CN102658127B - Selective hydrogenation dechlorination catalyst for 1,2-dichloroethane, as well as preparation method and application thereof - Google Patents
Selective hydrogenation dechlorination catalyst for 1,2-dichloroethane, as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a bimetallic catalyst prepared by a continuous light deposition method, and a method for degrading 1,2-dichloroethane by selective hydrogenation dechlorination. The bimetallic catalyst is A-B/TiO2 type catalyst obtained by sequentially depositing binary metal on a titanium dioxide carrier by light deposition, wherein A is Pd, Pt, Au or Rh, and B is Ag, Cu or Ni. The catalyst is prepared by the steps of: adding TiO2, A salt solution and methyl alcohol into a photoreactor, filling N2 into the photoreactor under the dark condition, and carrying out reaction for 3-6h under the ultraviolet illumination; filtering, washing and then drying; and loading the metal B in the same way to prepare the catalyst. 1,2-dichloroethane is degraded by hydrogenation through selective catalysis of the A-B/TiO2 type catalyst, thus being converted into hydrocarbon taking ethylene as main product. The catalyst has technical feasibility, is free from secondary pollution, is used for degrading 1,2-dichloroethane with remarkable effect, and has good economic benefit and environmental benefit.
Description
Technical field
The present invention relates to a kind of noble metal carrier catalyst and preparation method thereof, be specifically related to a kind of 1,2-dichloroethanes selective hydrogenation dechlorination catalyst and preparation method thereof, and the application of this catalyst on selective hydrogenation dechlorination degraded 1,2-dichloroethanes.
Background technology
1,2-dichloroethanes is oily liquids colourless, volatile, that have chloroform smell, is fat-soluble nervous poison, belongs to hypertoxic type, is a kind of teratogenesis, material that carcinogenicity is strong.As industrial widely used organic products, main as industry synthetic raw material, industrial solvent, degreasing agent, pesticide, metal cleaner and adhesive etc.Because it has effumability, easily enter human body via respiratory tract and skin pore, the symptoms such as human body sucks after a small amount of can occur headache, feel sick, vomiting.Long-term low concentration contact can cause neurasthenia syndrome and disease of digestive tract.High concentration mainly causes central nervous system symptom after sucking, and toxic encephalopathy can appear in severe patient, shows as encephaledema, severe headache, frequent vomiting, tic and stupor, and being in a bad way to worsen to cause death.
Because 1,2-dichloroethanes is a kind of conventional solvent, the chance touching in life is more, is mainly derived from the paint using in Furniture manufacture process, and the adhesive glue using in shoe-making industry, the pesticide of cereal.Due to less to the understanding of 1,2-dichloroethanes toxicity and be neglectful in taking precautions, the intoxication accident of clinical report is more in recent years, and majority is owing to sucking due to human body.The safety standard regulation of labour health department of China, in workshop air 1, the highest permission mass concentration of 2-dichloroethanes is 15mg/m
3.
At present, the processing method of 1,2-dichloroethanes is had to burning method, photocatalytic degradation method, hydrogenation catalyst reducing process etc.Burning method and photocatalytic method are all that 1,2-dichloroethanes is decomposed, and product comprises carbon dioxide and water, and burning method also can produce carbon monoxide in the situation that of incomplete combustion, all cannot realize the utilization again of product.And hydrogenation catalyst reducing process is because of can be by 1,2-dichloroethanes is converted into the ethene that industrial value is higher, obtains our concern.
In the processing of 1,2-dichloroethanes, conventional bimetallic catalyst is prepared with infusion process.Detailed process is by A, and two kinds of metal salt solutions of B mix in certain proportion, adds evaporate to dryness calcining after quantitative carrier, then at H
2under condition, with certain temperature high temperature reduction.The catalyst of preparing by the method, two kinds of active components evenly mix, and cannot effectively utilize the strong advantage of the metallic element such as Ag or Cu dechlorination ability.
Summary of the invention
The object of this invention is to provide a kind of 1,2-dichloroethanes selective hydrogenation dechlorination titanium dioxide load-type noble metal catalyst, and utilize Photodeposition to prepare the method for this catalyst.
Another object of the present invention is to provide one and utilizes the method for described catalyst to 1,2-dichloroethanes selective hydrogenation dechlorination.
For realizing object of the present invention, by the following technical solutions:
A kind of catalyst of 1,2-dichloroethanes selective hydrogenation dechlorination, is characterized in that this catalyst is taking titanium dioxide as carrier, and light deposition binary metal obtains A-B/TiO successively
2type catalyst, wherein A is precious metals pd, Pt, Au or Rh, B is Cu, Ag or Ni.
In described catalyst, the noble metal A of load accounts for 0.5 ~ 1.5% of total catalyst quality, and the ratio of the molal quantity of metal A and metal B is that 1:0.5 is between 1:3.
Described catalyst deposits two kinds of metallic elements with continuous light sedimentation on titanium dioxide, its surface forms the core of precious metals pd or Pt etc., form the shell of the elements such as Ag or Cu at noble metal core outer surface, thereby effectively utilize the characteristic of two kinds of metals, the activity of catalyst and selective excellence, and can keep good stability.
Described catalyst adopts the method preparation of light deposition, and concrete grammar comprises the following steps:
1) by TiO
2, metal A salt solution and methyl alcohol add in Photoreactor, logical N under the condition of lucifuge
2qi exhaustion is except O
2, under ultraviolet light prolonged exposure, react after 3～6h, it is neutral filtering and being washed till pH with distilled water, dries;
Then according to the method described above, metal B is loaded to carrier TiO
2upper, that is:
2) step 1) products therefrom, metal B salting liquid and methyl alcohol are added in Photoreactor to logical N under lucifuge condition
2remove O
2after, under ultraviolet light continuous light, react 3～6 hours, it is neutral filtering and being washed till pH with distilled water, dries and obtains described catalyst.
The catalyst that said method of the present invention makes is A-B/TiO
2the bimetallic catalyst of type load, wherein A is precious metals pd, Pt, Au or Rh, B is Cu, Ag or Ni.
Chloride, nitrate or sulfate that described metal A salt is metal A; Described metal B salt is chloride, nitrate or the sulfate of metal B.The concentration of metal A salt or B salt is 0.0001 ~ 0.001g/ml.
A-B/TiO prepared by Photodeposition of the present invention
2type supported bimetal catalyst, can be used for gas phase selective hydrogenation catalytic degradation and processes 1,2-dichloroethanes, the invention still further relates to described catalyst A-B/TiO
2application in 1,2-dichloroethanes selective hydrogenation dechlorination, the technical scheme adopting is:
A kind of method of 1,2-dichloroethanes selective hydrogenation dechlorination, is characterized in that, with described A-B/TiO
2for catalyst, in gas phase, 1,2-dichloroethanes is carried out to hydrogenating reduction, the dechlorination of 1,2-dichloroethanes is converted into the hydrocarbon taking ethene as primary product.
In said method, ethene selective >=70%.
Described method specifically comprises the following steps:
1) use Photodeposition at titanium dioxide surface successively carried metal A and B, obtain titanium dichloride load bimetallic A-B/TiO
2catalyst;
2) with A-B/TiO
2for catalyst, by 1,2-dichloroethanes, H
2after mixing with carrier gas He, 1,2-dichloroethanes is carried out to gas phase hydrogenation, reaction temperature is 230 ~ 250 DEG C, and 1,2-dichloroethanes selective hydrogenation dechlorination, is converted into the hydrocarbon taking ethene as primary product.
Wherein A-B/TiO
2catalyst and preparation process thereof are as described above.
The reaction of selective catalytic hydrogenation dechlorination degraded 1,2-dichloroethanes adopts the method for in-situ reducing.Catalyst can be first at 300 DEG C after reductase 12 h, carry out 1,2-dichloroethanes hydrogenation-dechlorination after being down to 250 DEG C.
In described catalytic hydrogenation reaction, the flow velocity of gaseous mixture is 40 ~ 50ml/min; In volumetric concentration, the concentration of hydrogen is 30000 ~ 40000ppm, and the concentration of 1,2-dichloroethanes is 7000 ~ 7500ppm.
The A-B/TiO that adopts light deposition method to prepare according to the present invention
2the bimetallic catalyst of type load, shows significant degradation effect to 1,2-dichloroethanes selective hydrogenation dechlorination, degradation efficiency to 1,2-dichloroethanes is high, the selective height of target product ethene, the good stability of catalyst, reaches the selective stable time fast.Catalyst of the present invention and 1,2-dichloroethanes selective hydrogenation dechlorination method 1, the 2-dichloroethanes that is used for degrading, technical feasible, non-secondary pollution, obvious processing effect, has good economic benefit, and environmentally friendly.
Detailed description of the invention
Embodiment 1
Method with continuous light deposition is prepared Pt-Ag/TiO
2catalyst, concrete grammar is: in the solution that contains a certain amount of titanium dioxide and a certain amount of Pt salt to 480ml, add 10ml methyl alcohol, add in Photoreactor, logical N under the condition of lucifuge
2gas 30min, then opens uviol lamp (500w), under illumination condition, reacts 4h, and it is neutral filtering and being washed till pH with distilled water, dries.Then according to the method identical with above-mentioned carried metal Pt, metal A g is loaded in catalyst carrier.The catalyst obtaining leaves in drier for subsequent use.
As a comparison, utilize Photodeposition prepare Pt or Ag single-metal reforming catalyst and utilize infusion process to prepare titanium dioxide load-type catalyst simultaneously.
The characterization result of the catalyst that two kinds of methods prepare is as shown in table 1 below, and the catalyst that in table 1, infusion process prepares is labeled as:
im-A (x)-B (y)/TiO
2, the catalyst that Photodeposition prepares is labeled as:
pd-A (x)-B (y)/TiO
2.Wherein x represents the mass content of metal A, and y represents the mass content of metal B.
The character of table 1 catalyst
From table 1, we can see, the catalyst preparing by the method for light deposition, and metallic is less than the catalyst that under respective amount, infusion process obtains, consistent with chemisorbed amount.The size of chemisorbed amount indirectly proved the Pt metal coming out on surface content number.As can be seen here, continuous light sedimentation can make metal B well cover the outer surface of metal A.This conclusion has also obtained the support of surface metal content.From table 1, we can see, the catalyst that the ratio of catalyst surface Ag/Pt prepared by Photodeposition obtains higher than infusion process.These digital proofs, catalyst prepared by Photodeposition makes more metal B be exposed to the outside of metal A, can improve the service efficiency of metal B in catalytic reaction process.
Embodiment 2
With continuous light deposition preparation Pt-Ag/TiO
2catalyst, Pt load capacity approximately 1% wherein, the mol ratio of Pt and Ag is about 1:0.5, in embodiment 1
pd-Pt (1.04)-Ag (0.25)/TiO
2catalyst.With above-mentioned Pt-Ag/TiO
2as catalyst, gas phase hydrogenation catalytic degradation 1,2-dichloroethanes.The consumption of catalyst is 100mg, and reaction temperature is 200 ~ 250 DEG C, H
2concentration be 30000 ~ 40000ppm, the concentration of 1,2-dichloroethanes is 7000 ~ 7500ppm, taking He as carrier gas, the flow velocity of gaseous mixture is 40 ~ 50ml/min, synthesis under normal pressure 18 ~ 21h adopts the gas-chromatography of being furnished with fid detector to detect online.Result shows, for target product ethene is selectively 74.3 ~ 89.0%.
Comparative example 1
The Pt/TiO of the Pt load capacity approximately 1% of preparing with the method for light deposition
2as catalyst, in embodiment 1
pd-Pt (1.05)/TiO
2catalyst, gas phase hydrogenation catalytic degradation 1,2-dichloroethanes.The consumption of catalyst is 100mg, and reaction temperature is 200 ~ 250 DEG C, H
2concentration be 30000 ~ 40000ppm, the concentration of 1,2-dichloroethanes is 7000 ~ 7500ppm, taking He as carrier gas, the flow velocity of gaseous mixture is 40 ~ 50ml/min, synthesis under normal pressure 19 ~ 21h, selective 1.5 ~ 1.6% of catalyst.
Selectively lower to ethene of the visible catalyst that utilizes only supporting Pt prepared by Photodeposition.
Comparative example 2
The Ag/TiO of the Ag load capacity approximately 1% of preparing with the method for light deposition
2as catalyst, in embodiment 1
pd-Ag (0.97)/TiO
2catalyst.Gas phase hydrogenation catalytic degradation 1,2-dichloroethanes.The consumption of catalyst is 100mg, and reaction temperature is 200 ~ 250 DEG C, H
2concentration be 30000 ~ 40000ppm, the concentration of 1,2-dichloroethanes is 7000 ~ 7500ppm, taking He as carrier gas, the flow velocity of gaseous mixture is 40 ~ 50ml/min, synthesis under normal pressure does not show any activity and selectivity.
The degraded to 1,2-dichloroethanes of the visible catalyst that utilizes only loaded Ag prepared by Photodeposition does not have activity.
Comparative example 3
Prepare Pt-Ag/TiO with infusion process
2catalyst, wherein Pt load capacity approximately 1%, the mol ratio of Pt and Ag is about 1:0.5, is in embodiment 1
im-Pt (1.03)-Ag (0.25)/TiO
2catalyst.With this Pt-Ag/TiO
2as catalyst, gas phase hydrogenation catalytic degradation 1,2-dichloroethanes.The consumption of catalyst is 100mg, and reaction temperature is 200 ~ 250 DEG C, H
2concentration be 30000 ~ 40000ppm, the concentration of 1,2-dichloroethanes is 7000 ~ 7500ppm, taking He as carrier gas, the flow velocity of gaseous mixture is 40 ~ 50ml/min, synthesis under normal pressure 36 ~ 39h, selective 16.9 ~ 18.2% of catalyst.
The visible selective catalyst of significantly preparing lower than Photodeposition of the present invention that utilizes bimetallic catalyst prepared by infusion process selective.
Embodiment 3
The Pt load capacity approximately 1% of preparing with the method for light deposition, the atomic molar of Pt and Ag is than the Pt-Ag/TiO for about 1:1
2as catalyst, be in embodiment 1
pd-Pt (1.05)-Ag (0.51)/TiO
2catalyst, gas phase hydrogenation catalytic degradation 1,2-dichloroethanes.The consumption of catalyst is 100mg, and reaction temperature is 200 ~ 250 DEG C, H
2concentration be 30000 ~ 40000ppm, the concentration of 1,2-dichloroethanes is 7000 ~ 7500ppm, taking He as carrier gas, the flow velocity of gaseous mixture is 40 ~ 50ml/min, synthesis under normal pressure 17 ~ 19h, selective 86.7 ~ 87.6% of catalyst.
Visible, the molar ratio of increase Pt and Ag can be accelerated catalyst and arrive the stable time, and improves the selective of catalyst.
Embodiment 4
The Pt load capacity 1% of preparing with the method for light deposition, the Pt-Ag/TiO that the atomic ratio of Pt and Ag is 1:2
2as catalyst, be in embodiment 1
pd-Pt (1.07)-Ag (1.05)/TiO
2catalyst, gas phase hydrogenation catalytic degradation 1,2-dichloroethanes.The consumption of catalyst is 100mg, and reaction temperature is 200 ~ 250 DEG C, H
2concentration be 30000 ~ 40000ppm, the concentration of 1,2-dichloroethanes is 7000 ~ 7500ppm, taking He as carrier gas, the flow velocity of gaseous mixture is 40 ~ 50ml/min, synthesis under normal pressure 17 ~ 19h, selective 89.1 ~ 90.0% of catalyst.
The visible mol ratio along with Pt and Ag improves constantly, the selective raising of catalyst to ethene.
Claims (8)
1. one kind 1, the catalyst of 2-dichloroethanes selective hydrogenation dechlorination, is characterized in that this catalyst is taking titanium dioxide as carrier, and light deposition binary metal obtains A-B/TiO successively
2type catalyst, wherein A is precious metals pd, Pt, Au or Rh, B is Cu, Ag or Ni;
Described catalyst adopts following methods to make:
1) by TiO
2, metal A salting liquid and methyl alcohol adds in Photoreactor, logical N under the condition of lucifuge
2remove O
2after, under ultraviolet light continuous light, react 3～6 hours, it is neutral filtering and being washed till pH with distilled water, dries;
2) step 1) products therefrom, metal B salting liquid and methyl alcohol are added in Photoreactor to logical N under the condition of lucifuge
2remove O
2after, under ultraviolet light continuous light, react 3～6 hours, it is neutral filtering and being washed till pH with distilled water, dries and obtains described catalyst.
2. according to claim 11, the catalyst of 2-dichloroethanes selective hydrogenation dechlorination, is characterized in that the noble metal A of load accounts for 0.5 ~ 1.5% of total catalyst quality, and metal A is 1:0.5 ~ 1:2 with the ratio of the molal quantity of metal B.
One kind claimed in claim 11, the preparation method of 2-dichloroethanes selective hydrogenation dechlorination catalyst, is characterized in that, described method comprises the following steps:
1) by TiO
2, metal A salting liquid and methyl alcohol adds in Photoreactor, logical N under the condition of lucifuge
2remove O
2after, under ultraviolet light continuous light, react 3～6 hours, it is neutral filtering and being washed till pH with distilled water, dries;
2) step 1) products therefrom, metal B salting liquid and methyl alcohol are added in Photoreactor to logical N under the condition of lucifuge
2remove O
2after, under ultraviolet light continuous light, react 3～6 hours, it is neutral filtering and being washed till pH with distilled water, dries and obtains described catalyst.
4. according to claim 31, the preparation method of 2-dichloroethanes selective hydrogenation dechlorination catalyst, is characterized in that nitrate, sulfate or chloride that described A salt is metal A; Described B salt is nitrate, sulfate or the chloride of metal B.
5. according to claim 31, the preparation method of 2-dichloroethanes selective hydrogenation dechlorination catalyst, is characterized in that, described A salt or the concentration of B salt are 0.0001 ~ 0.001g/mL.
6. one kind 1, the method for 2-dichloroethanes selective hydrogenation dechlorination, is characterized in that, with A-B/TiO claimed in claim 1
2for catalyst, in gas phase, 1,2-dichloroethanes is carried out to hydrogenating reduction, the dechlorination of 1,2-dichloroethanes is converted into the hydrocarbon taking ethene as primary product;
Described method comprises the following steps:
1) use Photodeposition at titanium dioxide surface successively carried metal A and B, obtain titanium dichloride load bimetallic A-B/TiO
2catalyst, wherein A is precious metals pd, Pt, Au or Rh, B is Cu, Ag or Ni; Described catalyst A-B/TiO
2in, the noble metal A of load accounts for 0.5 ~ 1.5% of total catalyst quality, and the ratio of the molal quantity of metal A and metal B is that 1:0.5 is between 1:2;
2) with A-B/TiO
2for catalyst, by 1,2-dichloroethanes, H
2after mixing with He, 1,2-dichloroethanes is carried out to gas-phase catalytic hydrogenation, reaction temperature is 230 ~ 250 DEG C, and 1,2-dichloroethanes selective hydrogenation dechlorination, is converted into the hydrocarbon taking ethene as primary product.
7. according to claim 61, the method for 2-dichloroethanes selective hydrogenation dechlorination, is characterized in that, in described catalytic hydrogenation reaction, and H
2concentration be 30000 ~ 40000ppm, the concentration of 1,2-dichloroethanes is 7000 ~ 7500ppm, the flow velocity of gaseous mixture is 40 ~ 50mL/min.
8. according to claim 71, the method for 2-dichloroethanes selective hydrogenation dechlorination, is characterized in that, the described catalytic hydrogenation reaction time is 17 ~ 21h.
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| CN102898266B (en) * | 2012-11-06 | 2015-04-01 | 南京大学 | Method for selectively hydrogenating acetylene in ethylene under normal pressure |
| CN104492429A (en) * | 2014-12-16 | 2015-04-08 | 上海华谊（集团）公司 | Catalyst and method for synthesizing methyl glycollate and ethylene glycol by virtue of dimethyl oxalate hydrogenation |
| CN105148907A (en) * | 2015-09-06 | 2015-12-16 | 南京大学 | 1, 2-dichloroethane selective hydrodechlorination reaction catalyst and preparation method and application thereof |
| CN110385138B (en) * | 2019-08-14 | 2022-02-01 | 重庆工商大学 | Preparation method of rhodium-loaded porous tubular carbon nitride photocatalyst applied to chlorophenol hydrodechlorination catalytic reaction |
| CN113083323B (en) * | 2021-04-13 | 2022-07-15 | 中国科学技术大学 | Copper-modified palladium-titanium dioxide nano composite material and preparation method and application thereof |
| CN113600163B (en) * | 2021-09-13 | 2022-06-14 | 厦门大学 | Photocatalyst and application thereof, and preparation method of N-alkyl piperazine and derivatives thereof |
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| CN102070407A (en) * | 2011-01-25 | 2011-05-25 | 中国科学院山西煤炭化学研究所 | Method for synthesizing ethylene glycol from noble metal load nanometer titanium dioxide through photocatalysis |
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| CN101385981A (en) * | 2008-10-30 | 2009-03-18 | 南京大学 | Catalyst for photocatalysis and degradation of benzene and nitrates |
| CN101961651A (en) * | 2010-11-01 | 2011-02-02 | 浙江大学 | Method for preparing noble metal modified one-dimensional titanium dioxide Hg-removing catalyst |
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