Molded ionite catalyst and a method for preparation thereof

FIELD: organic synthesis catalysts.

SUBSTANCE: invention relates to methods of preparing catalysts based on sulfurized styrene/divinylbenzene copolymer and thermoplastic polymer material, which are used in processes for preparing alkyl tert-alkyl ethers, hydration of olefins, dehydration of alcohols, preparation of esters, and the like. Invention provides molded ionite catalyst consisted of sulfurized styrene/divinylbenzene copolymer in the form of mixture of powdered copolymers with macroporous and gel structure and, as thermoplastic material, propylene polymers and propylene/ethylene copolymers. Preparation of catalyst is accomplished by extrusion at temperature of heating extruder cylinder 140-200°C and temperature of forming head equal to temperature of the last heated zone of heating cylinder.

EFFECT: increased catalytic activity.

10 cl, 3 tbl, 15 ex

 

The invention relates to methods of making catalysts, in particular catalysts based on sulfonated copolymer of styrene and divinylbenzene, and a thermoplastic polymeric material. These catalysts are widely used in producing alkyl tert-alilovic esters, hydration of olefins, dehydration of alcohols, obtaining esters and other

Known catalyst and method of its preparation on the basis of ion-exchange resins and thermoplastic polymeric materials by mixing, heating to the melting temperature of thermoplastic and forming the finished product by extrusion (USSR Author's certificate N 376984, CL 01 J 11/00, 1970). The catalyst prepared by this method has low activity. In addition, when the swelling in water observed increase in the volume of catalyst in two or three times and reducing its mechanical strength.

Known catalyst and method of its preparation on the basis of ion-exchange resins and thermoplastic polymeric materials with additives of organic substances which can be combined with a thermoplastic and can be dissolved in organic solvents (USSR Author's certificate N 448664, CL 01 J 11/00, 1971). The disadvantage of this method is the introduction of an additional stage in the process of its preparation, processing with an organic solvent.

<> The closest analogue is ionite the catalyst based on sulfonated copolymer of styrene and divinylbenzene, and a method thereof, including a mixture of sulfonated copolymer of styrene and divinylbenzene with a thermoplastic polymeric material and water, heating the mixture to the melting temperature of thermoplastic and molding the mixture by extrusion (USSR Author's certificate N 677191, CL 01 J 37/00, 01 J 31/08, 1972). At the stage of molding temperature of the material of the cylinder set at 20-40°C lower than the temperature of the forming head.

However, the catalyst obtained by this method has a relatively low activity in the processes of hydration isobutene (IB) to trimethylamine (TMK), dehydration TMK to information security, as well as in the synthesis of methyl tert-butyl ether (MTBE). So, are calculated from the examples describe how values of specific performance of the catalyst in the process of dehydration TMK (example 5) do not exceed 0,021 mol/(g cat·h), in the hydration IB (example 7) of 0.01 mol/(g cat·h), in the synthesis of MTBE (example 8) 0,026 mol MTBE/(g cat·h).

The aim of the present invention to provide a catalyst with increased activity.

This is achieved using ion exchangers molded catalyst consisting of sulforaphane what about a copolymer of styrene and divinylbenzene and thermoplastic material - polymers of propylene or copolymers of propylene and ethylene, in which the sulfonated copolymer of styrene and divinylbenzene take a mixture of powdered sulfonated copolymers of styrene and divinylbenzene macroporous and gel structure. You can get this catalyst was carried out by mixing the sulfonated copolymers of styrene and divinylbenzene, and a thermoplastic material, followed by molding the mixture by extrusion, which is conducted at the temperature of the material of the cylinder of the extruder 140-200°and the temperature of the forming head, equal to the temperature in the last heated zone of the material of the cylinder of the extruder.

Preferably as a sulfonated copolymer of styrene and divinylbenzene take a mixture of powdered sulfonated copolymers of styrene and divinylbenzene macroporous and gel structure when the mass ratio (1÷9):(9÷1) calculated on the dry weight of the copolymers.

Preferably as a sulfonated copolymer of styrene and divinylbenzene take a mixture of powdered sulfonated copolymers of styrene and divinylbenzene macroporous and gel structure with a water content of 5-25% wt.

Preferably as a sulfonated copolymer of styrene and divinylbenzene macroporous and gel structure using the coat is AI, containing not more than 15% wt. particles of the copolymer calculated on the dry product larger than 125 microns.

Preferably as a sulfonated copolymer of styrene and divinylbenzene gel structure using fractions, containing not less than 75% wt. particles of the copolymer calculated on the dry product with a size less than 100 microns.

Preferably as a sulfonated copolymer of styrene and divinylbenzene macroporous structures use fractions containing not less than 50% wt. particles of the copolymer calculated on the dry product with a size less than 100 microns.

Preferably as a sulfonated copolymer of styrene and divinylbenzene macroporous structures use fractions containing at least 99% wt. particles of the copolymer calculated on the dry product with a size less than 200 microns.

Preferable as thermoplastic material used polymers of propylene or copolymers of propylene and ethylene.

Preferably the formation of the mixture is conducted in an extruder having more than two heated zones.

Preferably the temperature in each subsequent heated zone of the extruder is maintained at 5-15°With more of the previous temperature of the heated zone.

As sulfonated copolymers of styrene and divinylbenzene can be used powdered gel and macroporous sulfate the ion exchangers according to THE 2227-025-39659962-2003, and, in particular, the sulfonic cation according to GOST 20298-74 and TU-93, shredded and dried to the above parameters.

As thermoplastic materials can be used polypropylene on THE other 2211-075-54155590-01 brands 21007 and 21015 and statcompiler propylene with ethylene brands and 23007 23015.

The following examples illustrate the method:

The preparation of the catalyst.

Example 1.

In a drum mixer with a volume of 1.5 m3through a special hatch load of 37.5 kg of powdery polypropylene brand 21007, 15,0 kg powder macroporous sulfonic cation exchanger containing 25% wt. water, and of 117.6 kg powder gel sulfonic cation exchanger containing 14 wt.%. water. The mass ratio of powder sulfonic cation macroporous and gel structure is 1:9 in dry weight. The content of sulfonic cation on the dry weight of the mixture with the polypropylene is equal to 75% wt. in terms of dry weight.

Mass fraction of particles above 125 μm powder macroporous sulfonic cation exchanger is of 15.0%, gel - 8,0%. Mass fraction of particles below 100 microns powder macroporous sulfonic cation exchanger is 58,0%, gel - 83.0 per cent. Mass fraction of particles below 200 microns powder macroporous sulfonic cation exchanger is 99,2%.

After components are loaded close the hatch, include the drive and rotation of the bar is Ana-mixer with a speed of 120 rpm for 4 hours thoroughly mixed polypropylene and sulfonic cation. After stirring through the open hatch unload the mixture from the drum mixer to the hopper, where it is dosed with a screw in a screw-press release chop-85.

In the worm-Timna press using two worm shafts of different length, rotating towards each other, the mixture of sulfonic cation with polypropylene is fed through four sequentially arranged and heated areas to the granulating head. The temperature in the case of the first heated zone support 155°C, second 170°C, third -185°C, fourth and granulating head - 200°C.

After all zones worm-drying machines catalyst mass is forced through the die plate and comes out in the form of cylinders or tubes, depending on the design of the forming head. Facing cylinders or tubes are cut by the rotating knife with obtaining pellets of a certain length, which is governed by the number of revolutions of a rotating knife. Granules of the catalyst is cooled with water to prevent clumping, washed on a shaker and loaded in bags of 20 kg

Examples 2-7.

Illustrate the method of preparation of the catalyst under different conditions: mass ratios DIF/GI sulfonic cation, the content of sulfonic cation in a mixture with thermoplastic material, the dimensions used fractions of particles sulfonic cation, marks thermoplas the ranks of the material, the temperature of the heated zones and the number of heated zones.

Conditions of preparation of the catalysts are shown in table 1.

Testing of samples of catalysts in the synthesis of methyl tert-butyl alcohol, hydration isobutene and dehydration trimethylarsine.

Example 8.

Synthesis of methyl tert-butyl ether (MTBE) is performed on the continuous action using ionite molded catalyst obtained in experiment 3. In a tubular reactor with an inner diameter of 21 mm and a length of 1 m, equipped with a thermostatic jacket, loaded with 30 g of catalyst. The methanol content of the basic substance at 99.95% wt. continuously at a rate of 280 ml/hour (221,5 g/h, 6,92 mol/h) is fed to the line of the isobutylene content of the basic substance to 99.9% wt. The feed rate of isobutylene 320 ml/hour (191,0 g/h, 3,41 mol/hour). The molar ratio of methanol : isobutylene in the original mixture at the inlet of the reactor is 2:1. The temperature in the reactor support 90°filing in the shirt of the coolant from thermostat, a pressure of 2.0 MPa. Coming out of the reactor, the reaction mass contains, wt.%: MTBE 66,76; methanol 29,38; isobutylene 3,71; trimethylarsine (TMK) of 0.15. The degree of conversion of isobutylene 92%. The performance of the catalyst in 0.104 mol MTBE/(g cat · h) compared with 0,026 mol MTBE/(g cat · h) prototype.

Example 9.

Synthesis of MTBE carried out using the catalyst obtained in example 5 according to the technology described in example 8. The methanol content of the basic substance at 99.95% wt. continuously at a rate of 135 ml/h (107 g/h, 3,34 mol/h) is fed to the line isobutane-isobutilene fraction containing isobutylene 45% wt. The feed rate of the isobutane-isobutilene fraction 365 ml/h (299,5 g/h, 1,68 mol/h of isobutene). The molar ratio of methanol : isobutylene in the original mixture at the inlet of the reactor is 2:1. The temperature in the reactor support 90°C, a pressure of 2.0 MPa. Coming out of the reactor, the reaction mass contains, wt.%: MTBE 42,95; methanol 18,17; isobutylene 2,40; isobutane 36,40; trimethylarsine of 0.08. The degree of conversion of isobutylene 92%. The performance of the catalyst 0,051 mol MTBE/g cat · h compared with 0,026 g MTBE/ g cat · the hour in the prototype when using 100%of isobutylene.

Example 10.

Hydration of isobutylene is carried out at the installation of continuous operation using ionite molded catalyst obtained in experiment 2. In a tubular reactor with an inner diameter of 21 mm and a length of 1 m, equipped with a thermostatic jacket, loaded with 30 g of catalyst. In the lower part of the reactor continuously served the isobutylene content of the basic substance at 99.95% wt. with a speed of 40 ml/hour (23,9 g/HR, 0.43 mol/h), ve is hnwu part - water at a rate of 280 ml/h (280 g/h, 15,54 mol/hour). The volume ratio of water : isobutylene 7:1. The temperature in the reactor support 90°filing in the shirt of the coolant from thermostat, a pressure of 2.0 MPa. From the bottom of the reactor enters the reaction mass of the following composition, % wt.: TMK of 10.05; water 89,69; isobutylene 0,24; dimers of isobutylene 0,02. The degree of conversion of isobutylene 97%, selectivity 99,74. The performance of the catalyst 0.014 mol PMC /(g cat · h) compared with 0,0103 mol PMC/(g cat. · h) in the prototype.

Examples 11-14.

Illustrate the activity of the catalysts obtained in examples 1, 4, 6 and 7. The results are shown in table 2.

Example 15.

Dehydration of trimethylarsine spend on the installation of periodic action using ionite molded catalyst obtained in experiments 1-7. In a glass flask with a capacity of 500 cm3equipped with reflux condenser, placed 10±0.1 g dried at a temperature of 100-105°C to constant mass of the catalyst and the cylinder pour 50 cm3trimethylarsine. The process of dehydration is carried out at the boiling temperature of TMK (80°C), which is supported using the boiling water bath.

Generated by decomposition TMK isobutylene condense in a graduated vial, cooled in a Dewar vessel filled with the ohms with a mixture of acetone and solid carbon dioxide. Every 30 minutes, record the volume of the resulting isobutylene. At the end of the experiment (2 hours) measure the temperature of cooling the mixture to accurately determine the mass accumulated in the ampoule of isobutylene.

The catalyst is determined in percentage as the ratio of the mass of the spin-off of isobutylene to theoretically possible. The results are shown in table 3.

Table 3

Test samples of the catalysts in the dehydration of trimethylarsine.
CatalystThe time of measurement of the volume of isobutylene, hActivity, %The performance of the catalyst, mol/(g cat·h)
For example 11,5750,0264
For example 21,5810,0285
For example 31.0800,0422
In example 41,5780,0274
For example, 51,0760,0401
In example 62,0790,0208
In example 72,0810,0214

The use of PR is degenova ionite molded catalyst and method of its production can improve the performance of processes of production of alkyl tert-alilovic esters, hydration of olefins, dehydration of alcohols, obtaining esters and others, to increase the degree of conversion of the raw materials and, consequently, to reduce energy costs.

1. Ionite molded catalyst consisting of a sulfonated copolymer of styrene and divinylbenzene and thermoplastic material - polymers of propylene or copolymers of propylene and ethylene, characterized in that as a sulfonated copolymer of styrene and divinylbenzene, a mixture of powdered sulfonated copolymers of styrene and divinylbenzene macroporous and gel structure.

2. The method of obtaining ionite molded catalyst according to claim 1 by mixing sulfonated copolymer of styrene and divinylbenzene, and a thermoplastic material, and molding the mixture by extrusion at elevated temperature material extruder barrel and die head, characterized in that the molding mixture is conducted at the temperature of the material of the cylinder of the extruder 140-200°and the temperature of the forming head, equal to the temperature in the last heated zone of the material of the cylinder of the extruder.

3. Ionite molded catalyst according to claim 1, characterized in that as a sulfonated copolymer of styrene and divinylbenzene, a mixture of powdered sulfonated copolymers article is Rola and divinylbenzene macroporous and gel structure when the mass ratio (1÷ 9):(9÷1) calculated on the dry weight of the copolymers.

4. Ionite molded catalyst according to claim 1, characterized in that as a sulfonated copolymer of styrene and divinylbenzene, a mixture of powdered sulfonated copolymers of styrene and divinylbenzene macroporous and gel structure with a water content of 5-25 wt.%.

5. Ionite molded catalyst according to claim 1, characterized in that as a sulfonated copolymer of styrene and divinylbenzene macroporous and gel structures use fractions containing not more than 15 wt.% particles of the copolymer calculated on the dry product larger than 125 microns.

6. Ionite molded catalyst according to claim 1, characterized in that as a sulfonated copolymer of styrene and divinylbenzene gel structure using the fractions containing at least 75 wt.% particles of the copolymer calculated on the dry product with a size less than 100 microns.

7. Ionite molded catalyst according to claim 1, characterized in that as a sulfonated copolymer of styrene and divinylbenzene macroporous structures use fraction containing at least 50 wt.% particles of the copolymer calculated on the dry product with a size less than 100 microns.

8. Ionite molded catalyst according to claim 1, characterized in that as a sulfonated copolymer of styrene and divinylbenzene macroporous is tructure use fractions, containing not less than 99 wt.% particles of the copolymer calculated on the dry product with a size less than 200 microns.

9. The method according to claim 2, characterized in that the formation of the mixture is conducted in an extruder having more than two heated zones.

10. The method according to claim 2, characterized in that the temperature in each subsequent heated zone of the extruder is maintained at 5-15°With more of the previous temperature of the heated zone.



 

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