CN105565376A - Recovery process of SCR waste catalyst - Google Patents

Recovery process of SCR waste catalyst Download PDF

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CN105565376A
CN105565376A CN201410539548.3A CN201410539548A CN105565376A CN 105565376 A CN105565376 A CN 105565376A CN 201410539548 A CN201410539548 A CN 201410539548A CN 105565376 A CN105565376 A CN 105565376A
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胡运兴
刘枫
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Abstract

The invention discloses a recovery process of an SCR waste catalyst. The process includes the steps of pretreatment of SCR waste catalyst, leaching, preparation of titanium dioxide, preparation of ammonium metavanadate, preparation of tungstic acid and molybdic acid and the like. The process involved in the invention is relatively simple, the raw material and auxiliary material consumption and waste production are not great, and the recovery rate is high, so that the process has good environmental, economic, social benefits and implementability.

Description

The recovery process of SCR spent catalyst
Technical field
Notification number CN102557142B) individually disclose the method that can be applicable to reclaim tungstic oxide and ammonium meta-vanadate in waste and old SCR denitration, V after the undeclared recovery of the method 2o 5, WO 3yield and the purity of corresponding product, also TiO in not mentioned SCR denitration 2recovery and method of disposal; Chinese invention patent (application number 201210023122.3) discloses the method that can be applicable to reclaim titanium oxide concentrate, ammonium meta-vanadate, wolframic acid in waste and old SCR denitration, the yield of main products and the purity of corresponding product after the undeclared recovery of the method; Chinese invention patent (application publication number CN102936039A) discloses the method that can be applicable to reclaim rutile titanium dioxide, ammonium meta-vanadate, ammonium paratungstate in waste and old SCR denitration, the method extracting and separating supervisor is complicated, and consumption of raw and auxiliary materials and refuse produce all larger.
Summary of the invention
The problems such as the present invention aims to provide a kind of recovery process of SCR spent catalyst, and existing SCR waste catalyst recovery is incomplete to solve, cost is comparatively large, program is complicated.Technique of the present invention is particularly suitable for the board-like SCR catalyst of titaniferous, vanadium, tungsten, molybdenum.
The recovery process of SCR spent catalyst of the present invention comprises the following steps:
1, pre-treatment: after SCR spent catalyst is washed, broken, grinding to 120 ~ 130 order;
2, leach: in the pretreated SCR spent catalyst of step 1, add alkali lye and oxygenant, described alkali lye concentration expressed in percentage by weight is 2% ~ 9%, leaching solvent and solute weight ratio is 2 ~ 10, leaches 2 ~ 5h, obtain leach liquor and leached mud under the condition of temperature 95 ~ 185 DEG C, pressure 0.5 ~ 1.3MPa; Preferably, described alkali is NaOH or Na 2cO 3,described oxygenant is NaClO 3, KMnO 4or H 2o 2;
3, titanium dioxide is prepared: the leached mud positive sodium titanate (Na obtained to step 2 4tiO 4) in add excessive acid, control ph is 0.6 ~ 1.6, and temperature 95 ~ 100 DEG C, obtains positive metatitanic acid (H 4tiO 4); Calcine positive metatitanic acid, calcining temperature is 700 ~ 900 DEG C, and calcination time is 3 ~ 4h, obtained rutile titanium white powder (TiO 2); Preferably, described acid is hydrochloric acid or sulfuric acid;
4, leach liquor removal of impurities: add in the leach liquor that step 2 obtains mass concentration 20% ~ 30% MgCl 2or MgSO 4solution, temperature of reaction controls at 95 ~ 105 DEG C, filters, obtains Mg 3(PO 4) 2, MgSiO 3, HAsMgO 4throw out and filtrate;
5, prepare ammonium meta-vanadate: add in the filtrate that step 4 obtains mass concentration 30% ~ 35% NH 4cl, (NH 4) 2sO 4or NH 4nO 3solution, temperature controls at 80 ~ 100 DEG C, obtained ammonium meta-vanadate (NH 4vO 3); Filter, obtain filtrate;
6, prepare wolframic acid, molybdic acid: in the filtrate that step 5 obtains, add hydrochloric acid or sulphuric acid soln, mass concentration is 29% ~ 32%, and control temperature, at 90 ~ 100 DEG C, obtains wolframic acid; Filter to obtain wolframic acid and filtrate; NaOH or Na that mass concentration in 3%-8%, temperature is 5-20 DEG C is added in filtrate 2cO 3cold soln is cooled to 35 ~ 45 DEG C, and pH value is adjusted to 5.5 ~ 6.5, obtains molybdic acid solid.
Preferably, the wolframic acid that step 6 is obtained is dissolved in ammoniacal liquor, and ammonia soln mass concentration is 25% ~ 35%, and control temperature is at 75 ~ 85 DEG C, and filtration, evaporation, crystallization obtain ammonium paratungstate.
Preferably, in step 6, filter further and molybdic acid solid is separated with waste liquid, in waste liquid, add alkali (as NaOH), precipitation Mg 2+, Fe 3+obtain salt slurry; Filter salt slurry, obtain filtrate, in filtrate, add BaCl 2solution, obtains barium sulfate precipitate; After filtration, filtrate is obtained raw material saline solution through reverse osmosis, fresh water part is back to reclaimer; Described reclaimer comprises the washing of spent catalyst and prepares the calcining tail gas absorption operation of titanium dioxide.
Preferably, described SCR catalyst is board-like SCR spent catalyst; Further preferably, the Ingredients Weight percentage composition of described SCR spent catalyst is TiO 275% ~ 85%, V 2o 51.3% ~ 3.3%, WO 32.3% ~ 5.8%, MoO 33% ~ 7.5%.
Beneficial effect of the present invention comprises:
1, technique is relatively simple, consumption of raw and auxiliary materials amount and refuse generation all little;
2, obtained major product rutile titanium white powder, ammonium meta-vanadate, wolframic acid, molybdic acid, ammonium paratungstate purity is high, the rate of recovery is high;
3, rutile titanium white powder can continue the raw material as production SCR catalyst, is conducive to various material in denitrating flue gas industrial chain and forms closed circuit benign cycle;
4, can produce flexibly according to the market requirement the state of matter after tungsten recovery;
5, byproduct silicon magnesium slag, phosphorus magnesium slag, arsenic magnesium slag, salt slurry, high density sodium chloride salt liquid, barium sulfate slag are all that higher innoxious of purity has valency commodity;
6, waste water focused on and be back to the washing of spent catalyst and prepare the calcining tail gas absorption operation of titanium dioxide, be beneficial to water saving and waste water, exhaust emission reduction of discharging.
Based on above-mentioned, technique of the present invention has good environment, economical, societal benefits and exploitativeness.
Accompanying drawing explanation
Fig. 1 is the schema of present invention process.
Embodiment
Below by embodiment, the specific embodiment of the present invention is described further, but not therefore by protection scope of the present invention restriction in one embodiment.
embodiment 1:the technique reclaiming useful component from the board-like SCR spent catalyst of titaniferous, vanadium, tungsten, molybdenum comprises the steps:
1, pre-treatment: after board-like for 1kg SCR spent catalyst washing, broken, grinding to 130 order; In described spent catalyst, TiO 275%, V 2o 51.8%, WO 33.8%, MoO 35.5%;
2, leach: in the pretreated SCR spent catalyst of step 1, add NaOH alkali lye, the mass concentration of alkali lye is 2%, leaching solvent and solute weight ratio is 2, adds oxygenant NaClO 3, under the condition of temperature 95 DEG C, pressure 0.5MPa, leach 2h, obtain leach liquor and leached mud, filter and the two is separated;
3, prepare rutile titanium white powder: leached mud positive sodium titanate step 2 obtained drops in excessive hydrochloric acid, control ph is 1.6, and temperature is 95 DEG C, obtains positive metatitanic acid; Calcine positive metatitanic acid, calcining temperature is 700 DEG C, and the time is 3h, obtained rutile titanium white powder (TiO 2);
4, leach liquor removal of impurities: add the MgCl that mass concentration is 20% in the leach liquor that step 2 obtains 2solution, temperature controls, at 95 DEG C, to obtain Mg 3(PO 4) 2, MgSiO 3, HAsMgO 4throw out; Filtering separation;
5, ammonium meta-vanadate is prepared: in the filtrate that step 4 obtains, add the NH that mass concentration is 30% 4cl, temperature controls at 80 DEG C, obtained ammonium meta-vanadate; Filtering separation;
6, wolframic acid, molybdic acid is prepared: in the filtrate that step 5 produces, add the hydrochloric acid that mass concentration is 29%, control temperature is 90 DEG C, obtained wolframic acid; Filter wolframic acid, then in filtrate, add the NaOH cold soln that mass concentration is 4%, temperature is 15 DEG C make it to be cooled to 35 DEG C, it is 6.5 that pH value controls, obtained molybdic acid; Filtering separation obtains solid molybdic acid, and waste liquid enters Waste Water Treatment;
7, prepare ammonium paratungstate: the wolframic acid that step 6 is obtained is dissolved in ammoniacal liquor, and ammonia soln mass concentration is 25%, control temperature is at 75 DEG C, and filtration, evaporation, crystallization, obtain ammonium paratungstate;
8, Waste Water Treatment: add NaOH in the waste liquid that step 6 obtains, precipitation Mg 2+, Fe 3+obtain salt slurry; Filter, in filtrate, add BaCl 2solution, obtains barium sulfate (BaSO 4) precipitation; Filter, filtrate obtains raw material saline solution through reverse osmosis, and fresh water part is back to washing spent catalyst.
According to above-mentioned concrete technology step, obtain as shown in the results summarized in table 1.
The specific targets that table 1SCR waste catalyst recovery technique obtains
embodiment twothe technique reclaiming useful component from the board-like SCR spent catalyst of titaniferous, vanadium, tungsten, molybdenum comprises the steps:
1, pre-treatment: after board-like for 5kg SCR spent catalyst washing, broken, grinding to 125 order; In described SCR spent catalyst, TiO 280%, V 2o 53%, WO 35%, MoO 33%;
2, leach: in the pretreated SCR spent catalyst of step 1, add Na 2cO 3alkali lye, alkali lye concentration expressed in percentage by weight is 6%, and leaching solvent and solute weight ratio is 6, adds oxygenant NaClO 3, under the condition of temperature 140 DEG C, pressure 0.9MPa, leach 3.5h; Be separated leached mud positive sodium titanate;
3, prepare rutile titanium white powder: in the positive sodium titanate that step 2 produces, add excessive hydrochloric acid or sulfuric acid, control ph is 1.1, and temperature 98 DEG C, obtains H 4tiO 4; Calcine positive metatitanic acid, calcining temperature is 800 DEG C, and calcination time is 3.5h, obtained rutile titanium white powder (TiO 2);
4, leach liquor removal of impurities: add MgSO in the leach liquor that step 2 produces 4solution, mass concentration is 25%, and temperature controls at 100 DEG C, obtains Mg 3(PO 4) 2, MgSiO 3, HAsMgO 4throw out; Filtering separation;
5, ammonium meta-vanadate is prepared: in the filtrate that step 4 obtains, add (NH 4) 2sO 4solution, mass concentration is 33%, and temperature controls at 90 DEG C, obtained ammonium meta-vanadate; Filtering separation;
6, prepare wolframic acid: in the filtrate that step 5 obtains, add sulphuric acid soln, mass concentration is 31%, and control temperature is 95 DEG C, obtained wolframic acid; Filtering separation, add in filtrate mass concentration be 5%, temperature is the Na of 10 DEG C 2cO 3cold soln, makes to being cooled to 40 DEG C, and it is 6.0 that pH value controls, obtained molybdic acid; Filtering separation obtains solid molybdic acid, and waste liquid enters Waste Water Treatment;
7, prepare ammonium paratungstate: the wolframic acid that step 6 is obtained is dissolved in ammoniacal liquor, and ammonia soln mass concentration is 30%, control temperature is at 80 DEG C, and filtration, evaporation, crystallization, obtain ammonium paratungstate;
8, Waste Water Treatment: add NaOH in the waste liquid that step 6 produces, precipitation Mg 2+, Fe 3+obtain salt slurry; Filter to get filtrate, in filtrate, add BaCl 2solution, obtains barium sulfate (BaSO 4) precipitation; Filter, filtrate is obtained raw material saline solution through reverse osmosis, and fresh water part is back to the tail gas absorption of titanium white calcining.
According to above-mentioned concrete technology step, obtain result as shown in table 2.
The specific targets that table 2SCR waste catalyst recovery technique obtains
embodiment threethe technique reclaiming useful component from the board-like SCR spent catalyst of titaniferous, vanadium, tungsten, molybdenum comprises the steps:
1, pre-treatment: after board-like for 10kg SCR spent catalyst washing, broken, grinding to 130 order; Described SCR spent catalyst TiO 285%, V 2o 51.3%, WO 33%, MoO 36%;
2, leach: in the pretreated SCR spent catalyst of step 1, add NaOH alkali lye, alkali lye mass percentage concentration is 9%, leaching solvent and solute weight ratio is 10, adds oxygenant NaClO 3, under the condition of temperature 185 DEG C, pressure 1.3MPa, leach 5h; Separating and filtering, obtains leached mud positive sodium titanate and leach liquor;
3, rutile titanium white powder is prepared: in the leached mud positive sodium titanate that step 2 produces, add excessive hydrochloric acid, control ph is 0.6, and temperature 100 DEG C, obtains H 4tiO 4, calcining H 4tiO 4, calcining temperature is 900 DEG C, and calcination time is 4h, obtained rutile titanium white powder (TiO 2);
4, leach liquor removal of impurities: add MgCl in the leach liquor that step 2 produces 2solution, mass concentration is 30%, and temperature controls at 105 DEG C, obtains Mg 3(PO 4) 2, MgSiO 3, HAsMgO 4throw out; Filtering separation;
5, ammonium meta-vanadate is prepared: in the filtrate that step 4 produces, add NH 4cl solution, mass concentration is 35%, and temperature controls at 100 DEG C, obtained ammonium meta-vanadate (NH 4vO 3); Filtering separation;
6, wolframic acid is prepared: in the filtrate that step 5 produces, add hydrochloric acid, mass concentration is 32%, and control temperature is 100 DEG C, obtained wolframic acid; Filtering separation, add in filtrate 8%, temperature is that the NaOH cold soln of 20 DEG C is cooled to 45 DEG C, it is 5.5 that pH value controls, obtained molybdic acid; Filtering separation obtains solid molybdic acid, and waste liquid enters Waste Water Treatment;
7, prepare ammonium paratungstate: the wolframic acid that step 6 is obtained is dissolved in ammoniacal liquor, and ammonia soln mass concentration is 35%, control temperature is at 85 DEG C, and filtration, evaporation, crystallization, obtain ammonium paratungstate;
8, Waste Water Treatment: add NaOH in the waste liquid that step 6 produces, precipitation Mg 2+, Fe 3+obtain salt slurry; Filter, in filtrate, add BaCl 2solution, obtains barium sulfate (BaSO 4) precipitation; Filter, filtrate obtains raw material saline solution through reverse osmosis, and fresh water part is back to the tail gas absorption of titanium dioxide calcining.
According to above-mentioned concrete technology step, obtain result as shown in table 3.
The specific targets that table 3SCR waste catalyst recovery technique obtains
Can find out from above three embodiments, the major product rutile titanium white powder, ammonium meta-vanadate, wolframic acid, molybdic acid and the ammonium paratungstate purity that utilize present invention process to obtain are high, and the rate of recovery of its main component is also high, TiO in rutile titanium white powder 2content can reach 97% ~ 99%, TiO 2the rate of recovery can reach 88% ~ 90%, amounts to V in ammonium meta-vanadate 2o 5content can reach 75% ~ 77%, V 2o 5the rate of recovery can reach 86% ~ 88%, amounts to WO in wolframic acid or ammonium paratungstate 3content can reach 86% ~ 89%, WO 3the rate of recovery can reach 87% ~ 89%, amounts to MoO in molybdic acid 3content can reach 78% ~ 80%, MoO 3the rate of recovery can reach 80% ~ 82%.Byproduct silicon magnesium slag, salt slurry, barium sulfate slag, raw material saline solution are also all that higher innoxious of purity has valency commodity, silicon magnesium slag CaCO 3content 65% ~ 67%, salt slurry CaCO 3content 98% ~ 99%, barium sulfate slag BaSO 4content 98% ~ 99%.Technique of the present invention is discharged without any harmful secondary pollutant, belongs to the useless SCR catalyst recovery process of environmental protection, type capable of circulation, has good environment, economical, societal benefits and exploitativeness.

Claims (8)

1. a recovery process for SCR spent catalyst, comprising:
1), pre-treatment: after SCR spent catalyst is washed, broken, grinding to 120 ~ 130 order;
2), leach: in the pretreated SCR spent catalyst of step 1, add alkali lye and oxygenant, described alkali lye concentration expressed in percentage by weight is 2% ~ 9%, leaching solvent and solute weight ratio is 2 ~ 10, leaches 2 ~ 5h, obtain leach liquor and leached mud under the condition of temperature 95 ~ 185 DEG C, pressure 0.5 ~ 1.3MPa;
3), prepare titanium dioxide: in the leached mud positive sodium titanate that step 2 obtains, add excessive acid, control ph is 0.6 ~ 1.6, and temperature 95 ~ 100 DEG C, obtains positive metatitanic acid; Calcine positive metatitanic acid, calcining temperature is 700 ~ 900 DEG C, and calcination time is 3 ~ 4h, obtained rutile titanium white powder;
4), leach liquor removal of impurities: add in the leach liquor that step 2 obtains mass concentration 20% ~ 30% MgCl 2or MgSO 4solution, temperature of reaction controls at 95 ~ 105 DEG C, filters, obtains Mg 3(PO 4) 2, MgSiO 3, HAsMgO 4throw out and filtrate;
5), prepare ammonium meta-vanadate: add in the filtrate that step 4 obtains mass concentration 30% ~ 35% NH 4cl, (NH 4) 2sO 4or NH 4nO 3solution, temperature controls at 80 ~ 100 DEG C, obtained ammonium meta-vanadate (NH 4vO 3); Filter, obtain filtrate;
6), prepare wolframic acid, molybdic acid: in the filtrate that step 5 obtains, add hydrochloric acid or sulphuric acid soln, mass concentration is 29% ~ 32%, and control temperature, at 90 ~ 100 DEG C, obtains wolframic acid; Filter to obtain wolframic acid and filtrate; NaOH or Na that mass concentration in 3%-8%, temperature is 5-20 DEG C is added in filtrate 2cO 3cold soln is cooled to 35 ~ 45 DEG C, and pH value is adjusted to 5.5 ~ 6.5, obtains molybdic acid solid.
2. technique according to claim 1, comprises further, and the wolframic acid that step 6 is obtained is dissolved in ammoniacal liquor, and ammonia soln mass concentration is 25% ~ 35%, and control temperature is at 75 ~ 85 DEG C, and filtration, evaporation, crystallization obtain ammonium paratungstate.
3. technique according to claim 1, filters further and is separated with waste liquid by molybdic acid solid, in waste liquid, add alkali, precipitation Mg 2+, Fe 3+obtain salt slurry; Filter salt slurry, obtain filtrate, in filtrate, add BaCl 2solution, obtains barium sulfate precipitate; After filtration, filtrate is obtained raw material saline solution through reverse osmosis, fresh water part is back to recovery process.
4. technique according to claim 3, described reclaimer comprises the washing of spent catalyst and prepares the calcining tail gas absorption operation of titanium dioxide.
5. technique according to claim 1, wherein, in step 1, described alkali is NaOH or Na 2cO 3, described oxygenant is NaClO 3, KMnO 4or H 2o 2.
6. technique according to claim 1, wherein, in step 2, described acid is hydrochloric acid or sulfuric acid.
7. the technique according to any one of claim 1-6, wherein, described SCR spent catalyst is board-like SCR spent catalyst.
8. technique according to claim 7, wherein, the Ingredients Weight percentage composition of described SCR spent catalyst is TiO 275% ~ 85%, V 2o 51.3% ~ 3.3%, WO 32.3% ~ 5.8%, MoO 33% ~ 7.5%.
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Cited By (10)

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CN106480320A (en) * 2016-11-23 2017-03-08 河钢股份有限公司承德分公司 A kind of method for reclaiming valuable metal from discarded SCR denitration
CN107419104A (en) * 2017-07-24 2017-12-01 航天龙源(北京)环保科技发展有限公司 The comprehensive recovering process of useless SCR denitration
CN108687105A (en) * 2018-04-23 2018-10-23 清华大学 A kind of method of comprehensive utilization to discarding SCR denitration
CN109652664A (en) * 2018-12-18 2019-04-19 信丰华锐钨钼新材料有限公司 A kind of method of tungsten in high efficiency extraction waste denitration catalyst
CN110015686A (en) * 2018-01-08 2019-07-16 神华集团有限责任公司 Titanium slag recycles the method for titanium dioxide and the method from denitrating catalyst recycling tungsten, titanium and vanadium
CN110747339A (en) * 2019-10-17 2020-02-04 韶关市诚一金属材料科技有限公司 Treatment process of ship tail gas denitration waste catalyst
CN112408470A (en) * 2020-10-30 2021-02-26 甘肃盈华环保科技有限公司 Method for producing titanium dioxide by using waste denitration catalyst based on high-temperature calcination method
CN112609079A (en) * 2020-12-15 2021-04-06 武汉工程大学 Treatment and recovery method for regenerated waste liquid of inactivated denitration catalyst and application thereof
CN113249595A (en) * 2021-06-01 2021-08-13 中国科学院过程工程研究所 Method for recovering tungsten from waste alkali liquor generated by regenerating waste SCR catalyst and application of method
CN115872442A (en) * 2023-03-08 2023-03-31 国能龙源环保有限公司 Method for preparing titanium dioxide by using waste denitration catalyst

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CN106480320A (en) * 2016-11-23 2017-03-08 河钢股份有限公司承德分公司 A kind of method for reclaiming valuable metal from discarded SCR denitration
CN107419104A (en) * 2017-07-24 2017-12-01 航天龙源(北京)环保科技发展有限公司 The comprehensive recovering process of useless SCR denitration
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CN110015686A (en) * 2018-01-08 2019-07-16 神华集团有限责任公司 Titanium slag recycles the method for titanium dioxide and the method from denitrating catalyst recycling tungsten, titanium and vanadium
CN108687105A (en) * 2018-04-23 2018-10-23 清华大学 A kind of method of comprehensive utilization to discarding SCR denitration
CN109652664A (en) * 2018-12-18 2019-04-19 信丰华锐钨钼新材料有限公司 A kind of method of tungsten in high efficiency extraction waste denitration catalyst
CN110747339A (en) * 2019-10-17 2020-02-04 韶关市诚一金属材料科技有限公司 Treatment process of ship tail gas denitration waste catalyst
CN112408470A (en) * 2020-10-30 2021-02-26 甘肃盈华环保科技有限公司 Method for producing titanium dioxide by using waste denitration catalyst based on high-temperature calcination method
CN112609079A (en) * 2020-12-15 2021-04-06 武汉工程大学 Treatment and recovery method for regenerated waste liquid of inactivated denitration catalyst and application thereof
CN113249595A (en) * 2021-06-01 2021-08-13 中国科学院过程工程研究所 Method for recovering tungsten from waste alkali liquor generated by regenerating waste SCR catalyst and application of method
CN115872442A (en) * 2023-03-08 2023-03-31 国能龙源环保有限公司 Method for preparing titanium dioxide by using waste denitration catalyst

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