Method of alkene(s) and higher-boiling reagent reaction

FIELD: chemistry.

SUBSTANCE: invention refers to method of reaction of alkene(s) contained in hydrocarbon stream, and in a reaction-rectifying system provided with rectifying sections and in between reaction zones with subnatant catalyst. The fluid is poured from the top of each overlying zone to the bottom of underlying zone. It is followed with partial disperse passing of vapour flow from underlying zone through each reaction zone. Thus residual vapour flow from each underlying zone is backflow to the top of overlying reaction zone through overflow space to poured fluid. As a rule, higher-boiling reagent is nontertiary alcohol, carboxylic acid or benzene, while essential reaction product is ether, ester or alkylbenzene.

EFFECT: improved method.

7 cl, 3 dwg, 6 ex

 

The invention relates to the field of chemical interaction of alkenes or more high-boiling substances in the presence of selfactivity catalysts.

Known methods /Shuvalov and other Chemical industry, 1995, no 5-6, p.9-15/ chemical interaction of alkenes, served in the composition of the hydrocarbon mixture, and more high-boiling substances, in particular alcohol in a reactive distillation system comprising a distillation zone and located between a reaction zone with selfactivity catalyst, in which a counter-current movement of the liquid and steam flow. The disadvantage is the need for very large cross-section of this reaction zone and the difficulty of uniform distribution of liquid flow in its cross-section, in particular in the production of high power.

There is a method /Pat. EN-2063956, 20.07.96/ chemical interaction alkene(s) and more high-boiling substances (alcohol) in the apparatus of the reactive distillation type, having between distillation zones several reaction zones, the catalyst is partially or completely submerged in the liquid, provided with a distribution device for a pair at the bottom and overflow devices, in which the liquid from each of the upper reaction zone enters the lower part of the underlying reaction the th zone.

The disadvantage of this method is the high steam load of the reaction zones and the need for their large cross-section substantially greater than the cross section of the reaction zones.

Also known way /Pat. EN-2064919, 10.08.96/ chemical interaction alkene(s) and more high-boiling substances (alcohol) in the apparatus with separate zones rectification and multiple reaction zones, each of which is a layer sulfonate catalyst is immersed in a liquid, through which pass part (5-70%) steam flow coming from the lower zone, and the remaining part is passed into the upper part of the upstream zone on a separate hollow vertical channels.

The disadvantage of this method is the absence of mass-transfer contact between vapor and liquid in said hollow vertical ducts or passages and the need for installation of mass transfer plates between the reaction zones for transferring a part of alkene(s) from steam flow in flow down the fluid flow. In this space the reaction zone cluttered peritonei and pair-passing channels, or there is a necessity of the location of these pair-passing channels outside of the device.

We have found the way, does not have these disadvantages.

We say:

The way of interaction of the alkene(s)that contain(s)to ug is vodorodno thread and more high-boiling reagent in the presence of sulfonate catalyst in a reactive distillation system having a distillation zone and located between the reaction zone is immersed in the liquid catalyst, the overflow liquid from the upper part of each overlying zone in the lower part of the underlying zone and dispersed by passing steam flow from the lower zone through each reaction zone, wherein the remaining portion of the steam flow from each of the underlying zone is passed into the upper part of the upper reaction zone through the overflow space countercurrent to pour the liquid.

As complementary to the above we also declare methods, characterized in that:

- steam stream is passed through the specified overflow space is dispersed, preferably uniformly over the cross section of the filling space;

- alkene(s)containing hydrocarbon stream serves as a minimum below the bottom of the reaction zone, and the more high-boiling reagent serves at least in the upper reaction zone or above her distillation zone;

- alkene(s)containing hydrocarbon stream is distributed among multiple threads and some of them served in the intermediate reaction zone and/or between them;

stream more vysokoyebased the reagent is distributed on multiple threads and some of them served in the intermediate reaction zone and/or between them;

is specified more high-boiling reagent is a non-tertiary alcohol or carboxylic acid or benzene and the main product of the reaction is an ether or ester or alkyl benzene;

- the interaction of alkene(s) with more high-boiling reagent are also formed di - and/or trimers of alkenes, and the resulting material is removed from exhaustive distillation zone.

In the proposed method combines a General countercurrent flow of liquid and vapor in the system as a whole with their straight-through or flow-cross movement in each reaction zone. This achieves high conversion of the reacting substances with a relatively small cross-section of the reaction zones, the lack of local overheating in the reaction zones and the removal of high molecular weight impurities from the catalyst with the liquid stream.

The combination of countercurrent flow of liquid and transmission part of the steam flow in a single peritoneum space simplifies the design and provides the necessary mass transfer between the liquid stream and more rich in content alkene(s) steam flow.

The number of the reaction zones may be different depending on the requirements to the completeness of conversion and other circumstances. Preferably, the number of reaction zones 3 to 10.

We do not exclude the possibility of additional accommodation, massao the Menno devices between the reaction zones, however, their number is reduced, or they are not installed at all.

Unreacted(e) hydrocarbon(s) (possibly with an admixture of more high-boiling reagent) at least for the most part derive from the top to the strengthening of the distillation zone. Products of chemical interaction derive mainly from the bottom comprehensive distillation zone.

Placing the above reaction and distillation zones in one column apparatus is optional. It may be located in different devices, United countercurrent liquid and vapor flows in accordance with paragraph 1 of the claims.

Not excluded the possibility of combining the proposed reactive distillation system with the previous flow of the reaction zone in which is a partial chemical interaction of the reactants.

If necessary, warded off the hydrocarbon mixture and/or a mixture of the reaction product is subjected to separation using known methods (distillation, water extraction, heterotetrameric drying and the like).

The application of the invention illustrated in figures 1 to 3 and examples. Specified in figure 1-3 and in the examples do not preclude the application of other techniques, while respecting the characteristics specified in claim 1 of the claims.

Figure 1 and 2 legends essence: RT - rectifying plate, PN - RAS is realitalia device for steam flow, IN carrying steam vents, W - liquid flows, V - steam flows. Shaded (crossed out), the catalyst layers.

Liquid flow Well with each overlying zone enters the lower part of the underlying reaction zone or, respectively, in mass transfer (distillation) zone.

Steam flow V on the top of each zone below the reaction zone, partially passes through the switchgear RU in the upstream reaction zone and partially through the access holes (figure 1) enters the overflow space, barbthroat through transfused fluid and enters the upper part of the upper reaction zone.

Option, shown in figure 2 differs from figure 1 that the steam flow directed from the top of the reaction zone in the overflow space is dispersed in this space with switchgears, which contributes to a better mass transfer between rising vapor and flowing the liquid.

Figure 3 shows the scheme of the reactive distillation system as a whole. Denote the essence: RZ - reaction zone with a catalyst, protective relays and irz - firming and comprehensive distillation zone, BP is a more high-boiling reagent, KP - CC stream (product).

Source(s) hydrocarbon(s) is(are) on line 1 (hereinafter perhaps along the lines 1A, 1B, 1C, 1G, 1D), BP - line 2 (next POS of the but along the lines 2A, 2B, 2C). Product(s) of reaction(s) and the unreacted part of the BP output line 3, unreacted(e) hydrocarbon (s) in line 4 (line 4A). Perhaps part of the product(s) and BP output line 5.

Five reaction zones selected conditionally. Their number can be from 2 to 50, more realistically, from 3 to 10. The reaction and the two distillation zones do not necessarily have to be located in the same column. Possibly their location in two or more devices connected in liquid and gas streams and form a single reactive distillation system compliance with the characteristics indicated in claim 1 of the claims. Top (firming) distillation zone are not required to have a reflux condenser. Possible supply of high-boiling reagent in its upper part for the dissolution of part of the steam flow and create internal phlegmy for rectification.

In the examples, the concentrations are given in % of mass.

Legend: MTBE - methyl tert-butyl ether, ETBE - ethyl tert - butyl ether, BWA - sec-butyl acetate, cumene - cumene, MC - acetic acid, beef - butane-sabotinova fraction, BBF - butane-n-butenova fraction, propane - propene-propane fraction, RA - reaction(s) area(s), protective relays-firming distillation zone, irz - comprehensive distillation zone, D is the distillate, KP - CBM product, R - reflux h the words, SOY - static exchange capacity of the catalyst in mEq/g·cat, V1/V and V2/V - respectively the share of steam flow V from the top of the reaction zone, noise (V1through the upstream reaction zone and directed (V2through overflow space.

An example of the prototype EN-2064919.

Get MTBE from beef and methanol. In the middle part of the reactive distillation column has 3 reaction zone with a catalyst between them have three rectifying plates. Used sulphidity molded catalyst'KEEFE (SOY=3,6).

In the prototype is not specified dimensions of cross-sections (or diameters) of the reaction zones. Further comparison is carried out using loads of reaction zones in steam flow flowing through the catalyst.

Serves 10,9 t/h beef (45% isobutene) and is 2.74 t/h of methanol, which corresponds to a conversion of isobutene ~ 99% and a selectivity of ~ 99% obtaining 7.4 tonnes/h of MTBE (99,1% of the basic substance). The output of distillate (isobutane from 3.2% methanol and 0.75% of isobutene) is 6.3 t/h, R=3.

In protective relays steam load is 25.2 t/H. the Proportion of steam flow V1/V in the upper, middle and lower RH respectively of 0.05, and 0.4 and 0.7. Steam load in WA is from 1.3 (top RH) to 8.4 t/h MTBE Production per unit volume of catalyst is 0.92 kg/l cat·h

Other examples of the sludge is astronout the invention.

Example 1.

According to figures 1 and 3 hold receiving MTBE from beef (45% isobutene) and methanol (TKip=64°C). In the middle part is used 5 reaction zones (~ 1 m thick layer of catalyst in each). Used catalyst KIF-T (cylinders with a diameter of 6 mm and a length of 6-8 mm, SOY=3,6). The temperature in the reaction zones 60-70°C, R=2,3. Serves 11,0 t/h beef and 2.7 t/h of methanol.

Steam load in protective relays - 20.5 t/h V1/V in the reaction zone (from top to bottom) 0,08-0,15.

Steam load in WA with catalyst respectively 1.6 (top RH) up to 2.0 t/h (lower RH). When these loads with regard to 25-30%of porosity (fraction of free cross section) of catalyst required diameter of the reaction zone does not exceed the diameter of the distillation zones, which allows you to place the reaction and distillation zone in a single column with unchanging height diameter.

Output: 7,6 t/h KP (99.4% of MTBE, 0.3% methanol and 0.3% of dimers of isobutene) and 6.2 t/HR of isobutane distillate containing 0.4% isobutene and 2.8% methanol.

Compared with the prototype achieves a higher purity MTBE and the degree of extraction of isobutene requires 1.3 times smaller R and four times smaller section (based on load at the bottom RH).

Example 2.

Get ETBE from beef (45% isobutene) and ethanol (TKip=to 78.3°C). The processing performed according to figure 2 and 3. The catalyst'KEEFE, similar with the 1 ERU. In the system 4 the reaction zone with the height of the catalyst 1.1 m each. The temperature in the reaction zones 55-65°C, R=2,0.

Serves 11,0 t/h beef and 4.3 t/h of ethanol.

Steam load in protective relays is 18 t/h V1/V in the reaction zones, increasing from the upper to the lower RH, 0.15 to 0.3. Steam load in the reaction zones from 2.7 t/h in the upper zone to 3.3 t/h in the lower zone.

When the porosity of the catalyst 25-30% of the required diameter of the reaction zone does not exceed the required diameter of the distillation zones.

Output of 9.3 t/h KP (97,6% ETBE, 2.2% ethanol and 0.2% of dimers of isobutene) and 6 t/HR of isobutane distillate (0.3% isobutene, 0.1% ethanol).

Example 3.

Get the BWA from acetic acid (CA) and BBF (50% n-butenes) according to figure 2 and 3.

Use coarse sulphidity catalyst with a spherical granules with a diameter of 4-5 mm and SOY=2,7. In the system 4 the reaction zone. The temperature in them 90-100°C, R=1,7.

Serves 100 kg/h of BBF and 65 kg/h of the criminal code. Steam load in protective relays 137,7 kg/H. the Relationship V1/V in the reaction zones is practically identical and are 0,25. Steam load in WA is to 34.4 kg/h in the upper RH to 30.0 in the lower RH.

When the porosity of the catalyst 25% of the required diameter of the reaction and distillation zones are practically identical.

Take 51,0 kg/h butane of distillate (2% n-butenes) and 114 kg/h KP (85.7% of BWA, 14.0% for CC and 0.3% of dimers of n-butene is). After distillation of the criminal code are 98 kg/h flow with 99.7% of the BWA and 0.3% of dimers of n-butenes.

For comparison, in a similar process with counter-current vapor-liquid reaction zone cross-section of the reaction zone and the catalyst loading in the 3.0-3.5 times more than the proposed method.

Example 4.

Get cumene from benzene and propane (75% of propene) according to figure 1 and 3.

Use 5 reaction zones with coarse selfactivity catalyst, similar to example 3. The temperature in the reaction zones of 70-80°C.

High-boiling reagent benzene served in the upper part of the strengthening of the distillation zone, where it absorbs a portion of the hydrocarbon(s)3and creates an internal phlegm. Internal reflux number, defined as the ratio of the amount of water flowing down the hydrocarbons3to output steam flow (mainly propane), Rint=4.5 to 5.0.

Serves 100 kg/h propane and 520 kg/h of benzene. Steam load in protective relays - 178,2 kg/h Ratio V1/V in the reaction zones in the upper RH - 0,2, lower RH - 0,3 (in other RZ - intermediate values). Steam load in the upper RH - 35,6 kg/h, in the bottom RH - 36 kg/h

When the porosity of the catalyst 25% of the required diameter of the reaction and distillation zones are practically identical.

Output: 589 kg/h KP (67.4% of benzene, a 30.7% IPA, 1.7% diisopropylbenzene, 0.2% of di - and trimers of propene) and 31 kg/h propane the second distillate in line 4A (96.8% of the propane and 3.2% of propene).

Example 5.

Get trebujena (TBP) of beef (45% isobutene) and phenol (TKip=of 182.2°C).

In the middle part use 2 of the reaction zone (~0.9 m layer of the catalyst is a sulfonated cross-linked polystyrene on macroporous silica gel (diameter of 4 mm spheres, SOY=2,1). The temperature in the reaction zones 80-95°C), R=1,8. Serves to 1.87 t/h beef and 1.5 t/h of phenol, 1.0 t/h of cyclohexane. The ratio of V1/V in the reaction zones in the upper RH - 0,1, lower RH - 0,14.

Output: 1,05 t/HR of isobutane distillate (~2% of isobutene) and of 3.32 t/h cubic product containing 66.6% of TBP, 30,1% cyclohexane, and 2.0% of phenol, 1.3% of dimers of isobutene. After distillation (and return to the reaction) fractions of cyclohexane get to 2.2 t/h TBP.

1. The way of interaction of the alkene(s)containing(a)contacting the hydrocarbon stream, and more high-boiling reagent in the presence of sulfonate catalyst in a reactive distillation system having a distillation zone and located between the reaction zone is immersed in the liquid catalyst, the overflow liquid from the upper part of each overlying zone in the lower part of the underlying zone and dispersed by passing steam flow from the lower zone through each reaction zone, wherein the remaining portion of the steam flow from each of the underlying zone through verniest the upper reaction zone through the overflow space countercurrent to pour the liquid.

2. The method according to claim 1, characterized in that the steam flow passing through the specified overflow space, preferably dispersed uniformly over the cross section of the filling space.

3. The method according to claim 1, characterized in that the alkene(s)containing hydrocarbon stream serves as a minimum below the bottom of the reaction zone, and the more high-boiling reagent serves at least in the upper reaction zone or above her distillation zone.

4. The method according to claim 1, characterized in that the alkene(s)containing hydrocarbon stream is distributed among multiple threads and some of them served in the intermediate reaction zone or between them.

5. The method according to claim 1, characterized in that the flow over the high-boiling reagent distribute multiple threads and some of them served in the intermediate reaction zone and/or between them.

6. The method according to claim 1, characterized in that said more high-boiling reagent is a non-tertiary alcohol or carboxylic acid, or benzene, and the main product of the reaction is an ether or ester, or alkyl benzene.

7. The method according to claim 1, characterized in that in the interaction of alkene(s) with more high-boiling reagent are also formed di - and/or trimers of alkenes, and the resulting material is removed from exhaustive distillation zone.



 

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10 cl, 6 ex, 2 dwg

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to the improved method for oxidation of (C2-C4)-alkane and preparing the corresponding alkene and carboxylic acid. Method involves addition of this alkane to contact with molecular oxygen-containing gas in oxidative reaction zone and optionally at least one corresponding alkene and water in the presence of at least two catalysts with different selectivity. Each catalyst is effective in oxidation of alkane to corresponding alkene and carboxylic acid resulting to formation of product comprising alkene, carboxylic acid and water wherein the molar ratio between alkene and carboxylic acid synthesized in the reaction zone is regulated or maintained at the required level by regulation the relative amounts of at least two catalyst in the oxidative reaction zone. Also, invention relates to the combined method for preparing alkyl carboxylate comprising abovementioned stage in preparing alkene and carboxylic acid in the first reaction zone. Then method involves the stage for addition of at least part of each alkene and carboxylic acid prepared in the first reaction zone to the inter-contacting in the second reaction zone the presence of at least one catalyst that is effective in preparing alkyl carboxylate to yield this alkyl carboxylate. Also, invention relates to a method for preparing alkenyl carboxylate comprising the abovementioned stage for preparing alkene and carboxylic acid in the first reaction zone and stage for inter-contacting in the second reaction zone of at least part of each alkene and carboxylic acid synthesized in the first reaction zone and molecular oxygen-containing gas in the presence of at least one catalyst that is effective in preparing alkenyl carboxylate and resulting to preparing this alkenyl carboxylate.

EFFECT: improved method for oxidation.

30 cl, 1 dwg, 5 tbl, 14 ex

FIELD: petrochemical processes.

SUBSTANCE: invention relates to improved C2-C4-alkane oxidation process to produce corresponding alkene and carboxylic acid, which process comprises bringing indicated alkane in oxidation reaction zone into contact with molecular oxygen-containing gas and corresponding alkene and optionally with water in presence of at least one catalyst efficient for oxidation of alkane into corresponding alkene and carboxylic acid. Resulting product contains alkene, carboxylic acid, and water, wherein alkene-to-carboxylic acid molar ratio in oxidation reaction zone is controlled or maintained at desired level by way of controlling alkene and optional water concentrations in oxidation reaction zone and also, optionally, controlling one or several from following parameters: pressure, temperature, and residence time in oxidation reaction zone. Invention also relates to integrated process of producing alkyl carboxylate including above-indicated stage of producing alkene and carboxylic acid in first reaction zone and stage of bringing, in second reaction zone, at least part of each of alkene and carboxylic acid obtained in first reaction zone in contact with each other in presence of at least one catalyst effective in production of alkyl carboxylate to produce the same. Invention further relates to production of alkenyl carboxylate including above-indicated stage of producing alkene and carboxylic acid in first reaction zone and stage of bringing, in second reaction zone, at least part of each of alkene and carboxylic acid obtained in first reaction zone plus molecular oxygen-containing gas into contact with each other in presence of at least one catalyst effective in production of alkenyl carboxylate to produce the same.

EFFECT: enhanced process efficiency.

55 cl, 1 dwg, 7 tbl, 22 ex

Cleaning method // 2237652
The invention relates to an improved method of purification of the reaction products of the process of direct connection, comprising the reaction of ethylene with acetic acid in the presence of an acid catalyst to obtain ethyl acetate, and cleaning products, recycling, and this cleaning method includes the following stages: (I) feeding the reaction product in column (A) to remove the acid from the base which divert acetic acid, and with its top pick at least a fraction comprising boiling components containing, inter alia, hydrocarbons, ethyl acetate, ethanol, diethyl ether and water, and is directed to the apparatus (A1) for decanting in order to share these top shoulder straps on the phase rich in ethyl acetate, and water (rich in water) phase, (II) a separate return at least part of the rich ethyl acetate phase and almost all of the aqueous phase from the apparatus (A1) for decanting as phlegmy in the upper part of the column (A) or near its top, (III) the filing of the rest of the rich ethyl acetate phase from the apparatus (A1) for decanting in the upper part of the Westfalia refinery unit column (s) or near its top, (IV) the removal from the column (C): and nedogona, including significantly refined ethyl acetate, which is directed to the treatment of the colon is his, acetaldehyde and diethyl ether, which is sent to the column to remove aldehyde, and (C) lateral fraction comprising mainly ethyl acetate, ethanol and some water, which is directed to a point below the point of entry is rich in ethyl acetate phase is removed from the column (A), (V) challenging reset, including acetaldehyde, from the top or near the top of the column for removal of aldehyde and return diethyl ether, isolated from the base of the column to remove aldehyde, etherification reactor and (VI) purification of refined ethyl acetate in column (E)

Synthesis of esters // 2227138
The invention relates to an improved method for producing a lower aliphatic esters, including the interaction of lower olefin with a saturated lower aliphatic monocarboxylic acid, preferably in the presence of water in the vapor phase in the presence of heteropolyanions catalyst, characterized in that the reaction is carried out sequentially placed in several reactors or in one long reactor with several successive layers heteropolyanions catalyst and b) initial reagents practically cleared of metallic impurities or compounds of metals so that before coming in contact with heteropolyanions catalyst metals and/or metal compounds is not more than 0.1 ppm

The invention relates to a method for the synthesis of esters from olefins and lower carboxylic acids

The invention relates to an improved process for the preparation of secondary butyl alcohol, which is an intermediate for the production of methyl ethyl ketone

The invention relates to an improved method for producing sec-butyl acetate is used as solvent for paints and varnishes and as raw material for the production of sec-butyl alcohol

The invention relates to chemical technology, in particular to a method for producing sec-butyl acetate (BWA), used as a solvent for paints and varnishes and for the production of sec-butyl alcohol

FIELD: chemistry.

SUBSTANCE: claimed invention relates to method of selective isolation of recycling flow, which contains dimethyl ester (DME), from flow, which leaves zone of methanol conversion into olefins (MTO), where said leaving flow contains water, methanol, DME, ethylene, propylene, C4-C6-olefins. Claimed method includes stages: (a) cooling and separation of at least part of leaving flow into liquid flow, which contains methanol and DME, liquid hydrocarbon flow, which contains methanol, DME and C2-C6-olefins, and vaporous hydrocarbon flow, which contains DME, methanol, ethylene and propylene; (b) distillation of DME from at least part of liquid hydrocarbon flow, separated at stage (a) in zone of DME distillation, functioning in conditions of distillation, efficient for formation of vaporous main flow, which contains DME, methanol, ethylene and propylene, and liquid hydrocarbon bottom flow, which contains C4-C6-olefins; (c) mixing of at least part of vaporous hydrocarbon flow, separated at stage (a), with at least part of main vaporous flow, produced at stage (b), with formation of enriched DME vaporous flow of light hydrocarbons; (d) supply of formed enriched with DME vaporous flow of light hydrocarbons into zone of primary absorption of DME, where said vaporous flow is brought in contact with methanol-containing selective with respect to DME solvent in conditions of wet purification, which allows to form (1) liquid bottom solvent flow, containing methanol, DME, water and substantial and undesirable amount of ethylene and propylene, and (2) main vaporous flow of product, enriched with light olefins and depleted of DME; (e) directing of at least part of liquid bottom flow, separated at stage (d), into zone of light olefins distillation, functioning in conditions of distillation, efficient for distillation of at least considerable part of ethylene and propylene, contained in liquid bottom flow, without distilling from there any considerable part of methanol, which results in formation of main flow of distillation section, containing DME, ethylene and propylene, and liquid bottom flow, containing DME, methanol, water and light olefins in amount reduced in comparison with amount of light olefins in liquid bottom solvent flow, supplied to this stage, and (f) recycling of at least part of liquid bottom flow, separated at stage (e) into zone of conversion MTO, thus selectively introducing to it additional oxygenated reactants.

EFFECT: reduction of undesirable increase of C2 and C3-olefins in recycling DME flow.

10 cl, 4 tbl, 2 dwg, 2 ex

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