SU1234418A1 - Method of treating liquid products of hydrocarbon raw material pyrolysis - Google Patents

Description

2. Method POP.1, characterized in that when distillate distillate is taken fractions in the temperature range, ° C: 280-225 - naphtha

one

The invention relates to the production of hydrocarbon products from liquid pyrolysis products boiling above 200 ° C, fractions in which the resources of individual aromatic polycyclic compounds - acenaphthene, fluorene, phenanthrene, anthracene are concentrated, while simultaneously obtaining oil pyrolysis pitch and fractions containing naphthalene, monomethyl naphthalenes and dimethyl naphthalenes, and can be used in the petrochemical, shale and coke industry.

The aim of the invention is to expand the range of products and simplify the process technology.

FIG. 1 shows a schematic flow chart for the separation of liquid pyrolysis products into pyrolysis pitch and six target fractions. .

The feedstock — a desirable gasoline pyrolysis resin (TSP) —is fed through line 1 to the furnace 2 of the single evaporation, from which, via line 3, the heated raw material enters the evaporator 4.

The distillate obtained from the evaporator 4 in the course of a single evaporation, TSP via line 5 is sent to distillation column 6, in which a separation occurs in the fraction with boiling range 200-270 ° C (distillate) and 270-380 ° C (bottom product) . The ratio of distillate and bottom product in column 6 is 0.66: 0.34.

The resulting pyrolysis pitch is withdrawn through line 7, the distillate of column 6, which includes the light, naphthalene and alkylnaphthalene fraction, is fed as feed through line 8 to column 9.

In column 9, a light fraction (190-210 ° C) is separated as a head product along line 10, Ratio

linear, 245-250 - alkylnaphthalene, 275-280 - acenaphthenic, 290-295 - fluorene and 335-340 - anthracenephenanthrene.

distillate and bottom product in this column 0.2: 0.8.

The bottoms product (210-270 C) of column 9 is fed as feed by LII 11 to column 12, where it is divided (to naphthalene and alkylnaftline fractions, discharged along lines 13 and 14, ratio of fractions 0, 52: 0.48.

0 The bottom product of column 6 is sent via line 15 for processing to column 16. The final separation products of this column are the acenfenfluorene fraction, separable 5 as a distillate through line 17, a finanthracene fraction taken from one of the lower stages of the column. lines 18, and the cubic fraction representing the products of polymerization of the components of the distillate TSP. This product can be sent to the baking pan via line 19 and used as an additive to the high melting bake obtained in process 5 of single evaporation. The ratio of flows in the column is 16-distilled:: fraction: cube 0.43: 0.23: 0.34.

The azentafenfluorene fraction is fed as feed via line 17 to column 0 0.

In column 20, a narrow fraction is selected in the distillate along line 21, which includes the homologues of naphthalene and acenaphthene.

J The bottom product contains resinous, high-boiling unidentified components with an admixture of anthracene and phenanthrene. The acenaphthenic fraction (275-285 s) is selected at the level of the 35th theoretical level, calculated from the bottom of the column along the fluorene line - at the level of the 10th theoretical stage through the line 23. The ratio of the end products of the column 20, calculated from the top 5, is distilled: Fractions: Fractions:.: Bottom product 0.1: 0.3: 0.3: 0.3.

312344

 The distillate and the bottom product of the column 20, containing valuable components, are recycled: the distillate is fed to the power supply of the column 6, and the bottom product together with the power supply via the LI, NII 24 - to the column 16.

Example 1. Initial raw materials (gasoline tep) with the following physicochemical characteristics:

Density, g / cm 1.0681 MM225

Iodine number, g Ij / lOO g57

Kinematic viscosity, m / c 10, at T, ° C

7510.8

1005.4

1402.6

Driving, wt.%, Up to T, s

20011

25040

38074

Temperature C

195-200

50-55 1.22-1.23

0.1-0.2

outlets, С104

subjected to a single evaporation (he) on the installation of continuous operation at a pressure of 101.3 kPa, 365-370 speed of the resin in a coil of 0.04 m / s. Separated in an evaporator 4 in an amount of 25% by weight, the pitch is a dark mass with the following parameters.

Temperature

ras gcheni, ° C

Coke residue,

May %

Density, g / cm

Sulfur content

May.%

The distillate is subjected to rectification to the desired fraction.

In tab. 1 shows the characteristics of the distillate TSP, in table. 2 - the characteristic of target fractions.

Technological parameters of the distillation columns are given in table. 3

Example 2. The composition of the raw material, pressure and temperature correspond to the data given in Example 1. The speed of the resin in the coil is 0.06 m / s. Distillate ratio

,

0

five

0

five

0

0

five

184

and pitch, the quality of the pitch, the composition of the distillate and the fractions recovered by distillation correspond to the data of Example 1.

Example 3. The composition of the raw material, the pressure and the speed of the resin correspond to the data of Example 1.

SI temperature 350-355 s, mass ratio of distillate and pitch O, 7: 0.3. The quality of the pitch obtained with these parameters:

The softening temperature, s180-185 Coke residue, wt. Density, g / cm 1.21-1.22 Sulfur content, wt.% 0.2-0.1 The compositions of the distillate and the fractions emitted by distillation are identical (within the limits of a chromatographic analysis error of 5-10 rel,% ) given in example 1 (see table. 1). Example 4: Composition The main physico-chemical characteristics of the feedstock are similar to those shown in Example 1. The SI pressure is 40 kPa, the process temperature is 335-340 ° C, the resin speed is 0.04 m / s, the distillate mass ratio and pitch 0.75: 0.25.

The resulting pitch has the following properties: Temperature

size gcheni, from 180-185 Coke residue, wt.% 45-50 Density,

, 19-1.20

Content

sulfur, wt.% 0.1 The composition of the distillate obtained under these SI conditions is given in Table. four.

As can be seen from these data, the quality of the distillate is not fundamentally different from that given in Table. 1 (within the error of analysis). The composition of the narrow fractions emitted during the processing on the columns is also identical to that given in Table. one.

Example 5. The composition of the raw material, the pressure and the rate of movement of the resin correspond to those given in Example 4. The temperature is OH 315-320 s. The mass ratio of distillate and pitch is 0.7: 0.3.

Peck has the following properties: The softening temperature, from 165-170 Coke residue, May L35-40

Density, g / cm 1.19-1.20 Sulfur content, wt.% 0.1-0.2

The composition of the distillate and the narrow fractions is identical to that given in Example 4.

Example 6. The pressure of the SR is 25 kPa, the process temperature is 320– 325 ° C, the speed of the resin is 0.04 m / s, the mass ratio disptil tgpek is 0.75: 0.25.

The resulting pitch has the following properties:

Softening point, ° С160-165 Coke residue, - wt.% 35-40 Density, g / cm 1.19-1.2 Sulfur content, wt.%. 0.1-0.2 The composition of the distillate is given in table. 4 The operation parameters of the distillate separation columns into target fractions do not differ in principle from those described in examples 1-5.

Example 7. The pressure of the SR and the speed of movement of the raw materials correspond to that given in Example 6. The temperature is 295-300 ° C. The mass ratio distillate t: pitch 0.7-: 0.3. Pitch quality:

The softening temperature, С

150-155

Coke residue,

wt.% 30-35

Density, g / cm 1.18-1.19

Sulfur content

wt.% 0.1-0.2

At pressures below 25 kPa (200 mm Hg), the cost of the process of single evaporation increases sharply due to the increase in energy consumed under these conditions.

The change in the temperature of single evaporation in the selected pressure range occurs fairly smoothly (Fig. 2), so slight pressure fluctuations (temperatures) do not affect the quality of the distillates produced (see example 1 and 4).

ten

15

0

five

0

five

0

Phenomena associated with changes in the physicochemical characteristics of the raw materials at reduced pressures (convergence of boiling points and crystallization temperatures, increase in viscosity, increased sublimation of such components as naphthalene, anthracene, etc.) - clogging of communications, increase in apparatus resistance and associated with them, an increase in the power of pumps and drives is absent.

With a selected range of feed rates, the cfu into the single-evaporation furnace has time to undergo both polymerization processes and depolymerization processes, and the final products of the process are stabilized. Under these conditions, pyrolysis pitch containing a reduced amount of polymers is separated in the evaporator as a liquid phase.

FIG. Figure 3 shows the data on the output of the main components of the heavy pyrolysis resin to the distillation part, depending on the ratio of distillate and pitch during the process of single evaporation.

The proposed method, the essence of which is to apply the processes of single evaporation and rectification, allows to obtain six target fractions, from which further processing can be used for acenaphthene, fluorene, anthracene, phenanthrene, with simultaneous production of naphthalene, mono- and dimethyl-naphthalene with high output from the potential in the feedstock (acenaphthene 83, fluorene 77, anthracene 85 and phenanthrene 85%) and the content of the main substance 96–98 May%. Residual pitch obtained in the course of single evaporation with a softening temperature range of 150–200 ° C makes it possible for its specific use (not an acceptable polymer binder day) in the production of certain types of carbon-graphite materials, the technology of which involves the use of a high-melting binder, for example, high-temperature black brushes on the basis of a joint vibrating and vibrating components.

Soetm

cleavage of S1FY1 .7kta at 101.3 kPa,, X

v, 5 12.8

42, 72.0 1.3

t t 6 t c t 1

Yield from tep, wt.% 10

21

Temperature limits

boil

selection of fractions

N.K.-210 210-230 230-270 275-285 285-305 310-370

195-200220-225

Molecular weight 125135

p, g / smz 0,9351,005 Iodine number.

245-250 275-280 290-295 335-340

140 155 165 195 1,006 1,010 1,020 1,104

Place of supply of raw materials, t, Art. (counting from the bottom of the column)

The proportion of the selection of distillate (from the feedstock to the column)

Temperature, C

condensation distilled

boiling vat

 The feedstock to the columns is supplied as boiling (liquid

table 2

nineteen

3.3 3.3

5.9

245-250 275-280 290-295 335-340

140 155 165 195 1,006 1,010 1,020 1,104

ten

15

ten

22

0.2 0.52 0.43 0.1

200

225

295

270

Cocraa .icxoABoro of prodtggs p "i,. npB 101,3 KlU, Moc.Z

-

13, 2

14.0 29.1

11.2 10.5

10.2 3.0

3.3

5.5 6.5

7.0

9.5

5.6

19.7

42.0 g, 51.0

39.2 7,010,11,5

18.8 29,146,010.9

- 14,117,78,6

11,913,015,2

13,712,216,0

4.5-8.5

4.2

7.3

9.5

14.5

10.1

19.0 22.6

3.7

: atsvv kolov

16,1

 4.7 2.2

90.0 20.5 5.7 45.0 1.5

2.4 2.0

4.3 33.5 35.1 1.0 3.1

1.5

36.2 15.1

27.3 95.0

0.4 42.0

1.0

0.2 36.3 32.0 - 68.0

5

 Sh

"H

| 350

.

IG1-1-- 4i --Lgl L-, -f - ,,,, Mf ,, j-, l- | 11pl | w 1 LGsh-11ga

W 2/7/7 3/7/7 ffOO 500 fOO 700 800

Residual pressure mmrt. cm,. Phys .2

7/7 (7 EO

Nasrt

2-Methy l Naphthalene

, --- jlutpewn

so70SO

From & he distilled TSP, noo. %

Fig.Z

Nasrtolin

Compiled by E. Gorlov Editor L. Vesepovska Tehred L. Oleinik

Order 2952/30, Circulation 482: Subscription

VNISh State Committee of the USSR

for inventions and discoveries 113035, Moscow, Zh-35, Raushsk nab., 4/5

Tr |, one-one-graphic pre-tatie, Uzhgorod, st. Project, 4

Proofreader M.Samborsk

Claims (2)

1. METHOD FOR PROCESSING LIQUID PRODUCTS OF THE PYROLYSIS OF HYDROCARBON RAW MATERIALS, boiling above 200 C, by feeding raw materials to the furnace coil, a single evaporation to obtain distillate and pitch and distillate distillation with the selection of target fractions, characterized in that, with the aim of expanding the range and simplification of the range of products technologies, raw materials are fed into the furnace coil with a linear velocity of 0.04-0.06 m / s, a single evaporation is carried out at a pressure of 25-101.3 kPa while maintaining the mass ratio of distillate pitch 0.7-0.75: 0.25- 0.3 and rectification are carried out at atmospheric m pressure. 1/54418 2. The method of pop. 1, characterized in that during distillation distillation fractions are taken in the temperature range, ° C: 280-225 - naphtha, 245-250 - alkylnaphthalene, 275-280 - acenaphthenic, 290295 - fluorene and 335-340 - anthracenfenanthrene.