CN104498118A - Deoxidizer of low-concentration oxygen-containing coal bed gas, preparation method and application thereof - Google Patents
Deoxidizer of low-concentration oxygen-containing coal bed gas, preparation method and application thereof Download PDFInfo
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- CN104498118A CN104498118A CN201410651923.3A CN201410651923A CN104498118A CN 104498118 A CN104498118 A CN 104498118A CN 201410651923 A CN201410651923 A CN 201410651923A CN 104498118 A CN104498118 A CN 104498118A
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- reductor
- lower concentration
- carrier
- containing oxygen
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Abstract
The invention discloses a deoxidizer of low-concentration oxygen-containing coal bed gas, a preparation method and an application thereof. The deoxidizer is composed of an active component and a carrier, wherein, the weight percentage of the active component is 5-15%, and the balance is the carrier; the active ingredient is sulfide, the carrier is one of active carbon, NaY molecular sieve and alumina. and carrier particle size scope is 250-850mum. The active component sulfide is one or more of Li2S, Na2S, K2S and Rb2S. The deoxidizer has the advantages of high deoxidation rate, high deoxidation activity and low cost.
Description
Technical field
The invention belongs to the field category of coal bed gas deoxidation, be specifically related to a kind of reductor of lower concentration coalbed methane containing oxygen, also relate to preparation method and the application of the reductor of this lower concentration coalbed methane containing oxygen simultaneously.
Background technology
Coal-seam gas main component is CH
4, be a kind of clean air energy be present in a large number in coal seam.China buried depth 2000m with shallow Coal bed gas project for 36.81 × 10
13m
3, be equivalent to 490 × 10
9t standard coal or 38 × 10
9m
3natural gas, occupies third place in the world.In order to ensure Safety of Coal Mine Production, need down-hole extraction coal-seam gas, owing to mixing into large quantity of air in the process of extraction, therefore CH in coal-seam gas
4concentration is generally on the low side, and wherein about 2/3rds lower than 30%, belongs to low concentration coal-bed gas.Be only limitted to burning and generating at present to the utilization of low concentration coal-bed gas, utilization ratio only accounts for 5 ~ 7% of total emission volumn, and all the other are all emptying, not only waste the energy, cause environmental pollution again.Therefore the exploitation of low concentration coal-bed gas can not only improve gas utilization rate, make up energy shortage; Reduce the emptying Greenhouse effect caused of methane, reduce environmental pollution; Also strengthen coal mine production safety simultaneously.
Lower concentration coalbed methane containing oxygen CH
4concentration is 6 ~ 25%, O
2concentration is up to 20%.According to safety regulations in coal mine requirement, gas density can not be stored and carry lower than 30%; When the aerial concentration of methane reaches 5 ~ 16%, meeting naked light can explode.If to the direct enrichment concentrate of lower concentration coalbed methane containing oxygen, with CH in tail gas
4concentration constantly reduces, O
2concentration constantly rises, and will certainly penetrate limits of explosion, dangerous, therefore O
2it is the key restriction factors that lower concentration coalbed methane containing oxygen is able to Appropriate application.At present, the method for deoxidation of the coal-seam gas of report mainly contains both at home and abroad: membrane separation process, absorption method (pressure-variable adsorption, chemisorption), combustion method (coke burning and catalyticcombustion) and reduction method.
China Patent Publication No. CN1799679A discloses a kind of denomination of invention for " a kind of coalbed gas condensation method " on July 12nd, 2006, what it adopted is that pressure-variable adsorption and membrane separation technique are combined, by membrane separation technique separation of methane and oxygen, deoxidation process needs pressurized operation, the limits of explosion of methane is caused to expand, there is serious potential safety hazard, and the preparation of film and Cost Problems limit industrially scalable.
China Patent Publication No. CN1919986A discloses a kind of denomination of invention for " a kind of coal bed gas coke deoxidization technique " on February 28th, 2007, and it adopts coke deoxidization technique to remove oxygen in coal-seam gas.Temperature of reaction is between 600 ~ 1000 DEG C, and it is unsuitable that temperature controls, portion of methane loss, and create impurity CO
2deng gas.
It is " a kind of catalytic conversion deoxidation method of coal-seam gas " that China Patent Publication No. CN101250449A discloses a kind of denomination of invention on August 27th, 2008, and it adds a small amount of water vapour in coal-seam gas, makes portion of methane be converted into CO and H
2be used for deoxidation, but deoxygenation pressure is comparatively large, in High-Temperature Deoxygenation process, easily penetrates the limits of explosion of methane, there is potential safety hazard.
China Patent Publication No. CN102872883A discloses a kind of denomination of invention for " supported non-noble metal oxygen-containing coal bed gas deoxidation catalyst and method for making and application " thereof on January 16th, 2013, China Patent Publication No. CN102784639A discloses a kind of denomination of invention for " coal bed gas deoxidation catalyst and its preparation method and application " on November 21st, 2012, describes coal bed gas deoxidation catalyst and carries out deoxidation by catalytic methane burning.Catalyzer main active component is Cu, Fe, Pt, adds metal promoter, is carried on porous support.Temperature on fire is all below 400 DEG C, and deoxidation effectiveness is high, but causes methane losses.
China Patent Publication No. CN101659890A disclosed " a kind of method of deoxidation of coal-seam gas and a kind of catalyzer " on March 3rd, 2010, adopted FeSO
4make reductive agent, exogenously added alkali metal makees catalyzer, at normal temperatures and pressures catalyzed oxidation, and DNA vaccine is 88-98%, but its processed in units amount is low, raw material FeSO
4draw materials inconvenience, cannot recycle, cost is higher.
Summary of the invention
The object of the invention is to the reductor reductor that above-mentioned shortcoming and a kind of high DNA vaccine provided, high deoxy activity, cheap lower concentration coalbed methane containing oxygen are provided.
Another object of the present invention is to the preparation method of the reductor that this lower concentration coalbed methane containing oxygen is provided.
Another object of the present invention is the application of the reductor providing this lower concentration coalbed methane containing oxygen.
The reductor of a kind of lower concentration coalbed methane containing oxygen of the present invention, is made up of active ingredient and carrier, wherein: the weight percentage of active ingredient is 5 ~ 15%, and all the other are carrier; Active ingredient is sulfide, and carrier is the one of gac, NaY molecular sieve, aluminum oxide, and diameter of carrier scope is: 250 ~ 850 μm.
Described active ingredient sulfide is Li
2s, Na
2s, K
2s, Rb
2one or more of S.
The preparation method of the reductor of a kind of lower concentration coalbed methane containing oxygen of the present invention, comprises the following steps:
(1) active ingredient sulfide is mixed with the aqueous solution that sulfonium ion concentration is 1.5 ~ 3mol/L;
(2) porous support be impregnated in sulfide solution, after normal temperature dipping 2 ~ 10h, at N
2in atmosphere protection, 80 ~ 150 DEG C of drying 1 ~ 5h, and obtain.
It is 5 ~ 20wt% that described reductor controls its water content by above-mentioned drying process.
An application method for the reductor of lower concentration coalbed methane containing oxygen, comprises the following steps:
(1) reductor is placed in fixed bed, passing into oxygen volume content is 5 ~ 20% coalbed methane containing oxygens;
(2) lower concentration coalbed methane containing oxygen gas air speed is 50 ~ 200h
-1, deoxidation temperature is between 100 ~ 300 DEG C, and reaction pressure is normal pressure, reacts to oxygen outlet concentration below 0.4%.
The present invention compared with prior art, has obvious beneficial effect, as can be known from the above technical solutions: the present invention take sulfide as active ingredient, and porous medium is carrier, utilizes incipient impregnation method to be prepared into reductor.This reductor has that cost is low, deoxidation amount is large, deoxidation feature thoroughly; And operational condition is suitable for, and gets final product deoxidation, again without methane losses, be suitable for the deoxidation of lower concentration coalbed methane containing oxygen under low-temperature atmosphere-pressure.
Embodiment
A preparation method for lower concentration oxygen-containing coal bed gas deoxidation agent, comprises the following steps:
(1) 7.5gNa is weighed
2s and 1gLi
2s is also soluble in water, constantly stirs, and is mixed with the aqueous solution that sulfonium ion concentration is 2.5mol/L;
(2) in the aqueous solution granular active carbon incipient impregnation of 50g prepared in step (1), after normal temperature dipping 1h, at N
2in atmosphere protection, 100 DEG C of dry 2h, obtained reductor.
The application of reductor:
Obtained reductor is reacted in atmospheric fixed bed reactor, when temperature of reaction is 300 DEG C, can be 16% by oxygen level, air speed is 100h
-1lower concentration oxygen-containing coal bed gas deoxidation to 0.0467%, the effective deoxidation amount of its unit is 487.71mL/g.
embodiment 2
The preparation method of lower concentration oxygen-containing coal bed gas deoxidation agent, comprise the following steps:
(1) 15gK is weighed
2s is also soluble in water, constantly stirs, and is mixed with the aqueous solution that sulfonium ion concentration is 2.5mol/L;
(2) in the aqueous solution alumina granules incipient impregnation of 50g prepared in step (1), after normal temperature dipping 1h, at N
2in atmosphere protection, 100 DEG C of dry 2h, obtained reductor.
The application of reductor:
Obtained reductor is reacted in atmospheric fixed bed reactor, when temperature of reaction is 300 DEG C, can be 16% by oxygen level, air speed is 200h
-1lower concentration oxygen-containing coal bed gas deoxidation to 0.3422%, the effective deoxidation amount of its unit is 20mL/g.
embodiment 3
The preparation method of lower concentration oxygen-containing coal bed gas deoxidation agent, comprise the following steps:
(1) 7.5gNa is weighed
2s is also soluble in water, constantly stirs, and is mixed with the aqueous solution of 2mol/L;
(2) in the aqueous solution particulate state NaY molecular sieve incipient impregnation of 50g prepared in step (1), after normal temperature dipping 1h, at N
2in atmosphere protection, 100 DEG C of dry 2h, obtained reductor.
The application of reductor:
Obtained reductor is reacted in atmospheric fixed bed reactor, when temperature of reaction is 100 DEG C, can be 16% by oxygen level, air speed is 100h
-1lower concentration oxygen-containing coal bed gas deoxidation to 0.0548%, the effective deoxidation amount of its unit is 28.84mL/g.
embodiment 4
A preparation method for lower concentration oxygen-containing coal bed gas deoxidation agent, comprises the following steps:
(1) 6gNa is weighed
2s and 10gRb
2s is also soluble in water, constantly stirs, and is mixed with the aqueous solution that sulfonium ion concentration is 2.5mol/L;
(2) in the aqueous solution particulate state NaY molecular sieve incipient impregnation of 50g prepared in step (1), after normal temperature dipping 1h, at N
2in atmosphere protection, 100 DEG C of dry 2h, obtained reductor.
The application of reductor:
Obtained reductor is reacted in atmospheric fixed bed reactor, when temperature of reaction is 200 DEG C, can be 16% by oxygen level, air speed is 100h
-1lower concentration oxygen-containing coal bed gas deoxidation to 0.0516%, the effective deoxidation amount of its unit is 20mL/g.
embodiment 5
The preparation method of lower concentration oxygen-containing coal bed gas deoxidation agent, comprise the following steps:
(1) 3gNa is weighed
2s, 5gK
2s and 5gRb
2s is also soluble in water, constantly stirs, and is mixed with the aqueous solution that sulfonium ion concentration is 2.5mol/L;
(2) by gac in tube-type atmosphere furnace, 600 DEG C of logical H
2roasting 5h;
(3) in the aqueous solution that the granular gac incipient impregnation of 50g step (2) prepared is prepared in step (1), after normal temperature dipping 1h, at N
2in atmosphere protection, 100 DEG C of dry 2h, obtained reductor.
The application of reductor:
Obtained reductor is reacted in atmospheric fixed bed reactor, when temperature of reaction is 200 DEG C, can be 16% by oxygen level, air speed is 100h
-1lower concentration oxygen-containing coal bed gas deoxidation to 0.0504%, the effective deoxidation amount of its unit is 46.41mL/g.
The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, anyly do not depart from technical solution of the present invention content, the any simple modification done above embodiment according to technical spirit of the present invention, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (6)
1. a reductor for lower concentration coalbed methane containing oxygen, is made up of active ingredient and carrier, wherein: the weight percentage of active ingredient is 5 ~ 15%, and all the other are carrier; Active ingredient is sulfide, and carrier is the one of gac, NaY molecular sieve, aluminum oxide.
2. the reductor of lower concentration coalbed methane containing oxygen as claimed in claim 1, wherein: diameter of carrier scope is 250 ~ 850 μm.
3. the reductor of lower concentration coalbed methane containing oxygen as claimed in claim 1 or 2, wherein: described active ingredient sulfide is Li
2s, Na
2s, K
2s, Rb
2one or more of S.
4. a preparation method for the reductor of lower concentration coalbed methane containing oxygen, comprises the following steps:
(1) active ingredient sulfide is mixed with the aqueous solution that sulfonium ion concentration is 1.5 ~ 3mol/L;
(2) porous support be impregnated in sulfide solution, after normal temperature dipping 2 ~ 10h, at N
2in atmosphere protection, 80 ~ 150 DEG C of drying 1 ~ 5h, and obtain.
5. the preparation method of the reductor of a kind of lower concentration coalbed methane containing oxygen as claimed in claim 1, wherein: it is 5 ~ 20wt% that described reductor controls its water content by above-mentioned drying process.
6. the application of reductor in lower concentration coalbed methane containing oxygen.
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| CN101301611A (en) * | 2008-07-07 | 2008-11-12 | 西南化工研究设计院 | Sulfur-tolerance deoxidation catalyst and preparation and use thereof |
| CN101322942A (en) * | 2008-07-29 | 2008-12-17 | 西南化工研究设计院 | Oxygen-containing coal bed gas deoxidation catalyst and preparation thereof as well as applications |
| CN101412538A (en) * | 2008-11-10 | 2009-04-22 | 江苏康洁环境工程有限公司 | Method for extracting arsenic trioxide from roasting dust of arsenic-containing gold concentrate powder |
| CN101664679A (en) * | 2009-11-17 | 2010-03-10 | 中国科学院大连化学物理研究所 | Coal bed gas deoxidation catalyst as well as preparation method and application thereof |
| CN102086055A (en) * | 2009-12-03 | 2011-06-08 | 中国科学院成都生物研究所 | Method for removing sulfide from wastewater |
| CN103589450A (en) * | 2012-08-14 | 2014-02-19 | 中国科学院大连化学物理研究所 | Ultra-deep oxidative desulfurization method of diesel oil |
-
2014
- 2014-11-17 CN CN201410651923.3A patent/CN104498118A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101301611A (en) * | 2008-07-07 | 2008-11-12 | 西南化工研究设计院 | Sulfur-tolerance deoxidation catalyst and preparation and use thereof |
| CN101322942A (en) * | 2008-07-29 | 2008-12-17 | 西南化工研究设计院 | Oxygen-containing coal bed gas deoxidation catalyst and preparation thereof as well as applications |
| CN101412538A (en) * | 2008-11-10 | 2009-04-22 | 江苏康洁环境工程有限公司 | Method for extracting arsenic trioxide from roasting dust of arsenic-containing gold concentrate powder |
| CN101664679A (en) * | 2009-11-17 | 2010-03-10 | 中国科学院大连化学物理研究所 | Coal bed gas deoxidation catalyst as well as preparation method and application thereof |
| CN102086055A (en) * | 2009-12-03 | 2011-06-08 | 中国科学院成都生物研究所 | Method for removing sulfide from wastewater |
| CN103589450A (en) * | 2012-08-14 | 2014-02-19 | 中国科学院大连化学物理研究所 | Ultra-deep oxidative desulfurization method of diesel oil |
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Application publication date: 20150408 |