CN103808557A - Microwave digestion liquid and microwave digestion method for nickel-phosphorus catalyst - Google Patents
Microwave digestion liquid and microwave digestion method for nickel-phosphorus catalyst Download PDFInfo
- Publication number
- CN103808557A CN103808557A CN201410052795.0A CN201410052795A CN103808557A CN 103808557 A CN103808557 A CN 103808557A CN 201410052795 A CN201410052795 A CN 201410052795A CN 103808557 A CN103808557 A CN 103808557A
- Authority
- CN
- China
- Prior art keywords
- microwave digestion
- phosphorus catalyst
- micro
- nickel
- microwave
- 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.)
- Pending
Links
Abstract
The invention discloses a microwave digestion liquid and a microwave digestion method for a nickel-phosphorus catalyst. The microwave digestion liquid consists of the components in percentage by mass: 10-20 percent of H2SO4, 50-60 percent of H3PO4 and 25-35 percent of H2O. The microwave digestion method comprises the steps of adding the nickel-phosphorus catalyst into a microwave digestion tank and adding the microwave digestion liquid, wherein a ratio of the microwave digestion liquid to the nickel-phosphorus catalyst is 10mL: (0.1-0.3g); putting the microwave digestion tank into a microwave oven for microwave heating for 10-30min, taking out the microwave digestion tank, cooling the microwave digestion tank to room temperature, and fixing the volume. Due to a reasonable mixed acid constitution and a reasonable ratio of the microwave digestion liquid developed by the nickel-phosphorus catalyst, the aim of quickly digesting the nickel-phosphorus catalyst is fulfilled; furthermore, the nickel-phosphorus catalyst can be digested completely; the digestion time is short, and the using amount of a solvent is small; a subsequent sample injection requirement on an analysis instrument can be met, and detection can be executed; timely and accurate analysis data can be supplied to adiponitrile production.
Description
Technical field
The present invention relates to the production technical field of adiponitrile, relate to a kind of micro-wave digestion liquid and micro-wave digestion method of nickel phosphorus catalyst.
Background technology
Adiponitrile molecular formula is CN(CH
2)
4cN, English is abbreviated as ADN, is one of main raw material of producing new material nylon 66, and its proterties is colourless oil liquid, is slightly with sweet taste, toxic and corrosivity, density is 962g/cm
2, 1 ℃ of fusing point, 295 ℃ of boiling points (1atm).In addition, it also has wide application in electronics, light industry and other organic synthesis field.
Butadiene process Adiponitrile mainly divides hydrocyanation, isomerization, three steps of secondary hydrocyanation, and the reaction equation of these three steps is as follows:
Visible, nickel phosphorus catalyst participates in the three-step reaction of butadiene process Adiponitrile as homogeneous system, and nickel phosphorus catalyst plays key effect in butadiene process Adiponitrile process.Therefore, rapid and accurate determination nickel phosphorus catalyst content is even more important.
Traditional nickeliferous sample pretreating method has dry method, wet method.Dry method is first sample to be dried, more then calcination adds acid by its dissolving carbon removal in several hours in muffle furnace; Wet method is that acid adding is placed several hours.There is the defects such as consuming time, solvent load is large in above two kinds of methods.Most of molten sample pre-service Microwave Digestion now, compares that the first two method used time is short, solvent load is few.But it is bad that conventional Microwave Digestion and micro-wave digestion liquid are cleared up effect for this kind of nickel phosphorus catalyst, exist clear up not exclusively, by shortcomings such as durations.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of micro-wave digestion liquid and micro-wave digestion method of nickel phosphorus catalyst, clear up completely, the used time is few, solvent load is few, clears up the solution of rear formation clarification, can meet the sample introduction requirement of subsequent analysis instrument and complete detection.
For achieving the above object, the invention provides following technical scheme:
The micro-wave digestion liquid that the invention discloses a kind of nickel phosphorus catalyst, the component of described micro-wave digestion liquid and mass percent are: H
2sO
410% ~ 20%, H
3pO
450% ~ 60%, H
2o 25% ~ 35%.
Further, the component of described micro-wave digestion liquid and mass percent are: H
2sO
415%, H
3pO
456%, H
2o29%.
The invention also discloses a kind of method that uses described micro-wave digestion liquid nickel phosphorus catalyst to be carried out to micro-wave digestion, nickel phosphorus catalyst is added in micro-wave diminishing pot, then add described micro-wave digestion liquid, the proportioning of described micro-wave digestion liquid and nickel phosphorus catalyst is 10mL:0.1 ~ 0.3g, again micro-wave diminishing pot is put into after micro-wave oven microwave heating 10 ~ 30min, take out, be cooled to constant volume after room temperature.
Beneficial effect of the present invention is:
The micro-wave digestion liquid that the present invention is directed to the exploitation of nickel phosphorus catalyst consists of and proportioning rational nitration mixture, reach the object of rapid-digestion nickel phosphorus catalyst, and clear up completely, used time is few, solvent load is few, the solution of clearing up rear formation clarification, can meet the sample introduction requirement of subsequent analysis instrument and complete detection, produces and provides in time, analyzed accurately data for adiponitrile.
Embodiment
In order to make object of the present invention, technical scheme and beneficial effect clearer, will be described in detail the preferred embodiments of the present invention below.
embodiment 1
Component and the mass percent of the micro-wave digestion liquid of the present embodiment are: H
2sO
410%, H
3pO
460%, H
2o 30%.
Taking 0.2 g(and be accurate to 0.0001g) nickel phosphorus catalyst adds in micro-wave diminishing pot, then adds micro-wave digestion liquid described in 10mL, then micro-wave diminishing pot is put into after micro-wave oven microwave heating 20min, takes out, and is cooled to constant volume after room temperature, surveys its content.
embodiment 2
Component and the mass percent of the micro-wave digestion liquid of the present embodiment are: H
2sO
415%, H
3pO
456%, H
2o 29%.
Taking 0.2 g(and be accurate to 0.0001g) nickel phosphorus catalyst adds in micro-wave diminishing pot, then adds micro-wave digestion liquid described in 10mL, then micro-wave diminishing pot is put into after micro-wave oven microwave heating 20min, takes out, and is cooled to constant volume after room temperature, surveys its content.
embodiment 3
Component and the mass percent of the micro-wave digestion liquid of the present embodiment are: H
2sO
420%, H
3pO
450%, H
2o 30%.
Taking 0.2 g(and be accurate to 0.0001g) nickel phosphorus catalyst adds in micro-wave diminishing pot, then adds micro-wave digestion liquid described in 10mL, then micro-wave diminishing pot is put into after micro-wave oven microwave heating 10min, takes out, and is cooled to constant volume after room temperature, surveys its content.
Finally explanation is, above preferred embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is described in detail by above preferred embodiment, but those skilled in the art are to be understood that, can make various changes to it in the form and details, and not depart from the claims in the present invention book limited range.
Claims (3)
1. a micro-wave digestion liquid for nickel phosphorus catalyst, is characterized in that: the component of described micro-wave digestion liquid and mass percent are: H
2sO
410% ~ 20%, H
3pO
450% ~ 60%, H
2o 25% ~ 35%.
2. the micro-wave digestion liquid of nickel phosphorus catalyst according to claim 1, is characterized in that: the component of described micro-wave digestion liquid and mass percent are: H
2sO
415%, H
3pO
456%, H
2o29%.
3. right to use requires micro-wave digestion liquid described in 1 or 2 nickel phosphorus catalyst to be carried out to the method for micro-wave digestion, it is characterized in that: nickel phosphorus catalyst is added in micro-wave diminishing pot, then add described micro-wave digestion liquid, the proportioning of described micro-wave digestion liquid and nickel phosphorus catalyst is 10mL:0.1 ~ 0.3g, again micro-wave diminishing pot is put into after micro-wave oven microwave heating 10 ~ 30min, take out, be cooled to constant volume after room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410052795.0A CN103808557A (en) | 2014-02-17 | 2014-02-17 | Microwave digestion liquid and microwave digestion method for nickel-phosphorus catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410052795.0A CN103808557A (en) | 2014-02-17 | 2014-02-17 | Microwave digestion liquid and microwave digestion method for nickel-phosphorus catalyst |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103808557A true CN103808557A (en) | 2014-05-21 |
Family
ID=50705648
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410052795.0A Pending CN103808557A (en) | 2014-02-17 | 2014-02-17 | Microwave digestion liquid and microwave digestion method for nickel-phosphorus catalyst |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103808557A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1998020341A1 (en) * | 1996-11-08 | 1998-05-14 | Mountain States Analytical, Inc. | Sample preparation for metals analysis using accelerated acid digestion (aad) |
| CN101815579A (en) * | 2007-08-13 | 2010-08-25 | 旭化成化学株式会社 | Catalyst for carboxylic acid ester production, method for producing the same, and method for producing carboxylic acid ester |
| CN102213657A (en) * | 2011-03-30 | 2011-10-12 | 攀钢集团有限公司 | Digestion method and detection method of Tungsten-base class sample |
| CN102590181A (en) * | 2012-02-29 | 2012-07-18 | 成都中光电科技有限公司 | Method for detecting impurity components in alpha-alumina |
| CN102854238A (en) * | 2012-08-10 | 2013-01-02 | 同济大学 | Method for determination analysis of multiple heavy metals in environmental medium or biological sample |
-
2014
- 2014-02-17 CN CN201410052795.0A patent/CN103808557A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1998020341A1 (en) * | 1996-11-08 | 1998-05-14 | Mountain States Analytical, Inc. | Sample preparation for metals analysis using accelerated acid digestion (aad) |
| CN101815579A (en) * | 2007-08-13 | 2010-08-25 | 旭化成化学株式会社 | Catalyst for carboxylic acid ester production, method for producing the same, and method for producing carboxylic acid ester |
| US20110184206A1 (en) * | 2007-08-13 | 2011-07-28 | Ken Suzuki | Catalyst for producing carboxylic acid esters, process for producing same and process for producing carboxylic acid esters (as amended) |
| CN102213657A (en) * | 2011-03-30 | 2011-10-12 | 攀钢集团有限公司 | Digestion method and detection method of Tungsten-base class sample |
| CN102590181A (en) * | 2012-02-29 | 2012-07-18 | 成都中光电科技有限公司 | Method for detecting impurity components in alpha-alumina |
| CN102854238A (en) * | 2012-08-10 | 2013-01-02 | 同济大学 | Method for determination analysis of multiple heavy metals in environmental medium or biological sample |
Non-Patent Citations (4)
| Title |
|---|
| 周勇义等: "微波消解技术及其在分析化学中的应用", 《冶金分析》 * |
| 尹艳娥等: "微波消解-原子吸收光谱法测定催化剂中的铜、铁、镍、钠", 《分析测试技术与仪器》 * |
| 李丽华等: "微波消解光度法测定催化剂中镍", 《理化检验-化学分册》 * |
| 李静等: "微波消解-光度法测定镍基合金中的钼", 《广州化工》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104231539B (en) | A kind of process for dispersing of Graphene in phenolic resin and Graphene phenol-formaldehyde resin modified | |
| CN104357071B (en) | A kind of microwave catalysis pyrolysis biomass orientation is utilized to produce biomass carbon, bio-oil and the method for biogas | |
| CN104650938A (en) | Co-production technique of needle coke, mesocarbon microbeads and high-quality asphalt | |
| CN101456879B (en) | Method for preparing combustion inhibitor bisphenol A bis(diphenyl phosphate) | |
| EP3092209A1 (en) | Fertiliser having reduced biuret content | |
| CN102633604B (en) | Method for recovering phenol and acetophenone from phenol tar | |
| CN103723744A (en) | Method for extraction of high purity sodium thiocyanate from desulfurization waste liquid or desulfurization liquid mixed salt | |
| CN103923379B (en) | A kind of utilize boric sludge for the method for flame-retardant high-molecular composite | |
| CN105418675A (en) | Triazine charring agent, preparation method therefor and application thereof | |
| CN103808557A (en) | Microwave digestion liquid and microwave digestion method for nickel-phosphorus catalyst | |
| CN103396827B (en) | The separation method of liquefied coal coil neutral and alkali nitrogen compound | |
| CN102674405A (en) | Method for preparing potassium sulfate by using picromerite | |
| CN102515163A (en) | Method for recycling phosphoric acid from tail gas produced in carbonization and activation of active carbon in phosphoric acid process | |
| CN103849413B (en) | Asphalt additive, modified pitch, and preparation method thereof, the preparation method of application and pitch carbide | |
| CN104448179B (en) | A kind of Graphene modified furan resin and preparation method thereof and furane resins fiberglass | |
| CN111017966A (en) | Preparation method for preparing high-purity anhydrous lithium chloride by using butyl lithium residues | |
| Qu et al. | Investigation on the thermal decomposition and flame retardancy of wood treated with a series of molybdates by TG–MS | |
| CN102994138A (en) | Method for preparing biological aviation kerosene by using swell-cooked dirty oil | |
| CN102674282A (en) | Method for producing granular monoammonium phosphate | |
| CN109704289A (en) | A kind of method of sulphur cream extraction production high-purity sulphur | |
| CN104556029A (en) | Preparation of active carbon and fuel oil by use of petroleum residue and tar residue together | |
| CN103214513A (en) | Preparation method of bisphenol A bis(diphenyl phosphate) | |
| CN102633967A (en) | Preparation technology of bamboo-quality modified phenolic resin | |
| CN110563005A (en) | Process for producing potassium sulfate | |
| Chen et al. | Synthesis of Gd (III)-MOF: Dy 3+ phosphor and kinetics study of its thermal decomposition |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20140521 |