CN104678064A - Method for accurately measuring water content of reverse phase emulsion - Google Patents
Method for accurately measuring water content of reverse phase emulsion Download PDFInfo
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- CN104678064A CN104678064A CN201510107341.3A CN201510107341A CN104678064A CN 104678064 A CN104678064 A CN 104678064A CN 201510107341 A CN201510107341 A CN 201510107341A CN 104678064 A CN104678064 A CN 104678064A
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Abstract
The invention discloses a method for accurately measuring the water content of reverse phase emulsion. The method is applicable to testing the emulsion prepared according to a reverse phase emulsion polymerization method. The method provided by the invention integrates an organic solvent dissolution method and a Karl Fischer method; the water content of an organic solvent is tested according to the Karl Fischer method; the water content of the reverse phase emulsion into which the organic solvent is added is reversely deduced. According to the method provided by the invention, the water content of the reverse phase emulsion can be measured accurately and quickly; therefore, a central control method is provided for determining an end point for a concentrating process for preparing the reverse phase emulsion with high solid content.
Description
Technical field
The invention belongs to inverse emulsion polymerization field, be specifically related to accurate method of testing liquid water content in the emulsion obtained by inverse emulsion polymerization method.
Background technology
Inverse emulsion polymerization is one of important method of synthetic polymer, it can obtain the polymkeric substance of high molecular while keeping high reaction rate, reaction system is the dispersed system with aqueous medium, be easy to heat transfer, production safety, environmental pollution is little, obtain product can directly use, but its solid content of reversed-phase emulsion obtained by common inverse emulsion polymerization method is generally difficult to reach more than 50%, but the existence of a large amount of water and oil shows to there is open defect in volume, cost and sometimes added risk and/or toxic action.Present industrial conventional method is light isoparaffins and water decompression azeotropic by adopting 8 to 11 carbon atoms, and remove unnecessary water and oil, the solid content of the emulsion that the method obtains can up to 80%.So a kind of method of liquid water content in Measurement accuracy reversed-phase emulsion, and then provide middle control for the determination of the decompression distillation striking point preparing high solids content reversed-phase emulsion.
Summary of the invention
Technical matters to be solved by this invention is: the method providing liquid water content in a kind of Measurement accuracy reversed-phase emulsion, and then provides midpoint controlling method for the concentration process determination terminal of the reversed-phase emulsion preparing high solids content.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of method of liquid water content in Measurement accuracy reversed-phase emulsion, be applicable to test by the obtained emulsion of inverse emulsion polymerization method, have employed the method that organic solvent dissolution and Karl_Fischer method combine, by with Karl_Fischer method test Water in Organic Solvents content, then instead derive and add the liquid water content of the reversed-phase emulsion of this organic solvent;
Its concrete grammar is as follows: reversed-phase emulsion is placed in the organic solvent that can dissolve each other with water, abundant stirring, the water in reversed-phase emulsion is made to be dissolved in this organic solvent completely, centrifuging, get supernatant liquor, with the liquid water content in Karl_Fischer method test clear liquid, then according to the liquid water content in clear liquid, utilize inversion formula, the anti-liquid water content released in reversed-phase emulsion.
Described reversed-phase emulsion is a small amount of, the organic solvent that can dissolve each other with water is a large amount of, the organic solvent that can dissolve each other with water and the volume ratio of reversed-phase emulsion are 20-50, and the water in the too little polymkeric substance of ratio can not discharge completely, and when ratio is too large, the precision of testing tool may not reach; Concrete proportionate relationship must see that the liquid water content in the test specification of karl Fischer instrument used and emulsion is determined, organic solvent also should be the precipitation agent of polymkeric substance in reversed-phase emulsion in addition, and the water be beneficial to like this inside by reversed-phase emulsion is discharged in organic solvent and goes.
Described inversion formula is:
z＝w(x+y)/x
Wherein: x is the quality of reversed-phase emulsion, y is the quality of the organic solvent that can dissolve each other with water, and w is that z is the liquid water content in reversed-phase emulsion with the liquid water content in Karl_Fischer method test clear liquid.
The invention has the advantages that: the method can measure liquid water content in reversed-phase emulsion accurately and fast, and then provide midpoint controlling method for the concentration process determination terminal of the reversed-phase emulsion preparing high solids content.
Accompanying drawing explanation
Fig. 1 is the comparison diagram adding gauge water and volatile matter increase in reversed-phase emulsion;
Fig. 2 is the TGA figure of reversed-phase emulsion.
Embodiment
In order to preferably understand the present invention, below in conjunction with embodiment, the present invention is further described, but the scope of protection of present invention is not limited to the scope of embodiment statement.
Embodiment 1
Get 0.2g known water content be 10% reversed-phase emulsion karl Fischer moisture tester (K-F method) survey its liquid water content, instrument model is plum Teller V-20, drift value is 20, karl Fischer moisture teller used if not otherwise specified below, be all this kind of, when surveying amount of moisture by K-F method, reversed-phase emulsion produces into bulk, have partial inversion emulsion to wrap test electrode in whipping process, concrete test result is as shown in table 1.
Embodiment 2
Get 0.2g known water content be 10% reversed-phase emulsion halogen flash baking instrument survey its liquid water content, the temperature of setting flash baking instrument is 105 DEG C, and stop when reversed-phase emulsion quality no longer changes, concrete test result is as shown in table 1.
Embodiment 3
Getting three parts of 10g known water content is the reversed-phase emulsion of 10%, add 0.2g respectively, 0.5g, the deionized water of 1g, after stirring, get 0.2g reversed-phase emulsion halogen flash baking instrument respectively and survey its liquid water content, the temperature of setting flash baking instrument is 105 DEG C, stop when reversed-phase emulsion quality no longer changes, in reversed-phase emulsion, volatile matter increases the comparison diagram of percentage and moisture increase percentage as shown in Figure 1, computation process is as follows: it is Y=0.634+0.4046X that Fig. 1 obtains straight-line equation after linear fit, wherein Y is that moisture increases percentage, X is that moisture increases percentage, X is obtained as Y substitution straight-line equation using surveying volatilization score value 13.6 when not adding water in embodiment 2, concrete test result is as shown in table 1.
Embodiment 4
Get 10mg known water content be 10% reversed-phase emulsion thermogravimetry (TGA) survey its liquid water content, test condition is: nitrogen atmosphere, programming rate is 10 degrees/min, reversed-phase emulsion TGA schemes as shown in Figure 2, reversed-phase emulsion mainly contains two endothermic peaks in TGA test as shown in Figure 2, first is 131.3 DEG C, be mainly moisture evaporation, cause the weightlessness of 11.99% massfraction, the decomposition that second is 256.1 DEG C is partial polymer, cause the weightlessness of 55.98% massfraction, in reversed-phase emulsion, the concrete test result of liquid water content is as shown in table 1.
Embodiment 5
Getting 0.2g known water content is that the reversed-phase emulsion Ka Shi stove of 10% and the method for K-F combination survey its liquid water content, and test condition is: 160 DEG C, mixing 900s, and drift 15 stops relatively, and concrete test result is as shown in table 1.
Embodiment 6
Get 0.2g (x) known water content be 10% reversed-phase emulsion add in the organic solvent that 5g (y) and water can dissolve each other, select acetonitrile herein, abundant stirring, the water in reversed-phase emulsion is made to dissolve with this organic solvent completely, centrifugal, get clear liquid, with the liquid water content (w) in Karl_Fischer method test clear liquid, then according to the liquid water content in clear liquid, liquid water content (z) in anti-release reversed-phase emulsion, inversion formula is: z=w (x+y)/concrete test result of x is as shown in table 1.
The each test result statistical form of table 1.
The comparison of 6 kinds of schemes: directly with the liquid water content of K-F method test reversed-phase emulsion, the easy package testing electrode of reversed-phase emulsion, and the moisture in reversed-phase emulsion emulsion particle can not discharge completely, cause the on the low side of test result, and with organic solvent and reversed-phase emulsion mixing, fully stir, centrifugal, then can well solve the problem of simple K-F method test water content with the liquid water content of K-F method survey clear liquid, the test result obtained is also comparatively close to actual value; Flash baking instrument method and TGA method, all exist and steamed by the volatile matter of non-water, causes the problem that test result is higher; Add water anti-pushing manipulation, do not consider " grabbing water " ability of polymkeric substance in reversed-phase emulsion, cause the higher of test result; Purge water vapor with nitrogen in Ka Shi stove and K-F combined techniques process, but all water vapor can not be blown out, cause the less than normal of test result.
Claims (3)
1. the method for liquid water content in a Measurement accuracy reversed-phase emulsion, it is characterized in that: by testing the liquid water content be dissolved into from reversed-phase emulsion in the organic solvent that can dissolve each other with water with Karl_Fischer method, then anti-derivation adds the liquid water content of the reversed-phase emulsion of this organic solvent.
2. the method for liquid water content in a kind of Measurement accuracy reversed-phase emulsion according to claim 1, it is characterized in that: the concrete steps of the method are: reversed-phase emulsion is placed in the organic solvent that can dissolve each other with water, abundant stirring, make the water in reversed-phase emulsion be dissolved in this organic solvent completely, centrifuging, gets supernatant liquor, with the liquid water content in Karl_Fischer method test clear liquid, then according to the liquid water content in clear liquid, inversion formula is utilized, the anti-liquid water content released in reversed-phase emulsion;
Described inversion formula is:
z＝w(x+y)/x
Wherein: x is the quality of reversed-phase emulsion, y is the quality of the organic solvent that can dissolve each other with water, and w is that z is the liquid water content in reversed-phase emulsion with the liquid water content in Karl_Fischer method test clear liquid.
3. the method for liquid water content in a kind of Measurement accuracy reversed-phase emulsion according to claim 1 and 2, is characterized in that: the volume ratio of the described organic solvent that can dissolve each other with water and reversed-phase emulsion is 20-50.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102788864A (en) * | 2012-06-27 | 2012-11-21 | 中国科学院宁波材料技术与工程研究所 | Method for determining moisture content in polyacrylonitrile polymerized liquid |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102788864A (en) * | 2012-06-27 | 2012-11-21 | 中国科学院宁波材料技术与工程研究所 | Method for determining moisture content in polyacrylonitrile polymerized liquid |
Non-Patent Citations (1)
| Title |
|---|
| 李亚波等: "水性涂料、乳液及有机溶剂中水含量测定方法适用范围的探讨", 《现代涂料与涂装》 * |
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Application publication date: 20150603 |