Method of preparing palladium catalyst for hydrofining of hydrocarbon fractions to remove unsaturated hydrocarbons

FIELD: petrochemical synthesis catalysts.

SUBSTANCE: invention discloses a method for preparation of palladium catalyst comprising impregnation of alumina carrier with palladium chloride solution in presence of aqueous hydrochloric acid, treatment with reducing agent (hydrogen), washing with water, and drying, said carrier being preliminarily decoked exhausted catalyst containing alumina and group I and/or II, and/or VI, and/or VIII metals and subjected to washing with aqueous hydrochloric or nitric acid and then with water. Exhausted ethylene oxide production catalyst or methylphenylcarbinol dehydration catalysts can also be suitably used.

EFFECT: increased selectivity and activity of catalyst.

2 cl, 2 tbl, 21 ex

 

The invention relates to petrochemical synthesis and can be used to obtain catalysts for purification of hydrocarbon fractions from unsaturated hydrocarbons by hydrogenation.

A method of obtaining palladium catalyst for selective hydrogenation of acetylenes and dienes for the purification of olefins by impregnation of the carrier with clean solvent, and then the palladium salt solution, followed by drying and restoration. As media use γ-aluminum oxide containing zinc aluminates, magnesium and calcium, and as a solvent using water or toluene, or benzene, or acetone (RF Patent No. 1359961, IPC 01 J 37/02, publ. 20.08.99).

The catalyst obtained in the described manner, is characterized by insufficiently high selectivity in the reaction of hydrogenation of acetylene in the stream with ethylene.

A known method of producing catalyst for selective hydrogenation of acetylenic hydrocarbons in ethylene by impregnation γ-aluminum oxide with a solution of palladium chloride in concentrated hydrochloric acid at a mass ratio of PdCl2:Al2O31:9, 10-12 hours, drying at 120°With the processing solution of allyl alcohol in an organic solvent and annealing in vacuum at 200°C for three hours. The finished catalyst contains 3% of the mass. palladium (Sladkov the TA.., Galicia N.N., Besterberg VA /Kinetics and catalysis, 1986, .XXVII, issue 2, str).

The activity and selectivity of the catalyst obtained in this way is not high enough in the reaction of hydrogenation of acetylene in a mixture with ethylene, namely the hydrogenation of a mixture of C2H2and C2H4in the ratio of 1:100 at 70°and a pressure of 1 ATM, loss of ethylene due to its hydrogenation to ethane is 5%, and the residual content of acetylene - 0,3%.

Closest to the proposed invention is a method of producing catalyst for selective hydrogenation of acetylene and diene hydrocarbons (RF Patent No. 2118909, IPC601 J 37/02, publ. 20.09.98). Upon receipt of the catalyst carrier - α-aluminum oxide with a specific surface area of 2-40 m2/g or silica gel impregnated with a solution of palladium chloride in the presence of 1-4% of the mass. hydrochloric acid or a solution of ammonium complex of palladium in the palladium content of 0.03-0.30% of mass., maintain and process allyl alcohol or ZIOC scientists, washed with distilled water and dried.

The disadvantage of this method is not sufficiently high stability of the catalyst activity and selectivity.

The task of the invention to provide a catalyst having a high selectivity and activity when cleaning the hydrogenation of hydrocarbon fractions from opredelnnyh hydrocarbons.

To solve this problem is proposed a method of obtaining a palladium catalyst for the purification of hydrocarbon fractions from unsaturated hydrocarbons by hydrogenation, including impregnation aluminiumoxide carrier with a solution of palladium chloride in the presence of hydrochloric acid, the processing of reducing agent is hydrogen, washing with water and drying, the media used previously exempt from coke exhaust catalyst containing alumina and metals I and/or II and/or VI and/or VIII groups of the Periodic system, subjected to washing with an aqueous solution of hydrochloric or nitric acid, and then water.

As spent catalyst containing alumina and metals I and/or II and/or VI and/or VIII groups of the Periodic system may be used in the spent catalyst in the process of obtaining ethylene oxide or exhaust catalyst dehydration methylphenylcarbinol (IFC).

As the spent catalyst can be used, for example, the catalyst of the process of obtaining ethylene oxide, meets the requirements of THE 2175-123-00203335-2000 “Catalyst for the oxidation of ethylene “ETOX-111 or THE 2175-105-00203335-2000 “Catalyst for the oxidation of ethylene “ETOX-111, or the catalyst of the process of dehydration of methylphenylcarbinol, for example, correspond with the relevant requirements of GOST 8136-85 “active aluminium Oxide”.

The spent catalyst containing alumina and metals I and/or II and/or VI and/or VIII groups of the Periodic system, pre-release from coke by burning in air flow with a gradual increase in temperature up to 550°and holding at that temperature until the absence of CO and CO2the content of which are determined by the chromatographic method of analysis, washed with an aqueous solution of hydrochloric or nitric acid, water and impregnated with a solution of palladium chloride (0.003 to 0.15% of the mass. Pd based on the content in the catalyst) in the presence of 0.1 G. of hydrochloric acid. The carrier impregnated with a solution of palladium chloride can be carried out at different pH of the impregnating solution, using as the alkaline agent is KOH or NaOH. After impregnation the catalyst is reactivated by hydrogen at a temperature not exceeding 150°C, and then washed with water and dried.

The resulting catalyst was tested in the cleaning process of the hydrogenation of various hydrocarbon fractions from unsaturated hydrocarbons.

Implementation of the proposed method of obtaining a palladium catalyst and its tests are illustrated in the following examples.

Example 1

10 g of spent catalyst of the process of obtaining ethylene oxide in the form of spherical beads with a size of 4-5 mm, previously exempt from the Ochs and containing α -aluminium oxide and metals Ag, CA, BA, CR, Fe and Ni, respectively I, II, VI, and VIII groups of the Periodic table, immersed in 10 ml of 10%nitric acid solution, stirred and poured. Then washed three times with distilled water, soaked in 10 ml of a solution containing 0.025 g of PdCl20.1 N. the Hcl solution, in a water bath at a temperature of 60-100°With, then restore hydrogen, washed with distilled water to a pH of 6-8 and dried at a temperature of 110-120°C. the results of the experiment are shown in table 1.

Before the test of the obtained catalyst once again hold its activation by hydrogen at temperatures not exceeding 150°C. Hydrogenation of ethane-ethylene fraction is carried out at a temperature of 30°C, a pressure of 1.8 MPa, the space velocity of the feedstock 2500 h-1, the volumetric ratio of hydrogen: acetylene, equal to 4:1. The results of the experiment are shown in table 2.

Example 2

The catalyst was prepared as described in example 1, but the spent media was washed with 10 ml of 10%aqueous solution NGO3then washed three times with distilled water and immersed in 10 ml of impregnating solution containing 0.025 g of PdCl20.1 N. the solution of Hcl, with bringing the pH of the impregnation solution to 10 by adding 1 n NaOH solution. The results of the experiment are shown in table 1.

Testing of the catalyst is carried out as described in point is the iMER 1. Hydrogenation of ethane-ethylene fraction is carried out at 33°C, pressure of 1.0 MPa, space velocity of 2000 h-1, the volumetric ratio of hydrogen: acetylene, equal to 4:1. The results are given in table 2.

Example 3

The catalyst was prepared as described in example 1, but the spent media was washed with 2%Hcl solution. The results of the experiment are shown in table 1.

Testing of the catalyst is carried out as described in example 1. Hydrogenation of ethane-ethylene fraction is carried out at a temperature of 35°C, pressure of 1.5 MPa, space velocity of 1000 h-1, the volumetric ratio of hydrogen: acetylene, equal to 4:1. The results are given in table 2.

Example 4

The catalyst was prepared as described in example 3, but in the impregnating solution add NaOH in sufficient quantity to bring the pH of the solution to 12. The results of the experiment are shown in table 1.

Testing of the catalyst is carried out as described in example 1. Hydrogenation of ethane-ethylene fraction is carried out at a temperature of 38°C, a pressure of 1.8 MPa, flow rate 3000 h-1, the volumetric ratio of hydrogen:acetylene, equal to 4:1. The results are given in table 2.

Example 5

The catalyst was prepared as described in example 2, but as the alkaline agent using 1 n KOH solution. The results of the experiment are shown in table 1.

spymania catalyst spend the same way as described in example 1. The results are given in table 2.

Example 6

The catalyst was prepared as described in example 1, but the content of PdCl2in the impregnating solution is to 0.005, the results of the experiment are shown in table 1.

Testing of the catalyst is carried out as described in example 1, the results are given in table 2.

Example 7

The catalyst was prepared as described in example 1, but as the media use the spent catalyst dehydration IFC, containing γ-alumina and metals Na, Mo, respectively I and VI groups of the Periodic system, previously exempt from coke. The results of the experiment are shown in table 1.

Testing of the catalyst is carried out as described in example 1. The results are given in table 2.

Example 8

The catalyst was prepared as described in example 1. The results of the experiment are shown in table 1.

Testing of the catalyst is carried out in the cleaning process from acetylene and diene hydrocarbons propane-propylene fraction of the following composition, % by vol.: C3H8- 4,56; C3H6- 92,04; C3H4(methylacetylene) - 2,24; C3H4(PROPADIENE) is 1.16. The hydrogenation is carried out at a temperature of 45°C, pressure of 2.0 MPa, space velocity of 2000 h-1, a volume ratio of bodoro is:methylacetylene+PROPADIENE, equal (1.8-2.4m):1. The composition of the propane-propylene fraction after Hydrotreating, % vol.: With3H8- 5,7596; C3H6- 94,24; C3H4(methylacetylene) - OTS.; With3H4(PROPADIENE) -0,0004. The selectivity of the catalyst was: 100% methylacetylene and of 99.97% PROPADIENE.

Example 9

The catalyst was prepared as described in example 2. The results of the experiment are shown in table 1.

Testing of the catalyst is carried out in the cleaning process by hydrogenation With6-C8-fraction at a temperature of 60°C, a pressure of 4.0 MPa, flow rate 1 hour-1, the volumetric ratio of hydrogen:hydrocarbon fraction equal to 100:1. In the Hydrotreating bromine number decreased from 74 to 18.2 SHG/100 g, the diene number - from 20.2 to 1.8 J/100 g

Example 10

10 g of spent catalyst of the process of obtaining ethylene oxide in the form of spherical beads with a size of 4-5 mm, previously exempt from coke by burning in air flow with a gradual increase in temperature up to 550°and holding at that temperature until the absence of CO and CO2that has α-alumina and metals Ag and CA, respectively in groups I and II of the Periodic table, immersed in 10 ml of 10%nitric acid solution, stirred and poured. Then washed three times with distilled water and immersed in 10 ml of impregnating solution containing 0.025 g of PdCl 20.1 N. the solution of Hcl to bring the pH of the impregnating solution to 10 by adding 1 n NaOH solution. The impregnation is conducted in a water bath at a temperature of 60-100°With, then restore hydrogen, washed with distilled water to a pH of 6-8 and dried at a temperature of 110-120°C. the results of the experiment are shown in table 1.

Before the test of the obtained catalyst once again hold its activation by hydrogen at temperatures not exceeding 150°C. Hydrogenation of ethane-ethylene fraction is carried out at a temperature of 30°C, a pressure of 1.8 MPa, the space velocity of the feedstock 2500 h-1, the volumetric ratio of hydrogen: acetylene, equal to 4:1. The results of the experiment are shown in table 2.

Example 11

The catalyst was prepared as described in example 10, but as the media use the spent catalyst receiving α-ethylene oxide containing aluminum oxide and a metal of group II VA. The results of the experiment are shown in table 1.

Testing of the catalyst is carried out as described in example 10. The results are given in table 2.

Example 12

The catalyst was prepared as described in example 10, but as the media use the spent catalyst receiving α-ethylene oxide containing aluminum oxide and metals II, VI and VIII groups Ia, Mo and Ni, respectively. The results are shown in the table is 1.

Testing of the catalyst is carried out as described in example 10. The results are given in table 2.

Example 13

The catalyst was prepared as described in example 10, but as media use exhaust catalyst dehydration methylphenylcarbinol (IFC), containing γ-aluminum oxide and the metal of group VI - Mo. The results of the experiment are shown in table 1.

Testing of the catalyst is carried out as described in example 10. The results are given in table 2.

Example 14

The catalyst was prepared as described in example 10, but as the media use the spent catalyst in the process of obtaining ethylene oxide, containing α-aluminum oxide and the metal of group VIII - Ni. An impregnating solution containing 0,058 g of PdCl2. The results of the experiment are shown in table 1.

Testing of the catalyst is carried out as described in example 9. In the Hydrotreating bromine number6-C8fraction decreased from 74 to 19.1 g Br/100 g, a diene number - from 20.2 to 2.9 g 1/100,

Example 15

The catalyst was prepared as described in example 14, but the modifying component metals are Ag and Ni, respectively, I and VIII groups of the Periodic system. pH of the impregnating solution was adjusted to 12.0. The results of the experiment are shown in table 1.

Testing of the catalyst spend the AK, as described in example 9. In the Hydrotreating bromine number6-C8fraction decreased from 74 to 18.0 g Br/100 g, a diene number - from 20.2 to 2.9 g 1/100,

Example 16

The catalyst was prepared as described in example 10, but as the media use the spent catalyst in the process of obtaining ethylene oxide, containing α-alumina and metals II and VIII group - CA and Ni, respectively. The results of the experiment are shown in table 1.

Testing of the catalyst is carried out as described in example 8. The composition of the propane-propylene fraction after Hydrotreating, % vol.: C3H8-5,21; C3H6- 94,7891; C3H4(methylacetylene) - OTS.; With3H4(PROPADIENE) -0,0009. The selectivity of the catalyst was: 100% methylacetylene and 99,92%.

Example 17

The catalyst was prepared as described in example 10, but as media use exhaust catalyst dehydration methylphenylcarbinol containing γ-alumina and metals VI and VIII groups of the Periodic system of Mendeleev - Mo and Fe, respectively. The results of the experiment are shown in table 1.

Testing of the catalyst is carried out as described in example 1. The results of the experiment are shown in table 2.

Example 18

The catalyst was prepared as described in example 10, but as media use exhaust cat is the lyst process of dehydration of methylphenylcarbinol (IFC), containing γ-alumina and metals VA and Mo, respectively II and group VI of the Periodic table. The results of the experiment are shown in table 1.

Testing of the catalyst is carried out as described in example 1. The results of the experiment are shown in table 2.

Example 19

The catalyst was prepared as described in example 10, but as the media use the spent catalyst receiving of ethylene oxide, containing α-aluminum oxide and a metal of group II VA. The results of the experiment are shown in table 1.

Testing of the catalyst is carried out as described in example 10. The results of the experiment are shown in table 2.

Example 20

The catalyst was prepared as described in example 10, but as media use exhaust catalyst dehydration methylphenylcarbinol containing γ-alumina and metals Ag, W and Mo, respectively I, II and VI groups of the Periodic system. The results of the experiment are shown in table 1.

Testing of the catalyst is carried out as described in example 10. The results of the experiment are shown in table 2.

Example 21

The catalyst was prepared as described in example 10, but as the media use the spent catalyst in the process of obtaining ethylene oxide, containing α-alumina and metals Ag, Ba and Fe, respectively I, II, and VIII groups of the Periodic is eskay periodic system. The results of the experiment are shown in table 1.

Testing of the catalyst is carried out as described in example 10. The results of the experiment are shown in table 2.

As seen from the above examples, the proposed method allows to obtain the active palladium catalyst for selective hydrogenation of unsaturated hydrocarbons using waste in other processes catalysts. Exhaust catalysts that serve as the media already contain metals, modifying palladium catalyst, which allows not only to obtain a catalyst with high selectivity and activity, but also to reduce environmental pollution by reducing the export of spent catalysts for samoatel.

Table 1
No.View mediaThe content of Pd in the catalyst, % wt.Modifying metalsWash solutionImpregnating solutionpH of the impregnating solution
1The spent catalyst in the process of obtaining ethylene oxide0,15I, II, VI,

VIII group
10%PdCl21,02
  HNO3 of 0.1 n Hcl 
20,1510%PdCl210,0
  HNO3of 0.1 n Hcl 
   1 n NaOH 
30,152% HclPdCl21,02
   of 0.1 n Hcl 
40,15-<<-PdCl2to 12.0
   of 0.1 n Hcl 
   1 n NaOH 
50,1510%PdCl210,0
  HNO3of 0.1 n Hcl 
   1 Mr. COHN 
60,0110%PdCl21,02
  HNO3of 0.1 n Hcl 
7The spent catalyst of the process of dehydration were-carbinol0,10I, VI groups10%PdCl21,02
  HNO3of 0.1 n Hcl 
     
     
     
     
     
8The spent catalyst in the process of obtaining ethylene oxide0,15I, II, VI, VIII group10%PdCl21,02
  HNO3of 0.1 n Hcl 
     
90,3510%PdCl210,0
   HNO3of 0.1 n Hcl 
   1 n NaOH 
100,15I, II10% HNO3PdCl210,0
   of 0.1 n Hcl 
   1 n NaOH 

Continuation of table 1
No.View mediaThe content of Pd in the catalyst, % wt.Modifying metalsWash solutionImpregnating solutionthe pH of the impregnating solution
11The spent catalyst in the process of obtaining ethylene oxide0,15I10% HNO3PdCl2of 0.1 n Hcl 1 n NaOH10,0
120,15II, VI, VIII10% CME3PdCl2of 0.1 n Hcl 1 n NaOH10,0
13The spent catalyst dehydration IFC0,15VI10% HNO 3PdCl2of 0.1 n Hcl 1 n NaOH10,0
14The spent catalyst in the process of obtaining ethylene oxide0,35VIII10% CME3PdCl2of 0.1 n Hcl 1 n NaOH10,0
150,35I, VIII10% HNO3PdCl2of 0.1 n Hcl 1 n NaOHto 12.0
160,15II, VIII10% CME3PdCl2of 0.1 n Hcl 1 n NaOH10,0
17The spent catalyst of the process of dehydration were-carbinol0,15VI, VIII10% HNO3PdCl2of 0.1 n Hcl 1 n NaOH10,0
180,15II, VI10% NGO3PdCl2of 0.1 n Hcl 1 n NaOH10,0
19The spent catalyst in the process of obtaining ethylene oxide0.15II10% HNO3PdCl2of 0.1 n Hcl 1 n NaOH10,0

Modifying metals
Continuation of table 1
No.View mediaThe content of Pd in the catalyst, % wt.Wash solutionImpregnating solutionthe pH of the impregnating solution
20The spent catalyst of the process of dehydration were-carbinol0,10I, II, VI10% HNO3PdCl210,0
 groups of 0.1 n Hcl 
   1 n NaOH 
21The spent catalyst in the process of obtaining ethylene oxide0,10I, II, VIII10% NGO3PdCl2to 12.0
 groups of 0.1 n Hcl 
   1 n NaOH 

Table 2
# exampleContent, % mass.The selectivity of the catalyst, % (acetylene)
CH4With2H6With2H4With2 H2
Source ethane-ethylene fraction0,0624,4773,891,58 
10,0625,9274,01950,0005of 99.97
20,0625,0374,9100UTS.100
30,0625,7974,14970,0003of 99.98
40,0624,7875,1600UTS.100
50,0625,3774,5698is 0.000299,99
60,0625,0974,84960,0004of 99.97
70,0625,9973,9500UTS.100
100,0624,7475,2000OTC100
110,0625,9673,97940,0006of 99.96
120,0625,5274,41920,0008at 99.95
130,0626,0573,88890,0011 99,93
170,0625,3774,56910,000999,94
180,0625,7474,19960,0004of 99.97
190,0624,4975,44900,001099,94
200,0626,0573,88900,001099,93
210,0625,5274,41930,0007at 99.95

1. A method of obtaining a palladium catalyst for the purification of hydrocarbon fractions from unsaturated hydrocarbons by hydrogenation, including impregnation aluminiumoxide carrier with a solution of palladium chloride in the presence of hydrochloric acid, the processing of a reducing agent, washing with water and drying, characterized in that as the carrier used previously exempt from coke exhaust catalyst containing alumina and metals I and/or II and/or VI and/or VIII groups of the periodic system, subjected to washing with an aqueous solution of hydrochloric or nitric acid and then with water, and use as a reducing agent hydrogen.

2. The method according to claim 1, characterized in that as spent catalyst containing alumina and m is of Tallaght I, and/or II and/or VI and/or VIII groups of the periodic system, use the spent catalyst receiving ethylene oxide or exhaust catalyst dehydration methylphenylcarbinol.



 

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