CN109529920B - Supported titanium boride catalyst for light alkane isomerization and preparation method and using method thereof - Google Patents
Supported titanium boride catalyst for light alkane isomerization and preparation method and using method thereof Download PDFInfo
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- CN109529920B CN109529920B CN201811339876.3A CN201811339876A CN109529920B CN 109529920 B CN109529920 B CN 109529920B CN 201811339876 A CN201811339876 A CN 201811339876A CN 109529920 B CN109529920 B CN 109529920B
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/7049—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing rare earth elements, titanium, zirconium, hafnium, zinc, cadmium, mercury, gallium, indium, thallium, tin or lead
- B01J29/7057—Zeolite Beta
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C5/00—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
- C07C5/22—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by isomerisation
- C07C5/2206—Catalytic processes not covered by C07C5/23 - C07C5/31
- C07C5/222—Catalytic processes not covered by C07C5/23 - C07C5/31 with crystalline alumino-silicates, e.g. molecular sieves
Abstract
The invention provides a loaded titanium boride catalyst for light alkane isomerization as well as a preparation method and a using method thereof, belonging to the field of light alkane isomerization. Meanwhile, the catalyst has high activity, good stability and higher selectivity to isoparaffin. The technical scheme comprises a carrier, wherein the carrier consists of alumina and an H beta molecular sieve, and the weight ratio of the alumina to the H beta molecular sieve is 1:10-10: 1; and titanium boride, accounting for 1-30 wt% of the weight of the carrier. The method can be applied to the isomerization process of the light paraffin with the C5-C12.
Description
Technical Field
The invention belongs to the field of light paraffin isomerization, and particularly relates to a supported titanium boride catalyst for light paraffin isomerization as well as a preparation method and a use method thereof.
Background
Catalysts are a key issue for light paraffin isomerization technology. Currently, the light paraffin isomerization catalysts commonly used in industry are divided into two types, low-temperature catalysts and medium-temperature catalysts.
Low temperature isomerization catalysts in which a halogen (F or Cl) is added to the catalyst to lower the catalyst use temperature, such as the I-8 catalyst from UOP, the RD-291 catalyst from Engelhard, are low temperature catalysts having a reaction temperature of 115 ℃ to 150 ℃. The low-temperature catalyst has the advantages of low use temperature and high activity of catalyzing isomerization of the alkane. However, during the use of the catalyst, halogen is gradually lost along with the reaction, so that the activity of the catalyst is reduced, and the device is corroded. Halide is required to be continuously supplemented for maintaining the catalytic activity, but the method not only causes certain corrosion to equipment, but also causes pollution to the environment; meanwhile, the active components used in the catalyst are generally noble metals such as platinum and the like, and the preparation cost of the catalyst is high.
The commonly used intermediate-temperature isomerization catalyst is a noble metal dual-function catalyst represented by complete isomerization method series catalysts of American Shell oil company and United carbide company, and has the advantages of high activity, good selectivity, no halogen and the like, but the catalyst needs to be used under certain pressure and higher temperature by using H before use2The active components are reduced to be in a metal state for use, so that the operation is more complicated; in addition, the above-mentioned catalyst active component is mainly based on noble metals, and also adds no small burden on cost.
Therefore, how to provide a light alkane isomerization catalyst which does not contain halogen and precious metal, has low use temperature and does not need hydrogen pre-reduction before use is an important problem to be solved by the technical personnel in the field.
Disclosure of Invention
The invention provides a loaded titanium boride catalyst for light alkane isomerization and a preparation method and a using method thereof. Meanwhile, the catalyst has the advantages of high activity, good stability and good selectivity to isoparaffin.
In order to achieve the above object, the present invention provides a supported titanium boride catalyst for light paraffin isomerization, comprising the following components:
the carrier consists of alumina and an H beta molecular sieve, and the weight ratio of the alumina to the H beta molecular sieve is 1:10-10: 1; and
titanium boride, which accounts for 1-30 wt% of the weight of the carrier.
Preferably, the light alkane is a normal alkane having 5 to 12 carbon atoms.
Preferably, the catalyst has a particle size of 0.1mm to 1.0 mm.
The invention also provides a preparation method of the supported titanium boride catalyst for light alkane isomerization according to any one of the technical schemes, which comprises the following steps:
fully roasting the H beta molecular sieve at the temperature of 200-600 ℃, and uniformly mixing the roasted molecular sieve and alumina in proportion;
adding titanium boride, kneading, molding, and drying at 50-100 deg.C;
and grinding the dried material into particles, and then fully roasting the particles in a nitrogen atmosphere to obtain the titanium boride catalyst.
Preferably, the temperature at which the sufficient calcination is carried out under a nitrogen atmosphere is 100-400 ℃.
The invention also provides a method for using the supported titanium boride catalyst for light paraffin isomerization in any technical scheme, wherein the method comprises the following steps:
the reaction temperature is 230 ℃ and 350 ℃, the reaction pressure is 1.0-5.0MPa, the hydrogen-oil molar ratio is 1.0-6.0, and the mass space velocity is 0.5-3.0h-1。
Compared with the prior art, the invention has the advantages and positive effects that:
the titanium boride-loaded light alkane isomerization catalyst does not use noble metal or add halogen components, so that the cost of the catalyst is reduced, and the pollution to the environment is avoided. Meanwhile, the catalyst can be directly used when being used in an isomerization process, pre-hydrogenation reduction is not needed, the use temperature can be reduced to 230 ℃, side reactions in the isomerization process are greatly reduced, and the yield of the isoparaffin is improved. Tests prove that when the catalyst is used for catalyzing light alkane reaction, the activity is higher in the temperature range, and the isoparaffin selectivity and the catalyst stability are also better; in addition, the preparation process of the light paraffin isomerization catalyst loaded with titanium boride is simple and safe, high temperature and hydrogen are not needed, and the preparation cost of the catalyst can be greatly reduced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention provides a supported titanium boride catalyst for light alkane isomerization, which comprises the following components: the carrier consists of alumina and an H beta molecular sieve, and the weight ratio of the alumina to the H beta molecular sieve is 1:10-10: 1; and titanium boride, accounting for 1-30 wt% of the weight of the carrier.
The titanium boride catalyst provided by the above embodiment is composed of a carrier and titanium boride, wherein the carrier is composed of alumina and an H β molecular sieve, the H β molecular sieve has suitable acid strength, acid distribution and pore structure, and provides a good acid center and reaction site for normal paraffin isomerization, and simultaneously, alumina in the carrier provides a mesoporous structure for reaction, which is beneficial to rapid diffusion of raw materials and products; in addition, the catalyst is easier to form by adding alumina as a binder. It is understood that the weight ratio of the two can also be 1:9, 2:8, 3:7, 4:6, 5:5, 6:4, 7:3, 8:2, 9:1, etc., and the desired catalyst can be prepared by one skilled in the art within the above ranges. In addition, in the embodiment, titanium boride is used in combination with the carrier, which has the main advantages that titanium boride has very high abrasion resistance and certain physical and chemical stability, and can maintain good physicochemical properties under different reaction conditions, and when the titanium boride is used as an active component to prepare a catalyst, the catalyst has good abrasion resistance, catalytic stability and regeneration performance. Meanwhile, the titanium atom is easy to interact with hydrocarbons because the valence layer d orbital electron is in an unfilled state, and has good catalytic selectivity when being used as a metal hydrogenation/dehydrogenation center. Titanium boride and a carrier are organically combined to prepare the catalyst which has good stability, high activity and good selectivity to isoparaffin. In addition, the catalyst of the embodiment does not use noble metal, and does not need to add halogen components, thereby not only reducing the cost of the catalyst, but also avoiding the pollution to the environment, and being capable of carrying out high-efficiency isomerization on the normal paraffin containing 5-12 carbon atoms.
In a preferred embodiment, the catalyst has a particle size of 0.1mm to 1.0 mm. The particle size of the catalyst is limited in the embodiment, so that the phenomenon that the particles are too large, the internal diffusion effect of the catalyst is increased, the activity of the catalyst is reduced, and the conversion rate of raw materials is influenced is avoided; or the particles are too small, increasing the pressure drop in the reactor and plugging the catalyst bed.
An embodiment of the present invention also provides a method for preparing a supported titanium boride catalyst for light paraffin isomerization according to any one of the above embodiments, including:
fully roasting the H beta molecular sieve at the temperature of 200-600 ℃, and uniformly mixing the roasted molecular sieve and alumina in proportion; adding titanium boride, kneading, molding, and drying at 50-100 deg.C; grinding the dried material into particles, and then fully roasting the particles at the temperature of 100-400 ℃ in the nitrogen atmosphere to prepare the supported titanium boride catalyst.
The temperature for roasting the H beta molecular sieve in the above embodiment may also be 250, 300, 350, 400, 450, 500, 550 ℃ or any temperature value within the above range, the roasting time may vary from 1 to 5 hours, and those skilled in the art can adjust the roasting time according to the actual reaction conditions; the drying temperature is not particularly limited, and may be 60, 70, 80, 90 ℃ or any temperature value within the above range, based on the actual drying degree; similarly, the firing under a nitrogen atmosphere is not particularly limited, and the firing is carried out at 100, 200, 300, 400 ℃ or any temperature value within the above range, to the extent that the firing is sufficient.
Embodiments of the present invention also provide a method of using the supported titanium boride catalyst for light paraffin isomerization according to any one of the embodiments above for light paraffin isomerization under the following conditions: the reaction temperature is 230 ℃ and 350 ℃, the reaction pressure is 1.0-5.0MPa, the hydrogen-oil molar ratio is 1.0-6.0, and the mass space velocity is 0.5-3.0h-1. It should be noted that the catalyst described in this example can be directly used when used in an isomerization process, without pre-hydrogenation reduction, and the use temperature can be reduced to 230 ℃, which can greatly reduce the side reactions occurring in the isomerization process and improve the yield of isoparaffin. Wherein, the reaction temperature can be 250, 260, 280, 300, 320, 340 ℃ or any temperature value in the range, the reaction pressure can be 2.0, 3.0, 4.0MPa or any pressure value in the range, the hydrogen-oil molar ratio can be 2.0, 3.0, 4.0, 5.0 or any molar ratio in the range, and the mass space velocity can be 1.0, 1.5, 2.0, 2.5h-1Or any value within the above range.
In order to demonstrate the suitability of the catalysts of the invention for the isomerization of n-alkanes from C5 to C12, examples 1 to 13 are described in detail below, wherein examples 1 to 6 are the isomerization of n-alkanes from C5 to C6 using n-pentane/n-hexane as starting material and examples 7 to 12 are the isomerization of n-alkanes from C7 to C12 using n-heptane, n-octane, n-nonane, n-decane, n-undecane and n-dodecane, respectively.
Example 1
The light paraffin isomerization catalyst loaded with titanium boride in the embodiment comprises a carrier and titanium boride accounting for 5 wt% of the weight of the carrier, wherein the carrier consists of alumina and an H beta molecular sieve, and the weight ratio of the alumina to the H beta molecular sieve is 1: 3.
The preparation method of the titanium boride-loaded light paraffin isomerization catalyst in the embodiment comprises the following steps:
roasting the H beta molecular sieve at 500 ℃ for 4H, uniformly mixing 1 part by weight of alumina powder and 3 parts by weight of roasted H beta molecular sieve, adding 0.2 part by weight of titanium boride, uniformly mixing, extruding and molding, drying at 50 ℃, grinding into particles with the particle size of 0.45mm, and roasting the particles at 300 ℃ for 2H in a nitrogen atmosphere to prepare the catalyst A1.
The catalyst A1 prepared in the example has the reaction temperature of 300 ℃, the reaction pressure of 1.0MPa, the hydrogen-oil molar ratio of 2.0 and the mass space velocity of 1.0h-1Under conditions to catalyze the isomerization reaction of C5/C6.
Example 2
The light paraffin isomerization catalyst loaded with titanium boride in the embodiment comprises a carrier and titanium boride accounting for 10 wt% of the weight of the carrier, wherein the carrier consists of alumina and an H beta molecular sieve, and the weight ratio of the alumina to the H beta molecular sieve is 1: 10.
The preparation method of the titanium boride-loaded light paraffin isomerization catalyst in the embodiment comprises the following steps:
roasting the H beta molecular sieve at 300 ℃ for 6H, then uniformly mixing 1 part by weight of alumina powder and 10 parts by weight of roasted H beta molecular sieve, adding 1.1 part by weight of titanium boride, uniformly mixing, extruding and molding, drying at 80 ℃, grinding into particles with the particle size of 0.8mm, and roasting the particles at 350 ℃ for 0.8H in a nitrogen atmosphere to prepare the catalyst A2.
The catalyst A2 prepared in the example has the reaction temperature of 280 ℃, the reaction pressure of 2.0MPa, the hydrogen-oil molar ratio of 3.0 and the mass space velocity of 2.0h-1Under conditions to catalyze the isomerization reaction of C5/C6.
Example 3
The light paraffin isomerization catalyst loaded with titanium boride in the embodiment comprises a carrier and titanium boride accounting for 15 wt% of the weight of the carrier, wherein the carrier consists of alumina and an H beta molecular sieve, and the weight ratio of the alumina to the H beta molecular sieve is 5: 1.
The preparation method of the titanium boride-loaded light paraffin isomerization catalyst in the embodiment comprises the following steps:
roasting the H beta molecular sieve at 400 ℃ for 5 hours, then uniformly mixing 5 parts by weight of alumina powder and 1 part by weight of roasted H beta molecular sieve, adding 0.9 part by weight of titanium boride, uniformly mixing, extruding and molding, drying at 100 ℃, grinding into particles with the particle size of 1mm, and roasting the particles at 280 ℃ for 2.2 hours in a nitrogen atmosphere to prepare the catalyst A3.
The catalyst A3 prepared in the example has the reaction temperature of 320 ℃, the reaction pressure of 3.0MPa, the hydrogen-oil molar ratio of 4.0 and the mass space velocity of 3h-1Under conditions to catalyze the isomerization reaction of C5/C6.
Example 4
The light paraffin isomerization catalyst loaded with titanium boride in the embodiment comprises a carrier and the titanium boride accounting for 20 wt% of the weight of the carrier, wherein the carrier consists of alumina and an H beta molecular sieve, and the weight ratio of the alumina to the H beta molecular sieve is 10: 1.
The preparation method of the titanium boride-loaded light paraffin isomerization catalyst in the embodiment comprises the following steps:
roasting the H beta molecular sieve at 600 ℃ for 3H, then uniformly mixing 10 parts by weight of alumina powder and 1 part by weight of roasted H beta molecular sieve, adding 2.2 parts by weight of titanium boride, uniformly mixing, extruding into strips, forming, drying at 120 ℃, grinding into particles with the particle size of 0.4mm, and roasting the particles at 200 ℃ for 3H in a nitrogen atmosphere to prepare the catalyst A4.
The catalyst A4 prepared in the example has the reaction temperature of 250 ℃, the reaction pressure of 4.0MPa, the hydrogen-oil molar ratio of 5.0 and the mass space velocity of 1h-1Under conditions to catalyze the isomerization reaction of C5/C6.
Example 5
The light paraffin isomerization catalyst loaded with titanium boride in the embodiment comprises a carrier and titanium boride accounting for 1 wt% of the weight of the carrier, wherein the carrier consists of alumina and an H beta molecular sieve, and the weight ratio of the alumina to the H beta molecular sieve is 1: 6.
The preparation method of the titanium boride-loaded light paraffin isomerization catalyst in the embodiment comprises the following steps:
roasting the H beta molecular sieve at 200 ℃ for 6.8H, uniformly mixing 1 part by weight of alumina powder and 6 parts by weight of roasted H beta molecular sieve, adding 0.07 part by weight of titanium boride, uniformly mixing, extruding into strips, forming, drying at 150 ℃, grinding into particles with the particle size of 0.2mm, and roasting the particles at 400 ℃ for 0.5H in a nitrogen atmosphere to prepare the catalyst A5.
The catalyst A5 prepared in the example has the reaction temperature of 230 ℃, the reaction pressure of 5.0MPa, the hydrogen-oil molar ratio of 1.0 and the mass space velocity of 2h-1Under conditions to catalyze the isomerization reaction of C5/C6.
Example 6
The light paraffin isomerization catalyst loaded with titanium boride in the embodiment comprises a carrier and titanium boride accounting for 30 wt% of the weight of the carrier, wherein the carrier consists of alumina and an H beta molecular sieve, and the weight ratio of the alumina to the H beta molecular sieve is 8: 1.
The preparation method of the titanium boride-loaded light paraffin isomerization catalyst in the embodiment comprises the following steps:
roasting the H beta molecular sieve at 350 ℃ for 3H, uniformly mixing 8 parts by weight of alumina powder and 1 part by weight of roasted H beta molecular sieve, adding 2.7 parts by weight of titanium boride, uniformly mixing, extruding into strips, forming, drying at 90 ℃, grinding into particles with the particle size of 0.1mm, and roasting the particles at 100 ℃ for 4H in a nitrogen atmosphere to prepare the catalyst A6.
The catalyst A6 prepared in the example has the reaction temperature of 350 ℃, the reaction pressure of 2.0MPa, the hydrogen-oil molar ratio of 6.0 and the mass space velocity of 0.5h-1Under conditions to catalyze the isomerization reaction of C5/C6.
Example 7
In the example, the catalyst A1 was reacted at 260 deg.C under 1.0MPa hydrogen-oil molar ratio of 3.0 and mass space velocity of 2.0h-1Under the conditions of (1) catalyzing the isomerization reaction of n-heptane.
Example 8
In the example, the catalyst A1 was reacted at 290 deg.C under 3.0MPa hydrogen-oil molar ratio of 3.0 and mass space velocity of 0.5h-1The catalytic n-octane isomerization reaction is carried out under the conditions of (1).
Example 9
In the example, the catalyst A1 was reacted at 310 deg.C under 2.0MPa hydrogen-oil molar ratio of 1.0 and mass space velocity of 2.0h-1Under the conditions of (1) catalyzing the isomerization reaction of the n-nonane.
Example 10
In the example, the catalyst A1 was reacted at 330 deg.C under 4.0MPa hydrogen-oil molar ratio of 4.0 and a mass space velocity of 1.0h-1Under the conditions of (1) catalyzing the isomerization reaction of the n-decane.
Example 11
In the example, the catalyst A1 was reacted at 350 deg.C under 2.0MPa at 5.0 mol ratio of hydrogen to oil and 3.0 hr of space velocity-1Under the conditions of (1) catalyzing the isomerization reaction of the n-undecane.
Example 12
In the example, the catalyst A1 was reacted at a reaction temperature of 280 deg.C and a reaction pressure of 1.0MPa, a hydrogen-oil molar ratio of 2.0 and a mass space velocity of 1.0h-1Under conditions to catalyze the isomerization of n-dodecane.
Performance testing
The catalysts of examples 1-12 above were evaluated for their ability to catalyze the isomerization of n-paraffins, and the reaction products were analyzed by Agilent6820 gas chromatography. Wherein, the raw material conversion rate X, the isoparaffin yield Y and the product selectivity S are calculated according to the formula shown in (1-1), (1-2) and (1-3):
Y＝[B]product of (1-2)
S＝Y/X×100％ (1-3)
In the formula:
[A]raw materialsIs the proportion of the normal alkane peak area in the raw material,%;
[A]product ofThe percentage of the normal paraffin peak area in the product is percent;
[B]product ofFor all differences in the productThe ratio of the sum of the peak areas of the constituent alkanes is percent.
The results of the conversion of the raw material X, the yield of isoparaffin Y, and the selectivity of the product S in the case of catalyzing the isomerization of n-pentane in examples 1 to 12 are shown in Table 1:
TABLE 1 conversion of raw materials, isoparaffin yield, product selectivity for catalyzing isomerization of n-paraffins
Comparative example
The carriers of the catalyst in example 1 are respectively replaced by mordenite molecular sieves and Y molecular sieves to prepare catalysts B1 and B2, and the preparation process specifically comprises the following steps:
respectively drying the mordenite molecular sieve and the Y molecular sieve at 110 ℃ for 1h, respectively uniformly mixing 1 part by weight of alumina powder with 3 parts by weight of calcined mordenite molecular sieve and Y molecular sieve, respectively adding 0.2 part by weight of titanium boride, uniformly mixing, extruding into strips, drying at 50 ℃, grinding into particles with the particle size of 0.45mm, and calcining the particles at 200 ℃ for 2h in a nitrogen atmosphere to respectively prepare catalysts B1 and B2.
Using n-pentane and n-hexane as raw materials, and respectively carrying out catalyst catalytic activity evaluation on catalysts B1 and B2 under the same reaction conditions as those of example 1, namely, at the reaction temperature of 300 ℃, the reaction pressure of 2.0MPa, the hydrogen-oil molar ratio of 4.0 and the mass space velocity of 1.0h-1Under conditions to catalyze the isomerization reaction of C5/C6. Catalysts B1 and B2 catalyze the conversion rate X of raw materials, the yield Y of isoparaffin and the selectivity S of products as shown in Table 2.
TABLE 2 conversion of catalytic materials, isoparaffin yield, product selectivity of comparative example and example 1
From the results in table 2, it can be seen that the isomerization catalyst prepared by using the mordenite molecular sieve and the Y molecular sieve instead of the H β molecular sieve has a significantly lower normal paraffin conversion rate and a significantly lower isoparaffin yield than the titanium boride isomerization catalyst in example 1 of the present invention, and the active component and the carrier of the catalyst in the present invention have a more excellent catalytic effect than those in the prior art.
Claims (6)
1. The supported titanium boride catalyst for light alkane isomerization is characterized by comprising the following components:
the carrier consists of alumina and an H beta molecular sieve, and the weight ratio of the alumina to the H beta molecular sieve is 1:10-10: 1; and
titanium boride, which accounts for 1-30 wt% of the weight of the carrier.
2. The supported titanium boride catalyst for light paraffin isomerization according to claim 1 wherein the light paraffin is a normal paraffin containing 5 to 12 carbon atoms.
3. The supported titanium boride catalyst for light paraffin isomerization according to claim 1 or 2, wherein the particle size of the catalyst is 0.1mm to 1.0 mm.
4. The method of preparing a supported titanium boride catalyst for light paraffin isomerization according to any one of claims 1 to 3, comprising:
fully roasting the H beta molecular sieve at the temperature of 200-600 ℃, and uniformly mixing the roasted molecular sieve and alumina in proportion;
adding titanium boride, kneading, molding, and drying at 50-100 deg.C;
and grinding the dried material into particles, and then fully roasting the particles in a nitrogen atmosphere to obtain the titanium boride catalyst.
5. The method as set forth in claim 4, wherein the temperature for the sufficient calcination under the nitrogen atmosphere is 100-400 ℃.
6. The method of using the supported titanium boride catalyst for light paraffin isomerization according to any one of claims 1 to 3, characterized in that the light paraffin isomerization is carried out under the conditions:
the reaction temperature is 230 ℃ and 350 ℃, the reaction pressure is 1.0-5.0MPa, the hydrogen-oil molar ratio is 1.0-6.0, and the mass space velocity is 0.5-3.0h-1。
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