CN102590011A - Measuring method for monitoring content of siloxane in hydrochloride during organosilicone production process - Google Patents
Measuring method for monitoring content of siloxane in hydrochloride during organosilicone production process Download PDFInfo
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- CN102590011A CN102590011A CN2011103752232A CN201110375223A CN102590011A CN 102590011 A CN102590011 A CN 102590011A CN 2011103752232 A CN2011103752232 A CN 2011103752232A CN 201110375223 A CN201110375223 A CN 201110375223A CN 102590011 A CN102590011 A CN 102590011A
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Abstract
The invention provides a measuring method for monitoring the content of siloxane in hydrochloride acid during the organosilicone production process, and aims to provide a method which is simple to operate, is convenient and fast, and can accurately acquire the data about the content of siloxane in hydrochloride acid. The measuring method is realized through the technical scheme as follows: taking a clean reagent bottle, sampling from a production line a liquid phase sample with the sample amount between 100g and 1000g, and recording the total weight m2 of the sample and the reagent bottle; after taking back the sample, adding siloxane-soluble extraction agent 10 ml to 200 ml into a ventilation cabinet, oscillating violently for 5 min to 60 min, and weighing a constant weight beaker; taking lower level oil phase from a dryer into the beaker, placing oil phase in a water bath for evaporating to dryness, transferring oil phase into an oven under constant temperature at least for 1 hour and taking out oil phase, and then cooling oil phase in the dryer to the room temperature; and quantitatively calculating the content X of siloxane in the hydrochloride acid. The measuring method solves the problem that siloxane is separated out from the hydrochloride acid and accumulates to block the production device.
Description
Technical field
The invention relates to the assay method of hydrochloric acid content of siloxane in organic silicon production process.Especially relate to method through content of siloxane in the hydrochloric acid in the liquid-phase extraction analysis organic silicon production process.
Background technology
Organosilicon product is one of most widely used kind in the world.Can be divided into four big types by its grown form, that is: 1. silane (comprising downstream product silane coupling agent and silica-basedization reagent); 2. silicone oil; 3. silicon rubber; 4. silicones.Back three series products are the polymerizable organosilicon product, that is downstream product, and not only the kind trade mark is numerous for the latter, but also can further be processed into seriation, differentiated product and the goods of different shape, performance and purposes.
The organic silicon monomer and the downstream product organo-silicon compound of exploitation are divided into two big types usually at present, and one type is organosilyl low molecular compound, i.e. silane monomer and derivant thereof; Second type is the organosilicon macromolecule compound, comprises siloxane intermedium and polysiloxane product (like silicone oil, silicon rubber and silicones etc.).
Prior art is in organic silicon production process; Generally put in what system as raw material whom reacts the generation siloxane with concentrated hydrochloric acid, watery hydrochloric acid or water; After organic chlorosilane is processed siloxane intermedium (for D4 or DMC etc.); Chlorine is that by-product generates hydrochloric acid, in the hydrochloric acid that obtains, brings a small amount of siloxane inevitably into, makes and is dissolved with a spot of siloxane in the hydrochloric acid.The siloxane that generates belongs to two different phases with hydrochloric acid or water.Two out of phase siloxane and hydrochloric acid, in process of production, because the Long contact time of siloxane and hydrochloric acid; And under conditions such as high temperature, can generate a type polysiloxane by polymerization reaction take place; Type polysiloxane can be separated out from concentrated hydrochloric acid, is accumulated in the process units block system and influence carrying out smoothly that serialization produces; Therefore; Be necessary in process of production the content of siloxane of hydrochloric acid in the system is monitored, content of siloxane provides analytical approach in the monitoring hydrochloric acid, to guarantee the continuity of production run.And also do not see at present the relevant bibliographical information of the appropriate method of content of siloxane in the hydrochloric acid of can accurately analyzing in the production run.
Summary of the invention
Task of the present invention provides a kind of simple to operate, and is convenient and swift, can accurately obtain the method for content of siloxane data in the hydrochloric acid, with hydrochloric acid content of siloxane in the monitoring organic silicon production process, for the continuity of organosilicon production provides accurate instruction.
Above-mentioned purpose of the present invention can reach through following measure, and a kind of assay method of monitoring hydrochloric acid content of siloxane in the organic silicon production process is characterized in that may further comprise the steps; Get clean reagent bottle, weigh, be designated as m
1, on production line, get the liquid phase sample of sampling amount, the gross weight m of record sample and bottle at 100g-1000g
2After sample is fetched, in vent cabinet, add the extractant 10ml-200ml that is prone to dissolve siloxane, concuss 5min-60min; Fully wash out the oil in the hydrochloric acid, then the liquid in the reagent bottle all is transferred in the separating funnel static layering 5min-60min; Weighing is the beaker of constant weight, is designated as m
3Taking out separating funnel lower floor oil phase to beaker, oil phase is placed the water-bath evaporate to dryness, and beaker is transferred in the baking oven, is constant temperature 1h taking-up at least in 30 ℃-150 ℃ at oven temperature, in exsiccator, is cooled to room temperature again, and constant weight is designated as m
4Go out content of siloxane X in the hydrochloric acid with following formula quantitative Analysis:
The present invention has following beneficial effect.
The present invention utilizes siloxane to be soluble in the characteristic of some solvent; Isolate the siloxane in the hydrochloric acid through solvent-extracted method; Again siloxane in the organic phase is carried out quantitative test, thereby obtain content of siloxane in the hydrochloric acid, accurately obtain content of siloxane data in the hydrochloric acid; Realization is set up the analytical approach that siloxane in the concentrated hydrochloric acid is analyzed in extraction to the monitoring of concentrated hydrochloric acid content of siloxane in production or the scientific research process.Provide accurate instruction organosilyl continuity production through analysis, can from hydrochloric acid, separate out to solve siloxane, the problem of process units is stopped up in accumulation.Whole mensuration process operation is simple, convenient and swift, accurate, has stronger practicality.
Embodiment
In following examples, get clean brown narrow mouth reagent bottle, weigh, be designated as m
1, be accurate to 0.01g; Sample is taken in the reagent bottle, and sampling amount writes down the gross weight m of sample and bottle at 100-1000g
2, be accurate to 0.01g; In vent cabinet, add extractant 10-200ml after sample is fetched immediately, concuss 5-60min all is transferred to the liquid in the reagent bottle in the separating funnel static layering 5-60min fully to wash out the oil in the acid.Weighing is the beaker of constant weight, is designated as m
3, be accurate to 0.0001g; Taking out separating funnel lower floor oil phase to beaker, oil phase is placed the water-bath evaporate to dryness, and beaker is transferred to baking oven, is constant temperature 1h taking-up at least in 30 ℃-180 ℃ at oven temperature, in exsiccator, is cooled to room temperature, and constant weight is designated as m
4, be accurate to 0.0001g,
Content of siloxane X is in the hydrochloric acid so:
The separating effect of the siloxane effect of extracting of concentrated hydrochloric acid, extractant is relevant in measuring accuracy of the present invention and the analytic process.
Effect of extracting is bad, the content of siloxane that impact analysis obtains.And effect of extracting is relevant with sampling amount, extractant kind, extractant and inorganic phase ratio and extraction time in the analytic process.Experimental result shows that the extraction phase of extractant can comprise, sherwood oil (boiling range: 30-180 ℃), White Mineral Oil, benzene and derivant thereof, alkyl hydro carbons (C
x, x>=6), a kind of in the alkyl alcohols, siloxane, halogenated hydrocarbons.Preferred a kind of in sherwood oil (boiling range: 60-150 ℃), normal hexane, methenyl choloride, the phenixin.Extractant and inorganic ratio≤1: 1 mutually, preferred≤1: 5.Extraction time >=5min.
The extractant separating effect is relevant with selection of Extractant and oven temperature.Experiment shows that consistent at other analysis condition, under the extractant various conditions, the result who obtains has than big difference.Reason is that different extractant boiling points are different, causes in the siloxane residual extraction dosage different.In addition, the definite of oven temperature also has influence on precision of analysis, and be under condition of different temperatures, different with a kind of volatile grade of solvent.When temperature rises to one regularly, the lower boiling material of a small amount of short chain or ring-type is dried by the fire in the siloxane, same impact analysis result.Oven temperature is 30 ℃-150 ℃, preferred 90 ℃-120 ℃.
Under the same conditions, on production line, get respectively two groups totally 12 samples analyze content of siloxane in the hydrochloric acid, content of siloxane is identical in every group of sample, can obtain following parallel experiment data:
| ? | One group | Two groups |
| 1# | 0.0728 | 0.1708 |
| 2# | 0.0726 | 0.1699 |
[0018]
| 3# | 0.0731 | 0.1685 |
| 4# | 0.0753 | 0.1746 |
| 5# | 0.0740 | 0.1666 |
| 6# | 0.0750 | 0.1684 |
| Average | 0.0738 | 0.1698 |
Can find out that through above analysis result the relative error number percent of this method all about 1%, can be satisfied the demand, instruct and produce.
Claims (6)
1. an assay method of monitoring hydrochloric acid content of siloxane in the organic silicon production process is characterized in that may further comprise the steps; Get clean reagent bottle, weigh, be designated as m
1, on production line, get the liquid phase sample of sampling amount, the gross weight m of record sample and bottle at 100g-1000g
2After sample is fetched, in vent cabinet, add the extractant 10ml-200ml that is prone to dissolve siloxane, concuss 5min-60min; Fully wash out the oil in the hydrochloric acid, then the liquid in the reagent bottle all is transferred in the separating funnel static layering 5min-60min; Weighing is the beaker of constant weight, is designated as m
3Taking out separating funnel lower floor oil phase to beaker, oil phase is placed the water-bath evaporate to dryness, and beaker is transferred in the baking oven, is constant temperature 1h taking-up at least in 30 ℃-150 ℃ at oven temperature, in exsiccator, is cooled to room temperature again, and constant weight is designated as m
4Go out content of siloxane X in the hydrochloric acid with following formula quantitative Analysis:
2. the assay method of hydrochloric acid content of siloxane is characterized in that in the monitoring organic silicon production process as claimed in claim 1, and the extraction phase of described extractant can comprise, sherwood oil, White Mineral Oil, benzene and derivant thereof, alkyl hydro carbons (C
x, x>=6), alkyl alcohols, siloxane, halogenated hydrocarbons a kind of.
3. the assay method of hydrochloric acid content of siloxane is characterized in that in the monitoring organic silicon production process as claimed in claim 1, and described extractant is that boiling range is a kind of in 60-150 ℃ the sherwood oil, normal hexane, methenyl choloride, phenixin.
4. the assay method of hydrochloric acid content of siloxane is characterized in that in the monitoring organic silicon production process as claimed in claim 1, extractant and inorganic ratio≤1: 1 mutually, or≤1: 5.
5. the assay method of hydrochloric acid content of siloxane is characterized in that in the monitoring organic silicon production process as claimed in claim 1, extraction time >=5min.
6. the assay method of hydrochloric acid content of siloxane is characterized in that in the monitoring organic silicon production process as claimed in claim 1, and oven temperature is 90 ℃-120 ℃.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105547903A (en) * | 2015-12-14 | 2016-05-04 | 北方华锦化学工业集团有限公司 | Method for determining solid content of ABS by continuous bulk polymerization process |
| CN108982717A (en) * | 2018-07-23 | 2018-12-11 | 湖北兴瑞硅材料有限公司 | The detection method of content of siloxane in a kind of organosilicon slag inclusion waste water |
| CN112198078A (en) * | 2020-11-13 | 2021-01-08 | 中纺检测（福建）有限公司 | Method for measuring siloxane content in shoe material wear-resistant agent |
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| CN1663662A (en) * | 2004-12-24 | 2005-09-07 | 清华大学 | Hanging drop type liquid-liquid micro-extraction method |
| CN101343037A (en) * | 2007-07-10 | 2009-01-14 | 中国石油天然气股份有限公司 | Method for removing micro siloxane in hydrochloric acid hydrolyzation in organosilicon preparation |
| CN101975828A (en) * | 2010-09-25 | 2011-02-16 | 嘉兴学院 | Method for detecting residual dimethyl cyclosiloxane in water body |
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| CN1663662A (en) * | 2004-12-24 | 2005-09-07 | 清华大学 | Hanging drop type liquid-liquid micro-extraction method |
| CN101343037A (en) * | 2007-07-10 | 2009-01-14 | 中国石油天然气股份有限公司 | Method for removing micro siloxane in hydrochloric acid hydrolyzation in organosilicon preparation |
| CN101975828A (en) * | 2010-09-25 | 2011-02-16 | 嘉兴学院 | Method for detecting residual dimethyl cyclosiloxane in water body |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105547903A (en) * | 2015-12-14 | 2016-05-04 | 北方华锦化学工业集团有限公司 | Method for determining solid content of ABS by continuous bulk polymerization process |
| CN105547903B (en) * | 2015-12-14 | 2018-10-02 | 北方华锦化学工业股份有限公司 | A kind of assay method of substance law ABS solid contents |
| CN108982717A (en) * | 2018-07-23 | 2018-12-11 | 湖北兴瑞硅材料有限公司 | The detection method of content of siloxane in a kind of organosilicon slag inclusion waste water |
| CN112198078A (en) * | 2020-11-13 | 2021-01-08 | 中纺检测（福建）有限公司 | Method for measuring siloxane content in shoe material wear-resistant agent |
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Application publication date: 20120718 |