CN103846108A - Preparation method of catalyst carrier for preparing substitute natural gas from coal-based syngas - Google Patents
Preparation method of catalyst carrier for preparing substitute natural gas from coal-based syngas Download PDFInfo
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- CN103846108A CN103846108A CN201210493647.3A CN201210493647A CN103846108A CN 103846108 A CN103846108 A CN 103846108A CN 201210493647 A CN201210493647 A CN 201210493647A CN 103846108 A CN103846108 A CN 103846108A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 64
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 239000003245 coal Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000003345 natural gas Substances 0.000 title claims abstract description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 12
- 239000011777 magnesium Substances 0.000 claims abstract description 12
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract 3
- 239000002245 particle Substances 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 11
- 230000015572 biosynthetic process Effects 0.000 claims description 8
- 238000003786 synthesis reaction Methods 0.000 claims description 8
- 238000005469 granulation Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 4
- 238000000748 compression moulding Methods 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- CEGOLXSVJUTHNZ-UHFFFAOYSA-K aluminium tristearate Chemical compound [Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CEGOLXSVJUTHNZ-UHFFFAOYSA-K 0.000 claims description 2
- 229940063655 aluminum stearate Drugs 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 229910052799 carbon Inorganic materials 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 abstract 1
- 230000008021 deposition Effects 0.000 abstract 1
- 238000005453 pelletization Methods 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 6
- 230000001413 cellular effect Effects 0.000 description 4
- 229920002678 cellulose Polymers 0.000 description 4
- 239000001913 cellulose Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- -1 Magnesium aluminate Chemical class 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001802 infusion Methods 0.000 description 2
- CYPPCCJJKNISFK-UHFFFAOYSA-J kaolinite Chemical compound [OH-].[OH-].[OH-].[OH-].[Al+3].[Al+3].[O-][Si](=O)O[Si]([O-])=O CYPPCCJJKNISFK-UHFFFAOYSA-J 0.000 description 2
- 229910052622 kaolinite Inorganic materials 0.000 description 2
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- 229910003023 Mg-Al Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Substances OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Catalysts (AREA)
Abstract
The invention belongs to the technical field of catalysis, and relates to a preparation method of a catalyst carrier for preparing substitute natural gas from coal-based syngas. The catalyst carrier is prepared by the steps of mixing alumina (or pseudo-boehmite) with a soluble salt of magnesium, adding deionized water, fully mixing evenly, placing for a certain time, then drying, roasting, smashing, pelletizing with adding an adhesive, drying, carrying out tabletting forming, and roasting to obtain the catalyst carrier. The catalyst carrier prepared by the method has good hydrothermal stability, and has the water absorption rate of 35%-50%. A catalyst prepared by adopting the catalyst carrier and used for preparing the substitute natural gas from the coal-based syngas is suitable for a methanation reaction under conditions of relatively high CO content and relatively high reaction temperature, and can effectively prevent carbon deposition.
Description
Technical field
the invention belongs to catalysis technical field, be specifically related to a kind of preparation method of the catalyst carrier for preparing substitute natural gas by using coal based synthesis.
Background technology
natural gas is a kind of energy of high-efficiency cleaning.In recent years, along with " Shan gas is gone to the capital ", " in succession the building up and come into operation of the national combustion gas conveying engineering such as West-east Gas; the demand of natural gas is explosive growth; the insufficiency of supply-demand of natural gas is also increasing; and coal resources in China is relatively abundant; be an effective way that solves natural gas imbalance between supply and demand by coal based synthetic gas SNG, the coal chemical technology new bright spot of investment of coal to SNG project Cheng Liao China after coal liquefaction.
China is the country of " rich coal, oil-poor, weak breath ", utilize the coal resources of China's abundant, produce SNG by the methanation of coal based synthetic gas and there is good economic benefit at Waste Era of Oil, to solving the problem of complex utilization of coal resources, alleviate the present situation of Chinese Petroliferous shortage of resources, safeguard the energy security of China, realize CO
2reduce discharging, protection of the environment is all significant.China Petrochemical Industry will give priority to Coal Chemical Engineering Project during " 12 ", comprise MTO/MTP, coal to SNG, coal-ethylene glycol, coal artificial oil processed, and wherein, coal to SNG is the project of being badly in need of most in strategy.
Infusion process is one of important method of Kaolinite Preparation of Catalyst, preparation catalyst sample need to first be prepared the carrier of certain appearance and size, then soluble metal compound be impregnated in the endoporus of carrier, then obtain the catalyst of support type through suitable heat treatment.Catalyst activity component decentralization prepared by infusion process is high, and utilization rate is high, and in the industrial production of catalyst, application is very extensive.Carrier functions as follows catalyst: the mechanical strength that 1) improves catalyst; 2) increase active surface and suitable pore structure is provided; 3) improve the heat endurance of catalyst, save active component consumption, reduce the production cost of catalyst.
Mg-Al composite oxide to be to have acid and two kinds of activated centres of alkalescence, stable in properties, and the feature such as easy-sintering, does not more and more receive publicity, and becomes the important materials of Kaolinite Preparation of Catalyst.Magnesium aluminate spinel belongs to cubic system simultaneously, its unit cell is made up of oxonium ion and 16 aluminium ion and 8 magnesium ions in tetrahedron space in octahedral interstices of 32 cubic closest packings, this spinelle has higher heat endurance, its cell configuration at high temperature remains unchanged, and the fail temperature of lattice is 2135 ℃.The active spinelle that low-temperature bake is made, uses as catalyst carrier, has heatproof activity high, and the advantage that life cycle is long, is favored deeply.
At present, the catalyst of preparing substitute natural gas by using coal based synthesis is conventionally with Al
2o
3for carrier, methanation catalyst as disclosed in patent US 3933883 is take high-purity gama-alumina as carrier, supported active component nickel oxide and cobalt oxide.The disclosed methanation catalyst of patent CN 1043639A is with Al
2o
3for carrier, nickel is active constituent, with rare earth metal, or alkaline-earth metal, or alkali metal is co-catalyst.The disclosed methanation catalyst of patent CN 88109760.8 is with Al
2o
3for carrier.These methanation catalysts are take aluminium oxide as carrier, at trace amounts of CO
xmethanation reaction in use, reaction temperature is not high, in reacting gas, steam partial pressure is lower, catalyst has good stability.But the carrier hydrothermal stability of these catalyst is poor, be not suitable for using in the reaction of preparing substitute natural gas by using coal based synthesis.
Summary of the invention
the object of the invention is to provide a kind of preparation method for preparing substitute natural gas by using coal based synthesis catalyst carrier.
Catalyst carrier of the present invention is to mix with the soluble-salt of δ-aluminium oxide and magnesium, adds deionized water, fully mixes, through super-dry, roasting, pulverize, add binding agent granulation, dry, compression molding, roasting and make catalyst carrier.
Catalyst carrier of the present invention makes as follows: 1) a water aluminium oxide is heat-treated at 120 ℃ ~ 300 ℃ temperature; 2) soluble-salt of magnesium is joined in the aluminium oxide after roasting, add deionized water fully to mediate 0.5h, mix, at 100 ℃ ~ 140 ℃ temperature, dry, then at 350 ℃ ~ 550 ℃ roasting temperatures; 3) by roasting crushing material, mix with one or more in stearic acid, odium stearate, aluminum stearate, then add deionized water, mix rear granulation, obtain the particle of good fluidity, then particle is dried at 100 ℃ ~ 160 ℃ temperature; 4) particle of drying adds graphite to mix, compression molding; 5) tablet process is dried, then obtains catalyst carrier 700 ℃ ~ 1200 ℃ roastings.
Usually, in catalyst carrier preparation method of the present invention, at 120 ℃ ~ 300 ℃, a water alumina raw material is carried out to the heat treatment of 1h ~ 3h; At 350 ℃ ~ 550 ℃ temperature to magnesium and alumina mixture roasting 2 ~ 4h; After material adds deionized water to mix, material will be placed 10 ~ 24h, then carries out granulation with comminutor; At 700 ℃ ~ 1200 ℃, roasting 1h ~ 3h obtains catalyst carrier.
The catalyst carrier good hydrothermal stability that the inventive method is prepared, water absorption rate is 35% ~ 50%, the catalyst for preparing substitute natural gas by using coal based synthesis that adopts this catalyst carrier to prepare, be adapted at methanation reaction under higher CO content and higher reaction temperature, can effectively prevent carbon deposit.
The specific embodiment
describe the present invention below in conjunction with embodiment.
Embodiment 1: sample preparation
1) take 600g mono-water aluminium oxide, at 120 ℃ ~ 300 ℃, heat-treat, heat treatment time is 1h ~ 3h; 2) in the aluminium oxide after heat treatment, add the soluble-salt of 800g magnesium, add a certain amount of deionized water fully to mediate 0.5h, mix, at 100 ℃ ~ 140 ℃ temperature, dry, then at 350 ℃ ~ 550 ℃ roasting temperature 2 ~ 4h; 3) by roasting crushing material, add 24g cellulose and 500g deionized water, mediate the evenly rear 10h of placement; 4) be a granulated into by mediating uniform material the particle that particle diameter is about 1.2mm, at 120 ℃ of dry 3 ~ 5h; 5) particle of drying adds graphite to mix, and becomes cellular particle by tablet press machine compressing tablet; 6) tablet, 700 ℃ ~ 1200 ℃ roastings, obtains catalyst carrier I.
Embodiment 2: sample preparation
1) take 600g mono-water aluminium oxide, at 120 ℃ ~ 300 ℃, heat-treat, heat treatment time is 1h ~ 3h; 2) in the aluminium oxide after heat treatment, add the soluble-salt of 800g magnesium, add a certain amount of deionized water fully to mediate 0.5h, mix, at 100 ℃ ~ 140 ℃ temperature, dry, then at 350 ℃ ~ 550 ℃ roasting temperature 2 ~ 4h; 3) by roasting crushing material, add 24g cellulose and 500g deionized water, mediate the evenly rear 15h of placement; 4) be a granulated into by mediating uniform material the particle that particle diameter is about 1.2mm, at 120 ℃ of dry 3 ~ 5h; 5) particle of drying adds graphite to mix, and becomes cellular particle by tablet press machine compressing tablet; 6) tablet, 700 ℃ ~ 1200 ℃ roastings, obtains catalyst carrier II.
Embodiment 3: sample preparation
1) take 600g mono-water aluminium oxide, at 120 ℃ ~ 300 ℃, heat-treat, heat treatment time is 1h ~ 3h; 2) in the aluminium oxide after heat treatment, add the soluble-salt of 800g magnesium, add a certain amount of deionized water fully to mediate 0.5h, mix, at 100 ℃ ~ 140 ℃ temperature, dry, then at 350 ℃ ~ 550 ℃ roasting temperature 2 ~ 4h; 3) by roasting crushing material, add 24g cellulose and 500g deionized water, mediate the evenly rear 20h of placement; 4) be a granulated into by mediating uniform material the particle that particle diameter is about 1.2mm, at 120 ℃ of dry 3 ~ 5h; 5) particle of drying adds graphite to mix, and becomes cellular particle by tablet press machine compressing tablet; 6) tablet, 700 ℃ ~ 1200 ℃ roastings, obtains catalyst carrier III.
Embodiment 4: sample preparation
1) take 600g mono-water aluminium oxide, at 120 ℃ ~ 300 ℃, heat-treat, heat treatment time is 1h ~ 3h; 2) in the aluminium oxide after heat treatment, add the soluble-salt of 800g magnesium, add a certain amount of deionized water fully to mediate 0.5h, mix, at 100 ℃ ~ 140 ℃ temperature, dry, then at 350 ℃ ~ 550 ℃ roasting temperature 2 ~ 4h; 3) by roasting crushing material, add 24g cellulose and 500g deionized water, mediate the evenly rear 24h of placement; 4) be a granulated into by mediating uniform material the particle that particle diameter is about 1.2mm, at 120 ℃ of dry 3 ~ 5h; 5) particle of drying adds graphite to mix, and becomes cellular particle by tablet press machine compressing tablet; 6) tablet, 700 ℃ ~ 1200 ℃ roastings, obtains catalyst carrier IV.
In table, be the detection data of above-described embodiment gained carrier:
| ? | Catalyst I | Catalyst II | Catalyst III | Catalyst IV | Al 2O 3Carrier |
| Water absorption rate %(quality) | 35~38 | 36~40 | 38~43 | 38~45 | 28~35 |
| Intensity N/cm | 456 | 465 | 468 | 472 | 215 |
Embodiment 5: application
Get catalyst carrier I, II, III, IV and Al
2o
3carrier, takes identical preparation method and technique, for the preparation of catalyst I, II, III, IV and the V of preparing substitute natural gas by using coal based synthesis.
Catalyst I, II, III, IV and V are seated in respectively in fixed-bed tube reactor, and reaction condition is: pressure 3.0MPa, H
2/ CO=1.0 ~ 4.0, gas space velocity are 5000 ~ 30000h
-1, after 600 ℃ of reaction 500h, the activity keeping of catalyst I, II, III, IV is good, and wherein CO conversion ratio is 100%, and methane selectively is 100%, and the catalyst mechanical strength removing is still very high, and the surface of catalyst does not have carbon distribution; The activity decreased of catalyst V, the conversion ratio of CO declines, the area carbon of the catalyst removing.
Claims (7)
1. the preparation method for preparing substitute natural gas by using coal based synthesis catalyst carrier, it is characterized in that mixing with the soluble-salt of δ-aluminium oxide and magnesium, add deionized water, fully mix, through super-dry, roasting, pulverize, add binding agent granulation, dry, compression molding, roasting and make catalyst carrier.
2. the preparation method of catalyst carrier according to claim 1, is characterized in that catalyst carrier makes as follows: 1) a water aluminium oxide is heat-treated at 120 ℃ ~ 300 ℃ temperature; 2) soluble-salt of magnesium is joined in the aluminium oxide after roasting, add deionized water fully to mediate 0.5h, mix, at 100 ℃ ~ 140 ℃ temperature, dry, then at 350 ℃ ~ 550 ℃ roasting temperatures; 3) by roasting crushing material, mix with binding agent, then add deionized water, mix rear granulation, obtain the particle of good fluidity, then particle is dried at 100 ℃ ~ 160 ℃ temperature; 4) particle of drying adds graphite to mix, compression molding; 5) tablet process is dried, then obtains catalyst carrier 700 ℃ ~ 1200 ℃ roastings.
3. the preparation method of catalyst carrier according to claim 2, is characterized in that, at 120 ℃ ~ 300 ℃, a water alumina raw material is carried out to the heat treatment of 1h ~ 3h.
4. the preparation method of catalyst carrier according to claim 2, is characterized in that at 350 ℃ ~ 550 ℃ temperature magnesium and alumina mixture roasting 2 ~ 4h.
5. the preparation method of catalyst carrier according to claim 2, is characterized in that described binding agent is one or more in stearic acid, odium stearate, aluminum stearate.
6. the preparation method of catalyst carrier according to claim 2, after it is characterized in that material adds deionized water to mix, material will be placed 10 ~ 24h, then carries out granulation with comminutor.
7. the preparation method of catalyst carrier according to claim 2, is characterized in that roasting 1h ~ 3h obtains catalyst carrier at 700 ℃ ~ 1200 ℃.
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|---|---|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104475111A (en) * | 2014-11-24 | 2015-04-01 | 太原理工大学 | Catalyst for preparing methane by reaction of coal and carbon oxide and preparation method of catalyst |
| CN105435857A (en) * | 2014-09-09 | 2016-03-30 | 中国石油化工股份有限公司 | Preparation method for carbon dioxide methanation catalyst carrier |
| CN105457622A (en) * | 2014-09-09 | 2016-04-06 | 中国石油化工股份有限公司 | Preparation method for Cox methanation catalyst carrier |
| CN105562011A (en) * | 2014-10-11 | 2016-05-11 | 中国石油化工股份有限公司 | Preparation method of catalyst for preparing substitute natural gas from synthetic gas |
| CN105728060A (en) * | 2014-12-11 | 2016-07-06 | 中国石油化工股份有限公司 | Method for preparing catalyst carrier for preparing natural gas from coke oven gas |
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Application publication date: 20140611 |