Method of separating methanol from mixtures with hydrocarbons4or5

 

(57) Abstract:

Usage: in chemical technology for the separation of methanol from mixtures with hydrocarbons, C4or C5formed in the processes of obtaining highly active additives to motor fuels. The inventive product is methanol. Methanol from mixtures with hydrocarbons4and C5allocate passing through the adsorbent filled sulfonium molded catalyst having a static exchange capacity of not more than 1.7 mEq H+/, Adsorption is carried out at 10-30oC. 1 C.p. f-crystals.

The invention relates to a method of separating methanol from mixtures with hydrocarbons4or5. Such mixtures are detected, for example, in producing high-octane additives to motor fuels-tert-butyl ether (MTBE) or tert-amyl ether (tame) by the interaction of methanol and hydrocarbon fractions containing tert-olefin WITH4or C5. B these processes using rectificatio commodity MTBE or tame selected kubovy product and unreacted hydrocarbons WITH4or5and methanol top.

There is a method of separating methanol from hydrocarbon WITH4or

The disadvantage of these methods is their high energy consumption because of the separation of methanol and extractant used rectificatio.

Also known methods of recovery of methanol from mixtures with hydrocarbons4or5using adsorption followed by desorption. As adsorbents used, for example, silica gel, molecular sieves, Malopolskie and crystalline, and ion-exchange resin (U.S. Pat. USA N 4605787, Pat. USA N 4814517, European Pat. N205562, Pat. GERMANY N 3124293). For regeneration after adsorption through the sorbent miss nesorbiruyushchegosya liquids or gases.

Most deep cleaning hydrocarbons from methanol (20 PPT) was achieved by using as the adsorbent a special zeolites. In this way as desorbent used fresh hydrocarbon fraction, which after saturation with methanol is directed to the synthesis of MTBE (Int. application N 8/03483).

Closest to the present invention is a method of separating methanol from mixtures with hydrocarbons4or5that includes passing the mixture through adsorb is desorbent carry out desorption of methanol fresh portion of the hydrocarbon mixture, containing tert-olefin (U.S. Pat. USSR N 1456006, 1986).

In this way the depth of cleaning is somewhat lower and is equal to 1000 ppm. However, carrying out the process at lower temperatures leads to lower energy consumption in comparison with the known methods, using as liquid extractants, and other solid sorbents.

In the method according to the patent N 1456006 as adsorbents using a strongly acidic stiroldivinilbenzol cations in the salt form, weak acid ion exchangers or anion exchangers. It should be noted that the use of fine-grained ion-always complicated by their relative osmotic instability (grinding) and ash from the contact zone, which affects their consumption. Given the significant rates listed on the ion exchangers, the cost sorbents comprise a significant share in the cost of phase separation of methanol.

The task of the invention is to cheapen the process of separating methanol from hydrocarbon fractions WITH4or5while achieving almost the same sorption characteristics and high selectivity.

We propose a method of separating methanol from hydrocarbon fractions WITH4or5that includes passing scost (SOY) not more than 1.7 mEq H+/, Adsorption is carried out at a temperature of 10-30oC.

After adsorption recovery of methanol is carried out, for example, passing through the sorbent hydrocarbon fraction WITH4or5that after saturation of methanol is directed to the synthesis of MTBE or tame.

Used in the proposed method, the catalyst may be obtained from its natural poisoning with preservation of porosity in the implementation of processes, for example, the synthesis of MTBE, hydration of isobutylene, etc.

The same catalyst can be obtained by subjecting the alkaline processing solution of the catalyst prior to unloading from the reactor or after loading in the adsorber-desorber. The catalyst, if necessary, dehydrated, for example, with methanol, then to delete the last used IsolatedStorage fraction.

It should be noted that sulfonate molded catalysts inherently differ significantly from ionoobmennika used by the patent of the USSR N 1456006. Proposed in the invention ionite molded catalysts in its composition are thermoplastic materials such as, for example, polypropylene (KU-FPP) or sulphonated, politi the battle deterioration of their sorption properties relative to methanol. In practice this is not observed. This phenomenon can be explained by the presence in sulfonitric catalysts a certain number of SO3H - groups instead of SO3Na, -COOH, -OH and nitrogen-containing groups in the ion-exchange materials for the patent of the USSR N 1456006. Perhaps the acid strength of the proposed sorbent in combination with high porosity reduces the effect of the presence of thermoplastics-fillers ionite molded catalysts. While the invention the presence of SO3H-groups is limited by the amount not higher than 1.7 mg-EQ H+/, With a higher value of SOY deteriorating the selectivity of the adsorption process due to the chemical reactions on the basis of components4-C5fraction and methanol. The result can worsen the quality of waste fractions, as well as the target product. Furthermore, the high-boiling impurities can clog the pores of the catalyst and reduce its sorption properties. When SOY is not more than 1.7 mEq H+/g sorption properties of ion exchangers molded catalysts are saved in a wider temperature range (10-30oC) that is of interest in the CIS and the countries where the annual temperature variations are significant.

The catalyst, more granule size (5-10 mm vs. 0.3-1.5 mm in U.S. Pat. N 1456006). All this improves the hydrodynamics of the process and eliminates the problem of entrainment of catalyst, providing a lower flow rate.

Thus, it is proposed a method of separating methanol from mixtures with hydrocarbons4or5cheaper compared to well-known due to the reduction of consumption of sorbent, as well as through the use of the spent catalyst. This improves the ecology of the whole process, because it is still a question of the disposal of an additional quantity of ion exchange material required for the separation of methanol on the prototype.

Compared with known processes solvent extraction with methanol, followed by a significant flow of steam, the inventive method allows to reduce the energy intensity of the process, leads to the practical exclusion of wastewater.

Example 1. The adsorption-desorption was performed by running the installation contactor, made in the form of a tube of stainless steel, which was filled with a sorbent in 400 ml. Temperature in the contactor was maintained at the expense of water from a thermostat, supplied in a shirt contactor.

As sorbent was used partially swollen in methanol ionite molded kata is tion-adsorption.

Desorption of methanol produced isobutane-isobutilene fraction with 30% of isobutylene, which was served in a number 680 ml/h at a temperature of 40oC and a pressure of 0.8 MPa. The content of methanol in the stream at the outlet of the contactor determined chromatography with thermal conductivity detector, the first was 3 wt. then it fell off and after 1 h was 0.3% after 1.5 h,1% Then the contactor reduced the temperature to 10oC and started the cycle when submitting 480 ml/h isobutane fraction with 2% methanol. After 2 h 30 min, the methanol content at the outlet of the contactor was 0.1% and after 3 h of 1.1 wt.

Then raised the temperature in the contactor 50oC and started the desorption cycle with supply the same isobutane-isobutilene fraction, as in the initial cycle of desorption, in the amount of 750 ml/h After 2 h when the methanol content at the output of desorber of 0.1% reduced the temperature in the contactor to the 25oC and switched the setting on the adsorption cycle. Feed isobutane fraction with 2% methanol in the amount of 440 ml/h at 25oC was carried out for 3.5 hours While after 3 h, the methanol content at the outlet of the contactor was 0.1 wt. after 3.5 h 1%

Such operations switching contactor cycle desorption at temperatures of 40 and Oranta has not changed.

Example 2. In the same contactor as in example 1, was loaded exhaust on stage tame and optionally treated with a solution of caustic soda, washed and dehydrated with methanol catalyst KIF with SOY of 1.7 mEq H+/,

Desorption was performed by the fraction of hydrocarbons WITH5containing 37% tert-Milanov in the amount of 800 ml/h at a temperature of 50oC and a pressure of 1 MPA. After 1 h the methanol content at the outlet of the contactor amounted to 0.1% after 1 h 30 min 1% When it detected the presence of tame in trace quantities. Then in the contactor reduced the temperature to 30oC and started the cycle of adsorption in the flow of 600 ml/h of hydrocarbon fractions WITH5from 1.8% methanol and 0.1% tame. The content of methanol and tame in the stream at the outlet of the contactor, respectively after 2 h 0,1% 0,1% and 2 h 30 min to 0.9% and 0.1%

Such operation switch contactor from the desorption cycle at 50oC per cycle adsorption at 30oC was carried out 20 times. This adsorption capacity was almost unchanged.

Example 3. In the same contactor as in example 1, was loaded partially swollen in methanol, used in the production of isobutylene, optionally processed by an ammonia solution to SOY 1.0 mg s of hydrocarbons4the following composition, isobutylene 40,35; butane 7,5; isobutane 4,4; p-butylene, 48,8, which was applied in the amount of 400 ml/h at a temperature of 50oC and a pressure of 0.8 MPa. After 2 h, the methanol content in the stream at the outlet of the contactor amounted to 0.1% after 3 h 1% Then the temperature in the contactor has dropped to 20oC and pressure up to 0.5 MPa, began the cycle of adsorption in the flow of butane-butylene fractions of 500 ml/h of the following composition, isobutylene 3,1; p-propane 11,8; isobutene-6,9; n-butylenes 76,3 and methanol and 1.9. After 2 h 30 min, the methanol content at the outlet of the contactor was 0.1% in 3 hours 1%

Such operation switch contactor from the desorption cycle at 50oC per cycle adsorption at 20oC was carried out 20 times. This adsorption capacity of the sorbent was almost unchanged.

Example 4. (For comparison). In the same contactor that in examples 1-3, were loaded exhaust at the stage of synthesis of MTBE catalyst KU - FPP with SOY to 1.8 mEq H+/g, partially swollen in methanol.

Desorption and adsorption of methanol were carried out in the same conditions and in the same sequence as in example 3.

After 2 h, the methanol content at the outlet of the contactor (desorber) was 0.1% MTBE 0.5% of the dimer is Ola at the outlet of the contactor amounted to 0.1% after 3 h -1%

Such operation switch contactor from the desorption cycle to cycle adsorption at 20oC was carried out 20 times.

This adsorption capacity decreased slightly. So, starting with 10 switch in the faction after adsorption of traces of dimer of isobutylene, and the flow after 20 switch-methanol content after 2.5 hours was 0.2% MTBE 0.1% dimer of isobutylene 0,1%

Example 5. In the same contactor as in example 1 was loaded with the catalyst KU-2 FRR, pre-treated with alkali solution to a value of SOY 0,5 mEq H+/g, washed and dehydrated in methanol.

Operations desorption and adsorption was carried out under the same conditions and using the same feed and the composition of the hydrocarbon fractions With that in example 3.

The content of methanol in the stream of the first cycle was:

The output of desorber after 1.5 h of 0.1%

Through 3,0 h 1%

At the outlet of the adsorber after 2.5 h of 0.1%

Through 3,0 h 1%

Such switching operation of the contactor from the desorption cycle at 50oC on a cycle of adsorption at 20oC was carried out 20 times. This adsorption capacity of the sorbent has not changed.

1. Method of separating methanol from mixture with uglev is m, characterized in that as ionite material used sulphidity molded catalyst having a static exchange capacity of not more than 1.7 mmol H+/g, and spend adsorption at 10 30oC.

2. The method according to p. 1, characterized in that as sulfonates molded catalyst with static exchange capacity of not more than 1.7 mmol H+/g use the spent catalyst in the production of isobutylene, methyl tert-butyl ether or methyl tert-amyl ether.

 

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2 cl, 1 tbl, 8 ex

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