CN110252289A - A kind of preparation method of the platinum carbon catalyst based on microreactor - Google Patents
A kind of preparation method of the platinum carbon catalyst based on microreactor Download PDFInfo
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- CN110252289A CN110252289A CN201910513116.8A CN201910513116A CN110252289A CN 110252289 A CN110252289 A CN 110252289A CN 201910513116 A CN201910513116 A CN 201910513116A CN 110252289 A CN110252289 A CN 110252289A
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- Prior art keywords
- mixed liquor
- carbon black
- preparation
- carbon catalyst
- oil bath
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- 239000003054 catalyst Substances 0.000 title claims abstract description 31
- DSVGQVZAZSZEEX-UHFFFAOYSA-N [C].[Pt] Chemical compound [C].[Pt] DSVGQVZAZSZEEX-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000006229 carbon black Substances 0.000 claims abstract description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 7
- 239000012065 filter cake Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims abstract description 7
- 239000002002 slurry Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 4
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 4
- 239000012498 ultrapure water Substances 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims description 5
- 241000282320 Panthera leo Species 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims 1
- 239000007924 injection Substances 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- 238000001291 vacuum drying Methods 0.000 abstract description 3
- 239000008187 granular material Substances 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Catalysts (AREA)
Abstract
The preparation method of the invention discloses a kind of platinum carbon catalyst based on microreactor, the specially preparation technical field of platinum carbon catalyst.Preparation method: claim carbon black, add distilled water, ethylene glycol stirs to obtain carbon black slurry one；Claim chloroplatinic acid aqueous solution, claims sodium hydrate aqueous solution, the two is uniformly mixed, mixed liquor two is obtained；Both carbon black slurry one and mixed liquor two are injected separately into two isometric syringes, the two into first segment oil bath, after flowing out the last one oil bath, obtains mixed liquor three after first threeway mixes；The mixed liquor four that concentrated hydrochloric acid, ethylene glycol, ultrapure water are made into is injected into syringe and gets through second pump, and mixed liquor three is mixed by second threeway with mixed liquor four to get product mixture is arrived；Mixed liquor filtering, washing filter cake vacuum drying obtain platinum carbon catalyst.It is prepared using microreactor, preparation method is simple, and the platinum carbon catalyst granules for using this method to prepare is evenly distributed, chemical property is good.
Description
Technical field
The preparation method of the present invention relates to a kind of platinum carbon catalyst based on microreactor, the specially system of platinum carbon catalyst
Preparation Method technical field.
Background technique
Platinum carbon catalyst is a kind of carried catalyst loaded to platinum on active carbon, is belonged in noble metal catalyst most often
One kind.It can be used for the fields such as pharmacy, electronics, application is relatively broad, has biggish demand for the catalyst in the market.
In traditional still reaction, there are catalyst yields the case where small, active particle is unevenly distributed.Microreaction technology is urged for this
The increase of agent yield and the mass-and heat-transfer problem in synthetic reaction provide resolving ideas, therefore the application studies one kind
The preparation method of platinum carbon catalyst based on microreactor.
Summary of the invention
The preparation method of the purpose of the present invention is to provide a kind of platinum carbon catalyst based on microreactor, it is above-mentioned to solve
Itd is proposed in background technique the problem of.
To achieve the above object, the invention provides the following technical scheme: a kind of platinum carbon catalyst based on microreactor
Preparation method: Step 1: weighing 0.5-2.0g carbon black, distilled water 20-100g, ethylene glycol 30-150g, stirring, ultrasound point is added
It dissipates uniformly, obtains carbon black slurry one；
Step 2: weighing 50-200g mass fraction is the chloroplatinic acid aqueous solution of 0.1%-5%, and weigh mass fraction
For the sodium hydrate aqueous solution 5-20g of 0.5%-10%, the two is uniformly mixed, obtains mixed liquor two；
Step 3: both carbon black slurry one and mixed liquor two are injected separately into two isometric syringes, first
The flow velocity of pump is 1mL/min-20mL/min, and the two is after first threeway mixes, into 10-50 DEG C of first segment oil bath,
The long 3-6m of this segment pipe, the two is uniformly mixed；Then into 100-180 DEG C of oil bath of second segment, this segment pipe is long
0.5-1m, in entering 60-95 DEG C of oil bath, the long 0.5-1m of this segment pipe after flowing out the last one oil bath, obtains mixed liquor three；
Step 4: the mixed liquor four that 0.5-5mL concentrated hydrochloric acid, 50-200mL ethylene glycol, 200-1000mL ultrapure water are made into,
It is injected into syringe and is got through second pump, second flow rate pump is identical as first pump, mixed liquor three and mixed liquor four-way
Second threeway mixing is crossed to get product mixture is arrived；
Step 5: the product mixture that step 4 is obtained filters, benefit is washed with distilled water filter cake 5-10 times, filter cake is put
Enter 60-90 DEG C of vacuum drying oven dry 5-10h, is down to room temperature unlatching baking oven to temperature to get black platinum carbon catalyst is arrived.
Preferably, the carbon black is Cabot carbon black XC-72, in lion king's carbon black EC600, Czech CHEZACARB carbon black AC
One kind.
Compared with prior art, it the beneficial effects of the present invention are: being prepared during the preparation process using microreactor, makes
Preparation Method is simple, easily operated, and good using the platinum carbon catalyst activity even particle distribution of this method preparation, chemical property
It is good.
Detailed description of the invention
Fig. 1 is preparation flow figure of the present invention；
Fig. 2 is the black platinum carbon catalyst TEM figure of preparation of the embodiment of the present invention；
Fig. 3 is the cv curve graph that the embodiment of the present invention prepares black platinum carbon catalyst.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment: referring to Fig. 1, a kind of preparation method of the platinum carbon catalyst based on microreactor: Step 1: weighing
Distilled water 20-100g, ethylene glycol 30-150g is added in 0.5-2.0g carbon black, and stirring, ultrasonic disperse are uniform, obtain carbon black slurry
One；
Step 2: weighing 50-200g mass fraction is the chloroplatinic acid aqueous solution of 0.1%-5%, and weigh mass fraction
For the sodium hydrate aqueous solution 5-20g of 0.5%-10%, the two is uniformly mixed, obtains mixed liquor two；
Step 3: both carbon black slurry one and mixed liquor two are injected separately into two isometric syringes, first
The flow velocity of pump 1 is 1mL/min-20mL/min, and the two is after first threeway mixes, into 10-50 DEG C of first segment oil bath,
The long 3-6m of this segment pipe, the two is uniformly mixed；Then into 100-180 DEG C of oil bath of second segment, this segment pipe is long
0.5-1m, in entering 60-95 DEG C of oil bath, the long 0.5-1m of this segment pipe after flowing out the last one oil bath, obtains mixed liquor three；
Step 4: the mixed liquor four that 0.5-5mL concentrated hydrochloric acid, 50-200mL ethylene glycol, 200-1000mL ultrapure water are made into,
It is injected into syringe and is got through second pump 2, second 2 flow velocity of pump is identical as first pump 1, mixed liquor three and mixed liquor four
It is mixed by second threeway to get product mixture is arrived；
Step 5: the product mixture that step 4 is obtained filters, benefit is washed with distilled water filter cake 5-10 times, filter cake is put
Enter 60-90 DEG C of vacuum drying oven dry 5-10h, is down to room temperature unlatching baking oven to temperature to get black platinum carbon catalyst is arrived.It will preparation
Black platinum carbon catalyst carry out transmission electron microscope observation, Fig. 2 be black platinum carbon catalyst TEM scheme, black can be obtained by Fig. 2
Platinum carbon catalyst granules is evenly distributed；
Electro-chemical test is carried out to black platinum carbon catalyst, Fig. 3 is the cv curve graph of black platinum carbon catalyst, can by Fig. 3
The electro-chemical activity for obtaining black platinum carbon catalyst is good.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (2)
1. a kind of preparation method of the platinum carbon catalyst based on microreactor, it is characterised in that: specific preparation method: Step 1:
0.5-2.0g carbon black is weighed, distilled water 20-100g, ethylene glycol 30-150g is added, stirring, ultrasonic disperse are uniform, obtain carbon black
Material one；
Step 2: weighing 50-200g mass fraction is the chloroplatinic acid aqueous solution of 0.1%-5%, and weighs mass fraction and be
The sodium hydrate aqueous solution 5-20g of 0.5%-10%, the two is uniformly mixed, and obtains mixed liquor two；
Step 3: both carbon black slurry one and mixed liquor two are injected separately into two isometric syringes, first pump (1)
Flow velocity be 1mL/min-20mL/min, the two is after first threeway mixes, into 10-50 DEG C of first segment oil bath, this
The long 3-6m of segment pipe, the two is uniformly mixed；Then into 100-180 DEG C of oil bath of second segment, the long 0.5- of this segment pipe
1m, in entering 60-95 DEG C of oil bath, the long 0.5-1m of this segment pipe after flowing out the last one oil bath, obtains mixed liquor three；
Step 4: the mixed liquor four that 0.5-5mL concentrated hydrochloric acid, 50-200mL ethylene glycol, 200-1000mL ultrapure water are made into, injection
It is got into syringe through second pump (2), second pump (2) flow velocity is identical as first pump (1), mixed liquor three and mixed liquor
Four are mixed by second threeway to get product mixture is arrived；
Step 5: the product mixture that step 4 is obtained filters, benefit is washed with distilled water filter cake 5-10 times, filter cake is put into very
60-90 DEG C of empty baking oven dry 5-10h is down to room temperature unlatching baking oven to temperature to get black platinum carbon catalyst is arrived.
2. a kind of preparation method of platinum carbon catalyst based on microreactor according to claim 1, it is characterised in that: institute
Stating carbon black is one of Cabot carbon black XC-72, lion king's carbon black EC600, Czech CHEZACARB carbon black AC.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910513116.8A CN110252289A (en) | 2019-06-13 | 2019-06-13 | A kind of preparation method of the platinum carbon catalyst based on microreactor |
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| CN110252289A true CN110252289A (en) | 2019-09-20 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113555567A (en) * | 2021-07-22 | 2021-10-26 | 无锡威孚高科技集团股份有限公司 | Platinum-carbon catalyst and preparation method thereof |
Citations (5)
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|---|---|---|---|---|
| CN102107137A (en) * | 2009-12-28 | 2011-06-29 | 中国科学院大连化学物理研究所 | Preparation method of platinum-palladium bimetallic catalyst |
| CN103730668A (en) * | 2013-12-21 | 2014-04-16 | 南京大学昆山创新研究院 | Pt/C catalyst of fuel cell and preparation technology thereof |
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| BRPI1106528A2 (en) * | 2011-08-05 | 2016-09-06 | Comissão Nac De En Nuclear | platinum and bismuth electrocatalysts for application to alkaline fuel cells using ethanol directly as fuel |
| CN108855055A (en) * | 2018-05-31 | 2018-11-23 | 南京东焱氢能源科技有限公司 | A kind of preparation method of the high activity hydroxide palladium carbon based on microreactor |
-
2019
- 2019-06-13 CN CN201910513116.8A patent/CN110252289A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102107137A (en) * | 2009-12-28 | 2011-06-29 | 中国科学院大连化学物理研究所 | Preparation method of platinum-palladium bimetallic catalyst |
| BRPI1106528A2 (en) * | 2011-08-05 | 2016-09-06 | Comissão Nac De En Nuclear | platinum and bismuth electrocatalysts for application to alkaline fuel cells using ethanol directly as fuel |
| CN103730668A (en) * | 2013-12-21 | 2014-04-16 | 南京大学昆山创新研究院 | Pt/C catalyst of fuel cell and preparation technology thereof |
| CN105789641A (en) * | 2014-12-24 | 2016-07-20 | 上海汽车集团股份有限公司 | Fuel cell, platinum-carbon catalyst and preparation method of platinum-carbon catalyst |
| CN108855055A (en) * | 2018-05-31 | 2018-11-23 | 南京东焱氢能源科技有限公司 | A kind of preparation method of the high activity hydroxide palladium carbon based on microreactor |
Non-Patent Citations (1)
| Title |
|---|
| 周振华: ""直接甲醇燃料电池:高分散高负载铂基电催化剂的制备规律研究"", 《中国优秀博硕士学位论文全文数据库(博士) 工程科技Ⅱ辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113555567A (en) * | 2021-07-22 | 2021-10-26 | 无锡威孚高科技集团股份有限公司 | Platinum-carbon catalyst and preparation method thereof |
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Application publication date: 20190920 |