CN1632560A - Process for determining cyclohexyl hydrogen peroxide content in cyclohexane oxidation mixture - Google Patents
Process for determining cyclohexyl hydrogen peroxide content in cyclohexane oxidation mixture Download PDFInfo
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- CN1632560A CN1632560A CN 200310110679 CN200310110679A CN1632560A CN 1632560 A CN1632560 A CN 1632560A CN 200310110679 CN200310110679 CN 200310110679 CN 200310110679 A CN200310110679 A CN 200310110679A CN 1632560 A CN1632560 A CN 1632560A
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Abstract
This invention relates to a method to test the cyclohexyl auricome in the mixture of cyclohexane, which is characterized by the following: to join triphenylphosphine into the sample, together with cyclohexyl auricome to generate the equal molar peroxy triphenylphosphine; to isolate the sample by the color spectrum isolation column and to test the sample by the hydrogen ion tester; to adopt internal marker method to determine the content of the peroxy triphenylphosphine and indirectly to measure the content of the auricome cyclohexyl.
Description
One, technical field:
The present invention relates to a kind of method of measuring cyclohexyl hydroperoxide content in the cyclohexane oxidation potpourri.
Two, background technology:
Cyclohexyl hydroperoxide is the intermediate product that cyclohexane oxidation prepares the cyclohexanone process, based on its less stable, labile character, directly use the content of cyclohexyl hydroperoxide in the vapor-phase chromatography quantitative measurement potpourri, because sample is at the high-temperature evaporation of vaporizer, cyclohexyl hydroperoxide will inevitably be decomposed into cyclohexanone, cyclohexanol, even deep oxidation.The detection data that obtain can not reflect actual value.Home and abroad Cyclohexanone Production producer adopts its content of redox chemistry titrimetry indirect determination usually.Promptly accurately take by weighing the cyclohexane oxidation sample, add the potassium iodide (KI) of q.s, cyclohexyl peroxide is changed into iodine (I
2), with sodium thiosulfate (Na
2S
2O
3) standard solution titration iodine (I
2), the content of indirect determination superoxide cyclohexyl.This method running program is loaded down with trivial details, measures the about 40-50 minute analysis time of a sample, and this method accuracy is not high, time-consuming; Consume reagent such as a large amount of chloroforms, glacial acetic acid simultaneously, the glacial acetic acid pungency is stronger, and the phosgene toxicity of chloroform is very strong, and is bigger to health harm.
Three, summary of the invention:
The object of the present invention is to provide a kind of method of measuring cyclohexyl hydroperoxide content in the cyclohexane oxidation potpourri.The object of the present invention is achieved like this: add triphenylphosphine in blend sample sample is carried out pre-service, adopt internal standard method to carry out quantitatively.The concrete analysis step is as follows:
A, sample thief: cyclohexane non-catalyst oxidation or non-catalyst oxidation reactant liquor and described oxidation liquid are through the sample of aftertreatment.
B, selected internal standard compound: internal standard compound is and the nonreactive ester class of sample, as butylene phthalate, phthalic acid azelaoyl etc.Content all has the better linearity relation in the 40-200mg/L scope, and related coefficient is all greater than 0.999.
C, sample preparation: the triphenylphosphine of the excessive 10%-50% of disposable adding (w/w), accurately take by weighing internal standard compound suitable and 1.0g sample with sample size, place a period of time after having joined sample, add the 8ml solvent dilution, solvent can be the reagent miscible with sample such as toluene, benzene, acetone.
The preparation of D, standard solution: with analyzing pure toluene, preparation of chromatographically pure peroxide triphenylphosphine and the similar content of sample accurately add internal standard compound 0.01-0.3g, and standard solution 0.4-1.0g adds the 2-8ml solvent dilution, shakes up.
E, chromatographic column and analysis condition
Capillary column: 5m-30m, column temperature are temperature programme: 150 ℃-280 ℃, in, the low pole capillary column, as OV-101, HP-5, DB-5,0V-17 etc.
The packed column column temperature is temperature programme: 150 ℃-280 ℃.
Column material: glass column, stainless steel.
Immobile liquid: in, the low pole immobile liquid, the amount of being coated with: 5%-15%.
Column length: 0.5m-2m.
Good effect of the present invention is to provide effective analytical approach for the mensuration of cyclohexyl hydroperoxide in the cyclohexane oxidation potpourri.The present invention has that analysis result is accurate, and analysis speed is fast, and is easy and simple to handle, highly sensitive, characteristics such as heavy good linearity.
Four, embodiment:
Example 1: adopt the 8%OV-101 packed column
In volumetric flask, add the 0.04g triphenylphosphine, accurately add the 0.8230g sample, place 25min, accurately pipette 4ml inner mark solution (0.0080g/ml), add the 3ml dilution with toluene, shake up, get the 1ul sample analysis.Analysis condition: column temperature: 150 ℃ of initial temperatures, keep 1min to rise to 170 ℃ with 20 ℃/min, keep 2min; Rise to 230 ℃ with 30 ℃/min again and keep 8min.240 ℃ of injectors, 250 ℃ of detecting devices.Carrier gas: nitrogen 45ml/min, air 300ml/min, hydrogen 30ml/min.
Example 2:OV-17 capillary column, 25m * Φ 0.32.
In volumetric flask, accurately add the 0.1020g triphenylphosphine, add the 0.4850g sample, add the 6ml dilution with toluene, shake up, get the 0.4ul sample analysis.Chromatographiccondition is: column temperature rises to 250 with 40 ℃/min for 150 ℃ and keeps 6min.250 ℃ of injectors, 260 ℃ of detecting devices.Carrier gas: nitrogen 1.0ml/min, air 350ml/min, hydrogen 30ml/min.
Claims (3)
1, a kind of method of measuring cyclohexyl hydroperoxide content in the cyclohexane oxidation potpourri, comprise sample thief, selected internal standard compound, sample preparation, preparing standard solution, analyze with chromatographic column, it is characterized in that: sample is cyclohexane non-catalyst oxidation or non-catalyst oxidation reactant liquor or the described oxidation liquid sample through aftertreatment; Internal standard compound is and the nonreactive ester class of sample; Sample preparation is the triphenylphosphine that disposable adding adds excessive 10%-50% (w/w), accurately takes by weighing internal standard compound suitable with sample size and 1.0g sample, places a period of time after having joined sample, adds the 8ml solvent dilution; The preparation of standard solution is: with analyzing pure toluene, preparation of chromatographically pure peroxide triphenylphosphine and the similar content of sample accurately add internal standard compound 0.01-0.3g, and standard solution 0.4-1.0g adds the 2-8ml solvent dilution, shakes up; Described chromatographic column and analysis condition are: capillary column: 5m-30m, column temperature are temperature programme: 150 ℃-280 ℃, in, the low pole capillary column, as OV-101, HP-5, DB-5,0V-17 etc.; The packed column column temperature is temperature programme: 150 ℃-280 ℃; Column material: glass column, stainless steel; Immobile liquid: in, the low pole immobile liquid, the amount of being coated with: 5%-15%; Column length: 0.5m-2m.
2, the method for cyclohexyl hydroperoxide content in the mensuration cyclohexane oxidation potpourri according to claim 1 is characterized in that: the solvent that sample preparation adds can be the reagent miscible with sample such as toluene, benzene, acetone.
3, the method for cyclohexyl hydroperoxide content in the mensuration cyclohexane oxidation potpourri according to claim 1, it is characterized in that: internal standard compound can be butylene phthalate, phthalic acid azelaoyl.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310110679 CN1632560A (en) | 2003-12-22 | 2003-12-22 | Process for determining cyclohexyl hydrogen peroxide content in cyclohexane oxidation mixture |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310110679 CN1632560A (en) | 2003-12-22 | 2003-12-22 | Process for determining cyclohexyl hydrogen peroxide content in cyclohexane oxidation mixture |
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|---|---|
| CN1632560A true CN1632560A (en) | 2005-06-29 |
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|---|---|---|---|
| CN 200310110679 Pending CN1632560A (en) | 2003-12-22 | 2003-12-22 | Process for determining cyclohexyl hydrogen peroxide content in cyclohexane oxidation mixture |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1936586B (en) * | 2006-09-15 | 2010-05-12 | 北京工业大学 | Method for fully analyzing air (oxygen) oxidation cyclohexaane reaction mixture |
| CN103913521A (en) * | 2013-12-05 | 2014-07-09 | 烟台东诚生化股份有限公司 | Novel method for detecting hydrogen peroxide residues in heparin sodium |
-
2003
- 2003-12-22 CN CN 200310110679 patent/CN1632560A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1936586B (en) * | 2006-09-15 | 2010-05-12 | 北京工业大学 | Method for fully analyzing air (oxygen) oxidation cyclohexaane reaction mixture |
| CN103913521A (en) * | 2013-12-05 | 2014-07-09 | 烟台东诚生化股份有限公司 | Novel method for detecting hydrogen peroxide residues in heparin sodium |
| CN103913521B (en) * | 2013-12-05 | 2015-07-08 | 烟台东诚药业集团股份有限公司 | Novel method for detecting hydrogen peroxide residues in heparin sodium |
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