JPH0417092B2 - - Google Patents
Info
- Publication number
- JPH0417092B2 JPH0417092B2 JP61118898A JP11889886A JPH0417092B2 JP H0417092 B2 JPH0417092 B2 JP H0417092B2 JP 61118898 A JP61118898 A JP 61118898A JP 11889886 A JP11889886 A JP 11889886A JP H0417092 B2 JPH0417092 B2 JP H0417092B2
- Authority
- JP
- Japan
- Prior art keywords
- cadmium sulfide
- platinum
- sulfide
- hydrogen
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 claims description 22
- 229910052980 cadmium sulfide Inorganic materials 0.000 claims description 22
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 7
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 7
- 239000011941 photocatalyst Substances 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- 229910052763 palladium Inorganic materials 0.000 claims description 4
- 229910000272 alkali metal oxide Inorganic materials 0.000 claims description 3
- 150000001340 alkali metals Chemical class 0.000 claims description 3
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 239000002253 acid Substances 0.000 description 6
- 150000004696 coordination complex Chemical class 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 5
- 239000012300 argon atmosphere Substances 0.000 description 5
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- ABKQFSYGIHQQLS-UHFFFAOYSA-J sodium tetrachloropalladate Chemical compound [Na+].[Na+].Cl[Pd+2](Cl)(Cl)Cl ABKQFSYGIHQQLS-UHFFFAOYSA-J 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- KGYLMXMMQNTWEM-UHFFFAOYSA-J tetrachloropalladium Chemical compound Cl[Pd](Cl)(Cl)Cl KGYLMXMMQNTWEM-UHFFFAOYSA-J 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Landscapes
- Catalysts (AREA)
Description
【発明の詳細な説明】
〔技術分野〕
本発明は、光エネルギーを用いて硫化水素を分
解して水素を発生させる際に用いられる光触媒の
製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Technical Field] The present invention relates to a method for producing a photocatalyst used in decomposing hydrogen sulfide to generate hydrogen using light energy.
太陽エネルギーを化学エネルギーに変換する方
法として、硫化水素を光エネルギーにより分解し
て水素を得るプロセスが知られている。このプロ
セスで得られた水素は重油の水素化脱硫過程にあ
るいは化学原料として用いることができるため、
極めて有用である。
As a method of converting solar energy into chemical energy, a process of decomposing hydrogen sulfide using light energy to obtain hydrogen is known. The hydrogen obtained through this process can be used in the hydrodesulfurization process of heavy oil or as a chemical raw material.
Extremely useful.
光エネルギーを用いて硫化水素を分解する場
合、次に示す反応式に従つて、硫化水素をいつた
ん水酸化ナトリウム水溶液に吸収させた後、生成
する硫化ナトリウム水溶液に白金担持硫化カドミ
ウム粉末光触媒を分散させ、光を照射することに
より水素を発生させるという方法が既に知られて
いる。 When decomposing hydrogen sulfide using light energy, hydrogen sulfide is absorbed into a sodium hydroxide aqueous solution according to the reaction formula shown below, and then a platinum-supported cadmium sulfide powder photocatalyst is dispersed in the resulting sodium sulfide aqueous solution. A method of generating hydrogen by irradiating light is already known.
水酸化ナトリウム水溶液＋硫化水素→
硫化ナトリウム水溶液光
―――→
光触媒
水素＋イオウ＋水酸化ナトリウム水溶液
従来、光触媒となる白金担持硫化カドミウムの
製造法としては、ヘキサクロロ白金（）酸等の
酸性の白金錯体を硫化カドミウムに浸漬担持する
方法が知られているが、硫化カドミウムは酸性条
件下で化学的に不安定であるため、酸性の白金錯
体を担持することによつて、あるいは錯体担持後
の加熱処理で発生する塩化水素等によつて硫化カ
ドミウム自身が分解するという問題があつた。 Sodium hydroxide aqueous solution + hydrogen sulfide → Sodium sulfide aqueous solution light --- → Photocatalytic hydrogen + sulfur + sodium hydroxide aqueous solution Conventionally, as a method for producing platinum-supported cadmium sulfide, which serves as a photocatalyst, acidic platinum such as hexachloroplatinic () acid is used. A method of supporting the complex by immersion in cadmium sulfide is known, but since cadmium sulfide is chemically unstable under acidic conditions, it is possible to support the complex by supporting an acidic platinum complex or by heating after supporting the complex. There was a problem in that cadmium sulfide itself was decomposed by hydrogen chloride etc. generated during processing.
本発明は、従来技術に見られる前記問題を解決
することを目的とする。
The present invention aims to solve the aforementioned problems found in the prior art.
本発明によれば、硫化ナトリウム水溶液からの
水素発生用粉末光触媒の製造において、白金又は
パラジウム錯体の水溶液に硫化カドミウム粉末と
アルカリ金属又はアルカリ土類金属の水酸化物を
加えて、アルカリ性とし、全体を蒸発乾固した
後、不活性ガス中で加熱することを特徴とする白
金又はパラジウム担持硫化カドミウム粉末の製造
方法が提供される。
According to the present invention, in the production of a powder photocatalyst for hydrogen generation from an aqueous sodium sulfide solution, cadmium sulfide powder and an alkali metal or alkaline earth metal hydroxide are added to an aqueous solution of a platinum or palladium complex to make the entire solution alkaline. Provided is a method for producing platinum- or palladium-supported cadmium sulfide powder, which comprises evaporating to dryness and then heating in an inert gas.
本発明の粉末光触媒の製造においては、先ず、
白金又はパラジウム錯体の水溶液に硫化カドミウ
ム粉末を加える。この場合、金属錯体としては、
テトラクロロ白金（）酸、ヘキサクロロ白金
（）酸、テトラクロロパラジウム（）酸、ヘ
キサクロロパラジウム（）酸又はそれらの塩等
を用いることができる。硫化カドミウム粉末は微
細なものほど好ましく、特に5μｍ以下の粒径を
有するものが好ましい。金属錯体の使用量は、硫
化カドミウム１モルに対し、0.0001〜0.05モル、
好ましくは0.001〜0.02モルである。 In the production of the powder photocatalyst of the present invention, first,
Add cadmium sulfide powder to an aqueous solution of platinum or palladium complex. In this case, the metal complex is
Tetrachloroplatinic () acid, hexachloroplatinic () acid, tetrachloropalladium () acid, hexachloropalladium () acid, or salts thereof, etc. can be used. The finer the cadmium sulfide powder, the more preferable it is, and it is particularly preferable that the cadmium sulfide powder has a particle size of 5 μm or less. The amount of metal complex used is 0.0001 to 0.05 mol per 1 mol of cadmium sulfide.
Preferably it is 0.001 to 0.02 mol.
次に、カドミウム粉末を加えた金属錯体水溶液
に対して、アルカリ金属又はアルカリ土類金属の
水酸化物を加えてアルカリ性とする。この水酸化
物は、金属錯体１モルあたり、0.1〜500モル、好
ましくは５〜50モルである。 Next, an alkali metal or alkaline earth metal hydroxide is added to the aqueous metal complex solution containing cadmium powder to make it alkaline. The amount of this hydroxide is 0.1 to 500 mol, preferably 5 to 50 mol, per mol of metal complex.
次に、このようにして得られた硫化カドミウ
ム、金属錯体、水酸化物、水の混合物をよく撹拌
しながら蒸発乾固し、乳バチにより粉砕する。こ
れを石英ボートにとり、電気炉が挿入した石英管
中に置いて不活性ガス雰囲気中で0.1〜10時間加
熱する。この時の加熱温度は100℃〜700℃、好ま
しくは150℃〜400℃である。この加熱操作により
硫化カドミニウムに担持した金属錯体は分解還元
され、白金又はパラジウムの担持された硫化カド
ミウムが得られる。これらのものは、硫化ナトリ
ウム水溶液からの光照射下での水素発生に高い活
性を示す。 Next, the mixture of cadmium sulfide, metal complex, hydroxide, and water thus obtained is evaporated to dryness with thorough stirring and pulverized with a mortar. This is placed in a quartz boat, placed in a quartz tube inserted into an electric furnace, and heated for 0.1 to 10 hours in an inert gas atmosphere. The heating temperature at this time is 100°C to 700°C, preferably 150°C to 400°C. Through this heating operation, the metal complex supported on cadmium sulfide is decomposed and reduced, and cadmium sulfide on which platinum or palladium is supported is obtained. These materials exhibit high activity in hydrogen generation from an aqueous sodium sulfide solution under light irradiation.
次に本発明を実施例によりさらに詳細に説明す
る。
Next, the present invention will be explained in more detail with reference to Examples.
実施例 １
ヘキサクロロ白金（）酸（１×10-4モル）を
20mlの水に溶かし、硫化カドミウム（１×10-2モ
ル）を加え、さらに直ちに水酸化ナトリウムを水
溶液として加えてPHを調節する。全体を蒸発乾固
し、アルゴン雰囲気中において350℃で３時間加
熱し、その後冷却する。Example 1 Hexachloroplatinic acid (1×10 -4 mol)
Dissolve in 20 ml of water, add cadmium sulfide (1 x 10 -2 mol), and immediately add sodium hydroxide as an aqueous solution to adjust the pH. The whole is evaporated to dryness and heated at 350° C. for 3 hours in an argon atmosphere, then cooled.
次にこうして得られた白金担持硫化カドミウム
10mgを30mlの内容積を持ち、ゴム製ガス採取口を
備えたパイレツクスガラス製容器に入れ、さらに
硫化ナトリウム水溶液（0.1モル／×15ml）を
加え、アルゴンガスで空気を追い出した後、
500wキセノンランプを照射する。こうして得ら
れた水素生成速度を白金錯体担持の際とPHとの関
連で示すと、31μ／ｈ（PH6.4）、79μ／ｈ（PH
11.0）、452μ／ｈ（PH12.5）、1312μ／ｈ（PH
13.0）、574μ／ｈ（PH13.5）であり、PH13.0に調
節した場合に生成した白金担持硫化カドミウムの
活性が最も高いことがわかつた。また420nｍカ
ツトオフフイルターを用いて420nｍより短かい
波長の光をカツトした場合、水素生成速度はフイ
ルターなしの場合の約54％となつた。 Next, the platinum-supported cadmium sulfide obtained in this way
10 mg was placed in a Pyrex glass container with an internal volume of 30 ml and equipped with a rubber gas sampling port, an aqueous sodium sulfide solution (0.1 mol/x 15 ml) was added, and the air was expelled with argon gas.
Irradiate with a 500w xenon lamp. The hydrogen production rates obtained in this way are 31 μ/h (PH6.4), 79 μ/h (PH
11.0), 452μ/h (PH12.5), 1312μ/h (PH
13.0), 574μ/h (PH13.5), and it was found that the platinum-supported cadmium sulfide produced when the pH was adjusted to 13.0 had the highest activity. Furthermore, when a 420 nm cut-off filter was used to cut out light with wavelengths shorter than 420 nm, the hydrogen production rate was approximately 54% of that without a filter.
実施例 ２
実施例１において、PH13.0に調節後全体を蒸発
乾固して得た生成物を、アルゴン雰囲気下におい
て一定温度で３時間加熱し、その後冷却する。こ
うして得られた白金担持硫化カドミウム10mgをと
り、実施例１で述べたのと同様の反応条件を用い
て光照射する。こうして得られた水素生成速度を
アルゴン雰囲気下の加熱温度との関連で示すと、
17μ／ｈ（加熱無し）、297μ／ｈ（250℃）、
1312μ／ｈ（350℃）、750μ／ｈ（500℃）であ
り、アルゴン雰囲気下で350℃に加熱した白金担
持硫化カドミウムの活性が最も高いことがわかつ
た。Example 2 The product obtained in Example 1 by evaporating the entire product to dryness after adjusting the pH to 13.0 is heated at a constant temperature under an argon atmosphere for 3 hours, and then cooled. 10 mg of platinum-supported cadmium sulfide thus obtained is taken and irradiated with light using the same reaction conditions as described in Example 1. The hydrogen production rate obtained in this way is shown in relation to the heating temperature under an argon atmosphere.
17μ/h (no heating), 297μ/h (250℃),
The activity was 1312 μ/h (350° C.) and 750 μ/h (500° C.), and it was found that platinum-supported cadmium sulfide heated to 350° C. in an argon atmosphere had the highest activity.
実施例 ３
テトラクロロパラジウム（）酸ナトリウム
（１×10-2モル）を加え、さらに直ちに水酸化ナ
トリウム水溶液を加えてPH13.0とする。全体を蒸
発乾固し、アルゴン雰囲気中において350℃で３
時間加熱し、その後冷却する。こうして得られた
パラジウム担持硫化カドミウムを実施例１と同様
の条件で硫化ナトリウム水溶液からの水素発生実
験に供したところ、1200μ／ｈの水素生成速度
が得られた。Example 3 Sodium tetrachloropalladate (1 x 10 -2 mol) is added, and then immediately an aqueous sodium hydroxide solution is added to adjust the pH to 13.0. The whole was evaporated to dryness and heated to 350°C in an argon atmosphere for 3 hours.
Heat for an hour and then cool. When the palladium-supported cadmium sulfide thus obtained was subjected to a hydrogen generation experiment from an aqueous sodium sulfide solution under the same conditions as in Example 1, a hydrogen generation rate of 1200 μ/h was obtained.
Claims (1)
光触媒の製造において、白金又はパラジウム錯体
の水溶液に硫化カドミウム粉末とアルカリ金属又
はアルカリ土類金属の水酸化物を加えてアルカリ
性とし、全体を蒸発乾固した後、不活性ガス中で
加熱することを特徴とする白金又はパラジウム担
持硫化カドミウム粉末の製造方法。1. In the production of a powder photocatalyst for hydrogen generation from an aqueous sodium sulfide solution, cadmium sulfide powder and an alkali metal or alkaline earth metal hydroxide are added to an aqueous solution of platinum or palladium complex to make it alkaline, and the whole is evaporated to dryness. A method for producing platinum- or palladium-supported cadmium sulfide powder, which comprises heating in an inert gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61118898A JPS62277151A (en) | 1986-05-23 | 1986-05-23 | Production of hydrogen generating powdery photocatalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61118898A JPS62277151A (en) | 1986-05-23 | 1986-05-23 | Production of hydrogen generating powdery photocatalyst |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62277151A JPS62277151A (en) | 1987-12-02 |
| JPH0417092B2 true JPH0417092B2 (en) | 1992-03-25 |
Family
ID=14747895
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61118898A Granted JPS62277151A (en) | 1986-05-23 | 1986-05-23 | Production of hydrogen generating powdery photocatalyst |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62277151A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100301281B1 (en) * | 1999-06-18 | 2001-09-13 | 김충섭 | The Manufacturing Method of CdS Photocatalyst for Hydrogen Production and Method for Producing Hydrogen by use of the same |
| KR20040021074A (en) * | 2002-09-02 | 2004-03-10 | 한국화학연구원 | MxM'yS Photocatalyst for Hydrogen Production and Preparation Thereof and Method for Producing Hydrogen Use of the Same |
| KR100486388B1 (en) * | 2002-09-02 | 2005-04-29 | 한국화학연구원 | MyM'zS Photocatalys Supported by Semiconductor Particle and Preparation Thereof and Method Producing Hydrogen by Use of the Same |
-
1986
- 1986-05-23 JP JP61118898A patent/JPS62277151A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62277151A (en) | 1987-12-02 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |