Method of deparaffinization of hydrocarbon fractions

专利摘要:
A process for improving fluidity of hydrocarbon fractions by dewaxing thereof is described. In the process, hydrocarbon fractions are contacted with hydrogen in the presence of a specific type of catalyst, thereby lowering the pour point of the hydrocarbon fraction. The catalyst comprises a specific type of zeolite which is defined by a specific X-ray diffraction pattern (such as that shown in Fig. 1) and which has a mesitylene adsorption not less than 1.8 wt%.
公开号:SU1421261A3
申请号:SU843706624
申请日:1984-02-09
公开日:1988-08-30
发明作者:Иваяма Казуеси；Иноуе Такехиса；Сато Кимио；Хаякава Норио；Фудзии Масаки
申请人:Торэй Индастриз Инк (Фирма)；Фудзи Ойл Ко,Лтд (Фирма)；
IPC主号:

专利说明:

 Yu
Yu
ot

sn
The invention relates to a method for the dewaxing of hydrocarbon fractions and can be used in the refining industry,
The purpose of the invention is to increase the yield of deparaffinized fractions.
Example 1. 9.22 g of solid caustic soda and. 12.5 g of tartaric acid (L) are dissolved in 344.2 g of water. 17.5 g of sodium aluminate solution is added to the solution to form a homogeneous solution. To this stirring solution, 66.0 g of silicic acid are gradually added, thanks to which the aqueous reaction mixture is in the form of a uniform suspension. The reaction mixture has the following composition, mol:
 thirty
HzO / SiO 20
OH- / SiO, j0,17
. ,five
one
The reaction mixture is placed in a 500 ml autoclave and tightly closed. The contents are then heated at 160 ° C with stirring, followed by crystallization for 72 hours. After the crystallization is completed, the product obtained is taken out of the autoclave, then washed with distilled water until the creep is approximately neural (pH final), filtered and dried overnight at 11 The resulting product has the following molar composition: 1.01 Na O-A12.0z-25, SiOj 4.89-H, jp. The resulting zeolite has an X-ray diffraction pattern, which is shown in figure 1, and adsorption of mesitylene 2.1 %. Obtained in this way The zeolite powder is subjected to ion-exchange treatment in a batch process for 30 minutes by heating in an aqueous solution of ammonium chloride with a liquid / solid ratio of 5 liters / kg sefnecTBO and at a temperature of 80 to 90 ° C. Then the treated powder is washed with water and dried overnight at 110 ° C. The content of zeolite, washed from alkali, after treatment with a solution of ammonium chloride and drying at 110 ° C
1, -, -27, ISiO- -5.11
1,06NaiO AlaOs-24,8Si02-5,07
1, OONa20- Al Oj 26.1 SJ. -4.25
0, ,, 98
is 96.8%. In this way, to wash off the alkali from the alkali, the zeolite powder is mixed with alumina as a binder in an amount of 15% by weight based on alumina (ABO,), followed by stirring. After mixing, the mixture is formed into 10-24 mesh particles (yJScito), and then dried overnight and calcined at 500 ° C for 2 hours in air. The resulting catalyst is used to carry out the dewaxing reaction of the sweet crude oil vacuum gas oil. 10 days after the start of the reaction, the reaction temperature reaches 334 ° C and the solidification temperature of the 165 ° C fraction of the product is -15 ° C. The rate of increase in the reaction temperature, necessary to maintain this pour point, is 5.8 ° C / day. The yield of the 165 ° C fraction is 85.3% by weight, the bromine number of the fraction is 1.8,
Further, this catalyst is estimated using oil vacuum gas oil. As a result, 10 days after the start of the reaction, the reaction temperature reaches 327 ° C, and the pour point of the 165 ° C fraction of the product is -20 s. The rise temperature of the reaction temperature is necessary to maintain this temperature. solidification rate is 6.0 ° C / day. The yield of the fraction 165 ° C is 86.4% by weight,
The vacuum-free vacuum gas oil and gas oil used in the described reaction have the properties given in Table 1.
EXAMPLE 2 To prepare the catalysts, the procedure of Example 1 is used, using various carboxylic acids instead of tartaric acid. The reaction mixtures have the following compositions (see table 2).
Obtained after 24 hours overnight with zeolites have the following molar compositions:
31421261
These zeolites are diffractive
picture (FIG. 1) and have mesitylene adsorption of 1.8, 1.8, 2, O, and 1.9 wt.%, respectively.
The zeolites thus obtained are endowed with acidic properties as in Example 1 and molded to create catalysts. The content of zeolites in catalysts after washing from alkali and imparting acidic reaction according to example 1 is, wt.%: Succinic acid 98.2. O-Toluic acid 98.9. Citric acid 96.7. Salicylic acid 97.3. These catalysts are examined for evaluation their properties when using sweet gasoil.
swarm fraction has a temperature
The reaction temperature at which the desulfurized vacuum gas-gas is.
LA 5 days after the start of the reaction, the reaction temperature reaches and the freezing temperature of the fraction 165 is -15 C. The speed
Zyastan -15 With 10 days after the start of the reaction, the rate of rise of the reaction temperature is necessary
to maintain this temperature, to raise the reaction temperature, to set the temperature, and to exit the fraction of 165 ° C, to maintain this temperature, in table 3, the freezing temperature is
6.2 ° C / day The output of the fraction 165 is equal to
Froze The zeolite obtained 83.8% by weight, and the bromine number of this in example 1, is endowed with acidic properties of 2.7. and formed by the method of example 1. Then the particles of zeolite are impregnated with aqueous solutions of chloroplatinic acid, palladium nitrate and nickel nitrate, respectively, in amounts of Pt 0.2 wt.%} Pd 0.2 wt.%, and Ni 1,0 wt.% After soaking with each metal, the zeolite particles are dried overnight and calcined at 500 ° C for 2 hours in air. . The resulting catalysts are used for the dewaxing of a desulfurized vacuum gas oil.
For each of the considered catalysts, the reaction temperature.
35
40
45
Example 5 The procedure of Example 1 was repeated using an aqueous reaction mixture to obtain a zeolite, mol:
 95
H-20 / SiOi25
OH / SiOi 0.32
A / Al-2037.0
After drying, the final product of composition 1 is obtained. Al Oa-49.68102-10.4.
The zeolite is given acidic properties and molded to obtain the catalyst of Example 1. The content of zeolite after washing from alkali and imparting acidic reaction is 97.1% by weight. The catalyst is evaluated using sweet vacuum gas oil. 10 days after the start of the reaction, the reaction temperature reaches and the temperature of the fraction 165 ° C is 15 ° C. The rate of rise of the reaction temperature, which is necessary to maintain this pour point, is 7.1 ° C / day. Yield fraction 165 ° C
at which fraction. 165 ° C has a freezing temperature 5 days after the start of the reaction, the rate of rise of the reaction temperature is necessary to maintain this freezing temperature, and the yield of the fraction 165 ° C is given in Table 4,
Example 4: The general procedure of Example 1 is repeated except that an aqueous reaction mixture of the following composition, mol, is used:
SiO / AlOj 25
H O / SiOa 20
.j A / ACO,
0.16 1.0
After drying the final product overnight at 110 ° C, the zeolite has the following composition, 1, ACO3 x21.4Si02-5.00 H.0.
The resulting zeolite has a diffraction pattern of x-rays, presented in figure 1, and adsorption mesitylene, equal to 1.9 wt.%.
/
The zeolite is given acidic properties and molded to obtain a catalyst by the method of Example 1. The content of the zeolite after washing, from alkali and imparting acids to the reaction, is 98.0% by weight. The catalyst was evaluated by the method of example 1, using 165 ° C, is -15 ° C. Speed
83.8 wt.%, And the bromine number of this fraction is 2.7.
Example 5 The procedure of Example 1 was repeated using an aqueous reaction mixture to obtain a zeolite, mol:
 95
H-20 / SiOi25
OH / SiOi 0.32
A / Al-2037.0
After drying, the final product of composition 1 is obtained. Al Oa-49.68102-10.4.
The zeolite is given acidic properties and molded to obtain the catalyst of Example 1. The content of zeolite after washing from alkali and imparting acidic reaction is 97.1% by weight. The catalyst is evaluated using sweet vacuum gas oil. After 10 days after the reaction, the reaction temperature reaches and the fraction 165 ° C is 15 ° C. The rate of recovery of the reaction temperature, which is necessary to maintain this freezing temperature, is 7.1 ° C / day. Yield fraction 165 ° C
5U21261
79.3 wt.%, And the bromine number of this fraction is 4 p 3.
Example In accordance with a known method, zeolite ZSM-5 is prepared.
Table 5 presents the x-ray diffraction patterns of zeolites,
This freezing point is 8.3 C / day. The yield of the 165 C fraction is 77.8 mc o%, the bromine number of this fraction A, 1 °
Raw materials, g;
A.Water Silicon
acid68.3 10
B. Sodium aluminate solution 10.5
C. Aqueous solution of tetrapropylammonium hydroxide (25% aqueous solution) 439.4
The composition of the reaction mixture, mol: SiOj, 1, 0 - 0.02, 0.034 (CH,) 0.31
obtained in examples 1-6.
Example 7. Synthetic mordenite (Zeolon 100NA. Norton Co., LiMited) is endowed with acidic properties and molded to produce a catalyst in a manner similar to Example 1. This catalyst is evaluated using sweet gas. As a result, it is established that when the reaction temperature rises
20 to 400 ° C distillate with boiling point. The upper 165 ° C has a pour point of not less than -10 ° C. The mordenite catalyst has an adsorption value of mesitylene of 2.3% by weight and the requirements of this
The starting material B is added to C to form a uniform solution. K: Raw material A is gradually added to this solution, followed by stirring to obtain a uniform suspension of the reaction mixture. This reaction mixture was charged to an autoclave and heated to 160 ° C with stirring followed by crystallization for 72 hours. After the crystallization was completed, the crystals were washed with water until neutral. Then the washed crystals are dried at 120 ° C for 15 hours. After treatment at 120 ° C for 15 hours, a zeolite of composition is obtained
0.85 (), 15Na20 AlO-35.7SiO-7.7.
The ZSM-5 zeolite thus obtained is formed, calcined, exchanged with ammonium ions and calcined to form a catalyst. The content of zeolite after washing from alkali and exchange of ammonium ions is 95.7%. This catalyst is evaluated using desulfurized vacuum gas oil. 10 days after
the reaction’s reaction temperature — gg of furfural — starts to produce raffinate with pa and reaches 374 ° C, and the solidification temperature of the fraction .. 165 C is
yield 78.5 wt.%, having the following properties:
. The rate of rise of the reaction temperature, necessary to maintain this pour point, is 8.3 C / day, the yield of the fraction 165 C is 77.8 mc o%, the bromine number of this fraction A, 1 o
obtained in examples 1-6.
Example 7. Synthetic mordenite (Zeolon 100NA. Norton Co., Limed) is endowed with acidic properties and molded to produce a catalyst as in Example 1. This catalyst is evaluated using sweet gas. As a result, it is established that when the reaction temperature rises
0 to 400 ° C distillate with boiling point. The upper 165 ° C has a pour point of not less than -10 ° C. The mordenite catalyst has an adsorption value of mesitylene of 2.3% by weight and the requirements of this
5 of the invention are satisfied. However, the d space (da) obtained from the X-ray diffraction pattern, as can be seen from the data below, differs from the values found in Table 5.
d. A: 7.02, - 6.55, - 4.53; 4.00; 3.48; 3.39, 3.21.
PRI me R 8. As the raw material used, gas oil having the following
 Properties: 5 I
0
Density at 15/4 ° C, Stp Pour point, ° C Kinematic viscosity at 98.9 ° C, cSt
0.9122 25.0
5,801 66
Viscosity index
The original SFE is fed to the cube of the extrusion column and subjected to countercurrent extraction with furfural, which moves from above the extraction column. The extraction temperature is 90 ° C at the inlet of furfural and
0 at its output. Furfural is used in the amount of 1.2 hours of volume per volume part of the hydrocarbon feedstock. The overhead of the column is distilled to remove from the
him furfural and get raffinate with
yield 78.5 wt.%, having the following properties:
Density
at 15/4 s, Stp 0.8902
Pour point, ° C Kinematic viscosity at ge., CSt Viscosity index

The raffinate thus obtained is subjected to a dewaxing reaction using a β catalyst obtained in the leg in Example 1,
The reaction temperature is changed in accordance with the activity of the catalyst, so that the freezing temperature of the product is 270 ° C and is regulated as the desired temperature. 10 days after the start of the reaction, the reactive temperature reaches 335 ° C, and the pour point of the 270 ° C fraction is. The rate of temperature rise, necessary to maintain this temperature, is 5.0 ° C / day,
The yield and properties of the product are as follows:
Exit ,,, May,
C, -C ,, Fraction output
10.4
85.6 0.9072
.-10.0
6.132 81
С5-270 С, masl
Lraction output
 % wt.%
Density at 15/4 With,
Temperature
solidification, ° C
Kinematic
viscosity at 98.9 C, cSt
Index (; viscosity)
Example 9. The zeolites obtained in Example 2 were used for the dewaxing reaction as in Example 8 10 days after the start of the reaction, the reaction temperatures at which the 270 sec fraction had a pour point, the rate of temperature rise necessary to maintain this pour point, and the yield of the fraction were as follows ( Table 6).
Example 10. The catalyst prepared according to Example 5 was used for the raffinate dewaxing reaction obtained by furfural extraction as in Example 8. 10 days after the start of the reaction, the reaction temperature reached 396 ° C and the pour point of the 270 ° C fraction of the product was -10 ° C. The rate of rise of the reaction temperature is necessary to maintain this freezing temperature.
14212618
it is 6.9 C / day. The yield and properties of the product were as follows.
ten
15
20
25
-
thirty
40
Vpsod CJ-GX, mas%
5.1 15.3
79.6
0.9101 -10,
6,056 80
Fraction yield
Cs-2704 ,, wt.%
Exit of fraction 270 C,
wt.%
Density is 15/4 ° C. Pour point
Kinematic viscosity
at 98.9 ° C, cSt
Viscosity index
Example 11. The ZSM-5 zeolite catalyst obtained in Example 6 is used for the dewaxing reaction of a raffinate prepared by furfural as in Example 8.
10 days after the start of the reaction, the reaction temperature reaches 375 ° C and the freezing temperature of the 270 ° C fraction of the product is 10 ° C. The rate of rise of the reaction temperature, necessary to maintain this freezing temperature, is 8.1 C / day. The yield and properties of the obtained product were as follows:
Yield, wt.% 5.7
The output fraction Cr-270 ° C
wt.% 16.2
The output of the fraction 270 ° C 78,1
Density at
15/4 ° С, Stp
The freezing temperature is 35 nn,
. Kinematic viscosity at 98.9 C, cSt
0.9095 -10.0
6,028
80
50 ,
Viscosity index
Example 12. The catalyst and gas oil of example 1 is used to carry out a dewaxing reaction by controlling the temperature of the reaction in such a way that the freezing temperature of the fraction 165 from each feedstock to a predetermined value is reached. The conditions of the reaction and the results obtained 10 days after the start of the reaction are shown in Table 7.
Example 13. Using the catalyst of example 1 and heavy gas oil (TGO), having the properties indicated below, the dewaxing reaction is carried out under the following conditions:
Properties of heavy gas oil
Boiling point
(10-90% by volume), ° C 307-435
55
Pour point, ° C25 Daily content of sulfur, wt.% Total nitrogen content, wt.% 320 Carbon residue, wt.% 0.02 Reaction conditions Volumetric liquid feed rate, h - Pressure during the reaction, MPa
N / raw materials, nm / m. The freezing point of the fraction at 165 C, C
2.0
3.5 500
-15
1421261. 10
Example 15. The procedure of Example 1 is repeated using the following com- J positions, mol, as the reaction mixture:
SiOa / Al Gj 45 H O / SiOj20
OH / SiO, 0.17
, 0
10 (A - tartaric acid)
As a result of the reaction, a zeolite of the general formula is obtained:
15
10 days after the start of the reaction, the following results were obtained:
reactions, C348
Speed increase: temperature rises
/ reaction, With / day 6,3
Fraction yield
165 C, wt.%
20
25
82.7
EXAMPLE 14 Using the catalyst of Example 1 and heavy gas oil (TGO) 5 with the properties listed below, the dewaxing reaction is carried out under the conditions given below.
Properties of heavy gas oil Boiling point
thirty
1.02Na20.Al203- 34.8Si02-5.2 RjO,
which provides for the adsorption of mesitylene to 1.8% by weight. Studies of the resulting zeolite by X-ray diffraction are presented in Table 7. The zeolite thus obtained is treated according to the method of Example 1 and is given a certain form for use as a catalyst.

In this case, the gas oil used in Example 1 is hydrodesulfurized using a Co-Mo type catalyst, whereby a feedstock having the following properties is obtained:
Boiling point
(10-90%), ° С
Pour point, ° С
Full content
215-355
-ten
(10-90% by volume) С
315-465
Pour point, s-32.5 Total sulfur content, wt.% .1.35 Full nitrogen content, pPA 540 Carbon residue, wt.% 0.03 Reaction conditions Volumetric feed rate for the reaction, 0, MPa3.5 Н2 / сфье, nm / m700 Pour point of fraction, С -20
60 days after the start of the reaction and 120 days after the start of the reaction, the following results were obtained:
Through Through

60 days 418 81.9
120 days 55 450 80.7
five
0
five
0
five
0
five
0
five
1.02Na20.Al203- 34.8Si02-5.2 RjO,
which provides for the adsorption of mesitylene to 1.8% by weight. Studies of the resulting zeolite by X-ray diffraction are presented in Table 7. The zeolite thus obtained is treated according to the method of Example 1 and is given a certain form for use as a catalyst.

In this case, the gas oil used in Example 1 is hydrodesulfurized using a Co-Mo type catalyst, whereby a feedstock having the following properties is obtained:
Boiling point
(10-90%), ° С
Pour point, ° С
Full content
sulfur, wt.%
Full content
nitrogen, ppm.
Carbon residue
wt.%
Using the original oil and catalyst mentioned above, the dewaxing reaction is carried out under the following conditions:
Reaction Conditions
Capacity feed rate
liquid raw materials, h
Holding pressure
reactions, MPa
N / raw, HMVM
Pour point
165 C fraction, s
10 days after the start of the reaction, the following results were obtained
Holding temperature
reaction, ° C
Speed increase
temperature increase
reaction, s / day
The output of the fraction 165 ° C
wt.%
215-355
-ten
0.05
35
Less than 0.01
2.0
35,500
-15
310
5.5
84.5
jl1
ep 16. Repeat method.
Prim
ku example 1 when using the reaction mixture having the following composition, mol:
SiOz / AljO 20
HjO / SiO-i25
OH- / Si020,15
A / A1gOz1,0
(A - tartaric acid)
As a result, a zeolite of the general formula was obtained:
1.01Na20-Al203 18.6Si02-3.6 HjO,
which ensures the adsorption of methyl, equal to 2.1 wt.%.
The research data of the obtained zeolite by the method of X-ray diffraction correspond to those presented in Table 2. The zeolite thus obtained is used according to the method of Example 1 and is given a certain shape for use as a catalyst.
The heavy gas oil used in Example 8 is hydrodesulfurized using a Co-Mo type catalyst to produce a starting oil with the following properties:
Boiling point

(10-90 vol.%), C Pour temperature, ° С Total sulfur content, wt.% Full content
285-431
-22,5
0.1
150
0.01
The carbon residue, wt.%
Using the starting material described above and the catalyst, the dewaxing reaction is carried out with the following conditions:
Volumetric feed rate liquid,, 0
The pressure during the reaction, MPa 35 H7 / raw materials, HMVM 500 The pour point fraction
165 С, ° С
-15
10 days after the start of the reaction, the following results are obtained: Reaction temperature, ° C 327 Increase in the rate of reaction temperature. C / day 4,5
0
five
five
about
0
Fraction yield
163 ° C% wt.% 83.5
EXAMPLE 17 The catalyst used in Example 1 is used. As a syf, a raffinate fraction obtained by deasphalting with propane and extraction of residual oil with furfural after vacuum distillation is used. The original oil has the following properties. The de-waxing reaction is carried out under the conditions below.
Oil properties
Specific gravity 15/4 from 0.8941
Kinematic
viscosity at 98.9 ° C,
cSt23,15
Carbon residue
wt.% 0,62
Pour point, c40.
Reaction Conditions
Bulk liquid
liquid feed
raw materials,, 8
Pressure at the reaction, MPa3,5
Ng / sfye, nm VM 500
Pour point
165 С, ° С-10
10 days after the start of the reaction, the reaction temperature is
constitutes
and the yield of the fraction 165 C is 78.3 wt.%.

权利要求:
Claims (1)
[1]
Invention Formula
. 1. A method for dewaxing carbohydrate fractions, 10-90% by volume of which boil in the range of 215-490 ° C, or a hydrocarbon fraction subjected to selective purification, or a vacuum residue subjected to sequential defaltizing with propane and selective purification by contacting the feedstock with hydrogen in the presence of a zeolite catalyst at 263-450 ° C, a pressure of 1.0-7.0 MPa, a bulk flow rate of 0.5 to 4.0, the ratio of hydrogen to raw material is 100-1000 nm / m to obtain the desired product, characterized by that, in order to get out the target of product as kataizatora zeolite of formula (1 ± 0,2) NaaO-A j Oj- 18,6-34,8) Sip, j, (3,6-5,2),
Reaction temperature, s
The rate of recovery of the reactionary temperatureMetal component
Reaction temperature, C 263
Rate of reaction temperature rise, ° С / day
1.9
165 C, mas 84,4
fractions
1.5
Table3
344
341
336337
Table4 PtPdNi
263
1.9
84.4
286
3.8 86.4
283
2.9 86.9
1.9 1.8
1L
tt and V to o) H
Reaction temperature, ° С 347 Recovery rate of reaction343
338
338
curing fraction 165 ° C% s
Reaction temperature, with
The output of the fraction 165 ° C., Wt.%
Table
-20 -20 -20 -20 -20 O
-thirty
351 329 326 330 325 309 341
86.3 85.8 86.7 85.7 86.5 93.1 82.6

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同族专利:

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公开号 | 公开日

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KR840007746A|1984-12-10|

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AU2371284A|1984-08-16|

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DD223162A5|1985-06-05|

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EP0119709B2|1997-01-29|

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AU569055B2|1988-01-21|

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EP0119709B1|1988-11-02|

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EP0119709A3|1986-01-29|

引用文献:

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法律状态:

优先权:

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申请号 | 申请日 | 专利标题

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JP58019629A|JPS6218595B2|1983-02-10|1983-02-10|

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JP6068283A|JPS59187089A|1983-04-08|1983-04-08|Preparation of base oil for lubricant|

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