CN1815190A - Method for determining styrene micro-emulsion polymerization conversion rate by ultraviolet spectrometry - Google Patents
Method for determining styrene micro-emulsion polymerization conversion rate by ultraviolet spectrometry Download PDFInfo
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- CN1815190A CN1815190A CN 200610038457 CN200610038457A CN1815190A CN 1815190 A CN1815190 A CN 1815190A CN 200610038457 CN200610038457 CN 200610038457 CN 200610038457 A CN200610038457 A CN 200610038457A CN 1815190 A CN1815190 A CN 1815190A
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- styrene
- cinnamic
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- emulsion polymerization
- conversion rate
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Abstract
Said invention discloses ultraviolet spectrometry determining styrene micro emulsion liquid conversion rate method in order to composing styrene, 1-pentanol, SDS and H2 O reaction system. Said cinnamic initial concentration C0 is 0.4 mol L<-1>-1.2mol L<-1>,Polymerization temperature as 20-60 degree centigrade, sampling in plurality of time quantum in process of ultrasound trigering micro emulsion liquid polyreaction, to proceed precipitation pretreatment using 95 per cent ethanol as precipitant, then taking supernatant, using 95 per cent ethanol dilution Cinnamic concentration as 9 X10<-6> mol L<-1>-7X10<-5> mol L<-1>, adopting ultraviolet spectrophotometer determining said rare faction cinnamic absorbance in 200 nm-300 nm position, through absorbance-styrene concentration relationship chart and extension rate calculating polymeric system styrene concentration C, according to x = c 0- 0- c ) / c 0 ] * 100 % calculating cinnamic conversion rate. Said invented method is simple, easy operation, and high sensitivity.
Description
Technical field
The present invention relates to measure the method for styrene micro-emulsion polymerization conversion rate, particularly measure the correlation technique of concentration of styrene with ultraviolet spectroscopy.
Background technology
The polymerization of polystyrene has a lot, and micro-emulsion polymerization is a kind of polymerization wherein.Microemulsion is appearance transparent, thermodynamically stable oil-aqueous dispersion, and it is the polymerization of preparation small particle diameter, narrow distribution polymerization composition granule as a kind of narrow distribution, the thermodynamic stable system of particle diameter between 10～100nm.The reaction velocity of micro-emulsion polymerization is fast, and easily heat radiation can be reacted and reacting balance at low temperatures, does not have the constant speed phase, plurality of advantages such as having the gel-free effect, need not to stir, polyplant is simple, processing ease, particulate are controlled.
Polystyrene microemulsion particle size is a nanoscale, and surface tension is very low, has good penetration, wetting state, levelability, rheological and film forming, the density height, and glossiness is good.The polystyrene microemulsion can infiltrate and have in atomic thin bump maps line, the fine capillary channel and the unusual complicated matrix surface of geometric configuration, can be used for the primary coat of the good stock of absorbabilities such as fabric, woodenware, paper, building stones, concrete and pours into coating etc.The shape that is processed into the bump maps line for needs is complex surfaces extremely; still can wetting well, abundant adhesion; so the polystyrene microemulsion not only is used for top finishing, also can be used for aspects such as printing-ink, tackifier, pad-ink, the transparency protected varnish in metal surface.
The conversion ratio of measuring the styrene micro-emulsion polymerization reaction is one of major issue that must solve in the Development and Production polystyrene microemulsion.The assay method of present cinnamic conversion ratio, both at home and abroad the more of usefulness is gravimetric method, operations such as this method need be washed, filtered, drying, in these operating process, can bring the loss of polymerizate, accuracy is relatively poor, especially when conversion ratio hour, cinnamic conversion ratio in the more difficult accurate mensuration micro-emulsion polymerization process.
Summary of the invention
The objective of the invention is at above the deficiencies in the prior art, provide that a kind of method is simple, accuracy is high, the method for easy-operating determining styrene micro-emulsion polymerization conversion rate by ultraviolet spectrometry.
Technical scheme of the present invention is: the method for determining styrene micro-emulsion polymerization conversion rate by ultraviolet spectrometry is characterized in that to consist of the reaction system of styrene, n-amyl alcohol, SDS and water, cinnamic initial concentration C
0Be 0.4molL
-1～1.2molL
-1Polymerization temperature is 20 ℃～60 ℃, a plurality of time period samplings in ultrasonic initiation styrene micro-emulsion polymerization course of reaction, and the ethanol with 95% is that precipitation agent precipitates pre-service, getting supernatant liquor then, is 9 * 10 with 95% ethanol dilution to cinnamic concentration again
-6MolL
-1～7 * 10
-5MolL
-1In, adopt ultraviolet spectrophotometer to measure this dilution in 200nm～cinnamic absorbance in 300nm place, calculate concentration of styrene C in the polymerization system by absorbance-concentration of styrene graph of a relation and extension rate, press
Formula calculates cinnamic conversion ratio.
Described micro-emulsion polymerization system is made up of styrene, n-amyl alcohol, SDS and water.The detection wavelength of described ultraviolet spectrophotometry is 245nm-250nm.
Section of the present invention emulates the advanced, and method is simple, operation easily, and instrument and equipment is popularized, the accuracy height.Concentration of styrene is 9 * 10
-6MolL
-1～7 * 10
-5MolL
-1The time, absorbance and concentration of styrene are linear relationship, are used for the mensuration of micro-emulsion polymerization process concentration of styrene and conversion ratio.Help researching and developing applying of production polystyrene microemulsion and polystyrene microemulsion.
Description of drawings
Fig. 1 is the graph of a relation of absorbance (ABS) and concentration of styrene;
Embodiment
In the ultrasonic initiation styrene micro-emulsion polymerization course of reaction,, add a certain amount of 95% precipitation with alcohol and isolate polymkeric substance, get supernatant liquor then, and be about 9 * 10 with 95% ethanol dilution to cinnamic concentration at different time sampling 1ml
-6MolL
-1～7 * 10
-5MolL
-1In, from this diluted sample, take a sample then, measure the absorbance of this diluted sample at the 247nm place, calculate cinnamic concentration C, calculate cinnamic conversion ratio X by following formula.
Cinnamic conversion ratio
In the formula: C
0Be cinnamic initial concentration, C is a cinnamic concentration under a certain reaction time, and X is cinnamic conversion ratio.
Embodiment one:
Consist of the system of 3.8ml styrene, 3.4ml n-amyl alcohol, 3.5gSDS, 70.0ml water, in ultrasonic frequency is that 19.6kHz, power are 180W, 30 ℃ were reacted 90 minutes down, sampling 1ml, add 95% ethanol 100ml precipitate and separate polymkeric substance, and then get supernatant liquor 1ml, with 50 times of 95% ethanol dilutions, recording the absorbance of this dilute sample at the 247nm place with ultraviolet spectrophotometer is 0.5640.Check in by accompanying drawing (Fig. 1) that cinnamic concentration is 3.94 * 10 in this dilute sample
-5MolL
-1, promptly cinnamic concentration is 0.197molL in the reaction system
-1, can get cinnamic conversion ratio by following formula calculating is 53.7%.
Embodiment two:
Consist of the system of 4.0ml styrene, 3.5ml n-amyl alcohol, 4.0gSDS, 72.5ml water, in ultrasonic frequency is that 19.6kHz, power are 180W, 40 ℃ were reacted 60 minutes down, sampling 1ml, add 95% ethanol 100ml precipitate and separate polymkeric substance, and then get supernatant liquor 1ml, with 50 times of 95% ethanol dilutions, recording the absorbance of this dilute sample at the 247nm place with ultraviolet spectrophotometer is 0.4629.Check in by accompanying drawing (Fig. 1) that cinnamic concentration is 3.25 * 10 in this dilute sample
-5MolL
-1, promptly cinnamic concentration is 0.163molL in the reaction system
-1, can get cinnamic conversion ratio by following formula calculating is 62.7%.
Claims (2)
1, a kind of method of determining styrene micro-emulsion polymerization conversion rate by ultraviolet spectrometry is characterized in that to consist of styrene, n-amyl alcohol, SDS and H
2The reaction system of O, cinnamic initial concentration C
0Be 0.4molL
-1～1.2molL
-1Polymerization temperature is 20 ℃～60 ℃, and a plurality of time period samplings in ultrasonic initiation styrene micro-emulsion polymerization course of reaction are that precipitation agent precipitates pre-service with 95% ethanol, getting supernatant liquor then, is 9 * 10 with 95% ethanol dilution to cinnamic concentration again
-6MolL
-1～7 * 10
-5MolL
-1In, adopt ultraviolet spectrophotometer to measure this dilution in 200nm～cinnamic absorbance in 300nm place, calculate concentration of styrene C in the polymerization system by absorbance-concentration of styrene graph of a relation and extension rate, press
Formula calculates cinnamic conversion ratio.
2, the method for determining styrene micro-emulsion polymerization conversion rate by ultraviolet spectrometry according to claim 1, the ultraviolet detection wavelength that it is characterized in that described ultraviolet spectrophotometer is 245-250nm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100384577A CN100427925C (en) | 2006-02-20 | 2006-02-20 | Method for determining styrene micro-emulsion polymerization conversion rate by ultraviolet spectrometry |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100384577A CN100427925C (en) | 2006-02-20 | 2006-02-20 | Method for determining styrene micro-emulsion polymerization conversion rate by ultraviolet spectrometry |
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| Publication Number | Publication Date |
|---|---|
| CN1815190A true CN1815190A (en) | 2006-08-09 |
| CN100427925C CN100427925C (en) | 2008-10-22 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100543456C (en) * | 2007-07-19 | 2009-09-23 | 广州天赐高新材料股份有限公司 | A kind of lithium bis (oxalato) borate content ultraviolet spectrophotometry |
| CN102768263A (en) * | 2012-07-23 | 2012-11-07 | 江苏长乐纤维科技有限公司 | Method for measuring concentration of pentaerythritol solution in polyester production |
| CN111879809A (en) * | 2020-06-10 | 2020-11-03 | 中国原子能科学研究院 | Method for measuring and calculating dilution times of reaction liquid in research of crystal nucleation rate |
| CN114813603A (en) * | 2022-03-09 | 2022-07-29 | 南京林业大学 | Method for rapidly representing halogenation conversion rate of phenolic hydroxyl compounds without standard substance |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1434284A (en) * | 2003-02-26 | 2003-08-06 | 华中科技大学 | Spectrum identifying resin microball capable of self-coding |
| JP2005189062A (en) * | 2003-12-25 | 2005-07-14 | Fuji Photo Film Co Ltd | Biosensor |
| CN100340853C (en) * | 2004-03-04 | 2007-10-03 | 华中科技大学 | Method for raising correctness of resin microspheric spectrum coding |
-
2006
- 2006-02-20 CN CNB2006100384577A patent/CN100427925C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100543456C (en) * | 2007-07-19 | 2009-09-23 | 广州天赐高新材料股份有限公司 | A kind of lithium bis (oxalato) borate content ultraviolet spectrophotometry |
| CN102768263A (en) * | 2012-07-23 | 2012-11-07 | 江苏长乐纤维科技有限公司 | Method for measuring concentration of pentaerythritol solution in polyester production |
| CN102768263B (en) * | 2012-07-23 | 2015-08-12 | 江苏长乐纤维科技有限公司 | The assay method of pentaerythrite solution concentration in a kind of production of polyester |
| CN111879809A (en) * | 2020-06-10 | 2020-11-03 | 中国原子能科学研究院 | Method for measuring and calculating dilution times of reaction liquid in research of crystal nucleation rate |
| CN114813603A (en) * | 2022-03-09 | 2022-07-29 | 南京林业大学 | Method for rapidly representing halogenation conversion rate of phenolic hydroxyl compounds without standard substance |
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| Publication number | Publication date |
|---|---|
| CN100427925C (en) | 2008-10-22 |
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Granted publication date: 20081022 Termination date: 20110220 |