CN111060464A - Method for measuring chroma of caprolactam heavy discharge liquid - Google Patents
Method for measuring chroma of caprolactam heavy discharge liquid Download PDFInfo
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- CN111060464A CN111060464A CN201911189045.7A CN201911189045A CN111060464A CN 111060464 A CN111060464 A CN 111060464A CN 201911189045 A CN201911189045 A CN 201911189045A CN 111060464 A CN111060464 A CN 111060464A
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/251—Colorimeters; Construction thereof
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Abstract
The invention discloses a method for measuring the chroma of caprolactam re-drainage liquid, which relates to the technical field of chroma measurement; the determination method comprises the following steps: s1: weighing 1-10g of the heavy liquid discharge sample; s2: placing the rearrangement liquid sample into a 500mL flask, injecting 50-100mL ethanol or methanol water solution, and stirring until the rearrangement liquid sample is dissolved; s3: quantitatively transferring the solution in the flask to a 250 or 500ml volumetric flask, adding ethanol or methanol water solution to constant volume, and staying for 8-15 min; s4: and (3) measuring the absorbance of the sample solution at the wavelength of 390nm by using a spectrophotometer, and calculating the chromaticity of the sample solution according to a formula. The method adopts a spectrophotometry method to detect the chroma of the heavy discharge liquid, has simple and convenient operation and accurate and reliable data, and can be widely applied to the caprolactam industry.
Description
Technical Field
The invention relates to the technical field of chromaticity determination, in particular to a method for determining chromaticity of caprolactam re-drainage liquid.
Background
Caprolactam is one of important organic chemical raw materials, and is mainly used for producing polyamide chips through polymerization and further processing the polyamide chips into materials such as fibers, engineering plastics, films and the like. The liquid phase rearrangement process of cyclohexanone oxime in caprolactam production process by ammoximation method is one of the key reactions in caprolactam production, and the main function of the process is that cyclohexanone oxime undergoes Beckmann rearrangement reaction to generate caprolactam under the catalysis of oleum, and the process has great influence on the quality of caprolactam products, the material consumption in the caprolactam production process and the like.
At present, rearrangement reaction conditions are generally known from three indexes of rearrangement liquid acid/hexane, titration value and SO3 content in industrial production, and the reaction process is not completely reflected.
Disclosure of Invention
The invention aims to provide a method for measuring the chromaticity of caprolactam re-drainage liquid, which aims to solve the problem of measuring the rearrangement reaction condition of the re-arrangement liquid.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for measuring the chroma of caprolactam heavy discharge liquid comprises the following steps: s1: weighing 1-10g of the heavy liquid discharge sample; s2: placing the rearrangement liquid sample into a 500mL flask, injecting 50-100mL ethanol or methanol water solution, and stirring until the rearrangement liquid sample is dissolved; s3: quantitatively transferring the solution in the flask to a 250 or 500ml volumetric flask, adding ethanol or methanol water solution to constant volume, and staying for 8-15 min; s4: measuring the absorbance of the sample solution at a wavelength of 390nm by using a spectrophotometer, and calculating the chromaticity of the sample solution according to the following formula:
in the formula: x-sample color, platinum-cobalt number;
143-absorbance to chromaticity conversion coefficient;
a-sample absorbance;
M1-determining the volume of the sample mass g;
M0sample weighing g.
On the basis of the technical scheme, the invention also provides the following optional technical scheme:
in one alternative: the mass percentage concentration of the ethanol or methanol water solution is 2%.
In one alternative: ethanol or methanol aqueous solution adopt absolute ethyl alcohol or methanol to pour into ultrapure water into and dispose and ethanol or methanol need filter through 0.45um organic filter membrane before the configuration, ultrapure water filters through 0.45um water filter membrane before the use.
In one alternative: the absorbance of the sample solution was measured a plurality of times and the number of measurements was not less than three.
In one alternative: the step S4 further includes stability determination of the prepared sample, measuring absorbance of the prepared sample multiple times and drawing a stability spectrum.
In one alternative: step S4 further includes determining the accuracy of the method of preparing the sample by: and (3) adding a quantitative 500-chroma standard solution into a 100ml volumetric flask, fixing the volume by using a known chroma sample diluent, and measuring the standard addition recovery rate of the method.
Compared with the prior art, the invention has the following beneficial effects:
the method adopts a spectrophotometry method to detect the chroma of the heavy discharge liquid, has simple and convenient operation and accurate and reliable data, and can be widely applied to the caprolactam industry.
Drawings
FIG. 1 is a chart of the stability profile of a sample of the present invention.
Detailed Description
The examples are given solely for the purpose of illustration and are not intended to limit the scope of the invention. Any obvious modifications or variations can be made to the present invention without departing from the spirit or scope of the present invention.
Example 1
A method for measuring the chroma of caprolactam heavy discharge liquid comprises the following steps:
s1: weighing 1g of heavy liquid discharge sample;
s2: placing the rearrangement liquid sample into a 500mL flask, injecting 50 ethanol or methanol water solution, and stirring until the rearrangement liquid sample is dissolved;
s3: quantitatively transferring the solution in the flask to a 250 volumetric flask, performing constant volume with ethanol or methanol water solution, and staying for 8 min;
s4: measuring the absorbance of the sample solution at a wavelength of 390nm by using a spectrophotometer, and calculating the chromaticity of the sample solution according to the following formula:
in the formula: x-sample color, platinum-cobalt number;
143-absorbance to chromaticity conversion coefficient;
a-sample absorbance;
M1-determining the volume of the sample mass g;
M0sample weighing g.
The mass percentage concentration of the ethanol or methanol water solution is 2%.
Ethanol or methanol aqueous solution adopt absolute ethyl alcohol or methanol to pour into ultrapure water into and dispose and ethanol or methanol need filter through 0.45um organic filter membrane before the configuration, ultrapure water filters through 0.45um water filter membrane before the use.
The absorbance of the sample solution was measured a plurality of times and the number of times was measured three times.
The step S4 further includes stability determination of the prepared sample, measuring absorbance of the prepared sample multiple times and drawing a stability spectrum.
Step S4 further includes determining the accuracy of the method of preparing the sample by: and (3) adding a quantitative 500-chroma standard solution into a 100ml volumetric flask, fixing the volume by using a known chroma sample diluent, and measuring the standard addition recovery rate of the method.
Example 2
A method for measuring the chroma of caprolactam heavy discharge liquid comprises the following steps:
s1: weighing 10g of heavy liquid discharge sample;
s2: placing the rearrangement liquid sample into a 500mL flask, injecting 100mL ethanol or methanol water solution, and stirring until the rearrangement liquid sample is dissolved;
s3: quantitatively transferring the solution in the flask to a 500ml volumetric flask, performing constant volume with ethanol or methanol water solution, and staying for 15 min;
s4: measuring the absorbance of the sample solution at a wavelength of 390nm by using a spectrophotometer, and calculating the chromaticity of the sample solution according to the following formula:
in the formula: x-sample color, platinum-cobalt number;
143-absorbance to chromaticity conversion coefficient;
a-sample absorbance;
M1-determining the volume of the sample mass g;
M0sample weighing g.
The mass percentage concentration of the ethanol or methanol water solution is 2%.
Ethanol or methanol aqueous solution adopt absolute ethyl alcohol or methanol to pour into ultrapure water into and dispose and ethanol or methanol need filter through 0.45um organic filter membrane before the configuration, ultrapure water filters through 0.45um water filter membrane before the use.
The absorbance of the sample solution was measured a plurality of times and the number of measurements was not less than three.
The step S4 further includes stability determination of the prepared sample, measuring absorbance of the prepared sample multiple times and drawing a stability spectrum.
Step S4 further includes determining the accuracy of the method of preparing the sample by: and (3) adding a quantitative 500-chroma standard solution into a 100ml volumetric flask, fixing the volume by using a known chroma sample diluent, and measuring the standard addition recovery rate of the method.
The stability of the sample is configured as shown in figure 1;
the method accuracy is as follows:
the above description is only for the specific embodiments of the present disclosure, but the scope of the present disclosure is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present disclosure, and all the changes or substitutions should be covered within the scope of the present disclosure. Therefore, the protection scope of the present disclosure shall be subject to the protection scope of the claims.
Claims (6)
1. The method for measuring the chroma of caprolactam heavy discharge liquid is characterized by comprising the following steps of: s1: weighing 1-10g of the heavy liquid discharge sample; s2: placing the rearrangement liquid sample into a 500mL flask, injecting 50-100mL ethanol or methanol water solution, and stirring until the rearrangement liquid sample is dissolved; s3: quantitatively transferring the solution in the flask to a 250 or 500ml volumetric flask, adding ethanol or methanol water solution to constant volume, and staying for 8-15 min; s4: measuring the absorbance of the sample solution at a wavelength of 390nm by using a spectrophotometer, and calculating the chromaticity of the sample solution according to the following formula:
in the formula: x-sample color, platinum-cobalt number;
143-absorbance to chromaticity conversion coefficient;
a-sample absorbance;
M1-determining the volume of the sample mass g;
M0sample weighing g.
2. The method for measuring the color of caprolactam heavy discharge liquid of claim 1, wherein the concentration of the ethanol or methanol aqueous solution is 2% by mass.
3. The method for measuring the chromaticity of caprolactam heavy discharge liquid according to claim 1, wherein the ethanol or methanol aqueous solution is prepared by injecting absolute ethanol or methanol into ultrapure water, and the ethanol or methanol is filtered by a 0.45um organic filter membrane before preparation, and the ultrapure water is filtered by a 0.45um water filter membrane before use.
4. The method for measuring the color of caprolactam rearrangement liquid according to claim 1, characterized in that the absorbance of the sample solution is measured a plurality of times and the number of times is not less than three.
5. The method for determining the chromaticity of caprolactam reliquefaction according to claim 1, wherein the step S4 further comprises stability determination of the prepared sample, measuring absorbance of the prepared sample multiple times and plotting a stability spectrum.
6. The method for determining the color of caprolactam re-drainage liquid of claim 1, wherein the step S4 further comprises determining the accuracy of the method for preparing the sample by: and (3) adding a quantitative 500-chroma standard solution into a 100ml volumetric flask, fixing the volume by using a known chroma sample diluent, and measuring the standard addition recovery rate of the method.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1485607A (en) * | 2002-09-29 | 2004-03-31 | 中国石油化工股份有限公司巴陵分公司 | Method for analizing cyclohexanone oxime in the cyclohexanone oxime rearrangement reaction mixture |
| CN102053120A (en) * | 2009-10-30 | 2011-05-11 | 中国石油化工股份有限公司 | Method for measuring content of cyclohexanone-oxime by liquid chromatography |
| CN105092758A (en) * | 2015-08-11 | 2015-11-25 | 成都易创思生物科技有限公司 | Method for measuring content of total flavones of licorice |
| WO2017097070A1 (en) * | 2015-12-10 | 2017-06-15 | 中国科学院大连化学物理研究所 | Method for quantitatively detecting content of proteins in alginate material by using bicinchoninic acid |
| WO2018040821A1 (en) * | 2016-08-30 | 2018-03-08 | 广东药科大学 | Method for measuring degree of deacetylation of chitosan oligosaccharide by using first-order derivative ultraviolet spectrophotometry |
| WO2019154131A1 (en) * | 2018-02-12 | 2019-08-15 | 山西振东安特生物制药有限公司 | Method for measuring free bismuth in colloidal bismuth pectin or preparation containing colloidal bismuth pectin |
-
2019
- 2019-11-28 CN CN201911189045.7A patent/CN111060464A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1485607A (en) * | 2002-09-29 | 2004-03-31 | 中国石油化工股份有限公司巴陵分公司 | Method for analizing cyclohexanone oxime in the cyclohexanone oxime rearrangement reaction mixture |
| CN102053120A (en) * | 2009-10-30 | 2011-05-11 | 中国石油化工股份有限公司 | Method for measuring content of cyclohexanone-oxime by liquid chromatography |
| CN105092758A (en) * | 2015-08-11 | 2015-11-25 | 成都易创思生物科技有限公司 | Method for measuring content of total flavones of licorice |
| WO2017097070A1 (en) * | 2015-12-10 | 2017-06-15 | 中国科学院大连化学物理研究所 | Method for quantitatively detecting content of proteins in alginate material by using bicinchoninic acid |
| WO2018040821A1 (en) * | 2016-08-30 | 2018-03-08 | 广东药科大学 | Method for measuring degree of deacetylation of chitosan oligosaccharide by using first-order derivative ultraviolet spectrophotometry |
| WO2019154131A1 (en) * | 2018-02-12 | 2019-08-15 | 山西振东安特生物制药有限公司 | Method for measuring free bismuth in colloidal bismuth pectin or preparation containing colloidal bismuth pectin |
Non-Patent Citations (3)
| Title |
|---|
| WANG HAO: "Research Progress in Refining Process for Production of Caprolactam by Beckman Rearrangement Reaction", 《CHINA PETROLEUM PROCESSING & PETROCHEMICAL TECHNOLOGY》 * |
| 全国化学标准化技术委员会有机分会秘书处编: "《有机化工产品及试验方法标准汇编1992》", 31 October 1992 * |
| 全国涂料和颜料标准化技术委员会: "《涂料工业用原材料检验方法标准汇编 基础 通用 树脂 溶剂 助剂卷》", 30 September 2004 * |
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