CN112391191B - Method for preventing catalyst from coagulating and scaling in Fischer-Tropsch synthesis process, catalyst and application - Google Patents
Method for preventing catalyst from coagulating and scaling in Fischer-Tropsch synthesis process, catalyst and application Download PDFInfo
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- CN112391191B CN112391191B CN202011194333.4A CN202011194333A CN112391191B CN 112391191 B CN112391191 B CN 112391191B CN 202011194333 A CN202011194333 A CN 202011194333A CN 112391191 B CN112391191 B CN 112391191B
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- tetraethoxysilane
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- 239000003054 catalyst Substances 0.000 title claims abstract description 115
- 238000000034 method Methods 0.000 title claims abstract description 45
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 27
- 230000008569 process Effects 0.000 title claims abstract description 27
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 27
- 230000001112 coagulating effect Effects 0.000 title claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000002791 soaking Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 34
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 238000007598 dipping method Methods 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 125000000962 organic group Chemical group 0.000 abstract description 3
- 230000015271 coagulation Effects 0.000 abstract description 2
- 238000005345 coagulation Methods 0.000 abstract description 2
- 238000005470 impregnation Methods 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 11
- 239000007788 liquid Substances 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 231100000989 no adverse effect Toxicity 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2/00—Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon
- C10G2/30—Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen
- C10G2/32—Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen with the use of catalysts
- C10G2/33—Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen with the use of catalysts characterised by the catalyst used
- C10G2/331—Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen with the use of catalysts characterised by the catalyst used containing group VIII-metals
- C10G2/332—Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen with the use of catalysts characterised by the catalyst used containing group VIII-metals of the iron-group
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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Abstract
The invention relates to a method for preventing catalyst from being condensed and scaled in a Fischer-Tropsch synthesis process, a catalyst and application, and belongs to the field of Fischer-Tropsch synthesis. The method for preventing the coagulation and the scaling of the catalyst in the Fischer-Tropsch synthesis process comprises the following steps: completely soaking the dried Fischer-Tropsch catalyst in an organic solution of tetraethoxysilane; and taking out the impregnated Fischer-Tropsch catalyst and drying the impregnated Fischer-Tropsch catalyst in the air to obtain the modified Fischer-Tropsch catalyst. According to the method, the Fischer-Tropsch catalyst is treated by a solution impregnation method, the Fischer-Tropsch catalyst is impregnated in a tetraethoxysilane solution, and the tetraethoxysilane modifies the oleophobic organic group on the surface of the Fischer-Tropsch catalyst, so that the surface of the Fischer-Tropsch catalyst obtains good oleophobic property, and the Fischer-Tropsch catalyst can be prevented from being mixed with an oil phase in Fischer-Tropsch synthesis and condensing a structure on a reactor.
Description
Technical Field
The invention belongs to the field of Fischer-Tropsch synthesis, and particularly relates to a method for preventing a catalyst from being condensed and scaled in a Fischer-Tropsch synthesis process, and the catalyst and application.
Background
In the coal chemical production, the most important process is a Fischer-Tropsch synthesis process, and the core process of the Fischer-Tropsch synthesis process is to synthesize required oil products and related derivatives in a slurry bed Fischer-Tropsch reaction synthesizer under the action of a catalyst, and then carry out subsequent hydrofining and the like.
However, in the actual process operation process, the final product is often doped with impurities such as catalyst, although a part of the catalyst can be removed by filtration, a considerable amount of catalyst is deposited in a pipeline of the next process flow to form some deposits, and after long-time use, the reactor must be stopped, overhauled and cleaned, thereby causing great influence on normal production and greatly increasing the cost. Therefore, how to avoid the catalyst from being in a condensed structure in the reactor is a technical problem which needs to be solved urgently in the field.
Disclosure of Invention
The invention provides a method for preventing the condensation and the scaling of a catalyst in a Fischer-Tropsch synthesis process in order to solve the technical problems.
The technical scheme for solving the technical problems is as follows: a method for preventing catalyst from coagulating and scaling in a Fischer-Tropsch synthesis process comprises the following steps:
s1: completely soaking the dried Fischer-Tropsch catalyst in an organic solution of tetraethoxysilane;
s2: and taking out the Fischer-Tropsch catalyst impregnated in the step S1, and drying the Fischer-Tropsch catalyst in the air to obtain the modified Fischer-Tropsch catalyst.
The method for preventing the catalyst from being condensed and scaled in the Fischer-Tropsch synthesis process has the beneficial effects that: this application is handled the ft catalyst through solution dipping method, through with the solution of ft catalyst flooding in tetraethoxysilane, the organic group that has oleophobic nature is decorated on the ft catalyst surface to the hydrolysis of four oxygen ethyl and catalyst surface hydroxyl reaction, makes the ft catalyst surface obtain good oleophobic nature, and then can prevent that the ft catalyst from mixing with the oil phase in the ft synthesis, the structure of condensing on the reactor.
Further, the organic solution of tetraethoxysilane is an ethanol solution of tetraethoxysilane. Tetraethoxysilane can be mixed and dissolved with ethanol, and the ethanol is cheap and easy to obtain and has stable property.
Further, in the ethanol solution of tetraethoxysilane, the volume ratio of tetraethoxysilane to ethanol is 1: 1.
Further, in the step S1, the dipping temperature is 25 to 35 ℃. In the embodiment disclosed by the invention, tetraethoxysilane can be fully contacted with the Fischer-Tropsch catalyst by dipping in a water bath at 25-35 ℃, and meanwhile, the organic solvent is prevented from volatilizing.
Further, in the step S1, the dipping is performed under a stirring condition, and the dipping time is 5 to 7 hours. After the catalyst is soaked for 5-7 hours, tetraethoxysilane can better modify the surface of the Fischer-Tropsch catalyst.
Further, in the step 2, the drying temperature is 150-170 ℃, and the drying time is 3-5 hours. The dried Fischer-Tropsch catalyst can remove the surface organic solvent.
Further, the Fischer-Tropsch catalyst is an iron-based catalyst taking silicon dioxide as a carrier. The Fischer-Tropsch catalyst treated in the application is an iron-based catalyst taking silicon dioxide as a carrier, the iron-based catalyst is inert to metal due to low price, high catalytic activity and high water gas shift reaction activity, and can effectively disperse and isolate metal particles, and the Fischer-Tropsch catalyst taking the silicon dioxide as the carrier has good stability and regeneration performance.
The application also provides a Fischer-Tropsch catalyst obtained by the treatment method.
The Fischer-Tropsch catalyst has the beneficial effects that: the Fischer-Tropsch catalyst after surface modification has good oleophobic property, thereby being capable of preventing the Fischer-Tropsch catalyst from being mixed with oil stains in the Fischer-Tropsch synthesis process, being beneficial to the liquidity of the Fischer-Tropsch catalyst in the pipeline, being not easy to condense and scale and being convenient to clean.
Further, the contact angle of the Fischer-Tropsch catalyst to oil is greater than 120 degrees.
The application also provides an application of the Fischer-Tropsch catalyst in a Fischer-Tropsch synthesis process.
The application of the Fischer-Tropsch catalyst in the Fischer-Tropsch synthesis process has the beneficial effects that: the catalyst after surface modification treatment has no adverse effect on Fischer-Tropsch reaction and product yield, and can prevent the coagulation and scaling of the Fischer-Tropsch catalyst in the Fischer-Tropsch reactor.
Drawings
FIG. 1 is a graph of the contact angle of the modified Fischer-Tropsch catalyst treated in example 1 herein with oil;
FIG. 2 is the contact angle of an untreated Fischer-Tropsch catalyst with oil.
Detailed Description
The principles and features of this application are described below in conjunction with the following drawings, the examples of which are set forth to illustrate the application and are not intended to limit the scope of the application.
In the description of the present specification, it is to be understood that the terms "center", "length", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "inner", "outer", "circumferential", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, and do not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the specification.
In the description of the present specification, "a plurality" means at least two, e.g., two, three, etc., unless explicitly defined otherwise.
In the description herein, reference to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the application. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
The terms used in the present specification are those general terms currently widely used in the art in consideration of functions related to the present disclosure, but they may be changed according to the intention of a person having ordinary skill in the art, precedent, or new technology in the art. Also, specific terms may be selected by the applicant, and in this case, their detailed meanings will be described in the detailed description of the present disclosure. Therefore, the terms used in the specification should not be construed as simple names, but rather based on the meanings of the terms and the overall description of the present disclosure.
Flowcharts or text are used herein to illustrate the operational steps performed in accordance with embodiments of the present application. It should be understood that the operational steps in the embodiments of the present application are not necessarily performed in the exact order recited. Rather, the various steps may be processed in reverse order or simultaneously, as desired. Meanwhile, other operations may be added to the processes, or a certain step or several steps of operations may be removed from the processes.
The following discloses many different embodiments or examples for implementing the subject technology described. The following describes particular embodiments of one or more arrangements of features for simplicity of disclosure, but the illustrated embodiments are not intended to be limiting of the present disclosure, and the first and second features set forth in the following description may be combined to include embodiments that are directly connected, or may form additional features, and further, may include the use of one or more additional intervening features to indirectly connect or combine the first and second features to each other such that the first and second features may not be directly connected.
Example 1
The embodiment discloses a method for preventing catalyst from being condensed and scaled in a Fischer-Tropsch synthesis process, which comprises the following steps:
s1: drying a Fischer-Tropsch catalyst, evaporating to remove liquid on the surface of the catalyst, putting the dried Fischer-Tropsch catalyst into an ethanol solution of tetraethoxysilane in a water bath at the temperature of 30 ℃ to ensure that the ethanol solution of tetraethoxysilane completely overflows the Fischer-Tropsch catalyst, and stirring and dipping for 6 hours.
Wherein the volume ratio of tetraethoxysilane to ethanol is 1:1, and the Fischer-Tropsch catalyst is an iron-based catalyst taking silicon dioxide as a carrier.
S2: and (4) taking out the Fischer-Tropsch catalyst impregnated in the step S1, drying the Fischer-Tropsch catalyst in the air at 170 ℃ for 3h, and testing that the liquid content in the Fischer-Tropsch catalyst is less than 1% to obtain the modified Fischer-Tropsch catalyst.
The contact angle to oil of the modified fischer-tropsch catalyst treated in this example was tested and the results are shown in fig. 1. the results in fig. 1 show that the contact angle to oil of the modified fischer-tropsch catalyst treated in this example is greater than 120 °, which indicates that the present application has good oleophobic properties.
The mechanism of this application is, through steeping the ft catalyst in tetraethoxysilane's solution, can make ft catalyst surface modification have oleophobic organic group based on flooding grafting technique, changes catalyst surface characteristic to make ft catalyst surface obtain good oleophobic nature, and then can prevent that the ft catalyst from mixing with the oil phase in the ft synthesis, the structure of condensing is on the reactor.
Example 2
The embodiment discloses a method for preventing a catalyst from being coagulated and scaled in a Fischer-Tropsch synthesis process, which comprises the following steps:
s1: drying a Fischer-Tropsch catalyst in the air, evaporating to remove liquid on the surface of the catalyst, putting the dried Fischer-Tropsch catalyst into an ethanol solution of tetraethoxysilane in a water bath at the temperature of 35 ℃ to ensure that the ethanol solution of tetraethoxysilane completely overflows the Fischer-Tropsch catalyst, and stirring and dipping for 7 hours.
Wherein the volume ratio of tetraethoxysilane to ethanol is 1:1, and the Fischer-Tropsch catalyst is an iron-based catalyst taking silicon dioxide as a carrier.
S2: and (4) taking out the Fischer-Tropsch catalyst impregnated in the step S1, drying the Fischer-Tropsch catalyst in the air at 150 ℃ for 5 hours, and testing that the liquid content in the Fischer-Tropsch catalyst is less than 1 wt% to obtain the modified Fischer-Tropsch catalyst.
The Fischer-Tropsch catalyst treated in this example was tested for contact angles to oil which were greater than 120 deg..
Example 3
The embodiment discloses a method for preventing catalyst from being condensed and scaled in a Fischer-Tropsch synthesis process, which comprises the following steps:
s1: drying a Fischer-Tropsch catalyst in the air, evaporating to remove liquid on the surface of the catalyst, putting the dried Fischer-Tropsch catalyst into an ethanol solution of tetraethoxysilane in a water bath at 25 ℃ to ensure that the ethanol solution of tetraethoxysilane completely lacks the Fischer-Tropsch catalyst, and stirring and soaking for 5 hours.
Wherein the volume ratio of tetraethoxysilane to ethanol is 1:1, and the Fischer-Tropsch catalyst is an iron-based catalyst taking silicon dioxide as a carrier.
S2: and (4) taking out the Fischer-Tropsch catalyst impregnated in the step S1, drying the Fischer-Tropsch catalyst in the air at 170 ℃ for 4 hours, and testing that the liquid content in the Fischer-Tropsch catalyst is less than 1 wt% to obtain the modified Fischer-Tropsch catalyst.
The Fischer-Tropsch catalyst treated in this example was tested for contact angles to oil which were greater than 120 deg..
Comparative example
On the basis, the application also provides a group of comparison examples.
The contact angle of the comparative example, which used the same fischer-tropsch catalyst as in example 1, i.e., the iron-based catalyst supported on silica, was measured without modification, and the results are shown in fig. 2, which shows that the contact angle of the unmodified fischer-tropsch catalyst is only 98 °.
Meanwhile, the Fischer-Tropsch synthesis process is carried out on the same batch of synthesis gas by respectively adopting the embodiment 1 and the comparative example, the yield difference of the finally obtained product is within 0.1 wt%, and the final converted gas is tested, wherein the content difference of CO and H is within 0.1 wt%, which shows that the modified Fischer-Tropsch catalyst does not influence the Fischer-Tropsch synthesis and does not influence the yield of the product too much.
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (6)
1. A method for preventing catalyst from coagulating and scaling in a Fischer-Tropsch synthesis process is characterized by comprising the following steps:
s1: completely soaking the dried Fischer-Tropsch catalyst in an organic solution of tetraethoxysilane; the organic solution of tetraethoxysilane is an ethanol solution of tetraethoxysilane; the dipping temperature is 25-35 ℃; the dipping is carried out under the stirring condition, and the dipping time is 5-7 h;
s2: and (4) taking out the Fischer-Tropsch catalyst impregnated in the step S1, and drying the Fischer-Tropsch catalyst in the air at the drying temperature of 150-170 ℃ for 3-5 hours to obtain the modified Fischer-Tropsch catalyst.
2. The method of claim 1, wherein the volume ratio of tetraethoxysilane to ethanol in the ethanol solution of tetraethoxysilane is 1: 1.
3. A method of preventing catalyst fouling by condensation in a fischer-tropsch synthesis process as claimed in any one of claims 1 to 2, wherein the fischer-tropsch catalyst is an iron based catalyst on silica.
4. A fischer-tropsch catalyst treated by the process of any one of claims 1 to 3.
5. A Fischer-Tropsch catalyst according to claim 4, having a contact angle with oil of greater than 120 °.
6. Use of a fischer-tropsch catalyst according to claim 5 in a fischer-tropsch synthesis process.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1444507A (en) * | 2000-07-24 | 2003-09-24 | 萨索尔技术(控股)有限公司 | Production of hydrocarbons from synthesis gas |
| CN103920496A (en) * | 2014-04-22 | 2014-07-16 | 武汉凯迪工程技术研究总院有限公司 | Mesoporous material coated cobalt-based fischer-tropsch synthesis catalyst and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1444507A (en) * | 2000-07-24 | 2003-09-24 | 萨索尔技术(控股)有限公司 | Production of hydrocarbons from synthesis gas |
| CN103920496A (en) * | 2014-04-22 | 2014-07-16 | 武汉凯迪工程技术研究总院有限公司 | Mesoporous material coated cobalt-based fischer-tropsch synthesis catalyst and preparation method thereof |
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