conversion of methanol into formaldehyde - 95.0%. The resulting reaction mixture containing formaldehyde 5.5% vol. and water vapor 7.9% vol. served in 5 parallel connected tubes with vanadium-titanium catalyst, placed in a fluidized sand layer with a temperature of 115°C. the Tubes have an internal diameter of 22 mm, the contact time of the gas in the tubes is 6 sec. In tube uploaded oxide vanadium-titanium catalyst containing 18 V2O5wt.%, with the surface 100 m2/g, made in the form of rings 5×3×5 mm Equivalent diameter of the catalyst pellet is 2.5 mm, the Degree of conversion of formaldehyde is 98.5%. After passing through the tubes with the vanadium-titanium catalyst gas mixture with the reaction products are cooled in a refrigerator to a temperature of -5°C, where the condensation of the vapors of formic acid and water. The amount of condensation with the content of formic acid 56.9 wt.% is 467 g/hour. In addition, 19 g/h of formic acid contained in leaving the eat gas. The yield of formic acid is 81.8%, and the selectivity of the oxidation of formaldehyde to formic acid 83%.

Example 10 (method of implementation).

Formaldehydefree the mixture is produced analogously to example 8. The resulting reaction mixture containing formaldehyde 5.5% vol. and water vapor 7.9% vol. served in 5 parallel connected tubes with vanadium-titanium catalyst, placed in a fluidized sand layer with a temperature of 100°C. the Tubes have an internal diameter of 25 mm, the contact time of the gas in the tubes is 1.5 C. In the tube uploaded oxide vanadium-titanium catalyst containing 18 V2O5wt.%, with the surface 100 m2/g, made in the form of rings 5×3×5 mm Equivalent diameter of the catalyst pellet is 2.5 mm, the resulting reaction mixture was fed to the second stage oxidation of formaldehyde in 5 parallel connected tubes with the same vanadium-titanium catalyst, placed in a fluidized sand layer with a temperature of 110°C. the Tubes have an internal diameter of 25 mm, the contact time of the gas in the tubes is 1.5 C. the resulting reaction mixture was fed to the third stage in 5 parallel connected tubes with the same vanadium-titanium catalyst, placed in a fluidized sand layer with a temperature of 120°C. the Tubes have internal the diameter of 25 mm, the contact time of the gas in the tubes is 1.5 S. the Overall grade is the conversion of formaldehyde is 98.7%. The final reaction mixture is cooled in a refrigerator to a temperature of -5°C, where the condensation of the vapors of formic acid and water. The amount of condensation with the content of formic acid 56.4 wt.% is 465 g/H. in Addition, 19 g/h of formic acid contained in the exhaust gas. The yield of formic acid is 83.9%, and the selectivity of the oxidation of formaldehyde to formic acid 85.0%.

Characteristics of the catalysts described in examples 1-8 shown in the table.

As can be seen from the table, the inventive catalysts are characterized by high selectivity, more active and show a higher yield than the catalyst of the prototype.

1. The catalyst based on oxides of vanadium and titanium for formic acid by gas-phase oxidation of formaldehyde oxygen containing 7,0-to 50.0 wt.% vanadium oxide, characterized in that it has the form of granules with one or more through-holes, and the equivalent diameter of the granules, defined as 6V/S, where V is the volume of the catalyst pellet, S - area of the outer surface of the catalyst pellet is in the range of 2.0-3.9 mm, mostly in the range of 2.4 to 3.5 mm

2. The catalyst according to claim 1, characterized in that its granules have the form of Raschig rings or trilistniku, or chetyrehlistnik, or wheels with spokes, or cilin the ditch with a few holes.

3. The catalyst according to claim 1, characterized in that it has a surface of at least 40 m2/year

4. The method of obtaining the formic acid by oxidation of formaldehyde oxygen in one or several tubular reactors, wherein the process is carried out in the presence of a catalyst according to any one of claims 1 to 3.

5. The method according to claim 4, characterized in that the process is carried out in the presence of water vapor.

6. The method according to any of claims 4 to 5, characterized in that for formic acid is used formaldehydefree gas mixture obtained by oxidation of methanol, or obtained in any other way.

7. The method according to claim 6, characterized in that formaldehydefree gas mixture is produced by passing a gas mixture containing methanol and oxygen, sequentially through the tubular reactor zhelezorudnom catalyst and through adiabatic layer of the same catalyst.



 

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