CN102417835A - Method for preparing hydrogen-rich gas by performing catalytic gasification on petroleum coke - Google Patents
Method for preparing hydrogen-rich gas by performing catalytic gasification on petroleum coke Download PDFInfo
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- CN102417835A CN102417835A CN2011103088491A CN201110308849A CN102417835A CN 102417835 A CN102417835 A CN 102417835A CN 2011103088491 A CN2011103088491 A CN 2011103088491A CN 201110308849 A CN201110308849 A CN 201110308849A CN 102417835 A CN102417835 A CN 102417835A
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Abstract
The invention discloses a method for preparing hydrogen-rich gas by performing catalytic gasification on petroleum coke. The method comprises the following steps of: fully mixing a catalyst with petroleum coke; undergoing a catalytic gasification reaction under the condition that the gasification temperature is 700-900 DEG C, the steam partial pressure is 40-70 percent and the gasification reaction time is 10-120 minutes; and leading coal gas produced by catalytic gasification, and removing steam by condensing to obtain hydrogen-rich gas. According to the invention, the reaction speed of petroleum coke can be raised by 1.5-4 times, the H2 content of the coal gas is increased by 1-15 percent, a novel method for preparing hydrogen-rich gas is opened up, and resource utilization of petroleum coke is realized; and moreover, a soluble salt catalyst in gasification residues can be recovered with a water dissolution method, so that cyclic utilization of the catalyst is realized.
Description
Technical field
The present invention relates to a kind of method for preparing hydrogen-rich gas, relate to the method that a kind of refinery coke catalytic gasification prepares hydrogen-rich gas specifically, belong to the derived energy chemical field.
Technical background
Refinery coke is the main sub product of petroleum chemical enterprise.In recent years, along with the continuous increase of petroleum demand amount and the heaviness of world's crude oil, the output of refinery coke constantly increases.According to statistics, the burnt ultimate production of China's oil in 2007 is above 1,800 ten thousand tons.The burnt output of China's oil improves constantly and domestic market demand is saturated basically, and the easy problem of state's refinery coke is more and more outstanding still.Therefore, how the inferior fuel that refinery coke, especially high sulfur petroleum coke are such turns waste into wealth, and rationally utilizing becomes the problem that presses for solution.Refinery coke has the characteristics of high heating value, high-carbon content, low ash content and low volatile, can be used as fuel, recycles through the mode of burning or gasification.But along with the increasingly stringent of environmental protection policy, to the raising that the air pollution emission thing requires, seek more efficiently refinery coke (especially high sulfur petroleum coke) utilization technology is the target of people's unremitting pursue always.
Energy dilemma is the common issue with that the whole world faces, and factors such as the non-renewable and greenhouse gas emission of fossil energy promote development renewable and clean energy.Hydrogen Energy is one of ideal clean energy, also is a kind of good energy carrier, and along with the breakthrough and the commercialization of fuel cell and hydrogen storage technology, Hydrogen Energy will become a kind of very important energy in this century on the energy stage.Hydrogen Energy is dirty to environment zero in utilizing process, plays a significant role at space industry as the energy.The hydrogen preparation technique of current comparative maturity mainly is that water electrolysis hydrogen production and mineral fuel are raw material hydrogen manufacturing.In recent years; There is the scholar to propose refinery coke to be changed into high value hydrogen, synthetic gas etc. by high-temperature gasification; Not only can solve the difficulty that needs hydrogen manufacturing in the modern refining of petroleum; And can the form of the sulphur in the raw material with elemental sulfur be reclaimed, be a very promising technology that realizes the refinery coke resource utilization, have promotion prospect widely.
At present refinery coke has begun to try out as the raw material of high-temperature gasification, find that its activity can not show a candle to coal tar, and this has greatly restricted the feasibility that refinery coke is used as gasified raw material.The gasification temperature of the Coal Gasification Technology of suitability for industrialized production is generally 1100～1700 ℃, and only under such high temperature, gasification reaction speed just can satisfy industrial production requirement.As to realize effective utilization of refinery coke, must under higher gasification temperature, carry out gasification reaction.The temperature of gasification is high more, need to consume more raw materials and keep the high-temperature gasification state, and the gas products of outlet can bring power loss because temperature is high in temperature-fall period.In addition, under the high-temperature gasification condition, receive the restriction of high-temperature gasification reaction mechanism, the content of CO is very high in the gas composition, in the technology of producing synthetic gas or hydrogen, must cause the complex energy utilising efficiency low the CO conversion of reforming.
The catalytic gasification technology can significantly reduce temperature of reaction because of it has after English Patent in 1867 is open first, improve speed of reaction, improves coal gas and forms, and increases plurality of advantages such as gas yield and has caused people's extensive concern.Wherein, cheap, efficient, callable catalyzer is the catalytic coal gasifaction hot research fields always.With regard to catalyzer, sylvite, sodium salt, calcium salt, molysite and an otheralkali metal and earth alkali metal soluble salt all have catalytic effect in various degree.But test finds, the soluble salt catalyzer of these basic metal and earth alkali metal in gasification, understand with coal in the mineral substance such as clay that exist react and deactivation phenomenom occurs.Moreover, original water-soluble soluble salt has become water-fast composition in the coal ash that obtains after the gasification, causes catalyzer to be difficult to reclaim recycle in addition.And the ash oontent of refinery coke extremely low (being generally less than 1%), the soluble salt catalyzer that adds in the gasification with can not react and inactivation with the ash content in the refinery coke.And, can adopt simple water-soluble method to reclaim soluble salt in the gasification resistates behind the gasification reaction to realize the recycle of catalyzer.Therefore; The catalytic gasification technology is applied to the refinery coke gasification reaction; Not only can guarantee that refinery coke still has higher speed of reaction satisfying industrial production requirement under lower temperature of reaction, and the content that can effectively improve hydrogen in the coal gas is to produce hydrogen-rich gas.In addition, can adopt simple water-soluble method to reclaim catalyzer in the gasification resistates behind the gasification reaction to realize the recycle of catalyzer.Therefore, method disclosed by the invention is practical, economic and practical, is a very promising technology that realizes the refinery coke resource utilization, has promotion prospect widely.
Summary of the invention
The invention discloses the method that a kind of refinery coke catalytic gasification prepares hydrogen-rich gas, to realize that refinery coke, especially high sulfur petroleum coke are efficient, the recycling of environmental protection.
The present invention realizes through following technical scheme:
A kind of refinery coke catalytic gasification prepares the method for hydrogen-rich gas, it is characterized in that, said method comprises the steps:
(1) with behind catalyzer and the refinery coke thorough mixing of particle diameter, at N less than 0.074mm (200 order)
2Atmosphere, 105～110 ℃ of following thorough drying to quality constant weights, wherein the addition of catalyzer is 0.5～50%, is 100% in the weight of refinery coke;
(2) be that 650～900 ℃, steam partial pressure are to carry out the catalytic gasification reaction under 40～70% the condition with the mixture of step (1) gained at gasification temperature; Reaction times is 10～120 minutes, and the gasification product gas of generation promptly obtains hydrogen-rich gas after condensation removes water vapour;
Wherein, described catalyzer is for being selected from soluble salt K
2CO
3, KNO
3, KAc, K
2SO
4, KCl, Na
2CO
3, NaNO
3, NaAc, Na
2SO
4, NaCl, Ca (NO
3)
2, Ca (Ac)
2, CaCl
2, Fe (NO
3)
3, Ni (NO
3)
2And Cu (NO
3)
2In one or more, or be selected from wood vinegar, black liquid, biomass ash, the gasification lime-ash one or more.
In technique scheme, the refinery coke of described refinery coke preferred dry basis ash content content＜1% (mass ratio).
In technique scheme, described soluble salt catalyzer K
2CO
3, KNO
3, KAc, K
2SO
4, KCl, Na
2CO
3, NaNO
3, NaAc, Na
2SO
4, NaCl, Ca (NO
3)
2, Ca (Ac)
2, CaCl
2, Fe (NO
3)
3, Ni (NO
3)
2And Cu (NO
3)
2In one or more and wood vinegar and black liquid, adopt pickling process to mix, or it is surperficial to refinery coke to be mixed with spray solution with said refinery coke.
Described biomass ash and gasification lime-ash catalyzer adopt wet mixing method to mix with refinery coke.
In technique scheme, described steam partial pressure is preferably 60%.
The soluble salt catalyzer that the present invention adopted can adopt simple water-soluble method to reclaim to realize the recycle of catalyzer behind gasification reaction.In addition; The part catalyzer that the present invention adopted is a trade waste; Adopt these trade wastes not only economic and practical, and can realize the utilization again of these trade wastes, have far-reaching social effect and economic implications as the catalyzer of refinery coke gasification reaction.
Beneficial effect
The present invention has following unusual effect:
1. the present invention is with H in the exit gas
2Content improves 1～15 percentage point, makes H
2Content accounts for more than 50% (volume ratio) of exit gas, improving refinery coke gasification reaction speed with when satisfying the suitability for industrialized production requirement, effectively improves H in the coal gas
2Content is with the preparation hydrogen-rich gas, thereby with refinery coke, especially the such inferior fuel of high sulfur petroleum coke is converted into the synthetic gas or the hydrogen-rich gas of high value, has realized the recycling of refinery coke.Widened the approach that refinery coke utilizes, realized that refinery coke is efficient, environmental protection ground trans-utilization.
2. with the catalyzer of trade wastes such as the industrial residue of wood vinegar, black liquid, biomass ash, steel-making and iron work and the lime-ash that gasifies, realized the utilization again of these trade wastes as the refinery coke gasification reaction.Extremely cheap, the wide material sources of these trade waste prices are convenient to the scale operation of enterprise.
3. contain a certain amount of organic matter that does not transform fully in the trade waste such as wood vinegar, the gentle ashing slag of black liquid, this part organic matter also can be converted into coal gas in gasification, thereby can effectively improve the gas yield of unit refinery coke.Meanwhile, these trade waste wherein contained organic content after gasification as catalyzer significantly reduce, and help these trade wastes as purposes such as cement, material of construction.
4. the reaction of refinery coke catalytic gasification can be carried out under lower temperature apace; Thereby can solve well in the high-temperature gasification that the coal gas cooling intensity is big, energy consumption big, to problems such as equipment requirements height and high temperature purification difficulties, can effectively avoid simultaneously under the high-temperature gasification condition CO is reformed that conversion prepares hydrogen-rich gas and the total energy approach inefficiency that causes.
5. because the ash oontent of refinery coke is extremely low, the soluble salt catalyzer that wherein adds can be through water-soluble method efficient recovery behind gasification reaction, thus the recycle of realization catalyzer.
6 the present invention are simple to operate applied widely, go for the catalytic gasification reaction process of any low gasification reactivity carbonaceous material.
Embodiment
Below by embodiment the present invention is further set forth, its objective is be beneficial to better understand content of the present invention and and unrestricted protection scope of the present invention.The experimental technique of not marked actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.Except as otherwise noted, all per-cent and umber are by weight.
Comparative Examples 1: take by weighing the 1g refinery coke, be at gasification temperature that 1000 ℃, steam partial pressure are 60%, the gasification reaction time is to gasify under the 120min condition, adopts online gaseous mass analyzer that the composition of coal gas is detected.The percentage composition of each gaseous fraction is as shown in table 1 in the coal gas of gained.
Embodiment 1: take by weighing the 10g particle diameter less than 0.074mm refinery coke and 0.69g K
2CO
3(K
2The content of CO3 is 6.90%, is 100% in the weight of refinery coke) adopt the method thorough mixing of solution impregnation, with processing laboratory sample after the above-mentioned sample oven dry; Take by weighing the 1.069g laboratory sample, be at gasification temperature that 750 ℃, steam partial pressure are 60%, the gasification reaction time is to gasify under the 60min condition.The percentage composition of each gaseous fraction is as shown in table 1 in the coal gas of gained.
Embodiment 2: take by weighing the 10g particle diameter and adopt the method thorough mixing of spray solution less than 0.074mm refinery coke and 0.098g KAc (content of KAc is 0.98%, is 100% in the weight of refinery coke), with processing laboratory sample after the above-mentioned sample oven dry; Take by weighing the 1.01g laboratory sample and gasify, gasification condition such as embodiment 1.The percentage composition of each gaseous fraction is as shown in table 1 in the coal gas of gained.
Embodiment 3: take by weighing the 10g particle diameter less than 0.074mm refinery coke and 0.085g NaNO
3(NaNO
3Content be 0.85%, be 100% in the weight of refinery coke) adopt the method thorough mixing of solution impregnation, with processing laboratory sample after the above-mentioned sample oven dry; Take by weighing the 1.01g laboratory sample and gasify, gasification condition such as embodiment 1.The percentage composition of each gaseous fraction is as shown in table 1 in the coal gas of gained.
Embodiment 4: take by weighing the 10g particle diameter less than 0.074mm refinery coke and 1g Ca (NO
3)
2(Ca (NO
3)
2Content be 10%, be 100% in the weight of refinery coke) adopt the method thorough mixing of solution impregnation, with processing laboratory sample after the above-mentioned sample oven dry; Take by weighing the 1.10g laboratory sample and gasify, gasification temperature is that 850 ℃, steam partial pressure are 40%, and the gasification reaction time is 90min.The percentage composition of each gaseous fraction is as shown in table 1 in the coal gas of gained.
Embodiment 5: (content of cotton bar ash is 25% less than the cotton bar ash of 0.074mm less than 0.074mm refinery coke and 2.5g granularity to take by weighing the 10g particle diameter; Weight in refinery coke is 100%) adopt the method thorough mixing of wet mixing, with processing laboratory sample after the above-mentioned sample oven dry; Take by weighing the 1.25g laboratory sample and gasify, gasification temperature is that 800 ℃, steam partial pressure are 50%, and the gasification reaction time is 50min.The percentage composition of each gaseous fraction is as shown in table 1 in the coal gas of gained.
Embodiment 6: (content of corn stalk ash is 25% less than the corn stalk ash of 0.074mm less than 0.074mm refinery coke and 2.5g granularity to take by weighing the 10g particle diameter; Weight in refinery coke is 100%) adopt the method thorough mixing of wet mixing, with processing laboratory sample after the above-mentioned sample oven dry; Take by weighing the 1.25g laboratory sample and gasify, gasification condition such as embodiment 1.The percentage composition of each gaseous fraction is as shown in table 1 in the coal gas of gained.
Embodiment 7: (content of cotton bar ash is 45% less than the cotton bar ash of 0.074mm less than 0.074mm refinery coke and 4.5g granularity to take by weighing the 10g particle diameter; Weight in refinery coke is 100%) adopt the method thorough mixing of wet mixing, with processing laboratory sample after the above-mentioned sample oven dry; Take by weighing the 1.45g laboratory sample and gasify, gasification condition such as embodiment 5.The percentage composition of each gaseous fraction is as shown in table 1 in the coal gas of gained.
Embodiment 8: take by weighing the 10g particle diameter and adopt the method thorough mixing of solution impregnation less than 0.074mm refinery coke and 0.98g wood vinegar (content of wood vinegar is 9.8%, is 100% in the weight of refinery coke), with processing laboratory sample after the above-mentioned sample oven dry; Take by weighing the 1.098g laboratory sample and gasify, gasification condition such as embodiment 1.The percentage composition of each gaseous fraction is as shown in table 1 in the coal gas of gained.
Embodiment 9: take by weighing the 10g particle diameter and adopt the method thorough mixing of spray solution less than 0.074mm refinery coke and 0.98g wood vinegar (content of wood vinegar is 9.8%, is 100% in the weight of refinery coke), with processing laboratory sample after the above-mentioned sample oven dry; Take by weighing the 1.098g laboratory sample and gasify, gasification temperature is that 850 ℃, steam partial pressure are 40%, the gasification time is to gasify under the 60min condition.The percentage composition of each gaseous fraction is as shown in table 1 in the coal gas of gained.
Embodiment 10: (gasification lime-ash mineral content is 30% less than the gasification lime-ash of 0.074mm less than 0.074mm refinery coke and 3.80g granularity to take by weighing the 10g particle diameter; Weight in refinery coke is 100%) adopt the method thorough mixing of wet mixing, with processing laboratory sample after the above-mentioned sample oven dry; Take by weighing the 1.38g laboratory sample and gasify, gasification temperature is that 900 ℃, steam partial pressure are 60%, the reaction times is to gasify under the 90min condition.The percentage composition of each gaseous fraction is as shown in table 1 in the coal gas of gained.
The percentage composition of all gases component in the coal gas of each instance gained of table 1
Can find out by table 1, compare that the gasification reaction activity that adds soluble salt or contain the refinery coke (embodiment 1～10) of the trade waste of mineral ion has improved 1.5～4 times, H in the coal gas with Comparative Examples 1
2Content has improved 1～15 percentage point.In addition, the soluble salt catalyzer of adding can be through water-soluble method efficient recovery, and catalyzer can be realized recycle, and the trade waste catalyst economy that adopts is suitable for, and need not to reclaim.Therefore, the method that a kind of refinery coke catalytic gasification disclosed by the invention prepares hydrogen-rich gas is practical, economic and practical, is a very promising technology that realizes the refinery coke resource utilization, has promotion prospect widely.
Claims (5)
1. a refinery coke catalytic gasification prepares the method for hydrogen-rich gas, it is characterized in that said method comprises the steps:
(1) with behind catalyzer and the refinery coke thorough mixing of particle diameter, at N less than 0.074mm (200 order)
2Atmosphere, 105～110 ℃ of following thorough drying to quality constant weights, wherein the addition of catalyzer is 0.5～50%, is 100% in the weight of refinery coke;
(2) be that 650～900 ℃, steam partial pressure are to carry out the catalytic gasification reaction under 40～70% the condition with the mixture of step (1) gained at gasification temperature; Reaction times is 10～120 minutes, and the gasification product gas of generation promptly obtains hydrogen-rich gas after condensation removes water vapour;
Wherein, described catalyzer is for being selected from soluble salt K
2CO
3, KNO
3, KAc, K
2SO
4, KCl, Na
2CO
3, NaNO
3, NaAc, Na
2SO
4, NaCl, Ca (NO
3)
2, Ca (Ac)
2, CaCl
2, Fe (NO
3)
3, Ni (NO
3)
2And Cu (NO
3)
2In one or more, or be selected from wood vinegar, black liquid, biomass ash, the gasification lime-ash one or more.
2. a kind of refinery coke catalytic gasification as claimed in claim 1 prepares the method for hydrogen-rich gas, it is characterized in that, described refinery coke is the refinery coke of dry basis ash content mass content＜1%.
3. a kind of refinery coke catalytic gasification as claimed in claim 1 prepares the method for hydrogen-rich gas, it is characterized in that, and in step (1), described soluble salt catalyzer K
2CO
3, KNO
3, KAc, K
2SO
4, KCl, Na
2CO
3, NaNO
3, NaAc, Na
2SO
4, NaCl, Ca (NO
3)
2, Ca (Ac)
2, CaCl
2, Fe (NO
3)
3, Ni (NO
3)
2And Cu (NO
3)
2In one or more and wood vinegar and black liquid, adopt pickling process to mix, or it is surperficial to refinery coke to be mixed with spray solution with said refinery coke.
4. a kind of refinery coke catalytic gasification as claimed in claim 1 prepares the method for hydrogen-rich gas, it is characterized in that, in step (1), described biomass ash and gasification lime-ash catalyzer adopt wet mixing method to mix with refinery coke.
5. a kind of refinery coke catalytic gasification as claimed in claim 1 prepares the method for hydrogen-rich gas, it is characterized in that, in step (2), described steam partial pressure is 60%.
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|---|---|---|---|
| CN2011103088491A CN102417835A (en) | 2011-10-13 | 2011-10-13 | Method for preparing hydrogen-rich gas by performing catalytic gasification on petroleum coke |
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Cited By (6)
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| CN104437563A (en) * | 2013-09-25 | 2015-03-25 | 中国石油化工股份有限公司 | Catalytic coal gasification catalyst and preparation method and application thereof |
| CN104538645A (en) * | 2014-12-22 | 2015-04-22 | 山西大学 | Preparation method of active coal coke powder for solid oxide fuel cells |
| CN106635175A (en) * | 2016-12-22 | 2017-05-10 | 中国科学院山西煤炭化学研究所 | Catalytic gasification method for petroleum coke |
| CN107349948A (en) * | 2017-06-15 | 2017-11-17 | 华东理工大学 | A kind of iron alkali composite catalyst for DCL/Direct coal liquefaction |
| CN107583658A (en) * | 2017-08-29 | 2018-01-16 | 华中科技大学 | A kind of preparation method of coal tar catalyst based on ash component and products thereof |
| CN108517225A (en) * | 2018-04-26 | 2018-09-11 | 东北大学 | A method of improving petroleum coke gasification reactivity |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437563A (en) * | 2013-09-25 | 2015-03-25 | 中国石油化工股份有限公司 | Catalytic coal gasification catalyst and preparation method and application thereof |
| CN104538645A (en) * | 2014-12-22 | 2015-04-22 | 山西大学 | Preparation method of active coal coke powder for solid oxide fuel cells |
| CN104538645B (en) * | 2014-12-22 | 2016-09-28 | 山西大学 | Active coke raw powder's production technology for SOFC |
| CN106635175A (en) * | 2016-12-22 | 2017-05-10 | 中国科学院山西煤炭化学研究所 | Catalytic gasification method for petroleum coke |
| CN107349948A (en) * | 2017-06-15 | 2017-11-17 | 华东理工大学 | A kind of iron alkali composite catalyst for DCL/Direct coal liquefaction |
| CN107583658A (en) * | 2017-08-29 | 2018-01-16 | 华中科技大学 | A kind of preparation method of coal tar catalyst based on ash component and products thereof |
| CN107583658B (en) * | 2017-08-29 | 2020-05-19 | 华中科技大学 | Preparation method of coal coke catalyst based on ash component and product thereof |
| CN108517225A (en) * | 2018-04-26 | 2018-09-11 | 东北大学 | A method of improving petroleum coke gasification reactivity |
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Application publication date: 20120418 |