CN110102323A - A kind of preparation method of TiC load atom level transition-metal catalyst - Google Patents
A kind of preparation method of TiC load atom level transition-metal catalyst Download PDFInfo
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- CN110102323A CN110102323A CN201910470597.9A CN201910470597A CN110102323A CN 110102323 A CN110102323 A CN 110102323A CN 201910470597 A CN201910470597 A CN 201910470597A CN 110102323 A CN110102323 A CN 110102323A
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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Abstract
The invention discloses a kind of preparation methods of TiC load atom level transition-metal catalyst, and steps are as follows for preparation method: 1) pretreatment of carrier: carrying out acid processing to TiC to remove the oxide layer on surface, then TiC is ultrasonically treated and is heat-treated again;2) drying in vacuum environment is washed with deionized after filtering in the mixture of acid and TiC, is finally ground simultaneously vacuum storage;3) preparation of catalyst: mixing and dried with TiC with equi-volume impregnating drying for metal precursor solutions, be then heat-treated under mixed gas, finally obtains the atom level transition-metal catalyst of TiC load.Preparation method of the present invention is simple, and active constituent is uniformly dispersed, and prepared catalyst is high-efficient, can be used for catalyzing oxidizing degrading volatile organic contaminant.
Description
Technical field
The invention belongs to catalyst application fields, and in particular to a kind of system of TiC load atom level transition-metal catalyst
Preparation Method.
Background technique
Volatile organic compounds (VOCs) is one of main source of atmosphere pollution and the emphasis that China administers at present
Object.So-called VOCs refers to that saturated vapour pressure is greater than one kind that boiling point under 133.3Pa, normal pressure is less than or equal to 260 DEG C under room temperature
Compound.VOCs's is many kinds of, mainly there is alkane, alkene, alkynes, aromatic hydrocarbon etc..Most of volatile organic compounds are not
It only causes damages to ozone depletion environment, more seriously, by the way that (i.e. nitrogen oxides and sulphur aoxidize with other air pollutants
Object) reaction forms photochemical fog, and also threat and leads to irreversible damage at human health.As industrialization and economic add
Speed development, the annual emissions of VOC sharply increase in recent years, especially in developing country.For example, Chinese VOC row in 2015
High-volume close to 31,120,000 tons.Industrial process, especially petrochemical industry, chemical engineering, coating and printing industry account for current year Chinese VOCs people
It is the 43% of source.Since extreme adverse effect and volatility of the volatile organic compounds to environment and human health are organic
The gradually growth of compound emission, countries in the world government have formulated the discharge standard being increasingly stringenter, to limit every profession and trade production
Raw volatile organic compounds.
In the destructive technology for reducing volatile organic compounds, thermal incineration and catalysis oxidation are by the way that VOC to be catalyzed
It is converted into harmless product (CO2, H2O etc.) or become intermediate concentration (> 5,000mg/m3) VOCs two kinds of common approach of removal.With
Traditional thermal incineration is compared, and catalysis oxidation is usually run under lower temperature (200~500 DEG C even lower), in lower temperature
(200~500 DEG C even lower) destroys the VOCs dioxin and toxic product of high concentration completely under degree, therefore more energy efficient.In addition,
Photocatalytic degradation, plasma-catalytic oxidation and biological decomposition are effective administration ways of low concentration VOCs.Due to catalysis oxidation
Particular advantages, be dedicated to extensively exploitation be used for catalysis oxidation VOC effective catalyst, wherein the metal or metal that load
Oxide has been widely used as promising candidate.However, handling various volatile organic compounds or mixed volatilization
Property organic compound when, it becomes complicated and inefficiency.In addition, there is also obstacle, the poisoning including catalyst, coking and burning
Knot, the imperfect combustion of VOC, to the low selectivity of product without secondary pollution, and under the reality of catalyst and longtime running
Inhibit VOCs oxidation.
Study the mainstream work that efficient and rational catalyst becomes current.The catalyst of support type atom level dispersion is because of tool
Have the characteristics that it is efficient, at normal temperatures and pressures can catalysis oxidation VOCs, reduce energy consumption, become VOCs improvement important new skill
Art.
Recently, document it has been reported that monatomic catalyst application in electrocatalytic reaction, such as Choi etc. by atom level
The Pt of dispersion is supported in zeolite carbon template, which contains a large amount of sulphur, the generation H for the property of can choose2O2.Document there has been reported
Chemical reaction of the monatomic catalyst of Yang et al. supporting Pt on TiN for selectivity.Although monatomic catalyst has non-
Often good activity, but it is unstable under harshness, the reaction condition with corrosivity and oxidisability that its major defect, which is monatomic,
Fixed.This needs to find excellent carrier and suitable made of metal just for effective catalyst.Publication No. CN1663679A's
Chinese invention patent discloses " a kind of c loaded noble metal catalyst and preparation method thereof ".Using porous active carbon as load
Body provides a kind of fluid unit to prepare catalyst, and the bullion content needed is high, and metal partial size reduces greatly catalysis
The activity of agent.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of TiC load atom level transition-metal catalyst, catalyst
Carrier and transition metal atoms bond strength are high, and active component is uniformly dispersed, and high catalytic efficiency is adapted to hot environment, system
Preparation Method is simple, at low cost, catalytic effect stability and high efficiency.The temperature needed in preparation process is lower, can reduce energy consumption, increases
Safety.
A kind of preparation method of TiC load atom level transition-metal catalyst of the present invention, comprising the following steps:
(1) oxide layer on the surface TiC, TiC nano particle are removed with the salt acid soak TiC nano particle of 1~3mol/L
Solid-to-liquid ratio with hydrochloric acid is 1:30~1:50g/mL;
(2) ultrasonic treatment is carried out 10~30 minutes to the TiC in hydrochloric acid at 0~30 DEG C, then by the mixing of TiC and hydrochloric acid
Object is heated 1~2 hour with 45~60 DEG C of heating temperature under an ar atmosphere;
(3) TiC solid is taken out from hydrochloric acid solution, be washed with deionized and filtered, then under vacuum conditions in
2~4 hours dry in drying box, drying temperature is 50~60 DEG C;
(4) TiC after drying is ground into powder in mortar, and be stored in vacuumizing case;
(5) precursor solution is mixed with the TiC after grinding with equi-volume impregnating, is put into 50~60 DEG C after mixing evenly
It is 4~6 hours dry in vacuum oven, the carried metal on TiC;
(6) there is the TiC of metal to be transferred in pottery load, be heat-treated at 100~300 DEG C under mixed gas
Obtain within 2~3 hours catalyst and by gained catalyst storage in vacuumizing case;Active metal component in the catalyst
Quality account for the 0.2~1.5% of TiC mass, in the mixed gas argon gas volume accounting be 90%, surplus is hydrogen.
The beneficial effects of the present invention are:
(1) present invention uses equi-volume impregnating, and this law mixes carrier and the dipping solution of its absorbable volume, by
Suitable in the volume of dipping solution and the micro pore volume of carrier, as long as being sufficiently mixed, dipping solution can be impregnated in carrier just
Particle can also be had using equi-volume impregnating to avoid the filtering and recycling of waste liquid convenient for active component in control catalyst
The advantages of content.
(2) present invention prepares catalyst using equi-volume impregnating, and during the preparation process, atom level metal active constituent is equal
The even ingredient and property being supported on carrier and do not change carrier, combines closely with catalyst, catalytic effect stability and high efficiency.System
The temperature needed during standby is lower, can reduce energy consumption, increases safety.
(3) transition metal is dispersed into atom level size, is carried on by atom level site catalysts prepared by the present invention
On nano titanium carbide, being formed by catalyst has efficient catalytic efficiency, under normal temperature and pressure conditions can catalysis oxidation
VOCs has many advantages, such as that operating cost is low, and safety coefficient is high.
(4) developing using single atom or several atoms as the atom level site catalysts of active site is that tradition is urged
The great-leap-forward for changing incineration technology is promoted, and catalytic reaction temperature can be greatly lowered, and is saved process energy consumption, is improved inflammable and explosive VOCs
The safety of destruction, room-temperature catalytic oxidation VOCs are the important technology innovations that environmentally friendly VOCs administers field.
Specific embodiment
The specific implementation step that the present invention will be described in detail combined with specific embodiments below, but embodiments of the present invention are unlimited
In this.
A kind of preparation method of TiC load atom level transition-metal catalyst of the invention, comprising the following steps:
A kind of preparation method of TiC load atom level transition-metal catalyst, comprising the following steps:
(1) oxide layer on the surface TiC, TiC nano particle are removed with the salt acid soak TiC nano particle of 1~3mol/L
Solid-to-liquid ratio with hydrochloric acid is 1:30~1:50g/mL.
(2) ultrasonic treatment is carried out 10~30 minutes to the TiC in hydrochloric acid at 0-30 DEG C, then by the mixing of TiC and hydrochloric acid
Object is heated 1~2 hour with 45~60 DEG C of heating temperature under an ar atmosphere, can change its pore structure in this way, and change
The functional group of carrier surface, so as to better loaded metal ion.
(3) TiC solid is taken out from hydrochloric acid solution, be washed with deionized and filtered, then under vacuum conditions in
2~4 hours dry in drying box, drying temperature is 50~60 DEG C;
(4) TiC after drying is ground into powder in mortar, and be stored in vacuumizing case;
(5) precursor solution is mixed with the TiC after grinding with equi-volume impregnating, is put into 50~60 DEG C after mixing evenly
It is 4~6 hours dry in vacuum oven, the carried metal on TiC.
The precursor solution is the acid solution of transition metal, and configuration process is the TiC nano particle for taking certain mass, root
Go out the quality of the metal acid solid needed according to content of metal inverse, then is added into metal acid solid before deionized water is configured to
The volume of liquid solution, deionized water is determined by the saturated water adsorptive value measured, and finally mixes precursor solution with TiC.
The maceration extract volume that equi-volume impregnating only needs TiC to absorb is equal with the pore volume of TiC.Measure the saturation of TiC
Water absorption uses existing method, can inquire to obtain on the net;
The saturated water adsorptive value specific method for measuring TiC can be with are as follows: takes 1gTiC sample to be placed in beaker, then rubber head dropper
Deionized water is added dropwise until just covering sample, stands 4~5 hours.Then the water for sucking sample surfaces, until sample
Until product surface does not have apparent water droplet.The volume of the of poor quality or attention plus water before and after adding water is weighed, the difference of front and back is
Saturated water adsorptive value.The measurement of saturated water adsorptive value need to only be done and be averaged three times, be learnt according to experiment, the saturation water suction of TiC
Amount is every 1g TiC water suction 0.4mL.
The precursor solution is H2PtCl6﹒ 6H2O, AgNO3, Cu (NO3)2﹒ 3H2O and Ni (NO3)2﹒ 6H2One of O
Or it is a variety of.
(6) there is the TiC of metal to be transferred in pottery load, be heat-treated at 100~300 DEG C under mixed gas
Obtain within 2~3 hours catalyst and by gained catalyst storage in vacuumizing case.Active metal component in the catalyst
Quality account for the 0.2~1.5% of TiC mass.Argon gas volume accounting is 90% in the mixed gas, and surplus is hydrogen.
Embodiment 1
(1) 1g TiC nanometer powder is weighed on balance, adds it to 30ml, sour processing is carried out in the hydrochloric acid of 1mol/L
To remove the oxide layer on surface.
(2) ultrasonic treatment is carried out 10 minutes to the TiC in hydrochloric acid at 0 DEG C, then by the mixture of TiC and hydrochloric acid in Ar gas
It is heated 1 hour under atmosphere with 45 DEG C of heating temperature;
(3) TiC solid is taken out from hydrochloric acid solution, be washed with deionized and filtered, then under vacuum conditions in
2 hours dry in drying box, drying temperature is 50 DEG C;
(4) TiC after drying is ground into powder in mortar, and be stored in vacuumizing case;
(5) precursor solution is mixed with the TiC after grinding with equi-volume impregnating, is put into 50 DEG C of vacuum after mixing evenly
It is 4 hours dry in drying box, the carried metal on TiC.
The precursor solution is H2PtCl6﹒ 6H2O solution, configuration process are the TiC nano particle for taking 80mg, according to negative
The quality that carrying capacity inverse goes out the metal acid solid needed is 0.425mg, then 32 μ L deionized waters are added into metal acid solid and match
It is set to precursor solution, finally mixes precursor solution with TiC.
(6) TiC of Pt metal is transferred in pottery load, heat treatment 2 is small at 100 DEG C under mixed gas
When obtain catalyst, and by gained catalyst storage in vacuumizing case.Active metal Pt component in the catalyst
Quality accounts for the 0.2% of TiC mass.Argon gas volume accounting is 90% in the mixed gas, and surplus is hydrogen.
The atom level catalyst of preparation is evaluated, specific steps are as follows:
(a) it will be sieved after powder catalyst tabletting, take catalyst of the size between 10~20 mesh to retain spare.
(b) catalyst remained is filled in the reactor of catalyst test apparatus, descends both ends on a catalyst
Sizeable cotton is filled in, prevents catalyst from blowing out reactor by gas.
(c) methanol, toluene, acetoneand ethyl acetate are chosen as reactant, initial concentration 400ppm, air speed is
5000/h.Ozone is oxidant, and reaction temperature is 50 DEG C.
The VOCs concentration before and after catalyst reaction is added with gas chromatographic detection, and calculates catalyst to different organic gas
Degradation rate;TiC load atom level transition-metal catalyst can be used for volatile organic contaminant (VOCs) and be catalyzed at normal temperature
Oxidation processes.Catalysis oxidation uses existing method: the process of the catalysis oxidation is as follows: initial concentration for 400~
The VOCs gas of 500ppm passes through the atom level transition-metal catalyst equipped with TiC load with the air speed of 5000~10000/h
Reactor.The nitrogen buffering gas of the ozone that flow is 100mL/min and flow 100mL/min with flow are 30mL/min after mixing
The nitrogen containing VOCs enter in mixer mixed together, the concentration of VOCs is 100ppm in mixer;In a mixer
Gas mixing it is complete after from reactor lower part enter reactor, catalyst is fitted into the reaction tube in reactor, then gas
Body is discharged from reaction tube top;Temperature of reactor control is 50 DEG C, and pressure control is 0.2MPa.
Testing result is as follows:
VOCs | Methanol | Toluene | Acetone | Ethyl acetate |
Initial concentration (ppm) | 400 | 400 | 400 | 400 |
Tail gas concentration (ppm) | 0 | 30.8 | 48.8 | 56.8 |
Degradation rate | 100% | 92.3% | 87.8% | 85.8% |
As can be seen from the table: having higher degradation rate to VOCs using atom level loading transition metallic catalyst, not only
It can handle simple organic gas, also have preferable removal rate to VOCs difficult to degrade.
Embodiment 2
(1) 1g TiC nanometer powder is weighed on balance, adds it to 40ml, sour processing is carried out in the hydrochloric acid of 2mol/L
To remove the oxide layer on surface.
(2) ultrasonic treatment is carried out 20 minutes to the TiC in hydrochloric acid at 15 DEG C, then by the mixture of TiC and hydrochloric acid in Ar
It is heated 1.5 hours under atmosphere with 50 DEG C of heating temperature;
(3) TiC solid is taken out from hydrochloric acid solution, be washed with deionized and filtered, then done under vacuum conditions
Dry 3 hours, drying temperature was 55 DEG C;
(4) TiC after drying is ground into powder in mortar, and be stored in vacuumizing case;
(5) precursor solution is mixed with the TiC after grinding with equi-volume impregnating, is put into 55 DEG C of vacuum after mixing evenly
It is 5 hours dry in drying box, the carried metal on TiC.
The precursor solution is Cu (NO3)2﹒ 3H2O solution, process for preparation are the TiC nano particle for taking 80mg, according to negative
The quality that carrying capacity inverse goes out the metal acid solid needed is 0.991mg, then 32 μ L deionized waters are added into metal acid solid and match
It is set to precursor solution, finally mixes precursor solution with TiC.
(6) there is the TiC of Cu metal to be transferred in pottery load, be heat-treated 2.5 at 200 DEG C under mixed gas
Hour obtains catalyst, and by gained catalyst storage in vacuumizing case.Active metal component in the catalyst
Quality accounts for the 1.0% of TiC mass.Argon gas volume accounting is 90% in the mixed gas, and surplus is hydrogen.
The atom level catalyst of preparation is evaluated, specific steps are as follows:
(a) it will be sieved after powder catalyst tabletting, take catalyst of the size between 10~20 mesh to retain spare.
(b) catalyst remained is filled in the reactor of catalyst test apparatus, descends both ends on a catalyst
Sizeable cotton is filled in, prevents catalyst from blowing out reactor by gas.
(c) methanol, toluene, acetoneand ethyl acetate are chosen as reactant, initial concentration 450ppm, air speed is
7500/h.Ozone is oxidant, and reaction temperature is 50 DEG C.
The VOCs concentration before and after catalyst reaction is added with gas chromatographic detection, and calculates catalyst to different organic gas
Degradation rate;Specific detection method is the same as embodiment 1
Testing result is as follows:
VOCs | Methanol | Toluene | Acetone | Ethyl acetate |
Initial concentration (ppm) | 450 | 450 | 450 | 450 |
Tail gas concentration (ppm) | 0 | 27.9 | 44.1 | 55.8 |
Degradation rate | 100% | 93.8% | 90.2% | 87.6% |
As can be seen from the table: having higher degradation rate to VOCs using atom level loading transition metallic catalyst, not only
It can handle simple organic gas, also have preferable removal rate to VOCs difficult to degrade.
Embodiment 3
(1) 1g TiC nanometer powder is weighed on balance, adds it to 50ml, sour processing is carried out in the hydrochloric acid of 3mol/L
To remove the oxide layer on surface.
(2) ultrasonic treatment is carried out 30 minutes to the TiC in hydrochloric acid at 30 DEG C, then by the mixture of TiC and hydrochloric acid in Ar
It is heated 2 hours under atmosphere with 60 DEG C of heating temperature;
(3) TiC solid is taken out from hydrochloric acid solution, be washed with deionized and filtered, then done under vacuum conditions
Dry 4 hours, drying temperature was 60 DEG C;
(4) TiC after drying is ground into powder in mortar, and be stored in vacuumizing case;
(5) precursor solution is mixed with the TiC after grinding with equi-volume impregnating, is put into 60 DEG C of vacuum after mixing evenly
It is 6 hours dry in drying box, the carried metal on TiC.
The precursor solution is AgNO3With Ni (NO3)2﹒ 6H2The mixed solution of O, process for preparation are that the TiC of 80mg is taken to receive
Rice grain is AgNO according to the quality that load capacity inverse goes out the metal acid solid needed31.260mg, Ni (NO3)2﹒ 6H2O
1.982mg, then 32 μ L deionized waters are added into metal acid solid and are configured to precursor solution, finally precursor solution and TiC are mixed
Conjunction.
(6) TiC of Ag and Ni are transferred in pottery load, heat treatment 3 is small at 300 DEG C under mixed gas
When obtain catalyst, and by gained catalyst storage in vacuumizing case.Active metal Ag component in the catalyst
Quality accounts for the 1.0% of TiC mass, and the quality of active metal Ni component accounts for the 0.5% of TiC mass, active metal component gross mass
Account for the 1.5% of TiC mass.Argon gas volume accounting is 90% in the mixed gas, and surplus is hydrogen.
The atom level catalyst of preparation is evaluated, specific steps are as follows:
(a) it will be sieved after powder catalyst tabletting, take catalyst of the size between 10~20 mesh to retain spare.
(b) catalyst remained is filled in the reactor of catalyst test apparatus, descends both ends on a catalyst
Sizeable cotton is filled in, prevents catalyst from blowing out reactor by gas.
(c) methanol, toluene, acetoneand ethyl acetate are chosen as reactant, initial concentration 500ppm, air speed is
10000/h.Ozone is oxidant, and reaction temperature is 50 DEG C.
The VOCs concentration before and after catalyst reaction is added with gas chromatographic detection, and calculates catalyst to different organic gas
Degradation rate;Specific detection method is the same as embodiment 1
Testing result is as follows:
VOCs | Methanol | Toluene | Acetone | Ethyl acetate |
Initial concentration (ppm) | 500 | 500 | 500 | 500 |
Tail gas concentration (ppm) | 0 | 28.5 | 42 | 59.5 |
Degradation rate | 100% | 94.3% | 91.6% | 88.1% |
As can be seen from the table: having higher degradation rate to VOCs using atom level loading transition metallic catalyst, not only
It can handle simple organic gas, also have preferable removal rate to VOCs difficult to degrade.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not limited by examples detailed above
System, others are any to be accordingly to be regarded as without departing from spirit of the invention and changes, modifications, substitutions, combinations, simplifications made under principle
It is equivalent.
Claims (2)
1. a kind of preparation method of TiC load atom level transition-metal catalyst, it is characterised in that the following steps are included:
(1) oxide layer on the surface TiC, TiC nano particle and salt are removed with the salt acid soak TiC nano particle of 1~3mol/L
The solid-to-liquid ratio of acid is 1:30~1:50g/mL;
(2) ultrasonic treatment is carried out 10~30 minutes to the TiC in hydrochloric acid at 0-30 DEG C, then the mixture of TiC and hydrochloric acid is existed
It is heated 1~2 hour under Ar atmosphere with 45~60 DEG C of heating temperature;
(3) TiC solid is taken out from hydrochloric acid solution, be washed with deionized and filtered, then under vacuum conditions in drying
2~4 hours dry in case, drying temperature is 50~60 DEG C;
(4) TiC after drying is ground into powder in mortar, and be stored in vacuumizing case;
(5) precursor solution is mixed with the TiC after grinding with equi-volume impregnating, is put into 50~60 DEG C of vacuum after mixing evenly
It is 4~6 hours dry in drying box, the carried metal on TiC;
(6) there is the TiC of metal to be transferred in pottery load, be heat-treated 2~3 at 100~300 DEG C under mixed gas
Hour obtains catalyst and by gained catalyst storage in vacuumizing case;The matter of active metal component in the catalyst
Amount accounts for the 0.2~1.5% of TiC mass, and argon gas volume accounting is 90% in the mixed gas, and surplus is hydrogen.
2. the preparation method of TiC load atom level transition-metal catalyst according to claim 1, it is characterised in that: institute
The precursor solution stated is H2PtCl6﹒ 6H2O、AgNO3、Cu(NO3)2﹒ 3H2O and Ni (NO3)2﹒ 6H2One of O or a variety of.
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Cited By (1)
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CN112452346A (en) * | 2020-10-14 | 2021-03-09 | 浙江大学 | Universal method for preparing metal single-atom carbon-based catalyst and application |
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- 2019-05-31 CN CN201910470597.9A patent/CN110102323A/en active Pending
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CN101694880A (en) * | 2009-10-22 | 2010-04-14 | 复旦大学 | Electrode catalyst of fuel cell |
KR20170073831A (en) * | 2015-12-18 | 2017-06-29 | 한국과학기술원 | Titanium carbide supported Pt single-atom catalyst for production of hydrogen peroxide, MEA including the same and Method for preparing the catalyst |
Non-Patent Citations (2)
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SANGYONG SHIN等: "Changes in the oxidation state of Pt single-atom catalysts upon removal of chloride ligands and their effect for electrochemical reactions", 《CHEM. COMMUN.》 * |
李路军: "常温高校催化氧化芳香族VOCs的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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