HU196348B - Combined selective adsorbtive process and apparatus for producing hydrocarbons of 1-6 carbon atoms and volatile materials of high quality - Google Patents

Abstract

A mixture of carbohydrates obtd. from water and other contaminated solns. can be separated into pure fractions by passing it through a column of polar/nonpolar absorbent. The resin in the column is regenerated by this process and the eluted cpds. are of high purity.

Description

The organic chemical industry, the plastic industry, the rapid development of instruments and electronics industry, and in these fields of intensive research and development work requires simulant thou ^c purity is ever increasing, primarily szcntih'ti genes, oxygen and other gases, such as hydrocarbons thermal and catalytic conversion reactions and syntheses for adsorption-catalytic assays in modern physical analysis methods (such as gas chromatography, spectroscopy) for identification and calibration tasks.

Recently, high purity gases are also used in various technological processes. For example, methane in the manufacture of high-hardness metal tools, carbon dioxide in the creation of lasers, and carbon monoxide in the manufacture of cabonic compounds.

Pure materials can be prepared by chemical (synthesis) or physical methods by separation of gaseous and / or liquid mixtures obtained from natural or industrial processes by distillation, absorption, adsorption and membrane separation.

Of the industrial adsorption processes for the enrichment and separation of hydrocarbon-containing gas mixtures, the use of continuous-bed chromatography (hypersorption) has been limited in the past [Berg: Trans. Am. Inst. Chem. Engrs. 42, 665 (1946)). However, the fractions thus obtained are generally subject to further separation into individual components and in each case have to be purified individually to obtain pure products.

Separation of hydrocarbon mixtures is the subject of U.S. Patents 176,724, 159,936, 165,385, and U.S. Patents 3,310,486, 4,350,501, and 4,436,533. Each of the processes described in the above patents relates to the separation of liquid paraffinic hydrocarbon fractions having a molecular weight of 6 to 30, in the range of normal paraffin and non-normal paraffin hydrocarbons.

The processes referred to do not produce high purity individual hydrocarbons, but a mixture of normal paraffinic and non-normal paraffinic (branched, naphthane, aromatic) hydrocarbons in high volume, technical purity and quality.

Each process uses a molecular filter as adsorbent.

In each of the methods referred to, an eluting and / or displacing agent is used. This is separated from the product by fractionation and therefore fractionation order is an integral part of the processes.

Patents 159,936 and 165,385 are characterized by a special molecular adsorbent (containing protonphil metal compounds).

A batch selective adsorption process for the preparation of gaseous hydrocarbons of high purity is described in Hungarian Patent No. 152,779.

The process is carried out on a series of columns of at least three sequentially connected tubular columns which can be heated. Feeding of the starting material (hydrocarbon gas mixture) to the column temperature column at atmospheric temperature is continued at atmospheric pressure until the least adsorbed hydrocarbon is found at the end of the column column. After saturation, the first member of the column, first with gradual heating of the column and then with water vapor, desorbs the adsorbed carbon 2 hydrogens and passes them through the other non-heated adsorbent columns. After completion of the water vapor desorption, the first column is bypassed from the desorption operation and regenerated by passing inert gas. The same applies to the 2nd, 3rd, 4th etc. column dcsorption and regeneration.

An essential feature of the process is that the gas mixture containing only normal saturated or unsaturated hydrocarbons is separated on an activated carbon column and, besides the normal chemical ethyl alcohol, isoforms containing a column of molecular weight adsorbent or Al ₂ O ₃ switch.

SUMMARY OF THE INVENTION The present invention relates to single and branched, saturated and / or unsaturated hydrocarbons having carbon atoms of at least 99 mol% purity and / or carbon and oxygen and / or nitrogen and oxygen and / or hydrogen and halogen and / or hydrogen and It relates to the preparation of nitrogenous materials by a combined selective adsorption process and to the appropriate equipment necessary for this.

A feature of the process apparatus of the present invention is the high degree of fluidity in which several (at least 8) high purity products are produced in a given apparatus, at one and the same time, by implementing several process variants (process combinations) using only domestic raw materials.

Efficient and energy-efficient separation and purification of starting materials and recycled product fractions, high purity and minimal material separation, cooling and heating design, variable coupling of pre-purification and separation columns, application of different types of (polar, non-polar) pressure and temperature are appropriately co-ordinated over time, recirculation of intermediate product fractions, and integration of separation and regeneration processes into a single production cycle.

The apparatus for carrying out the process, the coupling of which is illustrated in Figure 1, optionally comprises evaporator (s), one, two or more pre-purification columns, one, two or more separation columns, a feed pump (s) and a product compressor. of compressor (s). The pre-cleaning and separating columns are of cooled and heated design, optionally tubular. The column for the pre-cleaning)! polar and optionally non-polar adsorbents, one part of the separation column M is filled with polar adsorbent and the other part is filled with non-polar adsorbent. Pre-purification columns) directly at the inlet end of the polar adsorbed M column (s) and / or non-polar adsorbent A columns) or at the inlet end of the column polar adsorbent and / or non-polar adsorbent A column (s). or) the outlet end of the column is connected directly to the product compressor or the outlet end of the M column (s) filled with a polar adsorbent is connected to the inlet end of the column A or column filled with a non-polar adsorbent,

The essence and several steps of the combined selective adsorption process carried out in the above apparatus:

196 348 - extracting water and sulfur-containing impurities from the starting materials in a polar and optionally non-polar adsorbent packed Sz, ET column (s);

- a separating column (s) or column series I-10 filled with regenerated polar adsorbent starting material and / or product fraction filled with regenerated polar adsorbent and / or barrel with a gradually increasing pressure (e.g. in the production of isobutane, saturation of the propane) at the outlet end of the ambient temperature or cooled separation column or column first or second column or at the pressure specified in the previous column or after loading a specified amount of material, illustrated by depressurization (by expanding the loaded material into the product line or optionally in the second or second and third columns) and then the first and optionally the second or second and third columns. gradually separating and purifying the column temperature to 100-250 ° C and suctioning the columns;

- the substance in the M-column (s) filled with the polar adsorbent for high purity product (s) and / or product fractions with different chemical structure and / or different saturation and / or different polarity;

And separating the material contained in the non-polar adsorbent A column (s) into high purity product (s) and / or product fractions of different molecular weight and / or different volatility and / or different adsorption capacity;

Returning the product fractions directly or via intermediate storage to the separation column (s) M and / or A;

- regenerating the hot adsorbent fill by cooling and / or vacuum and cooling and / or inert gas rinsing followed by vacuum and cooling, in accordance with the separation operations, as a direct continuation thereof, and then repeating the separation and regeneration operations as necessary.

During the separation described and also shown in Figure 2, the desorption, flow and adsorption of the different adsorbent components of the mixture (the filled material) due to the pressure reduction and the subsequent temperature increase and suction results in zones, and two-component mixed zones connecting these zones, migrate towards the exit end of the column). The quantitative distribution of the components of the feed mixture between the pure and mixed zones, the relative amounts of the components, their adsorption capacity, and the size of the column series and the value of the operating parameters set.

Based on frequent patterning and analysis of the column vapor (vapor), the mixed fractions containing the two components are transferred to intermediate collectors, and the pure products are transferred to appropriately prepared (cleaned, evacuated) bottles (containers). The product is pressurized with methane, ethylene and other non-condensable gas products (eg carbon monoxide) to a high pressure diaphragm compressor in a gas state of ^{5 to} 100 bar to 250 bar, and the condensate and other high pressure condensate products (CO ₂ , N ₂ O, NH ₃ ). It is liquefied by compressing and cooling to a pressure of 15 to 75 bar, and liquefying the pr opane and heavier products by compressing and cooling to a pressure of 3 to 15 bar and bottling in this state. Pentane and higher molar mass hydrocarbons are liquefied by cooling and stored as a liquid.

The polar adsorbent used in the process is molecular sieve, silica gel, alumina, carbosilve, preferably type A molecular sieve, and non-polar adsorbent sulfur active carbons, preferably at least 1000 nV / g of microporous activated carbon.

In our process, depending on the starting raw material (its impurity components), some products are produced in a single production cycle, in one filler. For example, methane and ethane are produced in a column of optionally two activated carbon and columns of carbon monoxide, carbon dioxide, and nitrous oxide are prepared in a column of 5A, optionally connected in series.

Propane, iso- and normal butane, starting from the propane-butane (PB) fraction, are prepared in 5A molecular weight packed M and activated carbon packed A columns by first separating propane and normal butane from the isobutane in the M column and light and the resulting isobutane is purified in column A (s) from the light contaminants, and the propane and normal butane are fractionally desorbed from column M. If only a small amount of isobutane is available as a starting material in propane and normal butane, high purity isobutane can be produced in a 5A molecular weight column (M) in a single production cycle.

Thus, depending on the quality of the raw material, the device of the invention may employ several variations (combinations) of the process of the present invention, which may produce several (at least 8) products of desired purity (99-99.99 mol% or greater).

In the prior art part of the present invention, this is an improved version of this prior art patent No. 152,779.

It is common for the two processes to use each of the batch adsorption methods, multiple adsorption columns, polar and non-polar adsorbents.

There are the following significant differences between the 152,779 procedure and the currently refined process:

- Process 152 779 for the production of hydrocarbons only, whereas the process developed is a hydrocarbon and / or gaseous carbon and oxygen and / or nitrogen and oxygen and / or hydrogen and halogen and / or hydrogen and nitrogen-containing materials suitable for producing.

Process 152 779 requires at least a three-mesh tubular adsorbent column, the process now being developed can be carried out in most or one of two or at most three adsorbent columns.

196 348 - The columns used in process 152 779 are of a heatable design, the columns of the process of the present invention are of a coolable and heatable design, preferably of tubular construction. The heating and / or cooling of the adsorbent columns is optionally carried out with hot and / or cold heat transfer oils circulating in the adsorber jacket space. The heated and cooled structural design of the adsorbers allows for a 30-60% higher specific adsorption capacity, greater selectivity and significantly (twice, three times) faster cycle (cycle change), resulting in a significant reduction in specific production costs. [The production capacity per unit of time has increased significantly (approximately threefold) and the operating cost has been reduced accordingly.] - Drying and pre-purification column (s) for the water purification and desulphurisation of starting materials and removal of other (mainly polar) impurities. t. In process 152,779, they were not used, so the impurity components were loaded on the separation columns. As a result, after each separation operation, the columns had to undergo an in-depth regeneration (including steam). In the process we are currently developing, we do not use steaming, and for deeper regeneration (consisting of hot vacuuming)

5-8 cycles are required.

- The starting material is added to the chilled separation column (s) at ambient temperature or pre-cooled in the present process.

Addition of starting material to the separation columns in the process of the present invention is carried out at a pressure of 1 to 10 bar, with increasing pressure, until a characteristic component appears at the outlet end of the first or second separation column or until a certain amount of material is reached.

In process 152,779, the addition is carried out at atmospheric pressure at ambient temperature until the least adsorbed hydrocarbon is present at the end of the column of at least 3 columns.

- The separation (dcsorption) of the components in the columns according to Method 152 779 is the first, second, third, fourth, etc. step. is performed by sequential heating of the columns and successive displacement of water vapor.

According to the method now developed, the separation is effected by reducing the pressure (expanding the loaded material into the product line and possibly columns 2 and 3) and then gradually increasing the temperature of the first column and, if appropriate, columns 2 and 3 to 100-250. By raising it to 'C and suctioning the column (s), no displacement material is used.

Method 152 779 requires the water vapor to be removed from the adsorbent when regenerating the columns, and water vapor is not used in the present process, making regeneration much simpler and less expensive.

The foregoing clearly demonstrates that the presently developed process and apparatus, as compared to the process described in U.S. Patent No. 152,779, represents significant progress in the design of the apparatus, the circuit arrangement, and the major operational steps of the process.

Together, these have resulted in the implementation of an apparatus and process for the efficient, rapid and economical production of a plurality of (at least 8) high purity (optionally more than 99.99 mol%) products, which are in any case intended for technical progress. The importance of the developed process and equipment makes it possible to produce high value imported materials from domestic raw materials.

Further details of the process for the preparation of high purity propane, iso- and n-butane products from propane-butane feedstock and pre-enriched fractions, for the production of high purity tnetane product from natural gas, for the production of high purity ethylene from ethylene rich fractions, in the Examples for the preparation of high purity nitric oxide from commercial liquid dinox and for the preparation of high purity ammonia from commercial liquid ammonia.

Apparatus shown in Figure 1, which were carried out to manufacture the above materials W and a charcoal ET spent pre-treatment column, a sieve, pouring a type 5A molecular sieve M separating columns and three I200 m ^z / g of surface area micropore supersorbon type charcoal WS IV consists of a filled column A1-A3. Columns M and A1 contain 90 liters, columns A 2 and A3 contain 53 liters of adsorbent.

Example 1

The propane butane used as a raw material for the production of high purity propane, iso and n-butane products contained 3 wt% ethane and lighter components, 35 wt% propane, 42 wt% isobutane and 20 wt% n-butane. The above composition was added at 5-10 m / min incrementally to 3 bar under increasing pressure at 25 ° C with an M5 filled with A5 molecular weight adsorbent. A mixture of mostly isobutane and a small amount of ethane and lighter components that were not adsorbed on the molar culture filter was passed directly from the M column to the A-A3 adsorbent filled with activated carbon at 25 ° C. Raw material was added to column M until propane appeared in the gas mixture leaving the column. This was observed from frequent analysis of gas samples taken through taps 9, 13 and 17:

When propane emerged, the feed from the M column was shut off, the inlet end of the activated carbon plant was sealed, and the isobutane was rinsed from the gas space of the M column by expansion through pins 9, 13 and 15. In the above operation, which is used to separate isobutane from propane and n-butane, 8.51 kg of raw material is used.

The production of high purity isobutane was continued in an apparatus consisting of activated carbon filled Al-A3 adsorbers. The flow of the mixture in the column row, as shown in Figure 2, is first gradual pressure

This was achieved by reducing 196 348 (expanding the mixtures from A1 to A2 and A3), then gradually lowering the temperature of the lower column of A1 to subsequent column sections to 220 ° C. During the flow, repeated selective adsorption of g components occurred, resulting in the separation of ethane and lighter components from isobutane. From the activated carbon plant, a mixed fraction of ethane and lighter components was first flushed out, followed by a small fraction of ethaneisobutane ·, θ and a high purity isobutane product. During separation, the resulting 3.1 kg of high purity isobutane product was compressed with a diaphragm compressor to a pressure of 4.5 bar, liquefied in a water-cooled condenser and filled into a vacuum metal bottle.

At the same time as the above separation in the activated carbon apparatus, propane and n-butane were desorbed from the M column filled with a molar filter. This was accomplished by gradually lowering the pressure and gradually increasing the temperature of the lower, middle and upper column sections to 220 ° C, respectively. These operations first afforded a high purity propane product, a mixed fraction containing propane-n-butane, and finally a high purity n-butane product. The high purity products were collected in bottles after compression and liquefaction, and the mixed fraction was collected for reprocessing in an intermediate container.

The combined production cycles in the molecular sieve and activated carbon apparatus 30 described above gave the products and fractions shown in Table 1.

Larger amounts of high purity product can be produced in a single production cycle by starting from so-called pre-enriched fractions. The natural gas industry produces many such fractions. Such is the isobutane-rich fraction of about 1 wt% ethane, methane and lighter impurities, 2-6 wt% propane,

It contains 90-93% by weight of isobutane and 3-6% by weight of n-butane 40.

High purity isobutane products are prepared from the above isobutane-rich fraction by the combined process described above, except that about 10 kg of this fraction is processed in a single cycle and 6-8 kg of high purity isobutane product are obtained depending on the isobutane content of the fraction. In this case, the propane and n-butane depleted from the M column filled with molecular sieve, with a small amount of rnia, should not be recovered as a pure product, but collected as a mixed fraction and processed in larger portions (about 10 kg) products.

Example 2

High purity methane was produced from methane-rich natural gas containing 1.3 wt% air and other impurities (water vapor, CO ₂ , H ₂ S), 92.5 wt% methane, 5.7 wt% ethane and 0.5 wt% propane . Methyl rich natural gas was added gradually to 7 bars at increasing pressure, ambient temperature, 5 to 6 m / min through a flowmeter FI, a dryer Sz and an ET pre-purification column into a suitably prepared (regenerated) column filled with activated carbon columns A1-A3. The natural gas supply was continued until methane appeared in the gas leaving the A2 column. (This was determined by analyzing gas samples taken at taps 11, 12 and 16.) At this point, the gas supply was shut off, the inlet end of the Al column closed, and the mixture flow in the column row, as shown in Figure 2, first by gradually decreasing pressure and then by gradually increasing the temperature of subsequent column sections. In these operations, due to repeated selective desorption, flow, and selective adsorption of the components, a mixed fraction containing air and methane followed by a highly purified methane product followed by a mixed fraction containing methane and ethane (propane). The methane product, 99.98% pure, was compressed and cooled to 120 bar by a two-stage diaphragm compressor and the mixed fractions were collected for recycling in an intermediate container.

In the above manufacturing step, the products listed in Table 2 were obtained.

Table 1

Products and fractions obtained in Example 1

components feed raw material propane product isobutane product r-butane 'medal Mixed fractions from activated carbon M-adsorber 1% kg . ·% kg t% kg t% kg kg 1% kg Elan and easier 3.0 0.260 0.01 0.0002 45.61 0.260 propane 35.0 2.980 99.97 2.2294 0.01 0.0003 0.05 0.0005 54.35 0,750 Isobutyl 42.0 3.570 99.97 3.0990 54.39 0.310 n-butane 20.0 1,700 0.02 0.0004 0.02 0.0007 99.75 1.0695 45.65 0,630 100.0 8.510 100.00 2.2300 100.00 3.1000 100.00 1.0700 100.00 0.570 100.00 1,380

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Table 2

Products and fractions obtained in Example 2

components feed raw material Mctán- terriiék "Light" "Hard" mixed t% fraction kg mixed t% fraction kg t% kg t% kg Air + Other 1.3 0.032 0.01 0.0002 12.70 0.032 Methane 92.5 2,276 99.98 1.7070 87.30 0,220 69.74 0.349 Ethane 5.7 0140 0.01 0.0002 27.86 .1396 propane 0.5 0,012 2.40 0,012 ΠΚΙ, Ο 2.460 100.00 1.7074 100.00 0.252 100.00 .5006

Example 3

High purity ethylene was prepared by purification of an ethylene fraction from an olefin factory. Ethylene contamination contained methane and lighter components, as well as ethane.

To produce a high purity ethylene product, 6.5 kg of ethylene was added to the M adsorbent filled with molecular sieve adsorbent at a rate of 5-6 m / min, with increasing pressure of 6-7 bar. By removing the feed, the flow in the column was maintained by gradually decreasing the pressure (expanding the gas mixture) and then gradually heating the lower, then the middle and upper sections of the column. First, the lighter impurity components were removed from the column, followed by a mixed fraction containing ethane and ethylene. The loading of the ethylene as a product (bottling) was started when the ethane content in the gas exiting the column dropped below 0.08% by weight. The pelleting was carried out with a two-stage diaphragm compressor at a pressure of 120 bar. The high purity ethylene was collected until the ethylene was aspirated from the adsorbent heated to about 250 ° C. The M column was then purged (eluted) with nitrogen, vacuum and cooled.

In the above production cycle, 5.8 kg of 99.98 wt% ethylene product were obtained. The product contained 0.02% by weight of ethane as impurity.

needles to maintain a carbon dioxide flow rate of 5-6 m / min in the column row. After the pressure in the column row had dropped to nearly 1 bar, the temperature of the lower column first, and then of the subsequent column sections, was gradually raised to 220 ° C. During the separation, a mixed fraction containing air, methane, ethane and carbon dioxide was briefly discharged, followed by 8.75 kg of carbon dioxide of 99.99 mol% purity. High purity carbon dioxide is compressed and cooled for approx. It was liquefied at 60 bar and stored in high pressure steel bottles.

After harvesting the product, the M column was cooled and a new production cycle started. After 6-8 cycles, the M column packing was regenerated hot (200-240 ° C) by vacuum and cooling.

Example 4

High purity carbon dioxide was produced by purifying bottled liquid carbon dioxide. The liquid carbon dioxide contained water, 0.4-0.7 mol% of methane, 0.4%, 4 mol% of air and 0.1-0.3 mol% of heavier hydrocarbon contamination. Activated carbon was added to the ET pretreatment column to remove hydrocarbon contamination. Purification was performed in column M filled with molecular sieve 5A.

11.5 kg of crude carbon dioxide from a steel bottle were added to the ambient temperature column M through a flow meter FI, a dryer Sz and a pre-cleaner ET, and taps 3 and 4, gradually increasing to 3 bars. After completion of the dosing, the tap 4 is closed and the pressure in the column is gradually lowered through the tap 9 with the needle valve 13.

E0

E5 eo

Example 5

High purity nitric oxide was prepared from commercial liquid Dinox, which contained 98-99 'mol% N ₂ O, 0.4-0.8 mol% NO ₂ and CO ₂ , 0.20.6 mol% air and it contained little water. Purification was carried out in a 5 column molecular weight M column.

10.2 kg of crude dinox from a steel bottle was added to the chilled M column through gradually increasing pressure (up to about 5 bar) through the FI flowmeter, the Sz dryer and the ET pre-cleaner, and through taps 3 and 4. After the addition was completed, tap 4 was sealed and the pressure in the column was gradually reduced through tap 9 with tap valve 13 (the material was expanded from the adsorber to the product line). After the pressure in the column had dropped to 1 bar, the M column was gradually heated to 150-160 ° C (batchwise). The gas exhausted by the compressor contained a large amount of air and methane for a short period of time. After removal of 3 kg of a mixed fraction consisting mainly of N ₂ O, 6.5 kg of 99.98 mol% pure nitric oxide were obtained. The mixed fraction and product were charged in bottles at ambient temperature in a fluid pressure of 50-70 bar.

After harvesting the product, the M column was cooled and a new production cycle started. After 4-5 cycles, the M column packing was regenerated by hot vacuuming and subsequent cooling.

-611

196 348

Example 6

High purity ammonia was prepared from commercial liquid ammonia which contained impurities of 0.1, 15 mole% hydrogen, 0.4-0.6 mole% nitrogen, 0, ΙΟ, 3 mole% oxygen, carbon dioxide and little water. Purification was carried out in a column filled with molecular sieve 5A.

9.4 kg of crude ammonia was added to the chilled M column through gradually increasing pressure (up to about 6 bars) through the flowmeter FI, the Sz dryer and the ET pre-cleaner, and through taps 3 and 4. After the addition was completed, tap 4 was sealed and gas was expanded from column M through tap 9 and through the needle valve 13 to the product line to the compressor. After the pressure in the column had dropped to 1 bar, the M column was gradually heated to 160-180 ° C (batchwise). The first batch (about 300 liters) of gas exhausted with the compressor contained many (more mol%) light impurity components (H ₂ , N ₂ , O ₂ , CO), followed by approx. 2.5 kg so called liquid mixed fraction, then ca. 6.8 kg of liquid ammonia greater than 99.97% mof% were collected in the collection bottle. This mixed fraction and the pure product were liquefied after the compressor at 35-40 ° C and 13-16 bar.

After harvesting, the M column was cooled and a new production cycle started. After 6-8 production cycles, the M-column packing was regenerated by hot vacuuming and subsequent cooling.

Claims (5)

Claims A combined selective adsorption process, at least Single C 1 -C 6 straight and branched chain saturated and / or unsaturated hydrocarbons, hydrocarbon derivatives and / or gaseous-vapor-containing hydrocarbons and / or nitrogen and oxygen and / or hydrogen and halogen, 99% pure and / or for the production of hydrogen and nitrogen containing materials in an adsorption apparatus consisting of polar and non-polar adsorbent columns, characterized in that: subtracting in column (s) (SZ, ET); - the separation column (s) (M, A) or column series filled with the regenerated polar and / or non-polar adsorbent with the pre-purified ambient temperature or pre-cooled starting material and / or product fraction up to a pressure of 1 to 10 bar at ambient temperature or saturated chilled separation column or column at the outlet end of the first or second column or until the pressure specified in the first column is reached or a specified amount of material is loaded, followed by loading the material into the product line or optionally second or second and third and then expanding the first and optionally to the second column, or the second and the third column, the temperature gradually increased to ^this 100 250 ° C and carried out suction of the column (s) of separation process steps - of substance (s) in polar adsorbent filled column (s) with high purity product (s) and / or product fractions of different chemical structure and / or different saturation and / or polarity, g - non-polar adsorbent filled column (s) (A) separating the present material into high purity product (s) and / or product fractions of different molecular weight and / or different volatility and / or different adsorption capacity; 10 - tern ^- ékfrakciókat directly or via intermediate holding the polar adsorbent filled in a column (M) and / or recycled to the spent nonpolar adsorbent column (s) with (A); - in coordination with wind selection operations 15 and directly therewith, the hot adsorbent charge is regenerated by cooling and / or vacuum and cooling and / or inert gas rinsing followed by vacuum and cooling, followed by 20 - the separation and regeneration operations are repeated as necessary. Process according to Claim 1, characterized in that the starting materials and / or product fractions of different chemical structure and / or different saturation and / or polarity are filled with a polar adsorbent, preferably a 5Λ type molar filter, of the same structure and / or and column (s) filled with non-polar adsorbent, preferably microporous activated carbon, to separate starting materials and / or product fractions of saturated and / or polar but different molecular weight and / or volatility. Method according to claim 1 or 2, characterized in that the heating and / or cooling of the adsorbent column is optionally carried out with hot and / or cold heat transfer oil circulated in the adsorber jacket space. 4θ 4. Equipment according to Figures 1-3. A process according to any one of claims 1 to 4, optionally comprising a vaporizer (s), one, two or more pre-purification and one, two or more separation columns, a feed metering pump (s) and a product-compressing compressor (s). the separation columns (SZ, ET) are of heated and cooled design, optionally tubular, the pre-cleaning columns (Sz, ET) with polar and optionally non-polar adsorbent, the separation columns (M) are Part 5θ is filled with a polar adsorbent, preferably a type 5A molecular sieve, and the other part of the separation columns (A) is filled with a non-polar adsorbent, preferably microporous activated carbon, and the pre-purification column (s) (SZ, ET) are directly filled with polar adsorbent 55 ) (M) and / or inlet end of column (s) filled with non-polar adsorbent (A) or column (s) filled with polar adsorbent (M) and / or columns filled with non-polar adsorbent (A) or and the outlet end of the column is directly connected to the thermocompressor compressor (s), or the outlet end (M) of the polar adsorbent-filled column (s) is at the inlet end of the non-polar adsorbent-filled column (s) on.