CN108169223B - Method for measuring alkali value of dimethyl sulfoxide recovered from carbon fiber wastewater - Google Patents
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Abstract
A method for determining the base number of dimethyl sulfoxide recovered from carbon fiber wastewater comprises the steps of using bromocresol green as an indicator, titrating carbon dioxide-free water used for testing by using HCl standard solution to obtain a titration value of a blank reference sample, adding the bromocresol green indicator after fully mixing distilled recovered DMSO with the carbon dioxide-free water, titrating by using HCl standard solution until the solution is changed into yellow green and keeps unchanged for 30 seconds, namely, a titration end point, obtaining a determination result, and calculating to obtain the base number of the dimethyl sulfoxide. The method has the advantages of accurate and rapid detection of the alkalinity value of the recovered DMSO and simple operation.
Description
Technical Field
The invention relates to a method for measuring the base number of dimethyl sulfoxide, in particular to a method for measuring the base number of dimethyl sulfoxide recovered from carbon fiber wastewater.
Background
Dimethyl sulfoxide (DMSO) is currently the most commonly used solvent for making polyacrylonitrile precursors. It is colorless, transparent and slightly odorous liquid, and has a relative density of 1.1014(20/4 deg.C), boiling point of 189 deg.C, freezing point of 18.5 deg.C, flash point of 95 deg.C, burning point of 304 deg.C, and refractive index of 1.47833(20 deg.C). In the process of industrial production of polyacrylonitrile protofilament, the consumption of DMSO in a DMSO one-step method is large, and DMSO in a protofilament coagulation bath is generally rectified and recycled so as to reduce the production cost. GB-21395-2008 makes a specification on the technical requirements of industrial DMSO and makes a specification on items such as DMSO crystallization point, transmittance, refractive index, mass fraction of impurities, mass fraction of water and the like. The acid value of the starting DMSO material was also specified. In the process of industrial production of polyacrylonitrile protofilament, in order to improve the hydrophilicity of polyacrylonitrile and effectively control the double diffusion rate, the polymerization solution is ammoniated after acrylonitrile is polymerized, so that the polymerization solution is changed from weak acidity (pH 5-6) to medium strong alkalinity (pH 8-10). Thus, unlike the starting DMSO, the recovered DMSO from rectification is alkaline, whereas GBT9736-2008 gives only a method for testing acidity, and this standard cannot be used for recovered DMSO from rectification which is alkaline. The retrieval shows that the method for measuring the alkalinity value of the distilled and recovered DMSO provided by the invention is not found.
Disclosure of Invention
The invention aims to provide a method for measuring the alkalinity value of distilled and recovered DMSO (dimethyl sulfoxide) by accurate measurement.
Compared with the acidity index of industrial raw material DMSO, the invention provides a method for measuring the alkali value of dimethyl sulfoxide recovered from carbon fiber wastewater, so that the alkali value of dimethyl sulfoxide recovered from carbon fiber wastewater by rectification in different batches can be compared, and an important reference basis is provided for subsequent polymerization production.
The technical scheme of the invention is as follows:
a method for measuring the base number of dimethyl sulfoxide recovered from carbon fiber wastewater comprises the step of titrating a recovered dimethyl sulfoxide aqueous solution by using an acid standard solution to obtain the base number of the recovered dimethyl sulfoxide.
The method comprises the following specific steps:
(1) titrating carbon dioxide-free water used for testing by using a HCl standard solution by using bromocresol green as an indicator until the solution turns yellow green and keeps unchanged for 30 seconds to obtain an end point, repeatedly titrating for 5 times to obtain a volume value of the HCl standard solution, removing the highest value and the lowest value, taking the arithmetic mean value of the other 3 parallel titration results as the volume of the finally consumed HCl standard solution, and recording the volume value as V0；
(2) Recovering dimethyl sulfoxide from carbon fiber wastewater by using a rectification method, fully mixing the rectified and recovered dimethyl sulfoxide with carbon dioxide-free water according to a mass ratio of 1:1-6, adding a bromocresol green indicator after uniformly mixing, titrating with an HCl standard solution until the solution becomes yellow green and keeps unchanged for 30 seconds, namely a titration end point, repeatedly titrating for 5 times to obtain a volume value of the HCl standard solution, removing the highest and lowest values, and taking the arithmetic average value of the other 3 parallel titration results as the final consumed volume of the HCl standard solution and marking as V;
(3) the alkalinity value of the distilled recovered DMSO is calculated according to the following formula:
in the formula: v-the volume of HCl standard solution consumed by titration to endpoint in mL;
V0titration ofThe volume of HCl standard solution consumed by the blank is mL;
CHCl-the concentration of HCl standard solution in mol/L;
V1volume of distilled recovery of DMSO at test in mL.
The base number W is calculated as the base number in HCl, i.e. the mass of HCl required for titration of 1g of DMSO.
The method can accurately and quickly detect the alkalinity value of the recovered DMSO, and has simple operation and small error.
Detailed Description
Example 1:
the method for measuring the alkalinity value of the DMSO recovered by rectification comprises three steps of titration of a DMSO aqueous solution, titration of a blank control sample and data processing, and specifically comprises the following steps:
1) preparing 0.1mol/L HCl standard solution and calibrating the concentration. Using bromocresol green as an indicator, titrating with carbon dioxide-free water used for testing an HCl standard solution until the solution turns yellow green and keeps unchanged for 30 seconds to obtain an end point, repeatedly titrating for 5 times to obtain a volume value of the HCl standard solution, removing the highest value and the lowest value, taking the arithmetic mean value of the other 3 parallel titration results as the final consumed volume of the HCl standard solution, and recording as V0,V0＝0.20mL。
2) Get V125mL of DMSO recovered by rectification was thoroughly mixed with 25mL of carbon dioxide-free water. And (3) adding a bromocresol green indicator after uniformly mixing, titrating by using an HCl standard solution until the solution becomes yellow green and does not change color for 30 seconds, and thus obtaining a titration end point. After repeating the titration 5 times to obtain the volume value of the HCl standard solution, the highest and lowest values were removed, and the arithmetic mean of the remaining 3 parallel titration results was taken as the final volume of the HCl standard solution consumed, which was recorded as V, and 0.79 mL.
3) And (3) calculating the data measured in the steps 1) and 2) according to the following formula to obtain the alkalinity value of the DMSO.
In the formula: v-the volume of HCl standard solution consumed by titration to endpoint in mL;
V0-the volume of HCl standard solution consumed for titration of the blank in mL;
CHCl-the concentration of HCl standard solution in mol/L;
V1volume of distilled recovery of DMSO at test in mL.
The determination was repeated five times in accordance with step 2), giving base numbers of 0.077mg/g, 0.078mg/g, 0.079mg/g, respectively, with an average value of 0.078mg/g, i.e. a mass of 0.078mg HCl required for titration of 1g of DMSO. The Standard Deviation (SD) was 0.00084.
Example 2:
mixing the distilled and recovered DMSO with carbon dioxide-free water according to different mass ratios, and titrating by using HCl standard solutions respectively, wherein the method comprises the following specific steps:
1) preparing 0.1mol/L HCl standard solution and calibrating the concentration. Using bromocresol green as an indicator, titrating with carbon dioxide-free water used for testing HCl standard solution until the solution turns into yellow green and keeps unchanged for 30 seconds as an end point, and recording the volume of the consumed HCl standard solution as V0. After repeating titration for 5 times to obtain the volume value of HCl standard solution, removing the highest and lowest values, taking the arithmetic mean of the other 3 times of parallel titration results as the final consumed volume of HCl standard solution, and recording as V0,V0＝0.20mL。
2) Get V1The DMSO recovered by rectification was 25mL, and the volumes of carbon dioxide-free water were 50mL, respectively, and mixed thoroughly. And (3) adding a bromocresol green indicator after uniformly mixing, titrating by using an HCl standard solution until the solution becomes yellow green and does not change color for 30 seconds, and thus obtaining a titration end point. After repeating the titration for 5 times to obtain the volume value of the HCl standard solution, the highest and lowest values were removed, and the arithmetic mean of the remaining 3 parallel titration results was taken as the final volume of the HCl standard solution consumed, which was recorded as V, and V was 0.80 mL.
3) And (3) calculating the data measured in the steps 1) and 2) according to the following formula to obtain the alkalinity value of the DMSO.
In the formula: v-the volume of HCl standard solution consumed by titration to endpoint in mL;
V0-the volume of HCl standard solution consumed for titration of the blank in mL;
CHCl-the concentration of HCl standard solution in mol/L;
V1volume of recovered DMSO by rectification in mL.
The determination was repeated five times in accordance with step 2), giving base numbers of 0.079mg/g, 0.080mg/g, 0.079mg/g, 0.081mg/g, 0.079mg/g, with an average value of 0.080mg/g, i.e. a mass of 0.080mg of HCl required for titration of 1g of DMSO. The result had a Standard Deviation (SD) of 0.00089.
Example 3:
the method for measuring the alkalinity value of the DMSO recovered by rectification comprises three steps of titration of a DMSO aqueous solution, titration of a blank control sample and data processing, and specifically comprises the following steps:
1) preparing 0.1mol/L HCl standard solution and calibrating the concentration. Using bromocresol green as an indicator, titrating with carbon dioxide-free water used for testing an HCl standard solution until the solution turns yellow green and keeps unchanged for 30 seconds to obtain an end point, repeatedly titrating for 5 times to obtain a volume value of the HCl standard solution, removing the highest value and the lowest value, taking the arithmetic mean value of the other 3 parallel titration results as the final consumed volume of the HCl standard solution, and recording as V0,V0＝0.20mL。
2) Get V1The recovered DMSO was distilled off in 25mL, and 100mL of carbon dioxide-free water was thoroughly mixed. And (3) adding a bromocresol green indicator after uniformly mixing, titrating by using an HCl standard solution until the solution becomes yellow green and does not change color for 30 seconds, and thus obtaining a titration end point. After the titration is repeated for 5 times to obtain the volume value of the HCl standard solution, the highest value and the lowest value are removed, the arithmetic mean value of the rest 3 times of parallel titration results is taken as the final consumed volume of the HCl standard solution,the notation is V, 0.81 mL.
3) And (3) calculating the data measured in the steps 1) and 2) according to the following formula to obtain the alkalinity value of the DMSO.
In the formula: v-the volume of HCl standard solution consumed by titration to endpoint in mL;
V0-the volume of HCl standard solution consumed for titration of the blank in mL;
CHCl-the concentration of HCl standard solution in mol/L;
V1volume of recovered DMSO by rectification in mL.
The determination was repeated five times in accordance with step 2), giving base numbers of 0.080mg/g, 0.081mg/g, 0.082mg/g, 0.079mg/g, 0.081mg/g, respectively, with an average value of 0.081mg/g, i.e. a mass of 0.081mg of HCl required for titration of 1g of DMSO. The Standard Deviation (SD) was 0.0011.
Example 4:
the method for measuring the alkalinity value of the DMSO recovered by rectification comprises three steps of titration of a DMSO aqueous solution, titration of a blank control sample and data processing, and specifically comprises the following steps:
1) preparing 0.1mol/L HCl standard solution and calibrating the concentration. Using bromocresol green as an indicator, titrating with carbon dioxide-free water used for testing an HCl standard solution until the solution turns yellow green and keeps unchanged for 30 seconds to obtain an end point, repeatedly titrating for 5 times to obtain a volume value of the HCl standard solution, removing the highest value and the lowest value, taking the arithmetic mean value of the other 3 parallel titration results as the final consumed volume of the HCl standard solution, and recording as V0，V0＝0.20mL。
2) Get V1The recovered DMSO was distilled off in 25mL, and 150mL of carbon dioxide-free water was thoroughly mixed. And (3) adding a bromocresol green indicator after uniformly mixing, titrating by using an HCl standard solution until the solution becomes yellow green and does not change color for 30 seconds, and thus obtaining a titration end point. The titration was repeated 5 times to obtain the volume value of the HCl standard solutionAfter that, the arithmetic mean of the other 3 parallel titration results after removing the highest and lowest values is taken as the final consumed volume of HCl standard solution, which is recorded as V, V0＝0.80mL。
3) And (3) calculating the data measured in the steps 1) and 2) according to the following formula to obtain the alkalinity value of the DMSO.
In the formula: v-the volume of HCl standard solution consumed by titration to endpoint in mL;
V0-the volume of HCl standard solution consumed for titration of the blank in mL;
CHCl-the concentration of HCl standard solution in mol/L;
V1volume of recovered DMSO by rectification in mL.
The determination was repeated five times in accordance with step 2), giving base numbers of 0.080mg/g, 0.079mg/g, 0.081mg/g, 0.080mg/g, 0.079mg/g, respectively, with an average value of 0.080mg/g, i.e. a mass of 0.080mg of HCl required for titration of 1g of DMSO. The Standard Deviation (SD) was 0.00084.
As can be seen from the above examples, the alkali value standard deviation of the recovered DMSO measured by the mass ratio of the different distilled recovered DMSO to the carbon dioxide-free water is small, the operation is simple, and the error is small.
Claims (1)
1. A method for measuring the alkali value of dimethyl sulfoxide recovered from carbon fiber wastewater is characterized by comprising the following steps:
(1) titrating carbon dioxide-free water used for testing by using a HCl standard solution by using bromocresol green as an indicator until the solution turns yellow green and keeps unchanged for 30 seconds to obtain an end point, repeatedly titrating for 5 times to obtain a volume value of the HCl standard solution, removing the highest value and the lowest value, taking the arithmetic mean value of the other 3 parallel titration results as the volume of the finally consumed HCl standard solution, and recording the volume value as V0；
(2) Recovering dimethyl sulfoxide from carbon fiber wastewater by adopting a rectification method, fully mixing the rectified and recovered dimethyl sulfoxide with carbon dioxide-free water according to the mass ratio of 1:1-6, adding a bromocresol green indicator after uniformly mixing, titrating with an HCl standard solution until the solution becomes yellow green and keeps unchanged for 30 seconds, namely a titration end point, repeatedly titrating for 5 times to obtain a volume value of the HCl standard solution, removing the highest and lowest values, and taking the arithmetic average value of the other 3 parallel titration results as the final consumed volume of the HCl standard solution and marking as V;
(3) the alkalinity value of the distilled recovered DMSO is calculated according to the following formula:
in the formula: v-the volume of HCl standard solution consumed by titration to endpoint in mL;
V0-the volume of HCl standard solution consumed for titration of the blank in mL;
CHCl-the concentration of HCl standard solution in mol/L;
V1volume of distilled recovery of DMSO at test in mL;
the method is used for comparing the base numbers of different batches of carbon fiber wastewater, and dimethyl sulfoxide is recovered by rectification, so that an important reference basis is provided for subsequent polymerization production.
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