CN109342650A - 1,2- glycol connects the method for structural content in a kind of measurement polyvinyl alcohol - Google Patents
1,2- glycol connects the method for structural content in a kind of measurement polyvinyl alcohol Download PDFInfo
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- CN109342650A CN109342650A CN201811500450.1A CN201811500450A CN109342650A CN 109342650 A CN109342650 A CN 109342650A CN 201811500450 A CN201811500450 A CN 201811500450A CN 109342650 A CN109342650 A CN 109342650A
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- polyvinyl alcohol
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/162—Determining the equivalent point by means of a discontinuity
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Abstract
The invention discloses in a kind of measurement polyvinyl alcohol 1,2- glycol connects the method for structural content, it is after being dissolved in water polyvinyl alcohol sample to be measured, periodic acid is added to react completely, adds potassium iodide avoid light place 5-15min, quantitative titration is finally carried out under the display of starch indicator using hypo solution, to colourless for terminal, the volume of hypo solution consumed by recording connects the content of structure to calculate and obtain 1,2- glycol in polyvinyl alcohol to be measured.The present invention measures 1,2- glycol in polyvinyl alcohol and connects the method for structural content, easy to operate, data stabilization, accurate, has significant application value.
Description
Technical field
The invention belongs to chemical technology fields, are related to a kind of content assaying method of chemical substance, and in particular to Yi Zhongju
1,2- glycol connects the measuring method of structural content in vinyl alcohol.
Background technique
Polyvinyl alcohol (PVA) is a kind of widely used water-soluble high-molecular compound, can be used for fiber, construction material,
The industries such as optical film material.Liu Yinglong etc. is pointed out in " polyvinyl alcohol polyvinyl industrial data handbook ", is contained on PVA molecular backbone
1,3- glycol (end to end) and 1,2- glycol (head) structure (see formula (2)), wherein with 1, based on 3- diol structure, mixed with a small amount of
1,2- diol structure.Because 1,2- diol structure property is unstable, dilation, hot water resistance and the machinery of polyvinyl alcohol are affected
Intensity etc., and cracked vulnerable to oxidation, to limit the service performance of polyvinyl alcohol.Thus, it measures in polyvinyl alcohol
The content of 1,2- diol structure is significant, can instruct the optimization of technique to reduce the content of 1,2- diol structure.
The connect method of structural content of 1,2- glycol is using periodic acid or CeO in tradition measurement polyvinyl alcohol2-HNO3
Selective oxidation 1,2- diol structure measure the viscous (flat of oxidation front and back according to national standard GB/T 12010.5-2010 respectively
) molecular weight, according to formula:(MηFor (average) molecular weight viscous before PVA oxidation；After PVA oxidation
Viscous (average) molecular weight), calculate the content of 1,2- diol structure.But the measurement of this method medium viscosity needs more complex instrument
Device and operating technology.
Summary of the invention
To avoid above-mentioned existing deficiencies in the technology, the present invention provides in a kind of measurement polyvinyl alcohol 1,2-
Glycol connects the method for structural content, and technical problem to be solved is using periodic acid selective oxidation and indirect iodometric processes
The method combined accurately measures the content of 1,2- diol structure in polyvinyl alcohol using the redox titration being simple and efficient.
In order to solve the above technical problems, the present invention adopts the following technical scheme:
1,2- glycol connects the method for structural content in a kind of measurement polyvinyl alcohol, it is characterized in that: by polyethylene to be measured
After alcohol sample is dissolved in water, periodic acid is added and reacts completely, adds potassium iodide avoid light place 5-15min, finally uses sulphur
Sodium thiosulfate solution carries out quantitative titration under the display of starch indicator, until colourless is terminal, records consumed thio sulphur
The volume of acid sodium solution connects the content of structure to calculate and obtain 1,2- glycol in polyvinyl alcohol to be measured.
1,2- glycol connects the method for structural content in said determination polyvinyl alcohol, and application principle is as follows:
IO4 -+7I-+8H+→4I2+4H2O；
IO3-+5I-+6H+→3I2+3H2O；
I2+2Na2S2O3→2NaI+Na2S4O6。
Preferably, the periodic acid source be pure periodic acid or be periodate and hydrochloric acid mixture.It is furthermore preferred that institute
Stating periodate is sodium metaperiodate or potassium metaperiodate.Because of pure HIO4It is not present, the maximum concentration of aqueous solution is 86%, tool
There is very strong acid and oxidisability, it is heated easily to decomposite toxic iodide gas therefore not easy to operate.And sodium metaperiodate, height
Potassiumiodate property is relatively stable, is conducive to subsequent operation.
Preferably, it measures 1,2- glycol in polyvinyl alcohol to connect the method for structural content, specifically carry out as follows:
(1) it weighs A g polyvinyl alcohol to be measured to be added in conical beaker, adds 50-200mL deionized water, be warming up to 80-
It 100 DEG C, stirs to being completely dissolved, then is cooled to room temperature, obtain poly-vinyl alcohol solution, wherein 0.4≤A≤1.0；It is described to
The purity for surveying polyvinyl alcohol is denoted as B, unit %；
(2) dilute hydrochloric acid and C g periodate of 2-8mL 0.1000mol/L, shake are added in the poly-vinyl alcohol solution
It swings after shaking up, reacts 3~5min；After reaction, 0.5-1.2g potassium iodide is added into reaction solution to be protected from light after concussion shakes up
5-10min is placed, liquid to be titrated is obtained；
When periodate uses sodium metaperiodate, 0.07≤C≤1.5；When periodate uses potassium metaperiodate, 0.8≤C
≤1.6；
Or: the pure periodic acid of Cg is added in the poly-vinyl alcohol solution, after concussion shakes up, reacts 3~5min；Reaction terminates
Afterwards, the dilute hydrochloric acid and 0.5-1.2g potassium iodide of 1-7mL 0.1000mol/L are added into reaction solution to be protected from light and put after concussion shakes up
5-10min is set, liquid to be titrated is obtained；
(3) hypo solution for being 0.100mol/L with concentration titrates the liquid to be titrated, in titration
It shakes up, until 4~5 drop 1wt.% starch indicators are added dropwise when lighter, continues to be titrated to colourless for terminal, record thiosulfuric acid
The consumption of sodium solution is V mL；
(4) it is calculated by formula (1) and obtains 1,2- glycol in polyvinyl alcohol and connect the content X, unit % of structure:
In formula:
A is the quality of polyvinyl alcohol, unit g；
B is the purity of polyvinyl alcohol, unit %；
C is the quality of periodate or pure periodic acid, unit g；
D is the molal weight of periodate or pure periodic acid, unit g/mol；
E is the purity of periodate or pure periodic acid, unit %；
88 connect the molal weight of structure for 1,2- glycol in polyvinyl alcohol, unit g/mol；
V is the consumption of hypo solution, unit mL.
Compared with the prior art, the beneficial effects of the present invention are embodied in:
The present invention measures 1,2- glycol in polyvinyl alcohol and connects the method for structural content, easy to operate, data stabilization, standard
Really, there is significant application value.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, below with reference to embodiment to this hair
Bright specific embodiment is described in detail.The following contents is only to design example of the invention and explanation, institute
Belong to those skilled in the art to make various modifications or additions to the described embodiments or using similar
Mode substitutes, and as long as it does not deviate from the concept of invention or beyond the scope defined by this claim, should belong to the present invention
Protection scope.
Embodiment 1
The present embodiment use known its 1,2- glycol connect structural content for 3.634% raw material-purity 95% to be measured
Polyvinyl alcohol (degree of polymerization 1700, alcoholysis degree 99%), verifies the accuracy of the method for the present invention, the specific steps are as follows:
(1) it weighs A g polyvinyl alcohol to be measured to be added in conical beaker, adds 100mL deionized water, be warming up to 90 DEG C,
Stirring to being completely dissolved, then be cooled to room temperature, obtain poly-vinyl alcohol solution, wherein A be respectively 0.546g (being denoted as test 1),
0.5589g (being denoted as test 2), 0.5816g (being denoted as test 3).
(2) (purity E is the dilute hydrochloric acid and C g sodium metaperiodate that 3mL 0.1000mol/L is added in poly-vinyl alcohol solution
99.5%) after, concussion shakes up, 5min is reacted；After reaction, 0.6g potassium iodide is added into reaction solution to keep away after concussion shakes up
Light places 10min, obtains liquid to be titrated；Corresponding to test 1-3, C is respectively 0.8g, 0.0782g and 0.0839g.
(3) hypo solution for being 0.100mol/L with concentration titrates the liquid to be titrated, in titration
It shakes up, until 4~5 drop 1wt.% starch indicators are added dropwise when lighter, continues to be titrated to colourless for terminal, record thiosulfuric acid
The consumption of sodium solution is V mL；Corresponding to test 1-3, V is respectively 25.6mL, 24.9mL and 26.8mL.
(4) it is calculated by formula (1) and obtains 1,2- glycol in polyvinyl alcohol and connect the content of structure, correspond to test 1-3, calculation
Content is respectively 3.539%, 3.546% and 3.522%.
As can be seen that the present embodiment methods and results are accurate, reproducible.
Embodiment 2
The present embodiment use its known 1,2- glycol connect structural content for 3.421% raw material-purity 94.5% to be measured
Polyvinyl alcohol (degree of polymerization 500, alcoholysis degree 98.7%), verify the accuracy of the method for the present invention, the specific steps are as follows:
(1) it weighs 0.5192g polyvinyl alcohol to be measured to be added in conical beaker, adds 100mL deionized water, be warming up to 90
DEG C, it stirs to being completely dissolved, then is cooled to room temperature, obtain poly-vinyl alcohol solution.
(2) dilute hydrochloric acid and 0.0767g sodium metaperiodate (purity of 6mL 0.1000mol/L are added in poly-vinyl alcohol solution
99.5%), after concussion shakes up, to react 5min；After reaction, 0.6g potassium iodide is added into reaction solution, after concussion shakes up,
Avoid light place 10min obtains liquid to be titrated.
(3) hypo solution for being 0.100mol/L with concentration titrates the liquid to be titrated, in titration
It shakes up, until 4~5 drop 1wt.% starch indicators are added dropwise when lighter, continues to be titrated to colourless for terminal, record thiosulfuric acid
The consumption of sodium solution is 24.8mL.
(4) it is calculated by formula (1) and obtains 1,2- glycol in polyvinyl alcohol and connect the content 3.358% of structure.
Embodiment 3
The present embodiment use known its 1,2- glycol connect structural content for 3.532% raw material-purity 96% to be measured
Polyvinyl alcohol (degree of polymerization 2600, alcoholysis degree 99.8%), verifies the accuracy of the method for the present invention, the specific steps are as follows:
(1) it weighs 0.5098g polyvinyl alcohol to be measured to be added in conical beaker, adds 100mL deionized water, be warming up to 90
DEG C, it stirs to being completely dissolved, then is cooled to room temperature, obtain poly-vinyl alcohol solution.
(2) dilute hydrochloric acid and 0.0802g sodium metaperiodate (purity of 6mL 0.1000mol/L are added in poly-vinyl alcohol solution
99.5%), after concussion shakes up, to react 5min；After reaction, 0.6g potassium iodide is added into reaction solution, after concussion shakes up,
Avoid light place 10min obtains liquid to be titrated.
(3) hypo solution for being 0.100mol/L with concentration titrates the liquid to be titrated, in titration
It shakes up, until 4~5 drop 1wt.% starch indicators are added dropwise when lighter, continues to be titrated to colourless for terminal, record thiosulfuric acid
The consumption of sodium solution is 26.0mL.
(4) it is calculated by formula (1) and obtains 1,2- glycol in polyvinyl alcohol and connect the content 3.486% of structure.
Embodiment 4
The present embodiment use its known 1,2- glycol connect structural content for 3.967% raw material-purity 97.5% to be measured
Polyvinyl alcohol (degree of polymerization 3300, alcoholysis degree 99%), verify the accuracy of the method for the present invention, the specific steps are as follows:
(1) it weighs 0.5303g polyvinyl alcohol to be measured to be added in conical beaker, adds 100mL deionized water, be warming up to 90
DEG C, it stirs to being completely dissolved, then is cooled to room temperature, obtain poly-vinyl alcohol solution.
(2) dilute hydrochloric acid and 0.0758g sodium metaperiodate (purity of 6mL 0.1000mol/L are added in poly-vinyl alcohol solution
99.5%), after concussion shakes up, to react 5min；After reaction, 0.6g potassium iodide is added into reaction solution, after concussion shakes up,
Avoid light place 10min obtains liquid to be titrated.
(3) hypo solution for being 0.100mol/L with concentration titrates the liquid to be titrated, in titration
It shakes up, until 4~5 drop 1wt.% starch indicators are added dropwise when lighter, continues to be titrated to colourless for terminal, record thiosulfuric acid
The consumption of sodium solution is 23.7mL.
(4) it is calculated by formula (1) and obtains 1,2- glycol in polyvinyl alcohol and connect the content 3.837% of structure.
The above is only exemplary embodiment of the present invention, are not intended to limit the invention, all in spirit of the invention
With any modifications, equivalent replacements, and improvements made within principle etc., should all be included in the protection scope of the present invention.
Claims (4)
1. 1,2- glycol connects the method for structural content in a kind of measurement polyvinyl alcohol, it is characterised in that: by polyvinyl alcohol to be measured
After sample is dissolved in water, periodic acid is added and reacts completely, adds potassium iodide avoid light place 5-15min, finally using thio
Metabisulfite solution carries out quantitative titration under the display of starch indicator, until colourless is terminal, records consumed thiosulfuric acid
The volume of sodium solution connects the content of structure to calculate and obtain 1,2- glycol in polyvinyl alcohol to be measured.
2. 1,2- glycol connects the method for structural content in measurement polyvinyl alcohol according to claim 1, it is characterised in that:
The periodic acid source be pure periodic acid or be periodate and hydrochloric acid mixture.
3. 1,2- glycol connects the method for structural content in measurement polyvinyl alcohol according to claim 2, it is characterised in that:
The periodate is sodium metaperiodate or potassium metaperiodate.
4. 1,2- glycol connects the method for structural content in measurement polyvinyl alcohol according to claim 1, which is characterized in that
Specifically carry out as follows:
(1) it weighs A g polyvinyl alcohol to be measured to be added in conical beaker, adds 50-200mL deionized water, be warming up to 80-100
DEG C, it stirs to being completely dissolved, then is cooled to room temperature, obtain poly-vinyl alcohol solution, wherein 0.4≤A≤1.0；It is described to be measured poly-
The purity of vinyl alcohol is denoted as B, unit %；
(2) dilute hydrochloric acid of 2-8mL 0.1000mol/L is added in the poly-vinyl alcohol solution and C g periodate, concussion is shaken
After even, 3~5min is reacted；After reaction, 0.5-1.2g potassium iodide is added into reaction solution, after concussion shakes up, avoid light place
5-10min obtains liquid to be titrated；
When periodate uses sodium metaperiodate, 0.07≤C≤1.5；When periodate uses potassium metaperiodate, 0.8≤C≤
1.6；
Or: the pure periodic acid of Cg is added in the poly-vinyl alcohol solution, after concussion shakes up, reacts 3~5min；After reaction,
The dilute hydrochloric acid and 0.5-1.2g potassium iodide of 1-7mL 0.1000mol/L, after concussion shakes up, avoid light place 5- are added into reaction solution
10min obtains liquid to be titrated；
(3) hypo solution for being 0.100mol/L with concentration titrates the liquid to be titrated, shakes up in titration,
4~5 drop 1wt.% starch indicators are added dropwise when to lighter, continue to be titrated to colourless for terminal, record sodium thiosulfate is molten
The consumption of liquid is V mL；
(4) it is calculated by formula (1) and obtains 1,2- glycol in polyvinyl alcohol and connect the content X, unit % of structure:
In formula:
A is the quality of polyvinyl alcohol, unit g；
B is the purity of polyvinyl alcohol, unit %；
C is the quality of periodate or pure periodic acid, unit g；
D is the molal weight of periodate or pure periodic acid, unit g/mol；
E is the purity of periodate or pure periodic acid, unit %；
88 connect the molal weight of structure for 1,2- glycol in polyvinyl alcohol, unit g/mol；
V is the consumption of hypo solution, unit mL.
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| CN201811500450.1A CN109342650A (en) | 2018-12-10 | 2018-12-10 | 1,2- glycol connects the method for structural content in a kind of measurement polyvinyl alcohol |
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| CN201811500450.1A CN109342650A (en) | 2018-12-10 | 2018-12-10 | 1,2- glycol connects the method for structural content in a kind of measurement polyvinyl alcohol |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1199168A (en) * | 1997-05-13 | 1998-11-18 | 西安市中心血站 | Mannitol content measuring method for mixed preparation of mannitol and glucose |
| CN1869664A (en) * | 2005-05-25 | 2006-11-29 | 中国石油天然气股份有限公司 | Method for testing purity of recovered ethylene glycol |
| CN102441102A (en) * | 2010-10-14 | 2012-05-09 | 天津天士力之骄药业有限公司 | Method for measuring content of oligosaccharide components in medicinal materials |
| CN105300972A (en) * | 2015-10-10 | 2016-02-03 | 煤炭科学技术研究院有限公司 | Determination method of glycol content in phenol and oil-containing complicated system |
-
2018
- 2018-12-10 CN CN201811500450.1A patent/CN109342650A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1199168A (en) * | 1997-05-13 | 1998-11-18 | 西安市中心血站 | Mannitol content measuring method for mixed preparation of mannitol and glucose |
| CN1869664A (en) * | 2005-05-25 | 2006-11-29 | 中国石油天然气股份有限公司 | Method for testing purity of recovered ethylene glycol |
| CN102441102A (en) * | 2010-10-14 | 2012-05-09 | 天津天士力之骄药业有限公司 | Method for measuring content of oligosaccharide components in medicinal materials |
| CN105300972A (en) * | 2015-10-10 | 2016-02-03 | 煤炭科学技术研究院有限公司 | Determination method of glycol content in phenol and oil-containing complicated system |
Non-Patent Citations (3)
| Title |
|---|
| J.欧班斯基 等: ""α-二醇基的测定"", 《合成聚合物与塑料分析手册》 * |
| 张志贤 等: ""邻醇羟基的测定"", 《有机官能团定量分析》 * |
| 顧炎初: "高碘酸应用于有机定量分析的讨论", 《化学世界》 * |
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Application publication date: 20190215 |