CN108169223A - The base number assay method of dimethyl sulfoxide (DMSO) is recycled in carbon fiber waste water - Google Patents
The base number assay method of dimethyl sulfoxide (DMSO) is recycled in carbon fiber waste water Download PDFInfo
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Abstract
The base number assay method that dimethyl sulfoxide (DMSO) is recycled in a kind of carbon fiber waste water is using bromocresol green as indicator, it is titrated with HCl standard solution to testing carbon dioxide-free water used, obtain the titration value of blank sample, rectifying recycles after DMSO is sufficiently mixed with carbon dioxide-free water and adds in bromocresol green indicator, with HCl standard solution be titrated to solution become yellow green and keep 30 seconds it is non-discolouring, as titration end-point obtains measurement result, calculates the base number of dimethyl sulfoxide (DMSO).The present invention has the advantages of basicity value for quickly and accurately detecting recycling DMSO, easy to operate.
Description
Technical field
It is sub- the present invention relates to dimethyl is recycled in a kind of base number assay method of dimethyl sulfoxide (DMSO), especially carbon fiber waste water
The base number assay method of sulfone.
Background technology
Dimethyl sulfoxide (DMSO) (DMSO) is the current most common solvent for preparing polyacrylonitrile fibril.It slightly has for water white transparency
The liquid of stink, relative density 1.1014 (20/4 DEG C), 189 DEG C of boiling point, 18.5 DEG C of solidification point, 95 DEG C of flash-point, 304 DEG C of burning point,
Refractive index 1.47833 (20 DEG C).During industrial production polyacrylonitrile fibril, DMSO consumptions are larger in DMSO one-step method,
Rectifying recycling usually is carried out to the DMSO in precursor coagulating bath, to reduce production cost.GB-21395-2008 is to industrial
The technology of DMSO requires to have carried out specification, to the quality of DMSO crystalline temperatures, light transmittance, refractive index, the mass fraction of impurity and water
The projects such as score have carried out code requirement.Specification has also wherein been carried out for the acid value of raw material DMSO.In industrial production polypropylene
During nitrile precursor, in order to improve the hydrophily of polyacrylonitrile, double diffusion speed is effectively controlled, to polymerization after acrylonitrile polymerization
Liquid carries out ammoniated treatment so that polymer fluid is changed into middle strong basicity (PH=8-10) by faintly acid (PH=5-6).Therefore and raw material
DMSO is different, and the DMSO of rectifying recycling is rendered as alkalinity, and the method that test acidity is only gived in GBT9736-2008, for
The rectifying recycling DMSO that alkalinity is presented cannot then use this standard.A kind of rectifying recycling provided by the invention is not found through retrieval
The assay method of DMSO basicity values.
Invention content
The purpose of the present invention is to provide a kind of assay methods of rectifying recycling DMSO basicity values that can accurately measure.
The present invention gives and dimethyl Asia is recycled in a kind of carbon fiber waste water relative to the acidity index of raw material of industry DMSO
The base number assay method of sulfone is measured carbon fiber waste water using the base number of rectifying recycling dimethyl sulfoxide (DMSO) to compare different batches
Method provides important reference frame for subsequent polymerization.
Technical solution of the present invention is as follows：
The base number assay method of dimethyl sulfoxide (DMSO) is recycled in a kind of carbon fiber waste water, using sour standard solution to the two of recycling
Methyl sulfoxide aqueous solution is titrated, and can obtain the base number of recycling dimethyl sulfoxide (DMSO).
It is as follows：
(1) it using bromocresol green as indicator, is titrated with HCl standard solution to testing carbon dioxide-free water used,
It is titrated to solution to become yellow green and keep 30 seconds non-discolouring as terminals, repeats to titrate 5 obtained bodies of HCl standard solution
After product value, HCl of the arithmetic mean of instantaneous value of remaining 3 parallel titration results finally to be consumed is taken to mark after removing highest and minimum
The volume of quasi- solution, is denoted as V0；
(2) to carbon fiber waste water using rectificating method recycling dimethyl sulfoxide (DMSO), by rectifying recycling dimethyl sulfoxide (DMSO) and without two
Carbonoxide water is with mass ratio 1:The ratio of 1-6 is sufficiently mixed, and is added in bromocresol green indicator after mixing, is marked with HCl
Quasi- solution is titrated to solution and becomes yellow green and keep 30 seconds non-discolouring, as titration end-points, repeats to titrate 5 obtained HCl
After the bulking value of standard solution, it is final that the arithmetic mean of instantaneous value of remaining 3 parallel titration results is taken after removal highest and minimum
The volume of HCl standard solution consumed, is denoted as V；
(3) rectifying recycling DMSO basicity values are calculated according to the following formula：
In formula：The volume of HCl standard solution that V- titration is consumed to terminal, unit mL；
V0The volume of HCl standard solution that titration blank sample is consumed, unit mL；
CHClThe concentration of-HCl standard solution, unit mol/L；
V1The volume of rectifying recycling DMSO, unit mL during test.
The base number W for calculating gained is the basicity value in terms of HCl, that is, titrates the quality of HCl needed for 1gDMSO.
The present invention can quickly and accurately detect the basicity value of recycling DMSO, and easy to operate, error is small.
Specific embodiment
Embodiment 1：
The assay method of the basicity value of rectifying recycling DMSO, the titration including DMSO aqueous solutions, the titration of blank sample
With three steps of data processing, it is as follows：
1) it prepares the HCl standard solution of 0.1mol/L and demarcates concentration.It is molten with HCl standards using bromocresol green as indicator
Liquid test carbon dioxide-free water used is titrated, be titrated to solution become yellow green and keep 30 seconds it is non-discolouring be eventually
Point repeats after titrating 5 obtained bulking values of HCl standard solution, remaining 3 parallel titration is taken after removing highest and minimum
As a result arithmetic mean of instantaneous value is the volume of HCl standard solution finally consumed, is denoted as V0,V0=0.20mL.
2) V is taken1The DMSO of=25mL rectifying recycling, carbon dioxide-free water 25mL are sufficiently mixed.After mixing plus
Enter bromocresol green indicator, with HCl standard solution titrate, be titrated to solution become yellow green and keep 30 seconds it is non-discolouring, as
Titration end-point.Repeat after titration obtains the bulking value of HCl standard solution 5 times, remove take after highest and minimum remaining 3 times it is parallel
The arithmetic mean of instantaneous value of titration results is the volume of HCl standard solution finally consumed, is denoted as V, V=0.79mL.
3) data measured by step 1) and step 2) are calculated with the basicity value of DMSO according to the following formula.
In formula：The volume of HCl standard solution that V- titration is consumed to terminal, unit mL；
V0The volume of HCl standard solution that titration blank sample is consumed, unit mL；
CHClThe concentration of-HCl standard solution, unit mol/L；
V1The volume of rectifying recycling DMSO, unit mL during test.
According to step 2) replication five times, gained base number be respectively 0.077mg/g, 0.078mg/g, 0.079mg/g,
0.078mg/g, 0.079mg/g, average value 0.078mg/g, that is, the quality for titrating HCl needed for 1gDMSO are 0.078mg.As a result
Standard deviation (SD) is 0.00084.
Embodiment 2：
Rectifying recycling DMSO with carbon dioxide-free water according to different quality ratio is mixed, is carried out respectively with HCl standard solution
Titration, is as follows：
1) it prepares the HCl standard solution of 0.1mol/L and demarcates concentration.It is molten with HCl standards using bromocresol green as indicator
Liquid test carbon dioxide-free water used is titrated, be titrated to solution become yellow green and keep 30 seconds it is non-discolouring be eventually
Point, the volume of HCl standard solution consumed are denoted as V0.It repeats after titrating 5 obtained bulking values of HCl standard solution, goes
Except taking the arithmetic mean of instantaneous value of remaining 3 parallel titration results after highest and minimum as the HCl standard solution that is finally consumed
Volume is denoted as V0,V0=0.20mL.
2) V is taken1The DMSO of=25mL rectifying recycling, carbon dioxide-free water volume is respectively that 50mL is sufficiently mixed.It is mixed
Bromocresol green indicator is added in after closing uniformly, is titrated with HCl standard solution, solution is titrated to and becomes yellow green and kept for 30 seconds not
Discoloration, as titration end-point.It repeatedly titrates 5 times after obtaining the bulking value of HCl standard solution, it is taken after removal highest and minimum
The arithmetic mean of instantaneous value of 3 parallel titration results of remaininging is the volume of HCl standard solution finally consumed, is denoted as V, V=0.80mL.
3) data measured by step 1) and step 2) are calculated with the basicity value of DMSO according to the following formula.
In formula：The volume of HCl standard solution that V- titration is consumed to terminal, unit mL；
V0The volume of HCl standard solution that titration blank sample is consumed, unit mL；
CHClThe concentration of-HCl standard solution, unit mol/L；
V1The volume of DMSO, unit mL are recycled in rectifying.
According to step 2) replication five times, gained base number be respectively 0.079mg/g, 0.080mg/g, 0.079mg/g,
0.081mg/g, 0.079mg/g, average value 0.080mg/g, that is, the quality for titrating HCl needed for 1gDMSO are 0.080mg.As a result
Standard deviation (SD) is 0.00089.
Embodiment 3：
The assay method of the basicity value of rectifying recycling DMSO, the titration including DMSO aqueous solutions, the titration of blank sample
With three steps of data processing, it is as follows：
1) it prepares the HCl standard solution of 0.1mol/L and demarcates concentration.It is molten with HCl standards using bromocresol green as indicator
Liquid test carbon dioxide-free water used is titrated, be titrated to solution become yellow green and keep 30 seconds it is non-discolouring be eventually
Point repeats after titrating 5 obtained bulking values of HCl standard solution, remaining 3 parallel titration is taken after removing highest and minimum
As a result arithmetic mean of instantaneous value is the volume of HCl standard solution finally consumed, is denoted as V0,V0=0.20mL.
2) V is taken1The DMSO of=25mL rectifying recycling, carbon dioxide-free water 100mL are sufficiently mixed.After mixing plus
Enter bromocresol green indicator, with HCl standard solution titrate, be titrated to solution become yellow green and keep 30 seconds it is non-discolouring, as
Titration end-point.Repeat after titration obtains the bulking value of HCl standard solution 5 times, remove take after highest and minimum remaining 3 times it is parallel
The arithmetic mean of instantaneous value of titration results is the volume of HCl standard solution finally consumed, is denoted as V, V=0.81mL.
3) data measured by step 1) and step 2) are calculated with the basicity value of DMSO according to the following formula.
In formula：The volume of HCl standard solution that V- titration is consumed to terminal, unit mL；
V0The volume of HCl standard solution that titration blank sample is consumed, unit mL；
CHClThe concentration of-HCl standard solution, unit mol/L；
V1The volume of DMSO, unit mL are recycled in rectifying.
According to step 2) replication five times, gained base number be respectively 0.080mg/g, 0.081mg/g, 0.082mg/g,
0.079mg/g, 0.081mg/g, average value 0.081mg/g, that is, the quality for titrating HCl needed for 1gDMSO are 0.081mg.As a result
Standard deviation (SD) is 0.0011.
Embodiment 4：
The assay method of the basicity value of rectifying recycling DMSO, the titration including DMSO aqueous solutions, the titration of blank sample
With three steps of data processing, it is as follows：
1) it prepares the HCl standard solution of 0.1mol/L and demarcates concentration.It is molten with HCl standards using bromocresol green as indicator
Liquid test carbon dioxide-free water used is titrated, be titrated to solution become yellow green and keep 30 seconds it is non-discolouring be eventually
Point repeats after titrating 5 obtained bulking values of HCl standard solution, remaining 3 parallel titration is taken after removing highest and minimum
As a result arithmetic mean of instantaneous value is the volume of HCl standard solution finally consumed, is denoted as V0, V0=0.20mL.
2) V is taken1The DMSO of=25mL rectifying recycling, carbon dioxide-free water 150mL are sufficiently mixed.After mixing plus
Enter bromocresol green indicator, with HCl standard solution titrate, be titrated to solution become yellow green and keep 30 seconds it is non-discolouring, as
Titration end-point.Repeat after titration obtains the bulking value of HCl standard solution 5 times, remove take after highest and minimum remaining 3 times it is parallel
The arithmetic mean of instantaneous value of titration results is the volume of HCl standard solution finally consumed, is denoted as V, V0=0.80mL.
3) data measured by step 1) and step 2) are calculated with the basicity value of DMSO according to the following formula.
In formula：The volume of HCl standard solution that V- titration is consumed to terminal, unit mL；
V0The volume of HCl standard solution that titration blank sample is consumed, unit mL；
CHClThe concentration of-HCl standard solution, unit mol/L；
V1The volume of DMSO, unit mL are recycled in rectifying.
According to step 2) replication five times, gained base number be respectively 0.080mg/g, 0.079mg/g, 0.081mg/g,
0.080mg/g, 0.079mg/g, average value 0.080mg/g, that is, the quality for titrating HCl needed for 1gDMSO are 0.080mg.As a result
Standard deviation (SD) is 0.00084.
As seen from the above embodiment, different rectifying recycling DMSO and the recycling measured by carbon dioxide-free water mass ratio
The base number standard deviation of DMSO is small, and easy to operate, error is small.
Claims (1)
1. the base number assay method of dimethyl sulfoxide (DMSO) is recycled in a kind of carbon fiber waste water, it is characterised in that include the following steps：
(1) it using bromocresol green as indicator, is titrated, titrated to testing carbon dioxide-free water used with HCl standard solution
Become yellow green to solution and keep 30 seconds non-discolouring as terminals, repeat to titrate 5 obtained bulking values of HCl standard solution
Afterwards, take the arithmetic mean of instantaneous value of remaining 3 parallel titration results molten for the HCl standards finally consumed after removing highest and minimum
The volume of liquid, is denoted as V0；
(2) dimethyl sulfoxide (DMSO) and no titanium dioxide are recycled using rectificating method recycling dimethyl sulfoxide (DMSO), by rectifying to carbon fiber waste water
Carbon water is with mass ratio 1:The ratio of 1-6 is sufficiently mixed, and adds in bromocresol green indicator after mixing, molten with HCl standards
Liquid is titrated to solution and becomes yellow green and keep 30 seconds non-discolouring, as titration end-points, repeats to titrate 5 obtained HCl standards
After the bulking value of solution, the arithmetic mean of instantaneous value of remaining 3 parallel titration results is taken finally to be disappeared after removing highest and minimum
The volume of the HCl standard solution of consumption, is denoted as V；
(3) rectifying recycling DMSO basicity values are calculated according to the following formula：
In formula：The volume of HCl standard solution that V- titration is consumed to terminal, unit mL；
V0The volume of HCl standard solution that titration blank sample is consumed, unit mL；
CHClThe concentration of-HCl standard solution, unit mol/L；
V1The volume of rectifying recycling DMSO, unit mL during test.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112782261A (en) * | 2020-12-28 | 2021-05-11 | 新疆美克化工股份有限公司 | 1, 4-butanediol base number analysis method |
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| CN104230769A (en) * | 2013-06-19 | 2014-12-24 | 吴嘉隆 | Method for obtaining dimethyl sulfoxide from recovered solvent in p-xylene bicyclic body production |
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| WO2001055698A1 (en) * | 2000-01-28 | 2001-08-02 | Pion, Inc. | MEASUREMENT OF SOLUBILITY-pH PROFILES |
| CN104230769A (en) * | 2013-06-19 | 2014-12-24 | 吴嘉隆 | Method for obtaining dimethyl sulfoxide from recovered solvent in p-xylene bicyclic body production |
| CN106353306A (en) * | 2016-08-17 | 2017-01-25 | 中简科技股份有限公司 | Method for testing residual acrylonitrile monomer content in spinning solution during carbon fiber production |
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Cited By (1)
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| CN112782261A (en) * | 2020-12-28 | 2021-05-11 | 新疆美克化工股份有限公司 | 1, 4-butanediol base number analysis method |
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Effective date of registration: 20230313 Address after: 030100 Jinyi Village, Yangqu County, Taiyuan City, Shanxi Province Patentee after: SHANXI GANGKE CARBON MATERIALS CO.,LTD. Address before: No. 27, Taoyuan South Road, Yingze District, Taiyuan, Shanxi Patentee before: INSTITUTE OF COAL CHEMISTRY, CHINESE ACADEMY OF SCIENCES |