Method of regenerating basic anionite catalysts

FIELD: industrial organic synthesis catalysts.

SUBSTANCE: invention relates to regeneration of basic anionite catalysts for process of production of alkylene glycols via hydration of corresponding alkylene oxides. Method according to invention consists in treatment of spent catalyst with aqueous solution of inorganic salts of iodine and inorganic acids or with hydroiodic acid aqueous solution.

EFFECT: achieved complete restoration of initial volume and selectivity of catalyst and thereby prolonged lifetime of expensive anionite catalyst.

1 tbl, 8 ex

 

The invention relates to a method of regeneration of the basic anionite catalysts used for the process of hydration of the oxides alkylene to alkalophile components for antifreeze, antifreeze, hydraulic and hydro hydraulic brake fluids and intermediates in the production of solvents, plasticizers and other materials used in the plastics industry, pesticides, varnishes and paints.

There are several ways to obtain alkalophile hydration of oxides alkylene at elevated temperature and pressure, using as catalyst anion exchange resin - supported catalysts basic type (US 6580008, US 6448456, US 6479715, US 6137015, EN 2001901).

The main disadvantage of all known methods of hydration in the presence of anionite catalysts is that the hydration process all known anionite catalysts increases its volume, i.e. swell, and at the same time lose their activity and selectivity. This eventually leads to clogging of the reactor and, consequently, to stop the process.

Despite numerous attempts to reduce the swelling properties anionite catalysts, to completely eliminate this effect is to date no one has succeeded. Swollen catalyst after unloading is a friable polymer mass which obacentral for recycling.

The objective of the invention is the regeneration of the basic anionite catalysts, i.e. the restoration of their original volume, activity and selectivity of action.

This task is solved by processing waste anionite catalysts in an aqueous solution of inorganic salts of iodine and inorganic acids or aqueous solution itestosterone acid.

As the inorganic salts of iodine can be used water-soluble salt of iodine, in particular Na, K, etc. as inorganic acids can be used HCl, H2SO4and other

Preferably, the treatment is carried out in the reactor hydration passing an aqueous solution containing inorganic salts of iodine and inorganic acid salt or an aqueous solution itestosterone acid through the layer of waste swollen catalyst.

However, processing can be performed in other devices by mixing unloaded from the reactor catalyst with an aqueous solution of the above substances.

The concentration of inorganic salts of iodine and inorganic acids in solution and the temperature of processing, mainly affects the regeneration time. At low concentrations is observed only increase in time of regeneration. When using solutions with high concentration of salts and acids (more than 10 wt.%) time regenerat and decreases but this increases the time of washing the regenerated catalyst from the inorganic salts of iodine and/or inorganic acids. Carrying out the process at elevated temperatures reduces the regeneration time, however, increasing energy costs.

Preferably, the regeneration process to carry out when using solutions containing 1-8 wt.% salts and/or acids and the ambient temperature.

To remove residual salts and acids from the regenerated catalyst (to exclude the ingress of salts of iodine and inorganic acids in the reaction products) before the beginning of the hydration process, the regenerated catalyst is usually washed with water.

The following examples illustrate the method:

Examples 1-3 (Hydration of ethylene oxide)

The process is carried out in a tubular reactor displacement volume of 2.2 ml, filled with a catalyst in a quantity of 1 ml as a catalyst using the anion exchange resin grades AB-17-T, Dowex SBR, Amberjet 4400 in bicarbonate form, representing a cross-linked divinylbenzene polystyrene containing Quaternary ammonium groups, coordinated by anions of carbonic acid.

At the entrance of the reactor serves the initial charge is a mixture of ethylene oxide and water. The concentration of ethylene oxide in the initial charge of 20 wt.% (examples 1-2) and 10 wt.% (example 3). The feed rate of the mixture in the reactor 0,297 ml/min So is the temperature value in the reactor is maintained at level 115° With±2°With due submission to the jacket of the reactor coolant. At the exit of the reactor are selected reaction mass, which is analyzed by GLC, calculating the degree of conversion of the oxide alkylene, the selectivity of the formation of monoglycol. After a significant drop of activity of the catalyst for the hydration process is stopped, and recording the total time of the hydration process, measure the volume of the anion and calculate the rate of swelling according to the method described in US 6160187. Process conditions and results of hydration are shown in table 1.

Example 4 (Regeneration of the catalyst of example 1)

Through the reactor with swollen catalyst of example 1 let aqueous solution of NaI (3 wt.%) and HCl (5 wt.%) with a speed of 0.3 ml/min for 2 hours at ambient temperature (21°). After that, the supply of stop solution, washing the catalyst with water, feeding into the reactor water for 3 hours at a rate of 0.5 ml/hour, and measure the volume of the catalyst. The amount of regenerated catalyst is equal to 1 ml, This means that the catalyst is fully regained its original volume.

To determine the activity and selectivity of the regenerated catalyst to carry out the hydration process using the regenerated catalyst under the conditions of example 1. The results of the analysis of the reaction mixture at the outlet of the reactor witnesses shall stout about the catalyst was fully restored to its original activity (conversion rate - 97%) and selectivity (97%).

Example 5 (Regeneration of the catalyst according to example 2)

Through the reactor with swollen catalyst of example 1 let aqueous KI solution (2 wt.%) and HI (1 wt.%) with a speed of 0.4 ml/min for a period of 1.6 hours at ambient temperature (19°). After that, the supply of stop solution, washing the catalyst with water, feeding into the reactor water for 5 hours with a speed of 0.4 ml/h, and measure the volume of the catalyst. The amount of regenerated catalyst is equal to 1 ml, This means that the catalyst is fully regained its original volume.

To determine the activity and selectivity of the regenerated catalyst to carry out the hydration process using the regenerated catalyst under the conditions of example 1. The results of the analysis of the reaction mixture at the outlet of the reactor indicate that the catalyst is fully restored to its original activity (conversion rate - 96%) and selectivity (98%).

Example 6 (Regeneration of the catalyst according to example 3)

Through the reactor with swollen catalyst of example 1 let aqueous solution of HI (1 wt.%) at a rate of 0.5 ml/min for 5 hours at ambient temperature (25°). After that, the supply of stop solution, washed catalysis is EO water, feeding into the reactor water for 7 hours with a speed of 0.3 ml/h, and measure the volume of the catalyst. The amount of regenerated catalyst is equal to 1 ml, This means that the catalyst is fully regained its original volume.

To determine the activity and selectivity of the regenerated catalyst to carry out the hydration process using the regenerated catalyst under the conditions of example 1. The results of the analysis of the reaction mixture at the outlet of the reactor indicate that the catalyst is fully restored to its original activity (conversion rate - 95%) and selectivity (99%).

Example 7 (Regeneration of the catalyst according to example 3)

Through the reactor with swollen catalyst according to example 3 let aqueous solution of Nal (0.1 wt.%), MgI2(0.1%) and HCl (0.3 wt.%) with a speed of 0.01 ml/min for 358 hours at a temperature of 10°C.

After that, the supply of the solution, stop and measure the volume of the catalyst. The amount of regenerated catalyst is equal to 1 ml, This means that the catalyst is fully regained its original volume.

To determine the activity and selectivity of the regenerated catalyst to carry out the hydration process using the regenerated catalyst under the conditions of example 3. To remove residual salts and acids from the regenerated catalyst prior to the beginning of the scrap hydration process, the catalyst is washed with water, feeding into the reactor water for 10 hours at a rate of 0.2 ml/hour.

The results of the analysis of the reaction mixture at the outlet of the reactor indicate that the catalyst is fully restored to its original activity (conversion rate - 96%) and selectivity (99%).

Example 8 (Regeneration of the catalyst according to example 2)

Through the reactor with swollen catalyst according to example 2 let aqueous solution of NaI (0.1 wt.%), ZnI2(0.1%) and N2SO4(0.3 wt.%) with a speed of 0.01 ml/min for 250 hours at a temperature of 45°C.

After that, the supply of the solution, stop and measure the volume of the catalyst. The amount of regenerated catalyst is equal to 1 ml, This means that the catalyst is fully regained its original volume.

To determine the activity and selectivity of the regenerated catalyst to carry out the hydration process using the regenerated catalyst under the conditions of example 2. To remove residual salts and acids from the regenerated catalyst before the beginning of the hydration process, the catalyst is washed with water, feeding into the reactor water for 7 hours with a speed of 0.6 ml/hour.

The results of the analysis of the reaction mixture at the outlet of the reactor indicate that the catalyst is fully restored to its original activity (conversion rate - 95%) and selectivity (99%).

Example 9 (Regeneration of the catalyst of example 1)

Through the reactor with swollen catalyst of example 1 let aqueous solution NiI2(0.01 wt%), ZnI2(0,01%) and H2SO4(0.03 wt.%) with a speed of 0.1 ml/min for 325 hours at a temperature of 20°C.

After that, the supply of the solution, stop and measure the volume of the catalyst. The amount of regenerated catalyst is equal to 1 ml, This means that the catalyst is fully regained its original volume.

To determine the activity and selectivity of the regenerated catalyst to carry out the hydration process using the regenerated catalyst under the conditions of example 1.

The results of the analysis of the reaction mixture at the outlet of the reactor indicate that the catalyst is fully restored to its original activity (conversion rate - 95%) and selectivity (99%).

Carrying out the regeneration process in this way allows you to completely restore the original volume, the activity and selectivity of action and, consequently, to increase the service life of expensive catalyst anion-exchange resin.

Conditions and results of hydration. The volume of the loaded catalyst 1 ml
No.Mark anion-exchangeOverall the present work, hourThe degree of conversion of the oxide %Selectivity to glycol, %The amount of catalyst, ml
After 1 hourIn the end,After 1 hourIn the end,In the end,
1AV-17-T198977997942,0
2Dowex SBR180968098932,1
3Amberjet 4400275958299981,8

The regeneration method of the basic anionite catalysts of the process of obtaining alkalophile hydration of oxides alkylene, wherein the spent catalyst is treated with an aqueous solution of inorganic salts of iodine and inorganic acids or aqueous solution itestosterone acid.



 

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