CN1282624A - Process for preparing CO oxidant - Google Patents
Process for preparing CO oxidant Download PDFInfo
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- CN1282624A CN1282624A CN99115512A CN99115512A CN1282624A CN 1282624 A CN1282624 A CN 1282624A CN 99115512 A CN99115512 A CN 99115512A CN 99115512 A CN99115512 A CN 99115512A CN 1282624 A CN1282624 A CN 1282624A
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- oxidant
- solution
- sulfuric acid
- palladium
- carbon monoxide
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- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
A process for preparing CO oxidant for fully and rapidly oxidizing the CO in gas to CO2 at normal temp. and pressure uses palladium ammonium salfate as main active component. It can also be used to analyze trace quantity of CO. When the content of CO is less than 1%, its oxidation efficiency can reach 99%. Said oxidant can be regenerated repeatedly.
Description
The invention relates to a preparation method of a carbon monoxide oxidant.
The carbon monoxide oxidant can be applied to the removal of carbon monoxide in the field of gas purification in the chemical industry and the analysis and test of trace carbon monoxide and carbon dioxide in the field of chemical analysis.
The existing methods for removing carbon monoxide in the field of gas purification at home and abroad can be roughly divided into two categories: one is copper salt series adsorbent, such as CuCl-Al2O3CuCl-activated carbon, Cu-molecular sieve, etc., and the adsorbent mainly uses Cu+Can generate a coordination bond compound with CO to achieve the purpose of adsorption; the other is noble metal catalyst, which is a series of products comprising metals such as platinum, palladium, gold and the like and various carriers, and the catalyst can oxidize carbon monoxide into carbon dioxide in oxygen environment or achieve the purpose of adsorbing and removing carbon monoxide by means of pressure swing adsorption and the like.
The invention aims to provide a preparation method of a carbon monoxide oxidant.
The invention is realized by the following steps: dissolving a certain amount of palladium or palladium salt (palladium chloride, palladium nitrate and palladium sulfate) in a certain amount of sulfuric acid solution, and removing Cl possibly existing in the solution at high temperature-、NO3 -Completely converting palladium into palladium sulfate, diluting the sulfuric acid-palladium sulfate solution into a certain amount of water, and immersing a certain amount of diatomite carriers into the liquid to enable the carriers to fully adsorb the solution. Transferring the carrier soaked with palladium sulfate solution to an acid-resistant container with air holes at both ends, and introducing nitrogen (N) at one end2More than 99.99 percent) is put in a temperature-controllable heater, and the temperature is slowly raised to 150 ℃ and 160 DEG CTaking for about 2-3 hours. The effective proportion range of the oxidant is (W/W):
palladium, sulfuric acid, carrier = (0.2-10): (10-50): (90-50)
The optimal proportion of the oxidant is (w/w)
Pd/sulfuric acid/carrier = (1-5) to 40: 60
The preparation method comprises the following specific steps:
first, 1 to 5 parts of palladium are dissolved in a certain amount of hydrochloric acid (1: 1) and heated slightly until all palladium is dissolved and cooled (hereinafter referred to as solution ①) (note: the amount of palladium depends on carbon monoxide in the gas, and generally, when the carbon monoxide content is about 100PPm, 1 part of palladium is contained, and when the carbon monoxide content is 1%, 5 parts of palladium is contained).
Secondly, 40 parts of concentrated sulfuric acid (H)2SO498%) was slowly added to solution ① and the water and HCl were slowly removed by heating in a furnace until the solution was white-smoking with sulfur trioxide (designated solution ②)
And thirdly, diluting the solution ② into 120 parts of water (called solution ③) (the water consumption is determined according to the water absorption capacity of the carrier and is generally twice of the carrier).
And fourthly, 60 parts of red diatomite carrier is soaked into the solution ③, and the solution ③ is required to be in an amount which ensures that the carrier completely adsorbs the solution but does not have excessive solution.
Fifthly, mixingTransferring the obtained material to a container with acid resistance and gas holes at both ends, placing the container in a temperature-controllable heating furnace, and introducing nitrogen (N) into the steel cylinder from one end2Not less than 99.99%), the flow rate is 0.5L/min, the temperature is slowly raised to 150 ℃ and 160 ℃, the temperature is kept for about 2 hours until the outlet gas is observed by using a cold mirror surface and the mirror surface has no obvious condensed water vapor, and the heating is stopped.
And sixthly, after the drying is finished, stopping introducing thenitrogen, and enabling the oxidant to be normally used.
The principle of the oxidation of the oxidant is that when carbon monoxide gas flows through the palladium sulfate oxidant, CO can react with Pd in the presence of a trace amount of water2+Reaction to CO2。
The water required for the reaction is provided by the water adsorbed by the excess sulfuric acid in the oxidant, and the reaction equation is as follows:
the reaction can be quantitatively completed at normal temperature and normal pressure.
When the oxidant is used, for example, CO in the gas and its oxidation product CO are mixed2All the components are eliminated by mixing the oxidant with CO2All the components are eliminated by mixing the oxidant with CO2The absorbent is used in series to oxidize CO into CO2Then introducing CO2Removal, e.g. by conversion of CO only to CO2Only the present oxidizing agent is used.
The reaction of oxidizing CO by the oxidant is an equimolar reaction, and after a certain amount of CO is oxidized, the oxidizing effect is gradually reduced until the CO is ineffective. Therefore, after a period of use, the oxidant must be regenerated.
The invention has the positive effects that the oxidant takes palladium sulfate as a main active component and can directly oxidize CO into CO2The oxidation reaction is carried out at normal temperature and normal pressure, the oxidation speed is high, and the reaction is completed instantly. The oxidant has wide application range, high oxidation efficiency and complete reaction. Can be suitable for purifying common gases such as nitrogen, argon, helium, oxygen, carbon dioxide and the like or analyzing and testing CO in the gas, and when the content of carbon monoxide in the gas is less than 1 percent, the oxidation efficiency can be up to 99 percentThe oxidant can be regenerated repeatedly, and the regeneration method is simple and convenient.
Example 1: this example is the preparation of an oxidant, the heating device is an SCL-01 gas chromatography column aging box, and the gas source is steel cylinder nitrogen (N)2More than 99.99%) oxidant container is cylindrical stainless steel tube whose diameter is 8 mm and length is 300 mm, according to the ratio of palladium, sulfuric acid and carrierVolume = 3: 40: 60 ratio 50 grams of oxidant was prepared.
According to the preparation steps, 1.5 g of metal palladium is weighed and dissolved in 10ml of 1: 1HCl solution, after the solution is heated slightly until the metal palladium is completely dissolved, 20 g (about 11ml) of sulfuric acid (98%) is added dropwise and slowly heated on an electric furnace to volatilize all water and HCl until the solvent just emits SO3Stopping heating after white smoke, cooling, dissolving in 60ml water, soaking 30 g 6201 red chromatographic monomer in the water, filling the monomer soaked with palladium sulfate into stainless steel tube, filling small amount of quartz wool at two ends, loading into heating furnace, introducing N2About 500 ml/min, heating to 110-120 ℃ for 30min, and then heating to 150-160 ℃ for about 2 hours.
Example 2, the purpose of this example was to test the oxidizing effect of an oxidizing agent on carbon monoxide in nitrogen.
The testing instrument is a gas chromatograph with a methanation furnace and a hydrogen flame detector, and the sample gas is a steel cylinder standard gas, wherein
CO=0．313％，CO2= 0.412%, bottom gas: n is a radical of2
The chromatographic condition is as follows:
a host computer: GC-15A gas chromatograph with a methanation furnace and a six-way valve.
A detector: hydrogen flame ionization detector
A chromatographic column: porpayk Q L =3m
Column temperature: detector temperature at 60 ℃: 180 deg.C
The temperature of the conversion furnace: 375 ℃ sample introduction: 1ml of
The method comprises the following operation steps: the standard gas is filled with a pressure reducing valve to test CO and CO in the standard gas2After the content is detected, connecting an oxidant pipe to an outlet of the pressure reducing valve, adjusting the flow of the standard gas to about 100 ml/min, and then testing CO and CO in the outlet gas2The content of (a).
And (3) testing results:
before Oxidation (%) after Oxidation (%)
CO 0．313 0．001
CO20．412 0．724
The oxidation rate of CO is more than 99 percent
Note: after the continuous use of the oxidizing agent for 3 hours, the oxidation rate will gradually decrease as per the above procedure.
Claims (3)
1. A process for preparing CO oxidant includes dissolving Pd or Pd salt in sulfuric acid solution, heating to convert the Pd salt to Pd sulfate, diluting in water, immersing diatomite in the solution, transferring the carrier immersed in Pd sulfate solution to a container with acid resistance and air holes at both ends, and introducing nitrogen gas at one end of said container and drying at 160 deg.C for 2 hr. The effective proportion range of the oxidant is as follows:
palladium, sulfuric acid, carrier = (0.2-10): (10-50): (90-50)
2. The method for preparing a carbon monoxide oxidizing agent according to claim 1, wherein the optimal ratio of the oxidizing agent is as follows:
pd/sulfuric acid/carrier = (1-5) to 40: 60
3. A process for the preparation of a carbon monoxide catalyst as claimed in claim 1. It is characterized in that the water required for the oxidation reaction is provided by water adsorbed by excess sulfuric acid in the oxidizing agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99115512A CN1100593C (en) | 1999-07-30 | 1999-07-30 | Process for preparing CO oxidant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99115512A CN1100593C (en) | 1999-07-30 | 1999-07-30 | Process for preparing CO oxidant |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1282624A true CN1282624A (en) | 2001-02-07 |
| CN1100593C CN1100593C (en) | 2003-02-05 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99115512A Expired - Fee Related CN1100593C (en) | 1999-07-30 | 1999-07-30 | Process for preparing CO oxidant |
Country Status (1)
| Country | Link |
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| CN (1) | CN1100593C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108333284A (en) * | 2018-02-08 | 2018-07-27 | 北京雪迪龙科技股份有限公司 | The method and its system of carbon compound are detected based on catalytic conversion technique |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5926337B2 (en) * | 1980-10-07 | 1984-06-26 | 日本たばこ産業株式会社 | carbon monoxide remover |
| SU1027880A1 (en) * | 1981-07-23 | 1985-08-30 | Ордена Трудового Красного Знамени Институт Катализа Со Ан Ссср | Homogeneous catalyst for oxidizing carbon monoxide |
| US4482635A (en) * | 1982-03-29 | 1984-11-13 | E. I. Du Pont De Nemours & Company | Composition, indicator, process and device for detecting carbon monoxide |
| CN2124473U (en) * | 1992-06-05 | 1992-12-09 | 机械电子工业部第二十三研究所 | Optical fibre type co detecting and alarm device |
-
1999
- 1999-07-30 CN CN99115512A patent/CN1100593C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108333284A (en) * | 2018-02-08 | 2018-07-27 | 北京雪迪龙科技股份有限公司 | The method and its system of carbon compound are detected based on catalytic conversion technique |
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| Publication number | Publication date |
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| CN1100593C (en) | 2003-02-05 |
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