CN115814786A - A kind of anti-chlorine poisoning de-CVOCs catalyst and preparation method thereof - Google Patents
A kind of anti-chlorine poisoning de-CVOCs catalyst and preparation method thereof Download PDFInfo
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Abstract
本发明属于CVOCs催化燃烧技术领域，尤其涉及一种抗氯中毒的脱CVOCs催化剂及其制备方法。本发明公开的一种抗氯中毒的脱CVOCs催化剂以过渡金属V氧化物和贵金属Pd为活性组分，过渡金属V的负载质量比为载体重量的2～10％，贵金属Pd的负载质量比为0.1～1％，通过四氯化钛(TiCl4)辅助水热合成法调控TiO2载体结构来提升脱CVOCs性能及抗氯性能。采用浸渍法将活性组分及改性组分负载于不同结构的TiO2载体上，后经过磁力搅拌及干燥处理，最后在空气氛围中进行焙烧，得到本发明的抗氯中毒脱CVOCs催化剂。本发明提供的抗氯中毒脱CVOCs催化剂低温高效、抗Cl中毒、CO2选择性高且制备成本低。
The invention belongs to the technical field of CVOCs catalytic combustion, and in particular relates to a chlorine poisoning-resistant CVOCs removal catalyst and a preparation method thereof. A chlorine-poisoning-resistant CVOCs catalyst disclosed by the present invention uses transition metal V oxide and noble metal Pd as active components, the loading mass ratio of transition metal V is 2 to 10% of the carrier weight, and the loading mass ratio of noble metal Pd is 0.1-1%, through the titanium tetrachloride (TiCl 4 ) assisted hydrothermal synthesis method to adjust the TiO 2 carrier structure to improve the CVOCs removal performance and chlorine resistance performance. The active component and the modified component are supported on TiO 2 carriers with different structures by impregnation method, then subjected to magnetic stirring and drying treatment, and finally roasted in air atmosphere to obtain the anti-chlorine poisoning de-CVOCs catalyst of the present invention. The anti-chlorine poisoning de-CVOCs catalyst provided by the invention is low-temperature, high-efficiency, anti-Cl poisoning, high CO2 selectivity and low preparation cost.
Description
Technical Field
The invention belongs to the technical field of CVOCs catalytic combustion, and particularly relates to a chlorine poisoning resistant CVOCs removing catalyst and a preparation method thereof, which are mainly applied to CVOCs generated in petrochemical spraying, printing and dyeing and other treatment processes.
Technical Field
chlorine-Containing Volatile Organic Compounds (CVOCs) are one of the main sources of air pollution, have wide application in the chemical industry, and can be used as solvents, dry cleaning agents, degreasing agents, intermediates for producing plastics, etching in the semiconductor industry, and precursors of synthetic resins or medicaments. Therefore, with the acceleration of industrialization and urbanization, the usage amount of the organic fertilizer is increasing, and the organic fertilizer brings more harm to the environment. Most CVOCs are high in toxicity and volatile, have hazards of persistence, biological enrichment and the like, and some substances even have a 'three-cause' effect. Therefore, research and development of the efficient CVOCs removal technology have very important significance for human body health and atmospheric environment protection.
The prior CVOCs are mainly treated by a condensation method, an adsorption method, an absorption method, a direct combustion method, a catalytic combustion method, a biological method and the like. When a condensation method and an absorption method are adopted to treat low-concentration organic waste gas, the efficiency is low, and the organic waste gas is generally used as a pretreatment technology of the flue gas and is often combined with technologies such as activated carbon adsorption and combustion to treat the organic flue gas; the direct combustion method needs to supplement fuel when treating low-concentration waste gas, and has the defect of high energy consumption; the prior biological technology has limited treatment effect on treating high-concentration CVOCs waste gas; the catalytic combustion process has good purification efficiency on pollutants in the waste gas, can meet the strict environmental standard requirements, and is widely applied to the petrochemical industry.
The catalytic combustion for purifying CVOCs waste gas has the characteristics of high purification efficiency, no pollution, low energy consumption and the like, wherein the catalyst is the core for removing the CVOCs. The catalyst can be used industrially, needs excellent catalytic activity and has good stability and durability, but most of the catalysts have poor stability under the condition of catalytic oxidation of CVOCs, and the activity of the catalyst tends to be reduced along with the running of time. Therefore, in designing the catalyst, the reaction stability of the catalyst needs to be considered. In the catalytic oxidation of CVOCs, the resultant product contains Cl element, which may cause catalyst poisoning, so that the catalytic performance of the catalyst is weakened, and thus, the chlorine poisoning resistance of the catalyst needs to be studied.
Chinese patent with publication number CN 105289584A discloses a catalyst for catalytic combustion of chloralkane, the active component of which is MnO x -SnO 2 Composite oxides, tiO 2 -ZrO 2 The composite oxide is a carrier. The catalyst has certain chlorine poisoning inhibition capacity, but has low-temperature catalytic activity, and CO is not considered 2 And (4) selectivity.
Chinese patent with publication number CN 110404534A discloses a high-efficiency chlorine poisoning resistant volatile organic compound catalytic oxidation catalyst, and the active component of the catalyst is RuO 2 Modification of TiO by Sn 2 The doping improves the catalytic activity and chlorine poisoning resistance of the catalyst. The catalyst has high catalytic activity, strong chlorine poisoning resistance and CO 2 High selectivity, but the catalyst is a quaternary catalyst, a noble metal RuO 2 The high component content leads to high catalyst cost and complicated preparation process of the carrier structure.
Chinese patent with publication number CN 109529806A discloses a catalyst for catalytic combustion of CVOCs, which is a cerium-titanium solid solution nanotube catalyst. The catalyst has better chlorine poisoning resistance and catalytic activity, but CO 2 Poor selectivity and easy generation of by-products.
Disclosure of Invention
In order to overcome the defects of the existing catalyst, the invention aims to provide a catalyst with low-temperature high efficiency, cl poisoning resistance and CO 2 The catalyst has high selectivity and low cost and is used for removing the CVOCs with chlorine poisoning resistance; another object of the present invention is to provide a catalyst for removing CVOCs, which is resistant to chlorine poisoning, and which is simple in preparation method and easy to operate.
The invention relates to a chlorine poisoning resistant CVOCs removal catalyst, tiO with different structures 2 Is used as a carrier, oxides of transition metal V and noble metal Pd are used as active components, wherein the load mass ratio of the transition metal V is 2-10% of the weight of the carrier, and the load mass ratio of the noble metal Pd is 0.1-0.5%.
Preferably, tiO 2 Structure is TiO 2 -S or TiO 2 -Vo；TiO 2 -S and TiO 2 The preparation of-Vo is as follows: (1) TiO2 2 -S preparation: measure 2000. Mu.l TiCl 4 Added dropwise to 60ml of ethylene glycol under a magnetic stirrer, and when no white smoke (HCl) was generated, 2ml of H2O was added to the mixture, which was stirred at room temperature for 3-6h to produce a homogeneous yellow solution. And transferring the obtained mixed solution into a 100ml polytetrafluoroethylene lining, and reacting in a reaction kettle for 3-6h. Cooling to room temperature, repeatedly cleaning with deionized water and ethanol to remove redundant organic solvent, centrifuging and filtering to obtain a solid sample, drying in a forced air drying oven, and grinding to obtain white TiO2-S carrier;
(2) Preparing a TiO2-Vo carrier: and (2) placing the TiO2-S prepared in the step (1) into a tubular furnace, calcining for 2-5h in the N2 atmosphere, and taking out after cooling to obtain the black TiO2-Vo carrier.
Preferably, the precursor of the oxide of V in the chlorine poisoning resistant CVOCs removing catalyst is ammonium metavanadate.
Preferably, the precursor of the Pd oxide in the chlorine poisoning resistant CVOCs removing catalyst is palladium nitrate.
In particular, the TiO 2 The reaction temperature of the-S carrier in the reaction kettle is 130-180 ℃.
In particular toOf the TiO compound 2 The calcination temperature for the preparation of Vo vectors is 700-900 ℃.
Preferably, the loading amount of the transition metal V element as the active component in the catalyst is 2-6%.
The invention also provides a preparation method of the chlorine poisoning resistant CVOCs removing catalyst, which comprises the following steps:
(1) Weighing a TiO2 carrier, a transition metal V salt and a Pd salt according to the load requirement;
(2) Respectively adding the weighed transition metal V salt and Pd salt into deionized water to be fully dissolved, and obtaining an active component metal salt aqueous solution:
(3) TiO weighed in the step (1) 2 Soaking the powder in the metal salt aqueous solution obtained in the step (2), fully stirring to uniformly disperse the powder in the metal salt aqueous solution, and using ultrasound to more uniformly disperse the titanium dioxide carrier;
(4) Putting the solution obtained in the step (3) into a magnetic stirrer, and stirring at room temperature;
(5) Evaporating the fully and uniformly mixed turbid liquid (4) to dryness in a magnetic stirrer;
(6) Putting the dried sample in an oven, and drying;
(7) And roasting the dried sample in an air atmosphere, and cooling to room temperature to obtain the catalyst.
In particular, tiO in the preparation method 2 The carrier being TiO 2 -S or TiO 2 Vo or conventional TiO available on the market 2 -P。
Specifically, the roasting temperature in the step (7) is 350-550 ℃, and the roasting time is 4-6 hours.
Specifically, the salts in step (2) are metavanadate and nitrate.
The chlorine poisoning resistant CVOCs removing catalyst can effectively remove the CVOCs in a Cl-containing atmosphere.
The preparation principle is as follows: tiO2 2 -Vo is titanium tetrachloride (TiCl) 4 ) Assisted hydrothermal synthesis method, in which N is carried out 2 The catalyst is calcined at high temperature in the atmosphere, has rich oxygen vacancy structure, and is beneficial to the removal of Cl on the catalyst. Using ultrasonic enhanced impregnationThe process makes the active component more uniformly and dispersedly loaded on the TiO 2 -Vo vector surface. The vanadium oxide can provide more acid sites, the palladium heavy metal oxide provides active sites of the catalyst, and the low-temperature reduction performance of the catalyst is improved, so that the low-temperature activity and CO of the catalyst are improved 2 And (4) selectivity.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention is through to TiO 2 The structure of the carrier is regulated and controlled, and TiO with rutile type and rich oxygen vacancy structure is prepared by adopting a hydrothermal synthesis method 2 The Vo carrier has better oxygen transfer capacity compared with the traditional TiO2 carrier, and is beneficial to removing Cl components on the surface of the catalyst;
(2) Only trace amount of palladium oxide is added into the chlorine poisoning resistant CVOCs removing catalyst, the mass ratio of transition metal oxide in the catalyst is reasonably set, and an ultrasonic enhanced auxiliary means is adopted in the preparation process, so that the prepared chlorine poisoning resistant CVOCs removing catalyst not only has good chlorine poisoning resistance, but also has good low-temperature catalytic activity and CO 2 Selectivity;
(3) The chlorine poisoning resistant CVOCs removing catalyst can be used for catalytically oxidizing dichloromethane into CO at the temperature of 250-400 DEG C 2 、H 2 O and HCl are generated, and almost no by-product is generated, so that the deep oxidation of the dichloromethane is improved;
(4) 10% of a catalyst for the removal of CVOCs resistant to chlorine poisoning in 500ppm of methylene chloride 2 ，N 2 The removal of dichloromethane can reach more than 90 percent at 290 ℃ under the condition of being used as balance gas, and CO 2 The product selectivity can reach 100%.
(5) 10% of a catalyst for the removal of CVOCs resistant to chlorine poisoning in 500ppm of methylene chloride 2 ，N 2 As equilibrium gas, the catalyst always keeps 100 percent of removal rate in long-time test, and CO is removed 2 The selectivity was 100%.
(6) The chlorine poisoning resistant CVOCs removal catalyst also has good catalytic activity on pollutants such as benzene, chlorobenzene, alkane and the like;
(7) The addition of the noble metal elements is only about 10 per mill, so that the effect of efficiently removing the CVOCs can be achieved;
(8) The preparation method is simple and easy to operate.
Drawings
FIG. 1 shows a CVOCs catalyst PdV/TiO embodiment of this invention 2 -a scheme for the preparation of Vo;
FIG. 2 shows a catalyst PdV/TiO for removing CVOCs in an embodiment of the present invention 2 -a scheme for the preparation of S;
FIG. 3 shows a catalyst PdV/TiO for removing CVOCs in an embodiment of the present invention 2 The preparation flow chart of (1);
FIG. 4 is a chart of DCM conversion for the catalytic removal of methylene chloride (DCM) by the chlorine poisoning resistant CVOCs removing catalyst of the present invention;
FIG. 5 is a CO removal from methylene chloride (DCM) catalyzed by the chlorine poisoning resistant CVOCs removing catalyst of the present invention 2 A selectivity profile;
FIG. 6 is a graph showing stability test of catalytic removal of methylene chloride (DCM) over a chlorine poisoning resistant CVOCs removal catalyst of the present invention;
FIG. 7 shows TiO of the present invention 2 Vo and TiO 2 A comparison graph of EPR (from Aladdin);
FIG. 8 shows TiO of the present invention 2 Vo and TiO 2 XRD contrast pattern (from alatin);
FIG. 9 is PdV/TiO of the present invention 2 Removal of Benzene (Benzene), chlorobenzene (CB), alkanes (C) from the Vo catalyst x H y ) Test graph of (2).
Detailed Description
In order to better illustrate the idea of the invention, specific embodiments of the invention are described below with reference to the accompanying drawings, in which embodiments are described below, except for TiO 2 -S、TiO 2 Vo is self-made and other raw materials are all purchased from commercial sources.
Preparation of TiO2-S and TiO2-Vo Supports
TiO 2 -the preparation of S comprises the following steps:
measure 2000. Mu.l TiCl 4 Added dropwise to 60ml of ethylene glycol under a magnetic stirrer, in the absence of white smoke (HCl)) When generated, 2ml of H 2 O is added to the mixture and stirred at room temperature for 3-6h to give a homogeneous yellow solution. And transferring the mixed solution into a 100ml polytetrafluoroethylene lining, and reacting with a reaction kettle at 130-180 ℃ for 3-6h. Cooling to room temperature, repeatedly cleaning with deionized water and ethanol to remove excessive organic solvent, centrifuging to obtain solid sample, drying in a forced air drying oven at 60 deg.C for 12 hr, taking out, and grinding to obtain white TiO powder 2 -an S-vector;
TiO 2 the preparation of Vo comprises the following steps:
TiO to be prepared 2 S in a tube furnace, in N 2 Calcining at 700-900 ℃ for 2-5h in the atmosphere, cooling and taking out to obtain black TiO 2 -a Vo vector.
Example 1
CVOCs catalyst PdV/TiO 2 -Vo preparation method, as shown in fig. 1, comprising the following steps:
(1) Weighing 5g of TiO 2 -Vo,0.4593g ammonium metavanadate, 0.015g palladium nitrate;
(2) Adding ammonium metavanadate and palladium nitrate into 50ml of deionized water, fully stirring to dissolve metal salt, and slowly adding TiO while stirring after dissolving 2 -Vo powder, soaking the obtained solution at 20 ℃ for 20min by using ultrasonic waves with the frequency of 30kHz, then placing the solution in a magnetic stirrer, setting the rotating speed at 30r/s, soaking and stirring at room temperature for 4h, heating to 65 ℃, stirring and soaking until the solution is dried by distillation, then placing in a drying oven at 110 ℃ for 10h, grinding and sieving by using a 100-mesh sieve, and roasting the powder at 500 ℃ for 5h.
Example 2
CVOCs removing catalyst PdV/TiO 2 -S, as shown in FIG. 2, comprising the steps of:
(1) 5g of TiO are weighed 2 -S,0.8911g ammonium metavanadate, 0.020g palladium nitrate;
(2) Adding manganese nitrate and palladium nitrate into 50ml of deionized water, fully stirring to dissolve metal salt, slowly adding titanium dioxide powder while stirring after dissolution, dipping the obtained solution at 25 ℃ for 20min by using ultrasonic waves with the frequency of 20kHz, then placing the solution in a magnetic stirrer, setting the rotating speed at 30r/s, dipping and stirring at room temperature for 4h, heating to 65 ℃, stirring and dipping to dry, then placing in an oven at 105 ℃ for drying for 10h, grinding and sieving by using a 100-mesh sieve, and roasting the powder at 500 ℃ for 5h.
Example 3
CVOCs removing catalyst PdV/TiO 2 As shown in fig. 3, the preparation method comprises the following steps:
(1) Weighing 5g of titanium dioxide (purchased from alatin), 0.4593g of ammonium metavanadate and 0.015g of palladium nitrate;
(2) Adding ammonium metavanadate and palladium nitrate into 50ml of deionized water, fully stirring to dissolve metal salts, slowly adding titanium dioxide powder while stirring after dissolution, dipping the obtained solution at 25 ℃ for 20min by using ultrasonic waves with the frequency of 30kHz, then placing the solution in a magnetic stirrer, setting the rotating speed at 30r/s, dipping and stirring for 4h at room temperature, heating to 65 ℃, stirring and dipping to dry the solution, then placing the solution in an oven at 105 ℃ for drying for 10h, grinding and sieving by using a 100-mesh sieve, and roasting the powder for 5h at 500 ℃.
Test of catalytic Activity of CVOCs catalyst
PdV/TiO prepared as in examples 1-3 2 -Vo、PdV/TiO 2 -S、PdV/TiO 2 Grinding, tabletting and screening the catalyst, and taking 100mg of a 40-60-mesh sample for a catalytic activity test experiment in a CVOCs removal reaction furnace.
The activity test conditions are as follows: 500ppm Dichloromethane (DCM), 10vol.% O2 and N2 are balance gases, the total smoke gas amount is 100ml/min, each path of gas is introduced through a mass flow meter and enters air mixed gas to be fully mixed, the reactor is a 7mm quartz tube, a weighed sample is fixed in the quartz reaction tube by quartz wool, and the temperature required by the reaction is provided through a temperature control tube furnace. The outlet smoke composition was analyzed online by GC to determine the concentration of DCM, while outlet COx was quantitatively analyzed by a Testo350-XL type smoke analyzer. In the catalyst activity evaluation test, the DCM removal efficiency is calculated by the following formula:
wherein C is in And C out Respectively representing the concentration of inlet and outlet DCM.
The analysis results are shown in FIGS. 4 and 5, and it can be seen from FIGS. 4 and 5 that the low temperature performance of the catalyst for removing CVOCs prepared by the method of the invention is greatly improved, and CO is also greatly improved 2 The selectivity is high; in example 1 (PdV/TiO) 2 -Vo) catalyst, T 90％ Compared with the embodiment 3 (PdV/TiO) 2 ) The catalyst is reduced by 50 ℃ and T 90％ Reduced to 290 ℃ and the product is completely CO 2 ，CO 2 The selectivity reaches 100 percent. Under the reaction condition, pdV/TiO 2 Vo) the catalyst showed the best performance.
PdV/TiO 2 Vo stability test
100mg of PdV/TiO are taken 2 The Vo catalyst was subjected to a stability test at a temperature of 400 ℃ and the results are shown in FIG. 6. PdV/TiO in the entire test interval 2 DCM removal of-Vo catalyst was always maintained at 100% with almost no CO production (lower curve of FIG. 6 shows CO change, upper curve shows CO change) 2 Variation), see PdV/TiO 2 The Vo catalyst possesses better stability, i.e. there is better chlorine resistance.
EPR characterization
PdV/TiO are taken 2 Support TiO for the Vo catalyst 2 Vo and TiO 2 EPR characterization (from Aladdin) was performed and the results are shown in FIG. 7. In TiO 2 In Vo, there is a clear EPR peak, in contrast to TiO 2 No significant EPR peak was found in-P. In TiO 2 Symmetric signal of EPR peak in-Vo appears around g =2.003, indicating TiO 2 The Vo carrier introduces oxygen vacancy through structural regulation, and further improves catalytic activity.
XRD test
PdV/TiO is taken 2 Support TiO for the Vo catalyst 2 Vo and TiO 2 XRD measurements (from Aladdin) were performed and the results are shown in FIG. 8. By contrast, it was found that in TiO 2 The rutile phase exists on the structure of-Vo, which is beneficial to the active component in TiO 2 Dispersion on the Vo support, which has a certain degree of catalytic properties in combination with better catalytic propertiesAnd (4) relationship.
Benzene (Benzene), chlorobenzene (CB) and alkanes (C) x H y ) Test for removal Properties
Example 1 (PdV/TiO) was taken 2 Vo) catalyst 100mg, benzene (Benzene), chlorobenzene (CB) and alkane (C) were each carried out x H y ) The results of the removal performance test are shown in fig. 9. As can be seen in FIG. 9, pdV/TiO 2 The Vo catalyst shows better catalytic activity to various VOCs, and Benzene, CB and C can be prepared at 300 DEG C x H y And (4) completely oxidizing.
The invention is achieved by TiCl 4 Auxiliary hydrothermal synthesis method for preparing TiO 2 Carrier, structure regulation and control of the carrier, development of catalyst carrier TiO with better activity 2 -Vo. The results show that the compounds are in the form of TiO 2 PdV/TiO prepared from Vo vector 2 Vo catalyst T 90％ Compared with the conventional TiO 2 The temperature is reduced by 50 ℃, pdV/TiO 2 Vo catalytic T 90％ As low as 290 ℃ and exhibits better CO2 selectivity without CO and other organics. After long-term stability test, pdV/TiO 2 The Vo catalyst always keeps 100% of removal efficiency and has excellent anti-poisoning performance. Meanwhile, the catalyst also shows better activity to other VOCs and has better universality.
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