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CN103191710A - Method for preparing denitration catalyst and application of denitration catalyst prepared by the method in denitration - Google Patents

Method for preparing denitration catalyst and application of denitration catalyst prepared by the method in denitration Download PDF

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CN103191710A
CN103191710A CN2013100852153A CN201310085215A CN103191710A CN 103191710 A CN103191710 A CN 103191710A CN 2013100852153 A CN2013100852153 A CN 2013100852153A CN 201310085215 A CN201310085215 A CN 201310085215A CN 103191710 A CN103191710 A CN 103191710A
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black liquor
lignin
denitration
catalyst
dry
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项学敏
金佩玉
王刃
王晓坤
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Dalian University of Technology
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Dalian University of Technology
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Abstract

The invention provides a method for preparing a Selective Catalytic Reduction (SCR) denitration catalyst by using papermaking black liquor lignin and cerium nitrate as main raw materials and application of the denitration catalyst prepared by the method in denitration. The method adopts an acid precipitation method to extract the lignin of the papermaking black liquor, utilizes the lignin of the papermaking black liquor to prepare the active carbon, and utilizes the prepared active carbon to load the active component cerium oxide to prepare the catalyst product. The invention can not only solve NO in paper making enterprisesXNO polluting and applicable for other industriesXIn pollution control, the utilization value of black liquor lignin resource can be improved, the waste polluting the environment is converted into a product with huge industrial demand, the waste is treated by waste, and the method has obvious economic, environmental protection and social benefits. Meanwhile, the method has the advantages of low treatment cost, no need of an additional reducing agent, safe and simple operation, long service life of the catalyst and high denitration activityAnd the like.

Description

Prepare the method for denitrating catalyst and the application of denitrating catalyst in denitration that is prepared by this method
Technical field
The invention belongs to the denitrating catalyst preparing technical field, be specifically related to a kind of the prepare method of denitrating catalyst and the application of denitrating catalyst in denitration that is prepared by this method.
Background technology
In the water environment protection field, China's black liquid pollutes very serious, accounts for more than 90% of whole paper industry pollutional load.Therefore, solving the black liquor problem is the key of paper mill environmental disposal problem.Lignin in the black liquor is the main component that causes black liquor pollution.Administer, utilize the method for black liquor to mainly contain both at home and abroad: Silvola recovery, acid-precipitation method, flocculence, membrane separation process, bioanalysis etc.Though these methods all are main purpose with the separating lignin, present most of papermaking enterprises are because of fund and technical limitations, only by simply adding the lignin in the acid extractants black liquor.Because the black liquor lignin lacks market, have to be landfilled or burn, and not only causes environmental pollution, also wasted valuable lignin resource, if the black liquor lignin as a kind of resource rational utilization, not only can be reduced pollution, can also create considerable economic value.
The report of black liquor lignin resource was just arranged as far back as the eighties in 19th century.At present, lignin derivative both domestic and external is also more and more, use also more extensive, as the dispersant of slurries additive agent, desulfurizing agent, cationic flocculant, antisludging agent, synvaren, pulp additive, pesticide slow-releasing agent, fertilizer, ore floatation agent, cement plasticizer, oil field chemical, printing and dyeing industry and color additive etc., and also constantly occur in recent years about the report of being prepared the active carbon with difference in functionality by the lignin that from black liquid of straw pulp paper-making, reclaims by acid-precipitation method.But at present be applied to the routine absorption of the materials such as heavy metal, formaldehyde, oil gas, colourity in the sewage disposal or the storage of hydrogen by the active carbon of black liquor lignin preparation more, and do not appear in the newspapers as yet for the preparation of the application of SCR (SCR) method denitrating catalyst.
Numerous enterprises such as China paper mill, thermal power plant, nitric plant, chemical pharmaceutical factory all are NO XStationary source, NO XIndustrial source is big because of concentration, potential danger is high receives increasing concern.During the Chinese Ministry of Environmental Protection " 12 " with NO XAlso include overall control in, formulated concrete reduction of discharging standard.At present, denitration method for flue gas mainly contains catalysis method and on-catalytic method, and using is catalysis method more widely, mainly contains three-way catalyst method, catalytic decomposition method and SCR (SCR) method.Wherein, SCR technology flue gas treating capacity is big, denitration efficiency is high, technology maturation, has become one of main gas denitrifying technology.At present, the commercial SCR method denitrating catalyst of using always both at home and abroad is V 2O 5/ TiO 2, have advantages such as denitration efficiency height, good stability, add auxiliary agent WO simultaneously 3Improve its heat endurance, but the preparation condition strictness, the cost height, strong toxicity causes the obstruction of equipment and pipeline easily.In addition, at present both at home and abroad with Al 2O 3, TiO 2, active carbon, molecular sieve etc. need NH for the SCR method denitrating catalyst major part of preparing carriers 3, gas such as CO is as reducing agent, involves great expense, and easily causes secondary pollution, storage and operating difficulties, potential safety hazard is big.
CN102513095A is carrier with cocoanut active charcoal, active fruit shell carbon, coal mass active carbon, wood activated charcoal, NACF or CNT, and the oxide of cerium is active material, WO 3For co-catalyst prepares catalyst, denitration activity is better, but adds NH in this method 3As reducing gas.CN102078753A is carrier with the Alveolate activated carbon capable, and manganese oxide and cerium oxide mixture are that active material prepares denitrating catalyst, and the NO conversion ratio is higher, but still with NH 3As reducing agent, cost height, operation and complex process.CN102527369A only prepares denitrating catalyst with activated carbon supported rare earth metal cerium oxide and the lanthana of source water-purifying material factory of Gongyi City, Henan section, and technology is simple, need not to add reducing gas, and the denitration rate is more than 95%.Space Na Na (space Na Na. rare earth oxide is used for catalytic reduction and removes NO XExperimental study.The master of Dalian University of Technology thesis, 2012.) prepare SCR method denitrating catalyst with cocoanut active charcoal and coal mass active carbon load cerium oxide respectively, when finding not add reducibility gas, the denitration rate reaches more than 99% in the catalyst reaction 12h of coal mass active carbon preparation, and the catalyst denitration rate of cocoanut active charcoal preparation reduces obviously, is down to 65% behind the 13h.This shows, relevant with the active carbon kind with the denitration activity of the denitrating catalyst of Preparation of Activated Carbon.
If utilize black liquor lignin-base Preparation of Activated Carbon SCR method denitrating catalyst, not only can solve the NO of papermaking enterprise inside XPollute also and can promote the use of other industrial NO XPollute in the control, can also improve the value of black liquor lignin resource, the discarded object of contaminated environment is converted into the huge product of industrial water requirement, realize the treatment of wastes with processes of wastes against one another, thereby realize higher economy, environmental protection, social benefit.But at present these process conditions and effect still there is not report.
Summary of the invention
The object of the present invention is to provide a kind of black liquor lignin conversion with contaminated environment to become the method for the huge SCR method denitrating catalyst of industrial water requirement and the application of denitrating catalyst in denitration that is prepared by this method, realize the treatment of wastes with processes of wastes against one another.
Purpose of the present invention is achieved through the following technical solutions:
The invention provides a kind of method for preparing denitrating catalyst, it is characterized in that, this method is primary raw material with black liquid lignin and cerous nitrate, specifically may further comprise the steps:
(1) measures a certain amount of black liquid, under 60～65 ℃ condition, regulate pH value to 2～4 with concentrated hydrochloric acid (for example concentrated hydrochloric acid of mass concentration 36.5%), precipitation leaves standstill 30～45min, successively after filtration, dry and grind black liquid lignin (for example black liquid lignin of particle diameter 0.25～0.425mm);
(2) according to phosphoric acid: the mass ratio 3.5～4.0:1 of black liquid lignin (being called " phosphorus material ratio " among the present invention sometimes) adds phosphoric acid solution (for example phosphoric acid solution of mass concentration 50%), mix, dry behind normal temperature dipping 24～48h, under nitrogen protection, be warming up to 450～550 ℃, behind reaction 45～75min, taking-up is washed to filtrate neutrality, and filter cake oven dry, grinding after filtering are made active carbon (for example active carbon of particle diameter 0.15～0.18mm);
(3) an amount of cerous nitrate hydrate crystal of weighing is put into water, constantly be stirred to dissolving fully, the preparation cerous nitrate aqueous solution (for example cerous nitrate aqueous solution of mass concentration 6.83～8.35%), by the cerous nitrate hydrate crystal: when the mass ratio 0.2～0.25:1(of active carbon is scaled cerium oxide with the cerous nitrate hydrate crystal, the mass percent of cerium oxide and carrier active carbon is about 7.93～9.91%) the prepared active carbon of adding step (2), normal temperature leaves standstill 48～72h, oven dry, according to the sesbania powder: the mass ratio 0.1～0.2:1 of active carbon adds the sesbania powder, and (the sesbania powder can form full-bodied glue after absorbing water, is easy to the adhesion-molded of active carbon.In addition, the sesbania powder has good pore-creating effect under hot conditions, makes the catalyst that makes have loose structure, and this is conducive to improve the catalytic activity of catalyst in denitration reaction.), add again a certain amount of salpeter solution (salpeter solution that for example adds 4～6ml mass concentration 9% with respect to 2～2.5g cerous nitrate hydrate crystal) mix agglomerating after, (for example make little with plodder
Figure BDA00002925299300041
Cylindrical little), normal temperature is placed 12～24h and is made denitrating catalyst.
In the step (1), pH value to 3 is preferably regulated in the extraction of black liquor lignin under 65 ℃ of conditions, and precipitation leaves standstill 30min.
In the step (2), phosphorus material ratio is preferably 3.5:1; Preferably under nitrogen protection, be warming up to 500 ℃, reaction 60min.
In the step (3), the sesbania powder: the mass ratio of active carbon is preferably 0.1:1.
Oven dry described in the above-mentioned steps all refers to dry to constant weight under 80～105 ℃.
Be the precursor state of catalytic active component cerium oxide by the cerous nitrate in the catalyst that above-mentioned steps (1)～(3) prepare, under the hot conditions of denitration reaction, cerous nitrate changes cerium oxide into and brings into play catalytic action.
Use as catalyst after also can directly changing cerous nitrate into cerium oxide.That is, method of the present invention can also comprise step (4): the further high-temperature roasting under the condition of 500～700 ℃ (preferred 600 ℃) of catalyst that step (3) is obtained.
In addition, the present invention also provides the application of denitrating catalyst in denitration by method for preparing.Experimental result shows that the catalyst that the present invention obtains does not need to use NH 3, gas such as CO can reach good denitration effect as reducing agent.For example, the catalyst that the present invention is made places the stainless steel tube reactor to estimate, as nitric oxide volumetric concentration 700ppm, air speed 12000h -1, during 600 ℃ of reaction temperatures, the denitration rate reaches 92～99%.
Beneficial effect of the present invention is: the present invention not only can solve the NO of papermaking enterprise inside XPollute also and can promote the use of other industrial NO XPollute in the control, can also improve the value of black liquor lignin resource, the discarded object of contaminated environment is converted into the huge product of industrial water requirement, realize the treatment of wastes with processes of wastes against one another, have remarkable economical, environmental protection, social benefit.Simultaneously, the present invention also have processing cost low, need not additional reducing agent, characteristics such as handling safety is simple, catalyst life is long, denitration activity height.
The specific embodiment
Be further described below in conjunction with the present invention of embodiment, following non-limiting example can make those of ordinary skill in the art more fully understand the present invention, but does not limit the present invention in any way.
Embodiment 1:
(1) measure the 25ml black liquid, under 65 ℃ of conditions, regulate pH value to 3 with the concentrated hydrochloric acid of mass concentration 36.5%, precipitate and leave standstill 30min, successively after filtration, dry and grind the black liquor lignin of particle diameter 0.25～0.425mm.
(2) compare 3.5:1 according to the phosphorus material; phosphoric acid solution and the black liquor lignin of mass concentration 50% are mixed; dry behind the normal temperature dipping 24h; under nitrogen protection, be warming up to 500 ℃; behind the reaction 60min; taking-up wash to filtrate pH be 7, with the oven dry of the filter cake after filtering, grind and make the active carbon that particle diameter is 0.15～0.18mm.
(3) accurately weighing 2g cerous nitrate hydrate crystal constantly is stirred to dissolving fully in 20ml distilled water, is mixed with the cerous nitrate aqueous solution of mass concentration 6.83%.Accurately the prepared active carbon of weighing 10g step (2) adds in the cerous nitrate aqueous solution of preparing, and normal temperature leaves standstill 48h, oven dry, and the nitric acid of adding 1g sesbania powder and 5ml mass concentration 9% after mixing, is made with plodder
Figure BDA00002925299300061
Cylindrical little, normal temperature is placed 12h and is made catalyst, after wherein cerous nitrate was scaled cerium oxide, the mass percent of cerium oxide and active carbon was about 7.93%.
Be experimental subjects with the above-mentioned catalyst 5.0g that makes, as nitric oxide volumetric concentration 700ppm, air speed 12000h -1, during 600 ℃ of reaction temperatures, behind the successive reaction 8h, the denitration rate remains on 92～96%.
Embodiment 2:
(1) with embodiment 1.
(2) with embodiment 1.
(3) be that the mass concentration of the 2.5g(cerous nitrate aqueous solution is 8.35% except the quantitative change with the cerous nitrate hydrate crystal), other is with embodiment 1.After wherein cerous nitrate was scaled cerium oxide, the mass percent of cerium oxide and active carbon was about 9.91%.
Be experimental subjects with the above-mentioned catalyst 5.0g that makes, as nitric oxide volumetric concentration 700ppm, air speed 12000h -1, during 600 ℃ of reaction temperatures, behind the successive reaction 8h, the denitration rate remains on 97～99%.
Comparative example 1:
(1) with embodiment 1.
(2) except phosphorus material ratio being become 2.5:1, other is with embodiment 1.
(3) with embodiment 1.
Be experimental subjects with the above-mentioned catalyst 5.0g that makes, as nitric oxide volumetric concentration 700ppm, air speed 12000h -1, during 600 ℃ of reaction temperatures, behind the successive reaction 6h, its denitration rate is lower than 50%.
Comparative example 2:
(1) with embodiment 1.
(2) with embodiment 1.
(3) the accurate prepared active carbon of weighing 10g step (2) after mixing with the nitric acid of 1g sesbania powder and 5ml mass concentration 9%, is made with plodder Cylindrical little, normal temperature is placed 12h and is made the not sample of load cerium oxide.
Sample 5.0g with the above-mentioned not load cerium oxide that makes is experimental subjects, as nitric oxide volumetric concentration 700ppm, air speed 12000h -1, during 600 ℃ of reaction temperatures, behind the successive reaction 8h, its denitration rate is lower than 60%.

Claims (5)

1.一种制备脱硝催化剂的方法，其特征在于，该方法以造纸黑液木质素与硝酸铈为主要原料，具体包括以下步骤：1. a method for preparing denitration catalyst, is characterized in that, the method is main raw material with papermaking black liquor lignin and cerium nitrate, specifically comprises the following steps: （1）量取一定量的造纸黑液，在60～65℃的条件下，用浓盐酸调节pH值至2～4，沉淀静置30～45min，依次经过滤、烘干及研磨得造纸黑液木质素；(1) Measure a certain amount of paper-making black liquor, adjust the pH value to 2-4 with concentrated hydrochloric acid under the condition of 60-65°C, settle for 30-45 minutes, filter, dry and grind in turn to obtain paper-making black liquor liquid lignin; （2）按照磷酸：造纸黑液木质素的质量比3.5～4.0：1加入磷酸溶液，混合均匀，常温浸渍24～48h后烘干，在氮气保护下升温至450～550℃，反应45～75min后，取出洗涤至滤液中性，将过滤后的滤饼烘干、研磨制得活性炭；(2) According to the mass ratio of phosphoric acid:papermaking black liquor lignin 3.5~4.0:1, add phosphoric acid solution, mix evenly, soak at room temperature for 24~48h, then dry, heat up to 450~550°C under nitrogen protection, and react for 45~75min Finally, take out and wash until the filtrate is neutral, dry and grind the filtered filter cake to obtain activated carbon; （3）称量适量的硝酸铈水合晶体放入水中，不断搅拌至完全溶解，配制硝酸铈水溶液，按硝酸铈水合晶体：活性炭的质量比0.2～0.25:1加入步骤（2）所制得的活性炭，常温静置48～72h，烘干，按照田菁粉：活性炭的质量比0.1～0.2：1加入田菁粉，再加入一定量的硝酸溶液混合成团后，用压条机制成小条，常温放置12～24h即可。(3) Weigh an appropriate amount of cerium nitrate hydrated crystals into water, stir continuously until completely dissolved, prepare an aqueous cerium nitrate solution, and add the cerium nitrate hydrated crystals:activated carbon at a mass ratio of 0.2-0.25:1 to the prepared product in step (2). Activated carbon, let it stand at room temperature for 48-72 hours, dry it, add the safflower powder according to the mass ratio of safflower powder:activated carbon 0.1-0.2:1, add a certain amount of nitric acid solution, mix it into a ball, and use a layering machine to make small strips. Place it at room temperature for 12-24 hours. 2.如权利要求1所述的方法，其特征在于，步骤（2）中的磷酸：造纸黑液木质素的质量比为3.5：1。2. The method according to claim 1, characterized in that the mass ratio of phosphoric acid in step (2): lignin in papermaking black liquor is 3.5:1. 3.如权利要求1所述的方法，其特征在于，步骤（2）中，在氮气保护下升温至500℃，反应60min。3 . The method according to claim 1 , wherein in step (2), the temperature is raised to 500° C. under nitrogen protection, and the reaction is carried out for 60 minutes. 4.如权利要求1～3中任意一项所述的方法，其特征在于，所述方法还包括步骤（4）：将步骤（3）得到的催化剂进一步在500～700℃的条件下高温焙烧。4. The method according to any one of claims 1-3, characterized in that the method further comprises step (4): further calcining the catalyst obtained in step (3) at a high temperature of 500-700°C . 5.由权利要求1～4中任意一项所述的方法制备的脱硝催化剂在脱硝中的应用。5. The application of the denitration catalyst prepared by the method according to any one of claims 1 to 4 in denitration.
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Cited By (3)

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CN104128188A (en) * 2014-08-15 2014-11-05 安徽省元琛环保科技有限公司 Denitration catalyst used in waste incineration power plant and preparation method thereof
CN105170131A (en) * 2015-09-10 2015-12-23 广州中国科学院先进技术研究所 Preparation method of novel sludge carbon-based desulfurization and denitrification catalyst
CN114618514A (en) * 2022-03-08 2022-06-14 天津水泥工业设计研究院有限公司 Method for preparing low-temperature SCR catalyst and co-producing fertilizer by utilizing full-danger waste and solid waste

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104128188A (en) * 2014-08-15 2014-11-05 安徽省元琛环保科技有限公司 Denitration catalyst used in waste incineration power plant and preparation method thereof
CN105170131A (en) * 2015-09-10 2015-12-23 广州中国科学院先进技术研究所 Preparation method of novel sludge carbon-based desulfurization and denitrification catalyst
CN114618514A (en) * 2022-03-08 2022-06-14 天津水泥工业设计研究院有限公司 Method for preparing low-temperature SCR catalyst and co-producing fertilizer by utilizing full-danger waste and solid waste
CN114618514B (en) * 2022-03-08 2024-02-23 天津水泥工业设计研究院有限公司 Method for preparing low-temperature SCR catalyst by utilizing full-risk waste and solid waste and preparing chemical fertilizer simultaneously

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Application publication date: 20130710