CN104437563A - Catalytic coal gasification catalyst and preparation method and application thereof - Google Patents
Catalytic coal gasification catalyst and preparation method and application thereof Download PDFInfo
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- CN104437563A CN104437563A CN201310439546.2A CN201310439546A CN104437563A CN 104437563 A CN104437563 A CN 104437563A CN 201310439546 A CN201310439546 A CN 201310439546A CN 104437563 A CN104437563 A CN 104437563A
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- 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
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Abstract
The invention belongs to the technical field of catalytic coal gasification catalysts and provides a high-efficiency catalytic coal gasification catalyst prepared from a low-price halide ion metal salt and application thereof. According to the catalyst, the low-price halide ion metal salt serves as a precursor of the catalyst, a pH value regulator is adopted, active metal components are uniformly loaded on a coal base by virtue of an ion exchange technology, the active components are dispersed at an atomic scale, and corrosion of the halide ions to the reactor material is avoided. The catalyst prepared by the invention is applied to a fixed bed reactor for preparing natural gas by virtue of mild catalytic coal gasification, so that the conversion rate of converting the coal into gaseous products can be effectively improved, the composition of the coal gas can be changed, the content of methane is improved, and the coal utilization rate is greatly improved.
Description
Technical field
The present invention relates to a kind of Catalysts and its preparation method and purposes, particularly relate to a kind of Catalysts and its preparation method for catalytic coal gasifaction and purposes.
Background technology
Coal gasification, as one of the important means of coal machining and transform, is more and more subject to people's attention.This is because coal gasification can provide synthesis gas and substitute natural gas.If the colm such as dirty coal, fine coal can be utilized to gasify, protection of the environment is reduced costs significant.As the gentle gasification technology of one, the catalytic gasification of coal is that people quite feel must the research topic of interest always. key is wherein the selection of catalyst.So far the catalytic coal gasifaction catalyst studied almost includes the metallic element of the whole periodic table of elements.Mainly contain following several large class: his thing and salt of (1) metal oxide based on alkali and alkaline earth metal ions, metal hydrogen-oxygen, comprises NaOH, KOH, CaCO
3, K
2cO
3, Na
2cO
3, CaO etc.; (2) transition metal, mainly comprise iron, cobalt, nickel etc., wherein Ni shows preferably catalytic activity; (3) rare earth metal, mainly Ce (NO
3)
3, consider costliness and the not high factor of catalyst activity of price, the Coal Gasification research making catalyst with rare earth metal up to now does not cause the actual interest of people; (4) no matter the mineral matter in coal or ash content are which kind of coal is more or less always containing a certain amount of mineral matter (Fuel, 2000,79:427-438).Wherein alkali carbonate, as K
2cO
3, be the excellent catalyst of generally acknowledging at present, but this catalyst price is costly, is 10000 yuan/ton, meanwhile, due to the existence of clay mineral in coal, K in gasification
2cO
3to react generation lithium aluminium silicate with clay mineral, cause catalysqt deactivation; And lithium aluminium silicate is water insoluble, causes catalyst recovery difficulty, be difficult to recycle; And KCl price is relatively cheap, be 5000 yuan/ton, but directly adopt infusion process or mixing oxides method to be supported by KCl in coal-based material, its gasification efficiency is lower, and this is mainly owing to Cl
-electronegativity is comparatively strong, makes to have very strong affinity between anions and canons, and result causes cation can not bonding effective in the functional group of coal-based material surface well, thus can not show excellent catalytic effect, Cl simultaneously
-corrosion may be produced to reactor material, thus constrain cheap Cl
-slaine is applied in coal gasification (Energy & Fuels, 1987,1:308-309).
It is reported and found 80 number of chemical elements in current seawater, but its content difference is very large.Main chemical elements is 12 kinds, chlorine, sodium, magnesium, sulphur, calcium, potassium, bromine, carbon, strontium, boron, silicon, fluorine etc., and its content accounts for 99.8-99.9% of whole sewater chemistry constituent content, is therefore called as a great number of elements of seawater.Other element content in ocean is few, all at the trace element of 1 mg/litre hereinafter referred to as seawater.One of maximum feature of sewater chemistry element is that the ratio between above-mentioned 12 kinds of leading ion concentration is almost constant, is therefore called the constancy that seawater forms.In seawater, chloride content is the highest, accounts for 88.6%, is secondly that sulfate accounts for 10.8%.
Therefore, develop the cheap and halogen ion of abundance (as F
-, Cl
-and Br
-) slaine is a kind of invention technology of catalytic coal gasifaction catalyst, this to stride forward to industrialization for propelling third generation Coal Gasification Technology has important theoretical significance and actual application value.
Summary of the invention
The present invention is that catalytic coal gasifaction catalyst shows low gasification efficiency at coal gasification course according to halogen ionic metal salt cheap at present, providing a kind of ion exchange technique that utilizes effectively is distributed on coal-based material by the cationic components in chlorion slaine, cation is scattered on coal-based material with atom level, avoids halogen ion (as F simultaneously
-, Cl
-and Br
-) corrosion to reactor, the catalyst adopting the present invention to prepare is used for carrying out in catalytic coal gasification in fixed bed reactors, Activity Results shows to utilize catalyst provided by the present invention, and this catalyst shows conversion ratio and the methane-generated quantity that excellent coal changes gas-phase product in coal gasification reaction.
Catalytic coal gasifaction catalyst of the present invention, it is characterized in that the presoma of described catalyst is halogen ionic metal salt, catalyst active principle is the distribution in atom level on coal-based material, strong interaction is had to form mixture between catalyst and coal-based material, the particle diameter of this mixture is 60 order-100 orders, the loading of active component is metal quality and carbon-based material mass ratio, and loading is 6%-30%, and preferred loading is 10% ~ 25%.
Described coal-based material is brown coal, ub-bituminous coal, bituminous coal, coke, petroleum coke or anthracite;
Described halogen ionic metal salt, can be KCl, NaCl, CaCl
2, FeCl
3, MgCl
2, NiCl
2, a kind of, two or more combination in KBr, KF;
The preparation method of catalytic coal gasifaction catalyst of the present invention, is characterized in that, said method comprising the steps of:
1) with halogen ionic metal salt for catalyst precursor, it is soluble in water, and after it dissolves, be placed in one by coal-based material, fully stir and make it mix, the concentration of halogen ionic metal salt is 0.2-10 mol/L;
2) regulate solution ph by pH value regulator, adopt ion-exchange process to be effectively scattered in by metal component on coal-based material, by centrifugal, washing and dry, obtain the mixture of catalyst and coal-based material.
Usually, preparation method of the present invention is: coal-based material and chlorion slaine are placed in distilled water, regulate solution ph by pH value regulator, stir, again through centrifugal, washing and the process such as drying, after compressing tablet, fragmentation is screened to 40 order-80 orders, for coal gasification reaction.
Described pH value regulator, can be (NH
2)
2cO, NH
3, (NH
4)
2cO
3, NH
4hCO
3, NH
4cl, NH
4nO
3in a kind of, two or more combination.
Described solution ph is more than or equal to 7.
A kind of typical laboratory of the present invention preparation process is as follows:
The mixture taking 0.5-10 g KCl and NaCl is placed in beaker, measure 20-200 ml distilled water, being added drop-wise to by distilled water fills in the beaker of KCl and NaCl, stirring makes it dissolve, then 0.5-20 g coal is taken, joined in the aqueous solution of KCl and NaCl, stirring makes it mix, measure 60 ml ammoniacal liquor it to be dropwise added drop-wise in above-mentioned suspension, regulate the pH value of this suspension, continue to stir a period of time, until pH value is constant, through repeatedly centrifugal and washing process, until detect without Cl, then go in baking oven and carry out drying process, after compressing tablet, fragmentation is screened to 60 order-100 orders.
The significant advantage that the present invention presents shows as: the technology of the present invention changes the halogen ionic metal salt of cheapness into efficient catalytic coal gasifaction catalyst.The present invention gives a kind of presoma being catalytic coal gasifaction catalyst with the halogen ionic metal salt of cheapness, solution ph is regulated by pH value regulator, ion exchange technique is adopted to be distributed on coal-based material by effective metal component simple and fast, catalyst activity component penetrates in the micropore of coal-based material rapidly, and can be uniformly distributed, catalyst and coal-based material have stronger interaction force, simultaneously can the corrosion of skim halogen ion pair reactor material.The catalyst utilizing preparation technology provided by the present invention to prepare applies in the reaction of fixed bed coal catalytic gasification preparing natural gas, result display significantly reduces the gasification temperature of coal-based material, improve the gasification efficiency of coal-based material, in addition, within the identical time, utilize technology of preparing provided by the invention, the growing amount of methane prepares the methane content on catalyst higher than usual infusion process.This is conducive to the SNG process simplifying back segment operation, and therefore this meets the demand that people utilize the clean and effective of coal resources to a certain extent, accelerates the paces of the commercial Application of China's catalytic coal gasifaction preparing natural gas technology.
Detailed description of the invention
Below by way of specific embodiment, the inventive method is described in detail, but embodiment does not only form limitation of the scope of the invention for illustration of the present invention.
Embodiment 1:
Take 5.9 g KCl, add in 40 mL deionized waters, after dissolving completely, accurate for 1.5 g eastern coal is added wherein, continues stirring and make it mix, centrifugation, washing, carry out drying process, after compressing tablet, fragmentation is screened to 60 order-100 orders, and catalyst is labeled as KCl-ZD.
Catalytic coal gasification condition: de-ionized water flow rate 1.0 mL/min, reaction temperature 973 K, reaction system pressure 3.4 MPa.Efficiency of carbon con version curve and CH over time on this catalyst
4accumulation amount of precipitation is in table 1.
Embodiment 2:
Take 5.9 g KCl, be dissolved in 40 mL deionized waters, after dissolving completely, accurate for 1.5 g eastern coal added wherein, continuing stirring makes it mix, measure 40 mL ammoniacal liquor, it is dropwise joined in this suspension, continue to stir until solution ph remains unchanged, centrifugation, washing, carry out drying process, after compressing tablet, fragmentation is screened to 60 order-100 orders, and catalyst is labeled as KCl-1-ZD.
Catalytic coal gasification condition: de-ionized water flow rate 1.0 mL/min, reaction temperature 973 K, reaction system pressure 3.4 MPa.Efficiency of carbon con version curve and CH over time on this catalyst
4accumulation amount of precipitation is in table 1.
Embodiment 3:
Take 5.9 g KCl, be dissolved in 40 mL deionized waters, after dissolving completely, accurate for 1.5 g eastern coal added wherein, continuing stirring makes it mix, measure 60 mL ammoniacal liquor, it is dropwise joined in this suspension, continue to stir until solution ph remains unchanged, centrifugation, washing, carry out drying process, after compressing tablet, fragmentation is screened to 60 order-100 orders, and catalyst is labeled as KCl-2-ZD.
Catalytic coal gasification condition: de-ionized water flow rate 1.0 mL/min, reaction temperature 973 K, reaction system pressure 3.4 MPa.Efficiency of carbon con version curve and CH over time on this catalyst
4accumulation amount of precipitation is in table 1.
Embodiment 4:
Take 5.9 g KCl, be dissolved in 40 mL deionized waters, after dissolving completely, accurate for 1.5 g eastern coal added wherein, continuing stirring makes it mix, measure 80 mL ammoniacal liquor, it is dropwise joined in this suspension, continue to stir until solution ph remains unchanged, centrifugation, washing, carry out drying process, after compressing tablet, fragmentation is screened to 60 order-100 orders, and catalyst is labeled as KCl-3-ZD.
Catalytic coal gasification condition: de-ionized water flow rate 1.0 mL/min, reaction temperature 973 K, reaction system pressure 3.4 MPa.Efficiency of carbon con version curve and CH over time on this catalyst
4accumulation amount of precipitation is in table 1.
Embodiment 5:
Take 5.9 g KCl, 28.7g urea, add wherein by 80mL deionized water, until completely dissolved, accurate for 1.5 g eastern coal is added wherein, continue to be stirred to solution ph at 85 DEG C to remain unchanged, centrifugation, washing, carry out drying process, after compressing tablet, fragmentation is screened to 60 order-100 orders, and catalyst is labeled as KCl-4-ZD.
Catalytic coal gasification condition: de-ionized water flow rate 1.0 mL/min, reaction temperature 973 K, reaction system pressure 3.4 MPa.Efficiency of carbon con version curve and CH over time on this catalyst
4accumulation amount of precipitation is in table 1.
Embodiment 6:
Take 4 g KCl and NaCl mixture, be dissolved in 40 mL deionized waters, after dissolving completely, accurate for 2 g eastern coal is added wherein, continues stirring and make it mix, measure 80 mL (NH
4)
2cO
3solution, dropwise joins it in this suspension, continues to stir until solution ph remains unchanged, centrifugation, washing, and carry out drying process, after compressing tablet, fragmentation is screened to 60 order-100 orders, and catalyst is labeled as KCl-NaCl-5-ZD.
Catalytic coal gasification condition: de-ionized water flow rate 1.0 mL/min, reaction temperature 973 K, reaction system pressure 3.4 MPa.
Embodiment 7:
Take 8 g MgCl
2, be dissolved in 100 mL deionized waters, until completely dissolved, accurate for 6 g eastern coal added wherein, continues stirring and make it mix, measure 100 mL NH
4hCO
3solution, dropwise joins it in this suspension, continues to stir until solution ph remains unchanged, centrifugation, washing, and carry out drying process, after compressing tablet, fragmentation is screened to 60 order-100 orders, and catalyst is labeled as MgCl-6-ZD.
Catalytic coal gasification condition: de-ionized water flow rate 1.0 mL/min, reaction temperature 973 K, reaction system pressure 3.4 MPa.
Embodiment 8:
Take 9 g NaCl, be dissolved in 100 mL deionized waters, until completely dissolved, accurate for 12 g eastern coal is added wherein, continues stirring and make it mix, measure 100 mL NH
4cl solution, dropwise joins it in this suspension, continues to stir until solution ph remains unchanged, centrifugation, washing, and carry out drying process, after compressing tablet, fragmentation is screened to 60 order-100 orders, and catalyst is labeled as NaCl-7-ZD.
Catalytic coal gasification condition: de-ionized water flow rate 1.0 mL/min, reaction temperature 973 K, reaction system pressure 3.4 MPa.
From table 1, when not adding pH value regulator, KCl-ZD catalyst is when reaction proceeds to 50 min, and the conversion ratio that coal changes gas-phase product into is only 9.79%, and the output of methane is 0.56 mmol g
-1, when 250 min, the conversion ratio that on this catalyst, coal changes gas-phase product into is only 47.69%, and methane-generated quantity is 1.50 mmol g
-1and when taking ammoniacal liquor as pH value regulator, KCl-3-ZD catalyst is when experience 50 min gasification reaction, on this catalyst, carbon changes the conversion ratio of gas-phase product into is 19.2%, this result is 1.96 times of KCl-ZD catalyst prepared by conventional method, and when proceeding to 250 min, the conversion ratio that on KCl-3-ZD catalyst, coal changes gas-phase product into reaches 70.1%, far above 47.69% on KCl-ZD catalyst, now on this catalyst, methane-generated quantity is 1.7 times of KCl-ZD catalyst; Known additionally by table 1, with (NH
2)
2cO is pH value regulator, and the gasification efficiency of prepared KCl-4-ZD catalyst is pH value regulator not as good as ammoniacal liquor.
Shown by the above results, in catalytic coal gasifaction field, the technology of the present invention is utilized to change the halogen ionic metal salt of cheapness into efficient catalytic coal gasifaction catalyst, change on the conversion ratio of gas-phase product and methane-generated quantity at coal and all show good performance, the catalyst for catalytic coal gasifaction utilizing the inventive method to prepare, cost is low, and preparation method is simple, demonstrates good using value.。
Table 1 coal changes conversion ratio and the methane-generated quantity of gas-phase product into
Claims (8)
1. a catalytic coal gasifaction catalyst, it is characterized in that the presoma of described catalyst is halogen ionic metal salt, catalyst active principle is the distribution in atom level on coal-based material, strong interaction is had to form mixture between catalyst and coal-based material, the particle diameter of this mixture is 60 order-100 orders, the loading of active component is metal quality and carbon-based material mass ratio, and loading is 6%-30%.
2. catalytic coal gasifaction catalyst according to claim 1, is characterized in that the loading of described active component is 10% ~ 25%.
3. catalytic coal gasifaction catalyst according to claim 1, is characterized in that, halogen ionic metal salt is KCl, NaCl, CaCl
2, FeCl
3, MgCl
2, NiCl
2, a kind of, two or more combination in KBr, KF, NaF.
4. the preparation method of catalytic coal gasifaction catalyst according to claim 1, is characterized in that described coal-based material is the one in brown coal, ub-bituminous coal, bituminous coal, coke, petroleum coke or anthracite.
5. a preparation method for catalytic coal gasifaction catalyst, is characterized in that, said method comprising the steps of:
1) with halogen ionic metal salt for catalyst precursor, it is soluble in water, and after it dissolves, be placed in one by coal-based material, fully stir and make it mix, the concentration of halogen ionic metal salt is 0.2-10 mol/L;
2) regulate solution ph by pH value regulator, adopt ion-exchange process to be effectively scattered in by metal component on coal-based material, by centrifugal, washing and dry, obtain the mixture of catalyst and coal-based material.
6. the preparation method of catalytic coal gasifaction catalyst according to claim 5, is characterized in that, pH value regulator is (NH
2)
2cO, NH
3, (NH
4)
2cO
3, NH
4hCO
3, NH
4cl, NH
4nO
3in a kind of, two or more combination.
7. the preparation method of catalytic coal gasifaction catalyst according to claim 5, is characterized in that, the pH value of solution is more than or equal to 7.
8. the purposes of catalytic coal gasifaction catalyst according to claim 1, is characterized in that, described catalytic coal gasifaction catalyst as preparing methane from coal, coal hydrogen, the catalyst of producing synthesis gas from coal.
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CN107486244B (en) * | 2016-06-13 | 2020-04-28 | 中国石油化工股份有限公司 | Coal catalytic gasification catalyst and preparation method thereof |
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WO2020088398A1 (en) * | 2018-10-29 | 2020-05-07 | 中国石油化工股份有限公司 | Pulverized coal preprocessing method and pulverized coal gasiifying method |
AU2019372581B2 (en) * | 2018-10-29 | 2022-02-24 | China Petroleum & Chemical Corporation | Pulverized coal preprocessing method and pulverized coal gasiifying method |
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Application publication date: 20150325 |