CS269567B1 - Method of sulphur determination bound in form of sulphogroups in sulphonated polyphenylenoxide - Google Patents
Method of sulphur determination bound in form of sulphogroups in sulphonated polyphenylenoxide Download PDFInfo
- Publication number
- CS269567B1 CS269567B1 CS878781A CS878187A CS269567B1 CS 269567 B1 CS269567 B1 CS 269567B1 CS 878781 A CS878781 A CS 878781A CS 878187 A CS878187 A CS 878187A CS 269567 B1 CS269567 B1 CS 269567B1
- Authority
- CS
- Czechoslovakia
- Prior art keywords
- sulfur
- sample
- polyphenylene oxide
- analytical
- kbr
- Prior art date
Links
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 7
- 239000005864 Sulphur Substances 0.000 title 1
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 23
- 239000011593 sulfur Substances 0.000 claims abstract description 23
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 14
- 229920006380 polyphenylene oxide Polymers 0.000 claims abstract description 14
- 238000002835 absorbance Methods 0.000 claims abstract description 9
- 238000004458 analytical method Methods 0.000 claims abstract description 7
- 230000003595 spectral effect Effects 0.000 claims abstract description 5
- 238000001228 spectrum Methods 0.000 claims abstract description 5
- 238000005259 measurement Methods 0.000 claims abstract description 3
- 229920000642 polymer Polymers 0.000 claims description 6
- 230000002745 absorbent Effects 0.000 claims description 5
- 239000002250 absorbent Substances 0.000 claims description 5
- 238000002329 infrared spectrum Methods 0.000 claims description 5
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 claims description 5
- 230000033558 biomineral tissue development Effects 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 claims 5
- 238000007796 conventional method Methods 0.000 claims 1
- 239000000843 powder Substances 0.000 claims 1
- 238000009987 spinning Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000003892 spreading Methods 0.000 abstract 1
- 125000001273 sulfonato group Chemical group [O-]S(*)(=O)=O 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229920000930 2, 6-dimethyl-1, 4-phenylene oxide Polymers 0.000 description 1
- GVLZQVREHWQBJN-UHFFFAOYSA-N 3,5-dimethyl-7-oxabicyclo[2.2.1]hepta-1,3,5-triene Chemical compound CC1=C(O2)C(C)=CC2=C1 GVLZQVREHWQBJN-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000004870 electrical engineering Methods 0.000 description 1
- 239000012510 hollow fiber Substances 0.000 description 1
- 238000011089 mechanical engineering Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
Landscapes
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
Riešenie.sa týká spůsobu stanovenia I í síry vo formě sulfoskupin v sulíonovanom · : pólyfenylenoxide meraním transmisných lníra-ϊ ■ červených spektier. Podstata riešenia je me-| ' ranie spektier z KBr tabletiek obsahujúclch : · od 3 do 5 percent hmotnostných vzorky v ob- , ' ! lasti od 4000 do 400 cm ” , pričom sa hodno-· tí integrovaná absorbancia analytických ab- · sorgčných pásov s maximami při 561 a 663 , cm,1 a pásu vnůtorného Standardu pri 1610 · cm" za použitia vztahu hmot S Ai 561 * Ai 663 A CS 26 95 67 B l Ai 1610 kde A| A^ a A^ sú Integrované absorbancie pri vlnočtoch 561, 663 a 1610 cm"1, a empirické konštanty A a 8 sa stanovia vopred kalibráciou spektrálných meraní a analytického spůsobu stanovenia síry. Stanovením síry podía tohoto vynálezu možno · urychlif doteraz používaný analytický spůsob, •na základě' čoho presne kontrolovat technologický postup přípravy zvlákňovacích roztokov sulionovaných polyfenýlenoxiddv. ako ·’ aj kontrolovat kvalituchemického naviazan i a s í ry.The solution relates to the method of determination sulfur in the form of sulphonates in sulononated · polyphenyleneoxide by measuring transmissive ra ■ red spectra. The essence of the solution is | Spreading of spectra from KBr tablets containing: from 3 to 5 percent by weight of the sample in the? between 400 and 400 cm ”, while The integrated absorbance of the analytical bands and strips with peaks at 561 and 663, cm, 1 and the internal Standard band at 1610 · cm " Mass S Ai 561 * Ai 663 AND CS 26 95 67 B l Ai 1610 where A | A 1 and A 4 are Integrated absorbance at wave numbers 561, 663 and 1610 cm -1, and the empirical constants A and 8 are determined pre-calibration of spectral measurements and the analytical method for determining sulfur. By determining the sulfur of the present invention, the analytical method used so far can be accelerated. • based on what exactly control technology a process for preparing spinning solutions sulionated polyphenylene oxide. as · ’ I check qualuchemic bound i and s.
Description
CS 269 567 B1 l·'
Vynález sa týká spflsobu stanovenia síry v sulíonovanom polyf enylenoxddlei μ i rozsahuod 0 do 3 percent hmotnostných síry.
Nesulionovaný polyfenylenoxid / poly/2,6-dimethyl-l,4 phenylenoxid// je polymér s vý-bornými elektrickými, mechanickými, tepelnými a chemickými vlastnostami, ktoré sibuvedenénapr. v encyklopedii /Mark, H. F.: Encyclopedia ot Polymer Science and Technology!, Vol. 10,New York 1969/. Okrem hlavného využitia v elektrotechnike a strojárenstve sa výhodhe pou-žívá na výrobu poréznych membrán pře separačné procesy. Pre přípravu plochých membrána dutých vláken sa 3 výhodou používá polyfenylenoxid modifikovaný sulfuskupinami, ktorýmá vyššiu hydrofilitu a lepšie.separačné vlastnosti.
Sulfonovaný polyfenylenoxid má nasledovná chemická štruktáru
Podlá obsahu síry sa mění poměr medzi natívnymi a sulfonovanými jadrami. Předpokládá sa,že při obsahu síry cca 1,2 percent hmotnostných je nasulionované každé dvadsiate jádro po-lyméru.
Za účelom kontroly obsahu síry v sulíonovanom polyfenylenoxide před přípravou zvlák-óovacich roztokov je potřebné mat k dispozícii vhodnú analytická metodu. V sáčasnosti sapoužívá spčsob stanovenia síry mineralizáciou vzopky v atmosféře kyslíka na platinovomkontakte. Produkty spálenia sa kvantitativné zachytávajá v zriedenom peroxide vodíka podlápostupu vypracovanom vo VÚOS. Stanovenie síry podlá tohoto spósobu je časovo velmi nároč-né vzhladom k pomalej mineralizácii.
Podstata stanovenia síry vo formě sulfoskupin v sulíonovanom polyfenylenoxide podlátohoto vynálezu spočívá v tom, že z práškového polyméru sa připraví KBr tabletka o kon-centrácli od 3 do 5 percent hmotnostných vzorky a zmeria sa transmi3né infračervené spekt-rum v oblasti od 4000 cm-1 do 400 cm-1. V spektre sa hodnotia integrované absorbancie ana-lytických absorpčných pásov síry pri 561 a 663 cm-1 a absorpčného pásu vnútorného Stan-dardu polyfenylenoxidu při 1610 cm"1. Pre stanovenie obsahu síry sa použije vztah
hmot % S
Ai 561 + Ai 663
Ai 1610
v ktorom Ai A^ a A^ θύ integrované absorbancie pásov při vlnočtoch 561, 663 a 1610 cm _1, a empirické konštanty A a B sa vopred stanovia kalibráciou spektrálnýchmeraní a analytického spůsobu stanovenia síry. Výhodou stanovenia síry podlá tohoto vynálezu je značné urýchlenie doteraz používa- ného spůsobu, nakolko doba jednej analýzy nepřekračuje 1 hodinu. To dovoluje kontrolovat kvalitu vstupných surovin sulfonovaných polyfenylenoxldov tesne před přípravou zvlákňova- cích roztokov. Ďalšou výhodou je možnost zaregistrovania aj iných chemických vazieb síry
CS 269 567 B1 l · '
BACKGROUND OF THE INVENTION The present invention relates to a method for determining the sulfur content of a sulphonated polyphenylene oxide admixture from 0 to 3 percent by weight of sulfur.
The non-emulsified polyphenylene oxide / poly / 2,6-dimethyl-1,4-phenylene oxide // is a polymer with excellent electrical, mechanical, thermal and chemical properties, such as those described above. in Encyclopedia / Mark, HF: Encyclopedia ot Polymer Science and Technology !, Vol. 10, New York 1969; In addition to the main applications in electrical and mechanical engineering, the separation process is advantageously used to produce porous membranes. For the preparation of flat membranes of hollow fibers, it is advantageous to use a polyphenylene oxide modified with sulfo groups, which has higher hydrophilicity and better separation properties.
The sulfonated polyphenylene oxide has the following chemical structures
According to the sulfur content, the ratio between native and sulfonated nuclei changes. At a sulfur content of about 1.2 percent by weight, each twenty core polymer is believed to be emulsified.
In order to control the sulfur content of the sulphonated polyphenylene oxide prior to preparing the spinning solutions, a suitable analytical method should be available. In the present time, the method of determination of sulfur is used by mineralization of the flare in an oxygen atmosphere on a platinum contact. Combustion products are quantitatively captured in dilute hydrogen peroxide by a down-stream developed by VÚOS. The sulfur determination according to this method is very time consuming due to slow mineralization.
The essence of the determination of sulfur in the form of sulfo groups in the sulphonated polyphenylene oxide of the present invention is that a KBr tablet having a concentration of from 3 to 5 percent by weight of the sample is prepared from the powdered polymer and the transient infrared spectrum is measured in the range of 4000 cm -1 to 400 cm -1. In the spectrum, the absorbances of the absorbent absorbent bands of sulfur at 561 and 663 cm @ -1 and the absorbent band of the internal standard of polyphenylene oxide at 1610 cm @ -1 are evaluated.
% wt
Ai 561 + A1 663
Ai 1610
in which the A 1 and A 2 ύ integrated absorbances of the bands at wavelengths 561, 663 and 1610 cm -1, and the empirical constants A and B are predetermined by calibration of the spectral measurements and the analytical method for determining sulfur. The advantage of the sulfur determination according to the invention is the considerable acceleration of the method used so far, since the time of one analysis does not exceed 1 hour. This allows the quality of the feedstocks of the sulfonated polyphenylene oxides to be controlled just prior to the preparation of the spinning solutions. Another advantage is the possibility of registering other chemical bonds of sulfur
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS878781A CS269567B1 (en) | 1987-12-03 | 1987-12-03 | Method of sulphur determination bound in form of sulphogroups in sulphonated polyphenylenoxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS878781A CS269567B1 (en) | 1987-12-03 | 1987-12-03 | Method of sulphur determination bound in form of sulphogroups in sulphonated polyphenylenoxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CS878187A1 CS878187A1 (en) | 1989-09-12 |
| CS269567B1 true CS269567B1 (en) | 1990-04-11 |
Family
ID=5438838
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS878781A CS269567B1 (en) | 1987-12-03 | 1987-12-03 | Method of sulphur determination bound in form of sulphogroups in sulphonated polyphenylenoxide |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS269567B1 (en) |
-
1987
- 1987-12-03 CS CS878781A patent/CS269567B1/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| CS878187A1 (en) | 1989-09-12 |
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