The method of obtaining the fraction of aromatic hydrocarbons, c6-c9

 

(57) Abstract:

Use: petrochemical and chemical industry. The inventive fraction of aromatic hydrocarbons, C6-C9. Raw materials: 1 - phenolic resin (FS) - waste production of phenol and acetone. 2-isopropylbenzene (cumene) or recirculate process of production of phenol and acetone. The catalyst composition, wt.%: (1-) Pd 0,75, crystalline miniserial 5, -Al2O3100, (2) NiO 5; MoO315; crystalline miniserial 10; -Al2O3to 100, (3) the zeolite ZSM-8 - 45; ZnO - 1,0, -Al2O3to 100, (4) Pt 45; Sn - 0,25; F - 0,25; zeolite ZSM-8 or ZSM - 23 and 5-Al2O3up to 100. Conditions: the process are sequential contacting of the feedstock with 4 of these catalysts in the two reactors. The mass ratio of catalyst 1:2 1:9 and 3:4 1: 9, 300 - 380°C, 2.0 To 4.0 MPa, the volumetric feed rate of 1.5-2.5 h-1the volumetric ratio FS:IPA or recirculate 1:1 hydrogen: feedstock (900 - 1600): 1. 1 C.p. f-crystals, 1 table.

The invention relates to organic catalytic chemistry, in particular to the processing of hydrocarbon resins, namely phenolic resin in the fraction of aromatic hydrocarbons containing mainly benzene and isopropylbenzene (cumene), and m the FL fraction of aromatic hydrocarbons from acetophenones fraction of phenolic resin at 360-380aboutC, space velocity of the raw material 1 h-1, a pressure of 3.5 MPa, the ratio of N2raw materials (800-1000) 1 in the presence of aluminoborosilicate catalyst. The resulting hydrogenation product of the fraction of aromatic hydrocarbons containing monocyclic aromatic hydrocarbons WITH6-C9wt. 55,2, including benzene and 0.7, toluene 2; and-propylbenzoyl 0,2, -methylsterol 1,1, phenol 15,5, acetophenone 5,9, ethylbenzene 23,4, isopropylbenzene 27,8.

The disadvantage of method (1) is low activity, stability and selectivity of the catalyst in hydroperiod phenolic resin and the degree of conversion in benzene and cumene.

The closest in technical essence and the achieved effect is the method (2), including the hydrogenation of phenolic resin in the presence of hydrogen and aluminoborosilicate (AKM) of the catalyst composition, wt. Soo 4; NoO312, 0mm; -Al2O3else if T 350aboutC, Vc 1-1,2 h-1; P 4,9 MPa; filed hydrogen 1000 m3/m3of raw materials.

The original phenolic resin composition, acetone 0,15; water 10,1 O. m 0,35; IPA 30,40; alpha methylsterol 2,18; phenol 11,93; acetophenone 18,03; DMPC 0,80; dimer of alpha-methylstyrene 9,49, complex phenol resin 14,55 becomes 80% phenol, cclu aromatic hydrocarbon composition WITH6-C9(benzene, isopropylbenzene), there remains much resin, phenol and other hydrocarbon impurities, low stability and high coking ability of the used catalyst, mainegenealogy period is 250,0 PM

The resulting hydrogenation product has a black color (CNT more than 8 units). The method does not provide complete hydrogenation of alpha-methylstyrene and acetophenone; the temperature of the end of the boiling section of hydrogenated feed compared to the raw material phenol resin + IPA remains practically unchanged.

The aim of the invention is to obtain the fraction of aromatic hydrocarbons WITH6-C9with a predominant content of benzene and cumene.

This goal is achieved by the fact that as a starting raw material, a mixture of phenolic resin and IPA in a volume ratio of 1 to 1, which is subjected to hydrobromide in two sequential adiabatic reactors, the first of which layers are loaded during the feed catalysts (I) and (II) at a mass ratio of 1 to 9; the catalyst (I) has a composition, by weight. Pd 0,76; crystalline miniserial 5; -Al2O3else, the catalyst (II) has a composition, by weight. Ni 0,5; MoO315; crystalline miniserial (tellago reactor catalysts at a mass ratio of 1 to 9. The catalyst (III) has a composition, by weight. over high-silica zeolite with the module SiO2Al2O340 families pentelow (ZSM-8) 45; ZnO 1,0; -Al2O3else, the catalyst (IV) composition, wt. Pt 0,45; Sn 0,25; 0,25 F; servicecompany zeolite properties of pentelow (ZSM-23, ZSM8) (module SiO2Al2O340) 5; -Al2O3the rest of it.

The process of the proposed method in the proposed catalysts is carried out at 300-380aboutC, F 2-4 MPa; Vc 1.5 to 2.5 h-1, the ratio of hydrogen feedstock 900-1600 1, that is convertible composition of the raw material 1 (phenolic resin + isopropylbenzene (cumene) by about. the ratio of 1 1), wt. isopropylbenzene (cumene) 40,84; phenol 2,03; acetophenone (ACP) 2,14; dimer of alpha-methylstyrene (d-M-CT) 11,44; complex phenol 19,27; dimethylphenylcarbinol (DMPC) 0,58; heavy resin 23,39; fractional part;aboutWITH THE TC-90; QC-390;4200,972 g/cm3: iodine number 48,3 J2/100 g or raw material 2 a mixture of phenolic resin and recirculate (risaykl section of hydrogenated feed) at a volume ratio 1 1 composition, wt. benzene 20,02; ethylbenzene 0,87; IPA 16,15; phenol 0,34; -M-ST 0,62; ACF 2,01; dimer-M styrene 10,63; compound 19, 22 the phenol before. dimer-m styrene 1,31; DMPC 0,42, heavy hydrocarbons (tar) 28,41 get catalysate with the release of 100 wt. costulae of 0.03 to 4.0 from raw materials N 2 catalysate composition, wt. benzene 59,8-6; ethylbenzene 4-4,1; toluene 0,2-0,4; IPA 26-31; phenol 1.0 to 1.5; -m-styrene 0,4-0,5; complex phenol of 0.2-0.3; heavy leave the rest of the paraffin, naphthenic.

To date the literature has not described how to obtain a fraction of aromatic hydrocarbons from phenolic resin using catalysts of the specified structure, therefore it can be argued that the claimed combination of features of an object is new and, therefore, the corresponding solution has criterial feature of the "novelty."

On the other hand, the distinctive features of the proposed technical solutions (way) from the famous are.

The application of new catalysts (I), (II), (III), (IV).

The process of hydrobromide in 2 sequential reactors at different temperatures, thus ensuring that the necessary reactions of transformation of uglevodorodov of raw materials.

Layer-by-layer load reactors catalysts that provides in the first reactor in the upper layer on the catalyst (I) preliminary hydrogenation of resins, unsaturated hydrocarbons, in the lower layer on the catalyst (I) hydrocracking complex phenol, dimers, trimers-m-styrene, alkilirovanija, dealkylation, parallelomania and isomerization of aromatic hydrocarbons, preventing the catalyst (IV) from coking due to the content in the catalyst (III) zeolite Pancasila, which has anticariogenic component, and finally, in the lower layer on the catalyst (IV) of the 2nd reactor reactions proceed exhaustive hydrogenation alkylaromatics and unsaturated hydrocarbons.

Made certain ratio of the catalyst in the first reactor (I) (II) as 1 9, in the second reactor (III) (IV) 1 9.

At the start of the process as a diluent phenolic resin is used IPA, and then recirculating the hydrogenation product with a volumetric ratio of 1 to 1.

On the basis of these signs can be argued that the essence of the proposed facility is not obvious from the well-known in the industry prior art, therefore, it has criterial element of the invention "inventive step".

Technologically, the proposed method can be implemented in the chemical and petrochemical industry and allows you to receive waste from the production of phenol and acetone phenol resin fraction of aromatic hydrocarbons containing benzene 43-65 and the third criterion a symptom of the invention "industrial applicability".

P R I m e R 1. Phenolic resin mixed with IPA in a volume ratio of 1 to 1, the composition of the raw material 1 (see table), subject to hydrobromide in two sequential reactors with layers loaded catalysts during feed (top to bottom): R-1 CT I composition, wt. Pd 0,75; miniserial 5; -Al2O394,25, CT II composition, wt. NiO 5, MoO315; miniserial 10; -Al2O370 (the ratio of the catalysts 1 to 9), R-2, CT III composition, wt. CRS-zeolite 45; ZnO 1; -Al2O354, CT IV composition, wt. Pt 0,45; Sn 0,25; 0,25 F; CRS-5 zeolite; -Al2O394,05. The process is conducted at P 3 MPa, V 1.5 h-1N2raw 900 1; the temperature in the R-1 300aboutWith that in R-2 350aboutC. the Results of example 1 and for the subsequent in the table.

P R I m m e R 2. The process is carried out on raw materials in example 1, the catalyst composition of example 1 at a ratio of 1 to 9; P = 4 MPa; Vc 2.5 h-1; N2raw 1600 1; the temperature in the R-1 320aboutIn R-2 at 380aboutC.

P R I m e R 3 (for comparison). The process is carried out on raw materials in example 1, the catalyst of example 1 at a ratio of 2 8 P2,5 MPa; V 1,2 h-1; H2raw 800 1 at a temperature in the region of 1 280aboutWith that in R-2 at 340aboutC.

P R I m e R 4 (for comparison). The process is carried out on raw materials in example 1, the temperature value P-1,2 390aboutC. the Catalysts samakovlis, the product is a black, viscous, the process is not.

P R I m e R 5. The process is carried out on raw materials in Prime 1, the catalyst composition of example 1, the ratio of 1 9 P = 3.5 MPa, Vc 2 h-1; N2raw materials 1200 1, at a temperature in the R-1 320aboutWith that in R-2 at 350aboutC.

P R I m e R 6. The process is performed on the phenol resin in a mixture with a hydrogenation product (risaykl) (raw material 2) with a volumetric ratio of 1: 1 on the catalyst composition of example 1, at P 3 MPa; Vc 1,5; N2raw 900 1, at a temperature in the R-1 320aboutWith that in R-2 at 350aboutC.

P R I m e R 7. Spend on raw materials N 2, the catalyst composition of example 1, at mass ratio of 1 9, P = 4 MPa; Vc 2.5 h-1; N2raw 1600 1, at a temperature in the region of 1 300aboutWith that in R-2 at 380aboutC.

P R I m e R 8 (for comparison). The process is performed on the raw material 2, the catalyst composition of example 1 at a mass ratio of 1 9, P = 4.5 MPa, Vc 8 h-1; H2raw 2000 1, at a temperature in the region OF 1.2 390aboutC.

P R I m e R 9 (for comparison). The process is performed on the raw material 2, the catalyst composition of example 1, at a mass ratio of 2 to 8; P = 2.5 MPa; Vc 1,0 h-1; H2raw 800 1; the temperature in P-1,2 290aboutC.

P R I m e R 10 O395,3; (II) NiO 4; MoO313, the magnesium-silicate 7; -Al2O376; (CT III) CRS-zeolite 40; -Al2O360; (IV) Pt 0,4; SVK-zeolite 3; -Al2O396,6 when the parameters in example 6.

1. THE METHOD OF OBTAINING THE FRACTION OF AROMATIC HYDROCARBONS, C6-C9by catalytic hydrogenation of phenolic resins-waste production of phenol and acetone Kukolnik way at elevated temperature and pressure, wherein the phenolic resin is used in a mixture with cumene or recycled from the process of hydrogenation of the obtained hydrogenation product at their volumetric ratio of 1 to 1 and the process of hydrogenation lead by successive contact of the feedstock with four catalysts, having in the course materials the following composition, wt.

I. Palladium 0,75

Crystalline magnesium silicate 5

The aluminum oxide To 100

II. Nickel oxide (II) 5

Molybdenum oxide 15

Crystalline magnesium silicate 10

g-alumina To 100

III. High-silica zeolite type ZS M-8 45

Zinc oxide 10

g-alumina To 100

IV. Platinum 0,45

Tin 0,25

Fluorine 0,25

High-silica zeolite type ZS M-8 or ZS M-23 5

g-alumina To 100

taken in the mass is 380oC, pressure of 2.0 to 4.0 MPa, the space velocity of the raw material 1,5 2,5 h-1, the volumetric ratio of hydrogen: feedstock 900 1600 1.

 

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15 cl, 2 tbl, 5 ex

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13 cl, 2 tbl, 2 ex

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5 cl, 3 dwg, 6 tbl, 4 ex

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