CN105032416A - Four-element platinum-based catalyst and preparation method thereof - Google Patents
Four-element platinum-based catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a four-element platinum-based catalyst and a preparation method thereof. The four-element platinum-based catalyst is prepared by adopting a high-temperature combustion synthesis method, the washing and drying steps in the preparation process are omitted, and a technological process is simplified. When glycine or urea serves as a fuel, combustion can be completed within very short time, accordingly reaction is completed, and production efficiency is improved. In the preparation process, various precursors can be accurately added according to calculated amounts and are almost free of loss in the whole preparation process, and accordingly accurate control of component contents of the catalyst is achieved. In the high-temperature combustion process, lower temperature can also enable the glycine or the urea and the active components, namely the precursors, to strongly release heat, and accordingly energy consumption is partially saved. In addition, the active components of the catalyst prepared by means of the preparation method are evenly distributed, the reactivity of Bi contained in the catalyst is improved, the selectivity of the catalyst is improved by adopting Ba, the carbon depositing amount in the reaction process is decreased, and accordingly the service life of the catalyst is prolonged.
Description
Technical field
The present invention relates to platinum based catalyst technical field, specifically refer to a kind of quaternary platinum based catalyst of preparing propylene by dehydrogenating propane, the invention still further relates to the preparation method of above-mentioned platinum based catalyst.
Background technology
At present, continuous increase due to polypropylene, expoxy propane and acrylic acid demand causes propylene demand to present the trend constantly increased, but the rate of rise of production of propylene ability is but far below the rate of rise of propylene demand, and insufficiency of supply-demand strengthens year by year, therefore, Technologies For Increasing Propylene has become the study hotspot of petrochemical technology.Particularly in recent years, along with the development of shale gas technology and the surging of propylene price, by dehydrogenating propane technology that is inexpensive, that be easy to get prepare propylene in the whole world particularly China started upsurge.Therefore be that the research of catalytic material dehydrogenation producing propylene has very important significance with propane.
In prior art, the existing a large amount of report of Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane technology, but, the high manufacturing cost of catalyst that causes of noble metal component content is high, complex manufacturing process, cycle are long, the activity of catalyst and selective undesirable, the problems such as poor stability greatly limit the application of Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane.
Application publication number is that Chinese invention patent application " a kind of quaternary platinum based catalyst of preparing propylene by dehydrogenating propane and preparation method and application " (application number: CN201410406002.0) of CN104148069A discloses a kind of method preparing platinum based catalyst, the method with the aluminium oxide after alkaline gas process for carrier, with Pt and Sn for active component, with Na, K, Rb, Mg, Ca, one in Sr is auxiliary agent 1, with La, Ce, Pm, Sm, Ti, Ga, In, Zn, one in Fe is auxiliary agent 2, preparing propylene by dehydrogenating propane four-way catalyst is prepared by excessive infusion process.Although the method has, noble metal dosage is few, the advantages such as carbon distribution is few on active high, selective good, the catalyst of catalyst reaction, also there is the problem that operating procedure complexity, Active components distribution are uneven simultaneously.
Application publication number is Chinese invention patent application " platinum based catalyst and preparation method thereof of CN104226307A, application and the preparation method of propylene " (application number: CN201310229758.8) also disclose a kind of method preparing platinum based catalyst, the method take aluminium oxide as carrier, with Pt, Sn, In is active component, the dipping method of ultrasonic assistant is utilized to prepare preparing propylene by dehydrogenating propane platinum based three-way catalyst, although it is simple that the method has preparation process, active component is uniformly dispersed, catalytic activity high, but it is large also to there is precious metals pt consumption in the method, the defect that preparation cost is high.
Therefore, for current platinum based catalyst and preparation method thereof, await making further improvements.
Summary of the invention
Technical problem to be solved by this invention is the present situation for prior art, provides a kind of Active components distribution even and the quaternary platinum based catalyst that anti-carbon performance is strong.
Another technical problem to be solved by this invention is the present situation for prior art, a kind of preparation method of above-mentioned quaternary platinum based catalyst is provided, the method preparation technology is simple, production efficiency is high, production cost is low, and strictly can control the content of catalyst components as required, thus obtain the high platinum based catalyst of catalytic efficiency.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of quaternary platinum based catalyst, is characterized in that: described quaternary platinum based catalyst is with Al
2o
3for carrier, with Pt and Sn for main active component, with Ba and Bi for cocatalyst component.
In such scheme, the feed postition of described Ba is BaO, and the feed postition of described Bi is Bi
2o
3.
As a further improvement on the present invention, by weight percentage, the load capacity of described Pt is 0.1 ~ 0.3wt% of total catalyst weight, the load capacity of Sn is 0.2 ~ 3wt% of total catalyst weight, the load capacity of Ba is the load capacity of 0.4 ~ 4wt% of total catalyst weight, Bi is 0.2 ~ 1.5wt% of total catalyst weight.
A preparation method for quaternary platinum based catalyst, is characterized in that comprising the following steps:
(1) be respectively 0.1 ~ 0.3wt%, 0.2 ~ 3wt%, 0.4 ~ 4wt%, the 0.2 ~ 1.5wt% meter of catalyst weight according to the load capacity of Pt, Sn, Ba, Bi, take Pt, Sn, Ba, Bi and Al respectively
2o
3presoma;
(2) Pt, Sn, Ba, Bi and Al of will taking in step (1)
2o
3presoma to be dissolved in deionized water or ethanol and to stir, in this solution, then add urea or glycine and stir; By above-mentioned solution simmer down to saturated solution under the condition of water bath heating of 40 ~ 90 DEG C;
(3) first firing equipment is preheated to 350 ~ 700 DEG C, then step (2) gained saturated solution is placed in firing equipment burning 2 ~ 10min, namely obtains foamed solid catalyst;
(4) activation process is carried out to the foamed solid catalyst of step (3) gained, namely obtain described quaternary platinum based catalyst.
As improvement, described in step (2), the consumption of urea or glycine is Pt, Sn, Ba, Bi and Al
2o
30.4 ~ 2.0 times of presoma gross mass.
As preferably, high-temperature process 1 ~ 2h at the foamed solid catalyst that step (3) obtains first is placed in 350 ~ 700 DEG C before carrying out by step (4), to remove the impurity be attached on foaming solid catalyst surface.
Preferably, the activated process described in step (4) comprises grinding, compressing tablet, screening and high-temperature activation successively, and described high-temperature activation carries out in hydrogen atmosphere, and activation temperature is 600 ~ 850 DEG C, and soak time is 30 ~ 120min.
Preferably, the presoma of described Pt is the one in potassium platinic chloride, ammonium chloroplatinate, acetylacetone,2,4-pentanedione platinum; The presoma of described Sn is the one in stannous chloride, butter of tin, stannous oxalate.
Preferably, the presoma of described Ba is the one in barium nitrate, barium stearate, acetylacetone barium; The presoma of described Bi is the one in bismuth nitrate, bismuth chloride.
Preferably, described Al
2o
3presoma be one in aluminum nitrate, aluminium isopropoxide, aluminium secondary butylate, aluminium acetylacetonate.
Compared with prior art, the invention has the advantages that:
(1) the present invention adopts high-temp combustion synthetic method to prepare quaternary platinum based catalyst, does not occur adopting the method to prepare the report of platinum based catalyst in prior art;
(2) preparation method of the present invention is compared with the method preparing platinum based catalyst common in prior art, eliminates the washing in preparation process and dry run, simplifies technical process; And due to glycine or urea as fuel time, can be complete thus complete reaction in extremely short time combustion, substantially reduce the time of whole preparation process, improve production efficiency;
(3) in preparation process, the amount of various presoma accurately can be added according to amount of calculation, and each presoma is almost lossless in whole preparation process, thus achieves the accurate control to catalyst components content;
(4) in high-temp combustion process, lower temperature also can cause glycine or between urea and active component presoma, strong heat release occur, thus saves part energy consumption, reduces production cost to a certain extent; Meanwhile, after all burnt, products obtained therefrom has nanoscale structures, thus active component is uniformly distributed in the catalyst, guarantees that catalyst has good stability in use;
(5) Bi in catalyst of the present invention can improve the reactivity of catalyst, and the Ba in catalyst then can improve the selective of catalyst and reduce the formation of carbon distribution in course of reaction, thus the service life of extending catalyst.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1:
The preparation method of the present embodiment quaternary platinum based catalyst comprises the following steps:
(1) be respectively 0.1wt%, 0.2wt%, 2.0wt%, 1.5wt% meter of catalyst weight according to the load capacity of Pt, Sn, Ba, Bi, take potassium platinic chloride, butter of tin, barium nitrate, bismuth nitrate and aluminum nitrate respectively;
(2) potassium platinic chloride, butter of tin, barium nitrate, bismuth nitrate and the aluminum nitrate that take in step (1) to be dissolved in deionized water and to stir, then in this solution, add urea and stir, the addition of urea is 1.5 times of potassium platinic chloride, butter of tin, barium nitrate, bismuth nitrate and aluminum nitrate gross weight; By above-mentioned solution simmer down to saturated solution under the condition of water bath heating of 40 DEG C;
(3) first firing equipment is preheated to 350 DEG C, then step (2) gained saturated solution is placed in firing equipment to burn 10min, obtain foamed solid catalyst, high-temperature process 2h at this foamed solid catalyst is placed in 350 DEG C, to remove the impurity be attached on foaming solid catalyst surface;
(4) activation process is carried out to the foamed solid catalyst of step (3) gained, activated process comprises grinding successively, compressing tablet, 40 mesh sieves divide and high-temperature activation, high-temperature activation carries out in hydrogen atmosphere, and activation temperature is 600 DEG C, and soak time is 120min.
Embodiment 2:
The preparation method of the present embodiment quaternary platinum based catalyst comprises the following steps:
(1) be respectively 0.2wt%, 0.2wt%, 2.0wt%, 0.2wt% meter of catalyst weight according to the load capacity of Pt, Sn, Ba, Bi, take acetylacetone,2,4-pentanedione platinum, stannous oxalate, barium stearate, bismuth nitrate and aluminium isopropoxide respectively;
(2) the acetylacetone,2,4-pentanedione platinum, stannous oxalate, barium stearate, bismuth nitrate and the aluminium isopropoxide that take in step (1) to be dissolved in deionized water and to stir, then in this solution, add urea and stir, the addition of urea is 0.5 times of acetylacetone,2,4-pentanedione platinum, stannous oxalate, barium stearate, bismuth nitrate and aluminium isopropoxide gross weight; By above-mentioned solution simmer down to saturated solution under the condition of water bath heating of 90 DEG C;
(3) first firing equipment is preheated to 700 DEG C, then step (2) gained saturated solution is placed in firing equipment to burn 2min, obtain foamed solid catalyst, high-temperature process 1h at this foamed solid catalyst is placed in 700 DEG C, to remove the impurity be attached on foaming solid catalyst surface;
(4) activation process is carried out to the foamed solid catalyst of step (3) gained, activated process comprises grinding successively, compressing tablet, 60 mesh sieves divide and high-temperature activation, high-temperature activation carries out in hydrogen atmosphere, and activation temperature is 850 DEG C, and soak time is 30min.
Embodiment 3:
The preparation method of the present embodiment quaternary platinum based catalyst comprises the following steps:
(1) be respectively 0.3wt%, 0.2wt%, 0.4wt%, 1.2wt% meter of catalyst weight according to the load capacity of Pt, Sn, Ba, Bi, take potassium platinic chloride, butter of tin, barium nitrate, bismuth nitrate and aluminum nitrate respectively;
(2) potassium platinic chloride, butter of tin, barium nitrate, bismuth nitrate and the aluminum nitrate that take in step (1) to be dissolved in deionized water and to stir, then in this solution, add urea and stir, the addition of urea is 2 times of potassium platinic chloride, butter of tin, barium nitrate, bismuth nitrate and aluminum nitrate gross weight; By above-mentioned solution simmer down to saturated solution under the condition of water bath heating of 60 DEG C;
(3) first firing equipment is preheated to 500 DEG C, then step (2) gained saturated solution is placed in firing equipment to burn 6min, obtain foamed solid catalyst, high-temperature process 1.5h at this foamed solid catalyst is placed in 500 DEG C, to remove the impurity be attached on foaming solid catalyst surface;
(4) activation process is carried out to the foamed solid catalyst of step (3) gained, activated process comprises grinding successively, compressing tablet, 50 mesh sieves divide and high-temperature activation, high-temperature activation carries out in hydrogen atmosphere, and activation temperature is 750 DEG C, and soak time is 50min.
Embodiment 4:
The preparation method of the present embodiment quaternary platinum based catalyst comprises the following steps:
(1) be respectively 0.2wt%, 2.0wt%, 4.0wt%, 1.5wt% meter of catalyst weight according to the load capacity of Pt, Sn, Ba, Bi, take potassium platinic chloride, butter of tin, barium nitrate, bismuth nitrate and aluminum nitrate respectively;
(2) potassium platinic chloride, butter of tin, barium nitrate, bismuth nitrate and the aluminum nitrate that take in step (1) to be dissolved in deionized water and to stir, then in this solution, add urea and stir, the addition of urea is 1.0 times of potassium platinic chloride, butter of tin, barium nitrate, bismuth nitrate and aluminum nitrate gross weight; By above-mentioned solution simmer down to saturated solution under the condition of water bath heating of 50 DEG C;
(3) first firing equipment is preheated to 400 DEG C, then step (2) gained saturated solution is placed in firing equipment to burn 7min, obtain foamed solid catalyst, high-temperature process 1.5h at this foamed solid catalyst is placed in 400 DEG C, to remove the impurity be attached on foaming solid catalyst surface;
(4) activation process is carried out to the foamed solid catalyst of step (3) gained, activated process comprises grinding successively, compressing tablet, 60 mesh sieves divide and high-temperature activation, high-temperature activation carries out in hydrogen atmosphere, and activation temperature is 650 DEG C, and soak time is 60min.
Embodiment 5:
The preparation method of the present embodiment quaternary platinum based catalyst comprises the following steps:
(1) be respectively 0.1wt%, 0.5wt%, 2.0wt%, 1.5wt% meter of catalyst weight according to the load capacity of Pt, Sn, Ba, Bi, take potassium platinic chloride, butter of tin, barium nitrate, bismuth nitrate and aluminum nitrate respectively;
(2) potassium platinic chloride, butter of tin, barium nitrate, bismuth nitrate and the aluminum nitrate that take in step (1) to be dissolved in deionized water and to stir, then in this solution, add urea and stir, the addition of urea is 1.5 times of potassium platinic chloride, butter of tin, barium nitrate, bismuth nitrate and aluminum nitrate gross weight; By above-mentioned solution simmer down to saturated solution under the condition of water bath heating of 90 DEG C;
(3) first firing equipment is preheated to 500 DEG C, then step (2) gained saturated solution is placed in firing equipment to burn 5min, obtain foamed solid catalyst, high-temperature process 1h at this foamed solid catalyst is placed in 700 DEG C, to remove the impurity be attached on foaming solid catalyst surface;
(4) activation process is carried out to the foamed solid catalyst of step (3) gained, activated process comprises grinding successively, compressing tablet, 60 mesh sieves divide and high-temperature activation, high-temperature activation carries out in hydrogen atmosphere, and activation temperature is 600 DEG C, and soak time is 100min.
Embodiment 6:
The preparation method of the present embodiment quaternary platinum based catalyst comprises the following steps:
(1) be respectively 0.2wt%, 1.0wt%, 0.4wt%, 1.5wt% meter of catalyst weight according to the load capacity of Pt, Sn, Ba, Bi, take potassium platinic chloride, butter of tin, barium nitrate, bismuth nitrate and aluminum nitrate respectively;
(2) potassium platinic chloride, butter of tin, barium nitrate, bismuth nitrate and the aluminum nitrate that take in step (1) to be dissolved in deionized water and to stir, then in this solution, add urea and stir, the addition of urea is 1.0 times of potassium platinic chloride, butter of tin, barium nitrate, bismuth nitrate and aluminum nitrate gross weight; By above-mentioned solution simmer down to saturated solution under the condition of water bath heating of 50 DEG C;
(3) first firing equipment is preheated to 450 DEG C, then step (2) gained saturated solution is placed in firing equipment to burn 8min, obtain foamed solid catalyst, high-temperature process 1.2h at this foamed solid catalyst is placed in 400 DEG C, to remove the impurity be attached on foaming solid catalyst surface;
(4) activation process is carried out to the foamed solid catalyst of step (3) gained, activated process comprises grinding successively, compressing tablet, 40 mesh sieves divide and high-temperature activation, high-temperature activation carries out in hydrogen atmosphere, and activation temperature is 750 DEG C, and soak time is 45min.
Embodiment 7:
The preparation method of the present embodiment quaternary platinum based catalyst comprises the following steps:
(1) be respectively 0.2wt%, 3.0wt%, 2.0wt%, 1.5wt% meter of catalyst weight according to the load capacity of Pt, Sn, Ba, Bi, take potassium platinic chloride, butter of tin, barium nitrate, bismuth nitrate and aluminum nitrate respectively;
(2) potassium platinic chloride, butter of tin, barium nitrate, bismuth nitrate and the aluminum nitrate that take in step (1) to be dissolved in deionized water and to stir, then in this solution, add urea and stir, the addition of urea is 1.5 times of potassium platinic chloride, butter of tin, barium nitrate, bismuth nitrate and aluminum nitrate gross weight; By above-mentioned solution simmer down to saturated solution under the condition of water bath heating of 60 DEG C;
(3) first firing equipment is preheated to 700 DEG C, then step (2) gained saturated solution is placed in firing equipment to burn 2min, obtain foamed solid catalyst, high-temperature process 2h at this foamed solid catalyst is placed in 350 DEG C, to remove the impurity be attached on foaming solid catalyst surface;
(4) activation process is carried out to the foamed solid catalyst of step (3) gained, activated process comprises grinding successively, compressing tablet, 50 mesh sieves divide and high-temperature activation, high-temperature activation carries out in hydrogen atmosphere, and activation temperature is 600 DEG C, and soak time is 110min.
Carry out the evaluation of preparing propylene by dehydrogenating propane reactivity to catalyst prepared by the various embodiments described above, this preparing propylene by dehydrogenating propane reactivity evaluation is carried out on atmospheric fixed bed reactor, consisting of of reaction mixture gas: C
3h
8(volume fraction is 15%), H
2(volume fraction is 5%), Balance Air is Ar, and total volumetric flow rate is 40mL/min, and reaction temperature interval is 550 ~ 650 DEG C.Evaluation result is as shown in table 1.
Table 1
Claims (10)
1. a quaternary platinum based catalyst, is characterized in that: described quaternary platinum based catalyst is with Al
2o
3for carrier, with Pt and Sn for main active component, with Ba and Bi for cocatalyst component.
2. quaternary platinum based catalyst according to claim 1, is characterized in that: the feed postition of described Ba is BaO, and the feed postition of described Bi is Bi
2o
3.
3. quaternary platinum based catalyst according to claim 1, it is characterized in that: by weight percentage, the load capacity of described Pt is 0.1 ~ 0.3wt% of total catalyst weight, the load capacity of Sn is 0.2 ~ 3wt% of total catalyst weight, the load capacity of Ba is the load capacity of 0.4 ~ 4wt% of total catalyst weight, Bi is 0.2 ~ 1.5wt% of total catalyst weight.
4. a preparation method for quaternary platinum based catalyst, is characterized in that comprising the following steps:
(1) be respectively 0.1 ~ 0.3wt%, 0.2 ~ 3wt%, 0.4 ~ 4wt%, the 0.2 ~ 1.5wt% meter of catalyst weight according to the load capacity of Pt, Sn, Ba, Bi, take Pt, Sn, Ba, Bi and Al respectively
2o
3presoma;
(2) Pt, Sn, Ba, Bi and Al of will taking in step (1)
2o
3presoma to be dissolved in deionized water or ethanol and to stir, in this solution, then add urea or glycine and stir; By above-mentioned solution simmer down to saturated solution under the condition of water bath heating of 40 ~ 90 DEG C;
(3) first firing equipment is preheated to 350 ~ 700 DEG C, then step (2) gained saturated solution is placed in firing equipment burning 2 ~ 10min, namely obtains foamed solid catalyst;
(4) activation process is carried out to the foamed solid catalyst of step (3) gained, namely obtain described quaternary platinum based catalyst.
5. the preparation method of quaternary platinum based catalyst according to claim 4, is characterized in that: described in step (2), the consumption of urea or glycine is Pt, Sn, Ba, Bi and Al
2o
30.4 ~ 2.0 times of presoma gross mass.
6. the preparation method of quaternary platinum based catalyst according to claim 4, is characterized in that: high-temperature process 1 ~ 2h at the foamed solid catalyst that step (3) obtains is placed in 350 ~ 700 DEG C.
7. the preparation method of quaternary platinum based catalyst according to claim 4, it is characterized in that: the activated process described in step (4) comprises grinding, compressing tablet, screening and high-temperature activation successively, described high-temperature activation carries out in hydrogen atmosphere, activation temperature is 600 ~ 850 DEG C, and soak time is 30 ~ 120min.
8. the preparation method of quaternary platinum based catalyst according to claim 4, is characterized in that: the presoma of described Pt is the one in potassium platinic chloride, ammonium chloroplatinate, acetylacetone,2,4-pentanedione platinum; The presoma of described Sn is the one in stannous chloride, butter of tin, stannous oxalate.
9. the preparation method of quaternary platinum based catalyst according to claim 4, is characterized in that: the presoma of described Ba is the one in barium nitrate, barium stearate, acetylacetone barium; The presoma of described Bi is the one in bismuth nitrate, bismuth chloride.
10. the preparation method of quaternary platinum based catalyst according to claim 4, is characterized in that: described Al
2o
3presoma be one in aluminum nitrate, aluminium isopropoxide, aluminium secondary butylate, aluminium acetylacetonate.
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| CN105749986A (en) * | 2016-02-15 | 2016-07-13 | 中国石油大学(北京) | Catalyst for preparation of olefin through low-alkane dehydrogenation as well as preparation method and application thereof |
| CN106552645A (en) * | 2015-09-30 | 2017-04-05 | 中国石油化工股份有限公司 | A kind of loaded catalyst and its preparation method and application and Fischer-Tropsch synthesis method |
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Address after: 315803 No. 168 Hongyuan Road, Qijiashan Street, Beilun District, Ningbo City, Zhejiang Province Patentee after: Ningbo Golden Hair New Materials Co., Ltd. Address before: 315801 No. 168 Hongyuan Road, Beilun District, Ningbo City, Zhejiang Province Patentee before: NINGBO HAIYUE NEW MATERIAL CO., LTD. |