CN106334581B - N-alkane isomerization catalyst and preparation method thereof - Google Patents
N-alkane isomerization catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a normal paraffin isomerization catalyst, which comprises the following steps: (1) loading an active metal component platinum on an alumina carrier, and drying to obtain a first intermediate; (2) reducing the first intermediate obtained in the step (1) to obtain a second intermediate; (3) and (3) loading heteropoly acid on the second intermediate obtained in the step (2), and drying to obtain the catalyst. The invention also provides the normal paraffin isomerization catalyst prepared by the method. Compared with the normal paraffin isomerization catalyst in the prior art, the normal paraffin isomerization catalyst prepared by the method provided by the invention has better catalytic activity and isomerization product selectivity.
Description
Technical Field
The invention relates to the field of catalysts, in particular to an n-alkane isomerization catalyst and a preparation method thereof.
Background
High octane branched paraffins have been desirable gasoline components, while significant amounts of straight chain paraffins are present in crude oil. Therefore, it is important to convert a low octane linear paraffin into a high octane linear paraffin by an isomerization technique. Since normal paraffins are easily cracked upon isomerization, the yield of multi-branched paraffins, especially high octane paraffins, is reduced and the liquid yield is affected. The key point of catalyst development is to effectively control the generation of cracking products in the isomerization process and improve the selectivity of multi-branched isoparaffin.
CN100425583C discloses a preparation method of a paraffin isomerization catalyst, wherein the catalyst prepared by the method mainly contains inorganic carrier silica, metal platinum and chlorine and is mainly used for C4-C6 paraffin isomerization reaction.
CN1465436A discloses a catalyst for isomerization of alkane and its application, the catalyst contains 0.5-90% of heteropoly acid or heteropoly acid salt and 99.5-10% of inorganic substance, the inorganic substance is mainly carrier, but does not use VIII group noble metal. The catalyst is suitable for low-carbon alkane isomerization reaction, especially for normal butane isomerization reaction, but for higher-carbon alkane isomerization reaction, the selectivity and the yield of multi-branched alkane are lower.
CN102107142B discloses a C7-C10 alkane isomerization catalyst and a preparation method thereof, the catalyst comprises a composite carrier and platinum with the content of 0.05-3.0 mass percent calculated by taking the carrier as a reference, the composite carrier comprises 20-70 mass percent of MCM-41 molecular sieve, 10-35 mass percent of phosphotungstic acid and 10-50 mass percent of alumina. The invention disperses phosphotungstic acid with stronger acidity in pore channels of the mesoporous molecular sieve through impregnation, increases active sites and plays an acidic role, but the selectivity and the catalytic activity of the multi-branched isoparaffin of the catalyst can not meet the requirement of isomerization of normal paraffins.
Therefore, there is an urgent need to develop a catalyst having high catalytic activity and isomerization selectivity for normal paraffins.
Disclosure of Invention
The invention provides a preparation method of a catalyst, aiming at improving the catalytic activity and isomerization selectivity of the catalyst.
The invention aims to provide a preparation method of a normal paraffin isomerization catalyst, and the normal paraffin isomerization catalyst prepared by the method has higher catalytic activity and multi-branched chain isomerization selectivity.
The invention provides a preparation method of a normal paraffin isomerization catalyst, which comprises the following steps: (1) loading an active metal component platinum on an alumina carrier, and drying to obtain a first intermediate; (2) reducing the first intermediate obtained in the step (1) to obtain a second intermediate; (3) and (3) loading heteropoly acid on the second intermediate obtained in the step (2), and drying to obtain the catalyst.
The invention also provides the normal paraffin isomerization catalyst prepared by the method.
The method of the invention firstly loads active metal component platinum on an alumina carrier, and then loads heteropoly acid after reduction, and the prepared catalyst has higher catalytic activity and multi-branched chain isomerization selectivity when catalyzing normal paraffin isomerization.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The invention provides a preparation method of a normal paraffin isomerization catalyst, which comprises the following steps: (1) loading an active metal component platinum on an alumina carrier, and drying to obtain a first intermediate; (2) reducing the first intermediate obtained in the step (1) to obtain a second intermediate; (3) and (3) loading heteropoly acid on the second intermediate obtained in the step (2), and drying to obtain the catalyst.
In the method of the present invention, the method of supporting the platinum metal component on the alumina may employ an impregnation method. The impregnation method may be a saturated impregnation method or a supersaturated impregnation method, and a saturated impregnation method is preferable in the present invention, and for example, the alumina support may be impregnated with 70 to 150mL of an aqueous solution containing a platinum compound, wherein the platinum content is 0.14 to 20mg/mL, based on 100 parts by weight of the alumina support, and the impregnation time is preferably 1 to 12 hours. The platinum-containing compound may be at least one of chloroplatinic acid, tetraammineplatinum dichloride and hexaamminoplatinum tetrachloroplatinate, and is preferably chloroplatinic acid.
According to the method for preparing the normal paraffin isomerization catalyst, the platinum loading amount calculated by taking the dry-based alumina carrier as the reference in the catalyst is preferably 0.01-2.0 mass%, the heteropoly acid loading amount is 10-70 mass%, and more preferably, the platinum loading amount calculated by taking the dry-based alumina carrier in the catalyst is 0.1-1.3 mass%; the loading amount of the heteropoly acid is 30-70 mass%.
According to the preparation method of the normal paraffin isomerization catalyst, the alumina carrier can be alumina with various crystal phases, such as gamma-Al2O3、η-Al2O3、θ-Al2O3、δ-Al2O3And chi-Al2O3Preferably, the alumina carrier is gamma-Al2O3. The alumina support having the above crystal form can be obtained commercially, or can be obtained by molding and calcining an alumina precursor, and the alumina precursor is not particularly limited and may be at least one selected from the group consisting of alumina trihydrate, alumina monohydrate, and amorphous aluminum hydroxide, for example. The shape of the alumina carrier can be at least one selected from a sphere, a cylinder, a ring, a clover, a quadralobe, a honeycomb, a butterfly and the like.
According to the method for preparing the n-paraffin isomerization catalyst of the present invention, preferably, the obtained first intermediate is subjected to oxidation treatment before the reduction treatment in step (2). After the first intermediate is subjected to oxidation treatment, the ionic chloroplatinic acid radical is converted into platinum oxide, so that the platinum oxide is favorably and fully reduced to an active metal component platinum. The conditions of the oxidation treatment may include: the oxidation temperature is 100-550 ℃, and preferably 120-500 ℃; the oxidation time is 0.1 to 10 hours, preferably 1 to 8 hours; the volumetric space velocity of the oxidizing gas through the first intermediate is 5 to 1500 hours-1Preferably 30 to 1200 hours-1. The oxidizing gas may be oxygen and/or oxygen-containing nitrogen, preferably oxygen-containing nitrogen, such as air.
According to the method for preparing the n-paraffin isomerization catalyst, the alumina carrier is preferably soaked by ammonia water for pretreatment before the step (1), and then is dried and calcined. The alumina carrier is pretreated by ammonia water to adjust the surface property of the alumina, which is beneficial to the loading of active metal platinum components. The conditions of the pre-treatment may include: the concentration of ammonia water is 0.1-28 wt%, the treatment temperature is 30-250 deg.C, and the treatment time is 1-48 hr. Preferably, the conditions of the pretreatment include: the concentration of ammonia water is 3-20 wt%, the treatment temperature is 80-200 deg.C, and the treatment time is 1-24 hr. Preferably, the pretreatment is carried out under closed conditions, such as a closed impregnation vessel, which may be a closed reactor conventional in the art, such as a pressure-resistant stainless steel reaction vessel.
According to the preparation method of the normal paraffin isomerization catalyst, the roasting temperature of the pretreated alumina carrier can be 200-450 ℃, and the roasting time can be 0.5-10 hours.
According to the method for preparing the n-paraffin isomerization catalyst of the present invention, the drying conditions and method may be conventionally selected, and the present invention is not particularly limited, for example, the drying temperature may be 30 to 200 ℃, and the drying time may be 0.5 to 10 hours.
According to the method for preparing the n-paraffin isomerization catalyst of the present invention, in the step (2), the reduction treatment conditions may satisfy the platinum reduction conditions, and there is no particular limitation, for example, the reduction treatment conditions may include: the reduction temperature is 100-550 ℃, and preferably 200-500 ℃; the reduction time is 0.1 to 10 hours, preferably 1 to 8 hours; the volume space velocity of the reducing gas passing through the first intermediate is 5-1500 hours-1Preferably 30 to 1200 hours-1Wherein the reducing gas may be hydrogen.
According to the preparation method of the normal paraffin isomerization catalyst, in the step (3), the method for supporting the heteropoly acid on the second intermediate can adopt a supporting method which is well known by a person skilled in the art, and preferably adopts an impregnation method, namely, the heteropoly acid is prepared into an impregnation liquid, and then the second intermediate is impregnated by the impregnation liquid, wherein the heteropoly acid contained in the impregnation liquid is required to meet the requirement of supporting the heteropoly acid in the catalyst, for example, 70-150mL of phosphotungstic acid with the concentration of 71.4-467mg/mL can be adopted to impregnate for 1-12 hours relative to 100 parts by weight of alumina carrier.
According to the preparation method of the normal paraffin isomerization catalyst, the general formula of the heteropoly acid can be H8-n[AM12O40]Wherein A is P or Si, M is W or Mo, n is the valence state of A and the valence state is 4 or 5, preferably, the heteropoly acid comprises at least one of phosphotungstic acid, silicotungstic acid and phosphomolybdic acid.
According to the preparation method of the normal paraffin isomerization catalyst, the catalyst prepared by the method is suitable for normal paraffin isomerization, especially suitable for catalyzing isomerization of long-chain normal paraffin, preferably, the normal paraffin is C7-C8Of (a) is a normal alkane. In the invention, the catalyst of the invention is used for isomerizing normal paraffin to obtain the yield of multi-branched isoparaffin, wherein the multi-branched isoparaffin is isoparaffin with more than two branched chains in a carbon chain.
The catalyst prepared by the method of the invention catalyzes the isomerization reaction of normal paraffin under the hydrogen condition, and the hydrogen condition can comprise: the temperature is 100-300 ℃, the pressure is 0.1-3MPa, and the hydrogen/hydrocarbon molar ratio is (1-20): 1, the feed mass space velocity is 0.1-20 hours-1(ii) a Preferably, the hydrogen-contacting conditions include: the temperature is 150-: 1, the feed mass space velocity is 1-10 hours-1。
The invention also provides the normal paraffin isomerization catalyst prepared by the method.
The invention is further illustrated by the following examples, which are not intended to be limiting.
Example 1
10g of gamma-Al2O3Putting the mixture into a rotary evaporator, adding 15mL of chloroplatinic acid solution with the platinum content of 6.67mg/mL, soaking for 4 hours at 60 ℃, and performing rotary evaporation to obtain a first intermediate.
Loading the first intermediate into a reactor, and carrying out reduction treatment to obtain a second intermediate, wherein the reduction treatment conditions comprise: the volume space velocity of hydrogen is 1200 h-1The reduction temperature was 480 ℃ and the reduction time was 4 hours.
Then 15mL of 0.33g/mL aqueous solution of phosphotungstic acid is used for dipping the second intermediate for 2 hours at the temperature of 60 ℃, and the catalyst is obtained by rotary evaporation to dryness, and the composition of the catalyst is shown in Table 1.
Example 2
10g of eta-Al2O3Putting the mixture into a rotary evaporator, adding 8mL of chloroplatinic acid solution with the platinum content of 5.63mg/mL, soaking for 4 hours at 60 ℃, and performing rotary evaporation to obtain a first intermediate.
Loading the first intermediate into a reactor, and carrying out reduction treatment to obtain a second intermediate, wherein the reduction treatment conditions comprise: the volume space velocity of hydrogen is 30 hours-1And the reduction temperature is 200 ℃, and the reduction time is 8 hours, so as to obtain a second intermediate.
Then 8mL of 0.38g/mL aqueous solution of silicotungstic acid is used for dipping the second intermediate for 2 hours at the temperature of 60 ℃, and the catalyst is obtained by rotary evaporation to dryness, and the composition of the catalyst is shown in Table 1.
Example 3
10g of theta-Al2O3Putting the mixture into a rotary evaporator, adding 15mL of chloroplatinic acid solution with the platinum content of 2.33mg/mL, soaking for 4 hours at 80 ℃, and performing rotary evaporation to obtain a first intermediate.
Loading the first intermediate into a reactor, and carrying out reduction treatment to obtain a second intermediate, wherein the reduction treatment conditions comprise: the volume space velocity of hydrogen is 1000 hours-1The reduction temperature was 550 ℃ and the reduction time was 1 hour.
Then 15mL of 0.46g/mL phosphomolybdic acid aqueous solution is added to dip the second intermediate for 2 hours at 80 ℃, and the mixture is subjected to rotary evaporation to dryness to obtain the catalyst, wherein the composition of the catalyst is shown in Table 1.
Example 4
A catalyst was prepared in the same manner as in example 1, except that the first intermediate was charged into the reactor at an air flow volumetric space velocity of 1000 hours, and the composition thereof is shown in Table 1-1Oxidizing at 300 deg.c for 5 hr, replacing air flow with nitrogen and reducing.
Example 5
A catalyst was prepared in the same manner as in example 1, except that ammonia water was used for the reaction of gamma-Al, and the composition thereof is shown in Table 12O3The carrier is pretreated, and the pretreatment process comprises the following steps: weighing 200 g of gamma-Al2O3Placing the mixture into a stainless steel reaction kettle, soaking the mixture in 200mL of 3% ammonia water, sealing the stainless steel reaction kettle, and treating the mixture for 24 hours at 80 ℃; and cooling to 25 ℃, taking out the sample, drying for 8 hours at 120 ℃, and roasting for 4 hours at 300 ℃ to obtain the pretreated alumina carrier. And then the pretreated alumina carrier is used for preparing the catalyst.
Example 6
Weighing 200 g of gamma-Al2O3Placing the mixture into a stainless steel reaction kettle, soaking the mixture by using 200mL of 3% ammonia water, sealing the stainless steel reaction kettle, and treating the mixture for 1 hour at 200 ℃; and cooling to room temperature, taking out the sample, drying at 120 ℃ for 8 hours, and roasting at 300 ℃ for 4 hours to obtain the pretreated alumina carrier.
And (3) putting 10g of the pretreated alumina carrier into a rotary evaporator, adding 15mL of chloroplatinic acid solution with the platinum content of 6.67mg/mL, soaking at 60 ℃ for 4 hours, and performing rotary evaporation to dryness to obtain a first intermediate.
The first intermediate was charged to the reactor at an air flow volumetric space velocity of 1500 hours-1Oxidizing at 500 deg.C for 1 hr, then fully displacing the air flow in the reactor with nitrogen flow, and then making the hydrogen volume space velocity be hr-1And reducing for 4 hours at 480 ℃ to obtain a second intermediate.
Then 15mL of 0.33g/mL aqueous solution of phosphotungstic acid is used for dipping the second intermediate for 2 hours at the temperature of 60 ℃, and the catalyst is obtained by rotary evaporation to dryness, and the composition of the catalyst is shown in Table 1.
Comparative example 1
10g of gamma-Al2O3Putting the mixture into a rotary evaporator, adding 15mL of chloroplatinic acid solution with the platinum content of 6.67mg/mL, soaking for 4 hours at 60 ℃, and performing rotary evaporation to obtain a first intermediate.
The first intermediate was charged into a reactor and subjected to reduction treatment to obtain a catalyst having the composition shown in Table 1, supraThe conditions of the reduction treatment include: the volume space velocity of hydrogen is 1200 h-1The reduction temperature was 480 ℃ and the reduction time was 4 hours.
Comparative example 2
10g of gamma-Al2O3Dipping the catalyst in 15mL of 0.33g/mL phosphotungstic acid aqueous solution at 60 ℃ for 2 hours, and carrying out rotary evaporation to dryness to obtain the catalyst, wherein the composition of the catalyst is shown in Table 1.
Comparative example 3
10g of gamma-Al2O3Immersing in 15mL of 0.33g/mL aqueous solution of phosphotungstic acid at 60 ℃ for 2 hours, rotary evaporating to dryness, and evaporating to dryness to obtain gamma-Al2O3Immersing the reaction product in 15mL of 6.67mg/mL chloroplatinic acid solution at 60 ℃ for 4 hours, drying the solution by rotary evaporation, loading the solution into a reactor, and carrying out reduction treatment under the conditions of: the volume space velocity of hydrogen is 1200 h-1The reduction temperature was 480 ℃ and the reduction time was 4 hours, to obtain the catalyst, the composition of which is shown in table 1.
Test examples
This test example was conducted to test the catalysts prepared in examples 1 to 6 and comparative examples 1 to 3 for their catalytic activity and isomerization selectivity when used for catalyzing the isomerization of normal paraffins.
In a small fixed bed reactor, 3g of each of the catalysts prepared in examples 1 to 6 and comparative examples 1 to 3 was charged, heated to the temperatures given in Table 2, and contacted with n-heptane to conduct an isomerization reaction, wherein the conditions of the contact reaction include: the reaction pressure is 1.0MPa, and the mass space velocity of the reaction feeding is 3 hours-1Hydrogen/hydrocarbon molar ratio of 2.6: the results of the feedstock conversion, yield of multi-branched products and yield of cracked products are shown in Table 2, respectively.
TABLE 1
TABLE 2
As can be seen from Table 2, the catalysts prepared according to the present invention have better catalytic activity and multi-branched isoparaffin selectivity at different temperatures, lower yield of cracked products and higher yield of liquid products under the same reaction conditions, compared to the catalysts prepared according to comparative examples 1-3.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (9)
1. C7-C8The preparation method of the normal paraffin isomerization catalyst comprises the following steps:
(1) dipping the alumina carrier by ammonia water for pretreatment, then drying and roasting, wherein the roasting temperature is 200-450 ℃, and the roasting time is 0.5-10 hours;
(2) loading an active metal component platinum on an alumina carrier, and drying to obtain a first intermediate;
(3) reducing the first intermediate obtained in the step (2) to obtain a second intermediate;
(4) dipping the second intermediate obtained in the step (3) by using a heteropoly acid solution, loading the heteropoly acid on the second intermediate, and drying to obtain the catalyst, wherein the general formula of the heteropoly acid is H8-n[AM12O40]Wherein A is P or Si, M is W or Mo, n is the valence state of A, and the valence state is 4 or 5;
the platinum loading in the catalyst is 0.01-2.0 mass percent and the heteropoly acid loading is 10-70 mass percent, which are calculated by taking a dry-based alumina carrier as a reference.
2. The method of claim 1, wherein said alumina support comprises γ -Al2O3、η-Al2O3、θ-Al2O3、δ-Al2O3And chi-Al2O3At least one of (1).
3. The method of claim 1, further comprising: and (3) oxidizing the first intermediate obtained in the step (1) and then performing reduction treatment in the step (2).
4. The production method according to claim 3, wherein the conditions of the oxidation treatment include: the oxidation temperature is 100-550 ℃, the oxidation time is 0.1-10 hours, and the volume space velocity of the oxidation gas is 5-1500 hours-1The oxidizing gas is nitrogen containing oxygen.
5. The production method according to claim 1, wherein the conditions of the pretreatment are: the concentration of ammonia water is 0.1-28 wt%, the treatment temperature is 30-250 deg.C, and the treatment time is 1-48 hr.
6. The production method according to claim 5, wherein the conditions of the pretreatment are: the concentration of ammonia water is 3-20 wt%, the treatment temperature is 80-200 deg.C, and the treatment time is 1-24 hr.
7. The production method according to claim 1, wherein in the step (2), the conditions of the reduction treatment include: the reduction temperature is 100-550 ℃, the reduction time is 0.1-10 hours, and the volume space velocity of the reduction gas passing through the first intermediate is 5-1500 hours-1。
8. The production method according to claim 1, wherein the heteropoly-acid includes at least one of phosphotungstic acid, silicotungstic acid, and phosphomolybdic acid.
9. An n-paraffin isomerization catalyst produced by the production method according to any one of claims 1 to 8.
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