CN109821548A - A kind of preparation method of composite metal catalyst - Google Patents
A kind of preparation method of composite metal catalyst Download PDFInfo
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Abstract
The present invention discloses a kind of preparation method of composite metal catalyst, comprising the following steps: stirs after copper chloride, bismuth oxide and distilled water is added in the reactor, obtains premixed liquid；Oleyl amine, n-hexane and phenol are added into the premixed liquid, then under stirring, 2~3h of insulation reaction, is cooled to room temperature after being warming up to 40~50 DEG C, obtains generating the reaction solution for having solid matter；It is washed after isolating the solid matter in the reaction solution, obtains solid mixture；The solid mixture is mixed and ground with sodium sulphate, it is then cooling after 350~400 DEG C of 2~3h of temperature lower calcination, then calcined product is washed and is dried, obtain composite metal catalyst.The present invention is compound by Nanometer Copper and bismuth oxide progress by chemical reaction, and obtained composite material can be used as a kind of photochemical catalyst with excellent photocatalysis performance.
Description
Technical field
The present invention relates to catalyst preparation technical fields, in particular to metallic catalyst preparation technical field, and in particular to
A kind of preparation method of composite metal catalyst.
Background technique
Nano-copper base material is a kind of very important transition metal oxide nano-material, gas sensor, catalysis,
All there is potential application value in the various aspects such as lithium ion battery and heavy metal adsorption.With other transition metal oxide nanos
Material is compared, and nano-copper base material price is cheap, environmentally friendly and high catalytic activity becomes the heat of people's research
Point.In recent years, people have used different synthetic methods to synthesize the nano-copper base material of different-shape and size, and have studied
Its application in every field.Forefathers' studies have shown that developing different synthetic methods and efficiently controlling the shape of nano material
Looks, size, composition and specific surface area etc. can improve the performance of material in all fields, but what existing synthetic method was prepared
Nano-copper base material as photochemical catalyst in use, its photocatalysis performance remains to be further improved.
Summary of the invention
The main object of the present invention is to propose a kind of preparation method of composite metal catalyst, it is intended to improve photochemical catalyst
Photocatalysis performance.
To achieve the above object, the present invention proposes a kind of preparation method of composite metal catalyst, comprising the following steps:
It is stirred after copper chloride, bismuth oxide and distilled water is added in the reactor, obtains premixed liquid；
Oleyl amine, n-hexane and phenol are added into the premixed liquid, then under stirring, after being warming up to 40~50 DEG C
2~3h of insulation reaction, is cooled to room temperature, obtains generating the reaction solution for having solid matter；
It is washed after isolating the solid matter in the reaction solution, obtains solid mixture；
The solid mixture is mixed and ground with sodium sulphate, then after 350~400 DEG C of 2~3h of temperature lower calcination
It is cooling, then calcined product is washed and is dried, obtain composite metal catalyst.
Optionally, the mass ratio of the copper chloride, bismuth oxide, oleyl amine, n-hexane and phenol is (10~200): (5
~50): (5~15): (3~6): (3~9).
Optionally, it isolates the step of being washed, obtain solid mixture after the solid matter in the reaction solution, packet
It includes:
After reaction solution centrifugation, the solid matter isolated is washed, solid mixture is obtained.
Optionally, by after reaction solution centrifugation, the solid matter isolated is washed, solid mixture is obtained
In step:
The centrifugal rotational speed when centrifugation is 2000~5000r/min, centrifugation time is 10~15min.
Optionally, by after reaction solution centrifugation, the solid matter isolated is washed, solid mixture is obtained
In step:
The mode washed to the solid matter isolated is to be washed repeatedly using distilled water 5~8 times.
Optionally, the solid mixture is mixed and is ground with sodium sulphate, then in 350~400 DEG C of temperature lower calcinations 2
It is cooling after~3h, then in the step of being washed to calcined product and being dried, obtain composite metal catalyst:
The mass ratio of the solid mixture and the sodium sulphate is 1:(0.6~1.1).
Optionally, the solid mixture is mixed and is ground with sodium sulphate, then in 350~400 DEG C of temperature lower calcinations 2
It is cooling after~3h, then in the step of being washed to calcined product and being dried, obtain composite metal catalyst:
The mode washed to calcined product is to be washed repeatedly using the mixed liquor of distilled water and ethyl alcohol 2~4 times,
In, the mass ratio of distilled water and ethyl alcohol in the mixed liquor is (2~4): 1.
Optionally, the solid mixture is mixed and is ground with sodium sulphate, then in 350~400 DEG C of temperature lower calcinations 2
It is cooling after~3h, then in the step of being washed to calcined product and being dried, obtain composite metal catalyst:
Drying temperature when calcined product is dried is 80~90 DEG C, drying time is 30~40min.
In technical solution provided by the invention, by selecting copper chloride, bismuth oxide, oleyl amine, n-hexane and phenol to make
The composite material of Nanometer Copper and bismuth oxide is obtained, wherein nanometer after a series of chemical reaction for reaction raw materials
Both copper and bismuth oxide itself are good photochemical catalyst, after forming composite material by reaction, the composite material energy
The valence band of two kinds of photochemical catalysts and the difference of conduction level are enough utilized, after surface receives light radiation, two kinds of substances can be sent out simultaneously
Transition is given birth to, the recombination rate of electron-hole can be effectively reduced in the part electron transition between two kinds of substances, to improve photochemistry
Activity achievees the effect that improve photocatalysis performance.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
Other relevant attached drawings are obtained according to these attached drawings.
Fig. 1 is the flow diagram of an embodiment of the preparation method of composite metal catalyst provided by the invention.
The embodiments will be further described with reference to the accompanying drawings for the realization, the function and the advantages of the object of the present invention.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Nano-copper base material is a kind of very important transition metal oxide nano-material, gas sensor, catalysis,
All there is potential application value in the various aspects such as lithium ion battery and heavy metal adsorption.Studies have shown that the metal that incorporation is different
Or metal oxide can synthesize the nano-copper base material of different-shape and size, and efficiently control nano-copper base material
Pattern, size, composition and specific surface area etc. can improve the performance of nano-copper base material in all fields, but its photocatalytic
It can remain to be further improved.
In consideration of it, the present invention proposes a kind of preparation method of composite metal catalyst, Nanometer Copper and bismuth oxide are led to
It crosses chemical reaction and composite material is made, to achieve the effect that improve photocatalysis performance, Fig. 1 show provided by the invention compound
One embodiment of the preparation method of metallic catalyst.Referring to Fig. 1, in the present embodiment, the system of the composite metal catalyst
Preparation Method the following steps are included:
Step S10, it is stirred after copper chloride, bismuth oxide and distilled water being added in the reactor, obtains premixed liquid；
Step S20, oleyl amine, n-hexane and phenol are added in Xiang Suoshu premixed liquid and are then under stirring warming up to 40
2~3h of insulation reaction, is cooled to room temperature after~50 DEG C, obtains generating the reaction solution for having solid matter；
In the specific implementation, copper chloride, bismuth oxide are first added into reactor, distilled water is then added and is stirred
It mixes, agitating mode and stirring condition are not specifically limited, such as can be the modes such as mechanical stirring or ultrasonic agitation, as long as
Copper chloride and bismuth oxide can be made to be well dispersed in distilled water and obtain the premixed liquid, in the present embodiment specifically
The revolving speed that 200~500r/min can be used carries out 20~30min of mechanical stirring, to obtain the premixed liquid；Again to described pre-
Oleyl amine, n-hexane and phenol, then warming while stirring are added in mixed liquid, agitating mode at this time is preferably ultrasonic wave stirring,
Such as reactor can be placed in the ultrasonic stirrer that temperature setting is 40~50 DEG C, it is kept the temperature after being warming up to 40~50 DEG C
2~3h is reacted, is cooled to room temperature naturally after completion of the reaction, obtains reaction solution.Wherein, the n-hexane is as solvent；The oleyl amine
As reducing agent, while also there is certain peptizaiton to bismuth oxide；The phenol is ligand, is matched with copper ion formation
It closes object and nano-copper base material is easily become by oleyl amine reduction；The additions of these three reagents allows the nano-copper base composite material of generation
Particle is thinner, granular size is more uniform consistent, to obtain the solid product of nano-copper base composite catalyst.Further,
The wherein adding proportion of each raw material are as follows: the copper chloride, bismuth oxide, oleyl amine, n-hexane and phenol mass ratio be (10
~200): (5~50): (5~15): (3~6): (3~9), wherein the n-hexane is liquid, can be according to it in addition
Density (density under normal temperature and pressure is 0.66g/mL) measures mass conversion at volume, more convenient.
Step S30, it is washed after isolating the solid matter in the reaction solution, obtains solid mixture；
In the present embodiment, solid matter generated in reaction is isolated preferably by the mode of centrifugation, had solid
Liquid separative efficiency is high, advantage easy to operate, when specific operation, preferably selection centrifugal rotational speed be 2000~5000r/min,
The parameter setting that centrifugation time is 10~15min carries out centrifugal treating to the reaction solution, obtains the solid generated in step S20
Product.Further, the solid matter isolated is washed the reaction solution after centrifugation, is reused distilled water,
Washing times are preferably 5~8 times, and solid mixture is obtained after the completion of washing.
Step S40, the solid mixture is mixed and is ground with sodium sulphate, then in 350~400 DEG C of temperature lower calcinations
It is cooling after 2~3h, then calcined product is washed and is dried, obtain composite metal catalyst.
The sodium sulphate serves as calcining auxiliary agent in calcination process so that Nanometer Copper and bismuth oxide be combined into it is more stable
Composite material, in the specific implementation, by the solid mixture with sodium sulphate according to 1:(0.6~1.1) mass ratio mix
Afterwards, it is put into grinder and carries out 20~30min of grinding, the two is made to be sufficiently mixed to obtain hybrid solid, it is then again that the mixing is solid
Body is put into Muffle furnace and is calcined, cooled to room temperature after calcining, then uses the mixed liquor of distilled water and ethyl alcohol
Calcined product is washed, wherein the mass ratio of distilled water and ethyl alcohol in the mixed liquor is (2~4): 1, more preferably
Washed product after washing 2~4 times repeatedly, is placed in 30~40min of drying process under the conditions of 80~90 DEG C of temperature, is made by 3:1
Composite metal catalyst.
In technical solution provided by the invention, by selecting copper chloride, bismuth oxide, oleyl amine, n-hexane and phenol to make
The composite material of Nanometer Copper and bismuth oxide composition is obtained after a series of chemical reaction for reaction raw materials, wherein
Both Nanometer Copper and bismuth oxide itself are good photochemical catalyst, after forming composite material by reaction, the composite wood
Material can utilize the valence band of two kinds of photochemical catalysts and the difference of conduction level, and after surface receives light radiation, two kinds of substances can be same
Shi Fasheng transition, the recombination rate of electron-hole can be effectively reduced in the part electron transition between two kinds of substances, to improve light
Chemical activity achievees the effect that improve photocatalysis performance；The preparation method of the composite metal catalyst is being applied to industrial production
When, preparation process can be degraded rapidly using some organic pollutants in raw material, advantageously reduce to environment
Pollution.
Technical solution of the present invention is described in further detail below in conjunction with specific embodiments and the drawings, it should be understood that
Following embodiment is only used to explain the present invention, is not intended to limit the present invention.
Embodiment 1
(1) copper chloride 10g, bismuth oxide 5g are added in the reactor, distilled water is added to stir 20min；
(2) oleyl amine 5g, n-hexane 5mL, phenol 3g are successively added into reactor, ultrasonic wave stirring raises simultaneously temperature extremely
40 DEG C, keep temperature-resistant, after being stirred to react 2h, cooled to room temperature；
(3) reaction solution in reactor is centrifuged under the revolving speed of 5000r/min 15min, then washs 5 repeatedly with distilled water
Solid mixture is obtained after secondary, by solid mixture and sodium sulphate according to the quality of 1:0.6 than mixed grinding 30min after, place
3h, natural cooling after the completion of calcining are calcined in 350 DEG C of Muffle furnace, then use distilled water and ethyl alcohol according to the mass ratio of 3:1
The mixed liquor that example is mixed to form washs calcined product 2 times, dries 30min after washing at a temperature of 90 DEG C, obtains compound gold
Metal catalyst.
Embodiment 2
(1) copper chloride 200g, bismuth oxide 50g are added in the reactor, distilled water is added to stir 30min；
(2) oleyl amine 15g, n-hexane 9mL, phenol 9g are successively added into reactor, ultrasonic wave stirring raises simultaneously temperature
To 50 DEG C, keep temperature-resistant, after being stirred to react 3h, cooled to room temperature；
(3) reaction solution in reactor is centrifuged under the revolving speed of 2000r/min 10min, then washs 8 repeatedly with distilled water
Solid mixture is obtained after secondary, by solid mixture and sodium sulphate according to the quality of 1:1.1 than mixed grinding 20min after, place
2h, natural cooling after the completion of calcining are calcined in 400 DEG C of Muffle furnace, then use distilled water and ethyl alcohol according to the mass ratio of 3:1
The mixed liquor that example is mixed to form washs calcined product 4 times, dries 340min after washing at a temperature of 80 DEG C, obtains compound gold
Metal catalyst.
Embodiment 3
(1) copper chloride 110g, bismuth oxide 25g are added in the reactor, distilled water is added to stir 25min；
(2) oleyl amine 10g, n-hexane 8mL, phenol 7g are successively added into reactor, ultrasonic wave stirring raises simultaneously temperature
To 45 DEG C, keep temperature-resistant, after being stirred to react 2.5h, cooled to room temperature；(3) reaction solution in reactor is existed
It is centrifuged 14min under the revolving speed of 3000r/min, then obtains solid mixture after washing 7 times repeatedly with distilled water, by solid mixture
With sodium sulphate according to the quality of 1:0.8 than mixed grinding 26min after, be placed in 360 DEG C of Muffle furnace and calcine 3h, calcining complete
Natural cooling afterwards, then calcined product is washed 3 according to the mixed liquor that the mass ratio of 3:1 is mixed to form using distilled water and ethyl alcohol
It is secondary, 36min is dried after washing at a temperature of 85 DEG C, obtains composite metal catalyst.
Embodiment 4
(1) copper chloride 150g, bismuth oxide 40g are added in the reactor, distilled water is added to stir 26min；
(2) oleyl amine 11g, n-hexane 7mL, phenol 5g are successively added into reactor, ultrasonic wave stirring raises simultaneously temperature
To 44 DEG C, keep temperature-resistant, after being stirred to react 2.3h, cooled to room temperature；
(3) reaction solution in reactor is centrifuged under the revolving speed of 4000r/min 13min, then washs 7 repeatedly with distilled water
Solid mixture is obtained after secondary, by solid mixture and sodium sulphate according to the quality of 1:1.0 than mixed grinding 24min after, place
2h, natural cooling after the completion of calcining are calcined in 370 DEG C of Muffle furnace, then use distilled water and ethyl alcohol according to the mass ratio of 2:1
The mixed liquor that example is mixed to form washs calcined product 3 times, dries 38min after washing at a temperature of 86 DEG C, obtains compound gold
Metal catalyst.
Embodiment 5
(1) copper chloride 180g, bismuth oxide 30g are added in the reactor, distilled water is added to stir 28min；
(2) oleyl amine 12g, n-hexane 6mL, phenol 4g are successively added into reactor, ultrasonic wave stirring raises simultaneously temperature
To 46 DEG C, keep temperature-resistant, after being stirred to react 2.2h, cooled to room temperature；
(3) reaction solution in reactor is centrifuged under the revolving speed of 3000r/min 12min, then washs 6 repeatedly with distilled water
Solid mixture is obtained after secondary, by solid mixture and sodium sulphate according to the quality of 1:0.9 than mixed grinding 23min after, place
2.5h, natural cooling after the completion of calcining are calcined in 380 DEG C of Muffle furnace, then use distilled water and ethyl alcohol according to the quality of 4:1
The mixed liquor that ratio is mixed to form washs calcined product 3 times, dries 34min after washing at a temperature of 82 DEG C, obtains compound
Metallic catalyst.
Beneficial effect in order to further illustrate the present invention, as a comparison case with nanometer copper product, by the embodiment of the present invention 1
Composite metal catalyst and nanometer copper product to 5 preparations carry out photocatalysis experiment, verify its photocatalysis performance, specific method is such as
Under:
Precise 0.0500g methylene blue is configured to the methylene blue that concentration is 10.00mg/L with 500mL volumetric flask
Solution takes the methyl blue solution of five parts of 50mL, then the composite metal catalyzing for taking nanometer copper product and embodiment 1 to 5 to prepare respectively
Agent material 50mg is correspondingly placed into seven polytetrafluoroethylene (PTFE) magnetons in seven big quartz ampoule, in each big quartz ampoule and sticks
Label (stays a methylene blue solution to do blank control and is not put into any photochemical catalyst).The first dark reaction in photochemical reactor
0.5h makes system reach saturation state, draws about 5mL reaction solution with suction pipe, after centrifuge separates solid catalyst, takes
It is A0 that clear solution surveys its absorbance respectively；500W mercury lamp is then opened, hereafter per in half an hour with suction pipe absorption about 5mL reaction
Liquid separates solid catalyst with centrifuge, takes supernatant solution using blank solution as reference, with spectrophotometric measurement in 664nm
Absorbance A t and make a record, altogether illumination 3h.Each catalysis is calculated according to calculation formula W (%)=(A0-At)/A0 × 100%
The degradation rate of agent, calculated result are as shown in table 1 below.
The degradation rate calculated result of 1 catalyst of table
By the result in above-mentioned table 1 it is found that for directly using nanometer copper product as photochemical catalyst, composition metal
The degradation rate of catalyst is higher, illustrates that the composite metal catalyst of preparation of the embodiment of the present invention has higher photochemical activity,
Its photocatalysis performance is more preferably.
The above is only a preferred embodiment of the present invention, is not intended to limit the scope of the invention, for this field
For technical staff, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any
Modification, equivalent replacement, improvement etc. should all be included within the scope of the present invention.
Claims (8)
1. a kind of preparation method of composite metal catalyst, which comprises the following steps:
It is stirred after copper chloride, bismuth oxide and distilled water is added in the reactor, obtains premixed liquid；
Oleyl amine, n-hexane and phenol are added into the premixed liquid then under stirring to keep the temperature after being warming up to 40~50 DEG C
2~3h is reacted, room temperature is cooled to, obtains generating the reaction solution for having solid matter；
It is washed after isolating the solid matter in the reaction solution, obtains solid mixture；
The solid mixture is mixed and ground with sodium sulphate, it is then cooling after 350~400 DEG C of 2~3h of temperature lower calcination,
Calcined product is washed and is dried again, obtains composite metal catalyst.
2. the preparation method of composite metal catalyst as described in claim 1, which is characterized in that the copper chloride, three oxidations
Two bismuths, oleyl amine, n-hexane and phenol mass ratio be (10~200): (5~50): (5~15): (3~6): (3~9).
3. the preparation method of composite metal catalyst as described in claim 1, which is characterized in that isolate in the reaction solution
Solid matter after the step of being washed, obtaining solid mixture, comprising:
After reaction solution centrifugation, the solid matter isolated is washed, solid mixture is obtained.
4. the preparation method of composite metal catalyst as claimed in claim 3, which is characterized in that the reaction solution to be centrifuged
Afterwards, in the step of washing to the solid matter isolated, obtain solid mixture:
The centrifugal rotational speed when centrifugation is 2000~5000r/min, centrifugation time is 10~15min.
5. the preparation method of composite metal catalyst as claimed in claim 3, which is characterized in that the reaction solution to be centrifuged
Afterwards, in the step of washing to the solid matter isolated, obtain solid mixture:
The mode washed to the solid matter isolated is to be washed repeatedly using distilled water 5~8 times.
6. the preparation method of composite metal catalyst as described in claim 1, which is characterized in that by the solid mixture with
Sodium sulphate is mixed and is ground, then cooling after 350~400 DEG C of 2~3h of temperature lower calcination, then to calcined product carry out washing and
In the step of being dried, obtaining composite metal catalyst:
The mass ratio of the solid mixture and the sodium sulphate is 1:(0.6~1.1).
7. the preparation method of composite metal catalyst as described in claim 1, which is characterized in that by the solid mixture with
Sodium sulphate is mixed and is ground, then cooling after 350~400 DEG C of 2~3h of temperature lower calcination, then to calcined product carry out washing and
In the step of being dried, obtaining composite metal catalyst:
The mode washed to calcined product is to be washed repeatedly using the mixed liquor of distilled water and ethyl alcohol 2~4 times, wherein institute
The mass ratio for stating the distilled water and ethyl alcohol in mixed liquor is (2~4): 1.
8. the preparation method of composite metal catalyst as described in claim 1, which is characterized in that by the solid mixture with
Sodium sulphate is mixed and is ground, then cooling after 350~400 DEG C of 2~3h of temperature lower calcination, then to calcined product carry out washing and
In the step of being dried, obtaining composite metal catalyst:
Drying temperature when calcined product is dried is 80~90 DEG C, drying time is 30~40min.
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| CN113856668A (en) * | 2021-09-26 | 2021-12-31 | 许昌学院 | Bi/BiVO4Preparation method of composite heterojunction photocatalytic material |
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