CN100520399C - Fast measuring process of saponfication value of emulsion - Google Patents
Fast measuring process of saponfication value of emulsion Download PDFInfo
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- CN100520399C CN100520399C CNB2006100251607A CN200610025160A CN100520399C CN 100520399 C CN100520399 C CN 100520399C CN B2006100251607 A CNB2006100251607 A CN B2006100251607A CN 200610025160 A CN200610025160 A CN 200610025160A CN 100520399 C CN100520399 C CN 100520399C
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- emulsion
- saponification
- potassium hydroxide
- butanone
- saponification number
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Abstract
The process of measuring saponification value of emulsion fast, simply and accurately includes: the first microwave saponification reaction of emulsion with excessive potassium hydroxide in ethanol and butanone medium, the subsequent automatic electrometric titration with non-aqueous acid and alkali electrode as indication electrode, measuring the oil content in the emulsified liquid and calculating. Compared with available technology, the present invention has the advantages of less steps, lower consumption of organic solvent, shortened analysis period, and accurate and reliable measurement result.
Description
Technical field
The present invention relates to the assay method of emulsion saponification number, emulsion is extracted or extracts and direct rapid assay methods with fixed its saponification number of automatic potential titrator tests more specifically to a kind of need not.
Background technology
Emulsion has good lubricating function for cold rolling, thereby can reduce draught pressure, cuts down the consumption of energy, cooling roll and band steel prevent that roller from splitting and curling round the roll, and emulsion also have good spatter property, guarantee to roll back plate face cleanliness and certain vital role such as operation antirust ability.The height of emulsion saponification number is the important indicator of reaction ROLLING OIL quality quality.Influence the emulsion quality owing to emulsion its saponification number after using a period of time can reduce, therefore produce the saponification number situation that usually needs to analyze emulsion, so that the consumption of decision emulsion when producing how much.The mensuration of saponification number adopts many two kinds of methods that have at present both at home and abroad: volumetric method and infrared spectrophotometer.
Wherein, existing volumetric method has detailed introduction in " assay method of GB8021-87 petroleum products saponification number ", the step of this method is: with emulsion with sodium chloride breakdown of emulsion (promptly oily, moisture from) after, extract oil content with butanone, quantitatively be dissolved in the oil content of extracting in the butanone again, after certain amount of sodium hydroxide-ethanolic solution reflux generation saponification, with the alkali of hydrochloric acid overtitration, by calculating the emulsion saponification number.Afterwards, developed automatic potentiometric titration in this volumetric method again, the final step titration is improved to automatic potentiometric titration by the manual titration, but the loaded down with trivial details emulsion pre-treatment (being initial several steps such as oil and water separation) of this method still can't be saved.
The publication number that the OMODAKA KATAUJI of Japan and TANASE NORIKO are called " mensuration of oil saponification value, acid number and fatty acid iron " in the name of on November 25th, 1992 application is that the patent of JP06102177A has just been announced a kind of method of utilizing infrared spectrophotometer to measure the emulsion saponification number.This method is: at first emulsion is carried out breakdown of emulsion (i.e. oil, moisture from), with the oil content in the emulsion with phenixin or the extraction of methenyl choloride equal solvent after, with this sample sample groove of packing into, measure 2750-3100cm with infrared spectrophotometer
-1With 1670-1800cm
-1The area ratio or the ratio of peak of near the extinction spectrum the wave number are by calculating oil saponification value.Chinese patent open (bulletin) number: the denomination of invention that CN 1204055 announces is that " assay method of emulsion saponification number and hetero oil content " also discloses similar method, be that the oil that will extract from emulsion is coated on certain window materials, measure its 1745-1720cm
-1The feature absorbance and the 1465 ± 20cm of carbonyl near the wave number
-1The feature absorbance of hydrocarbon calculates emulsion saponification number and hetero oil content near the wave number.
Above method all is just can measure after with the oil content in various means extractions or the leaching emulsion, the process more complicated of extraction or leaching oil content, loaded down with trivial details, need to consume a large amount of chemical reagent and organic solvent, and the time that consumes is also longer, only be that oil and water separation and two steps of extraction oil content all will spend at least two hours time, had a strong impact on the efficient of soap value test.
Summary of the invention
Therefore, the purpose of this invention is to provide a kind of fast, the simple and measurement result detection method of emulsion saponification number accurately, to overcome above-mentioned deficiency, the use amount of also having saved organic solvent greatly simultaneously.
For achieving the above object, the invention provides a kind of rapid assay methods of emulsion saponification number, the invention core of this method is: with emulsion directly and the excessive hydrogen kali microwave saponification takes place in ethanol and butanone medium, be indicator electrode with non-water soda acid electrode then, carry out automatic potentiometric titration, record the oil content content of this emulsion simultaneously with solid part instrument or Moisture Meter, by calculating the saponification number that can record this emulsion.
According to an aspect of the present invention, a kind of rapid assay methods of emulsion saponification number, its step specifically comprises: 1. the oil content content of accurately measuring emulsion with solid part instrument or Moisture Meter; 2. quantitatively take by weighing emulsion to the sealable tank of microwave reactor, add the butanone solvent of equivalent, add excessive potassium hydroxide-ethanolic solution again; 3. opening microwave reactor makes saponification complete; 4. be indicator electrode to reaction mixture with non-water soda acid electrode, carry out automatic potentiometric titration; 5. the emulsion saponification number calculates according to following formula that (unit is mg; Potassium hydroxide/g): emulsion saponification number=[volume (the ml) * concentration of potassium hydroxide (mol/l) of the potassium hydroxide that the molecular weight of potassium hydroxide (56.1g/mol) * saponification consumes]/[emulsion sampling amount (g) * emulsion oil content content (%)].
Preferable, in above-mentioned steps 2, the ratio of the sampling gram number of the adding of butanone gram number and emulsion can be controlled in: emulsion: butanone=1:0.8～1.2.
Better, in above-mentioned steps 3, the opening program of microwave reactor can so be controlled: heating earlier 3～5 minutes, heated again 2～3 minutes after static 1～2 minute.
Compared with prior art, beneficial effect of the present invention have following some:
1. because the present invention directly carries out determination test with emulsion as sample, prior art then all is to test as sample with the oil content in the emulsion.Therefore, the present invention has saved the necessary breakdown of emulsion step of prior art and extraction subsequently or stripping step, simultaneously also just needn't to prior art will extract like that or the oil content of stripping in extraction solvent volatilize and just can obtain can continuing to test the oil content of usefulness after complete.Therefore, the present invention has omitted this pre-treatment process to the emulsion oil content fully, emulsion directly can be carried out saponification without any processing, and operation is oversimplified more.
2. the consumption of the organic solvent that uses in the process of the test of the present invention is very little, generally measure a sample and use butanone to be 10ml, and therefore prior art uses the amount of organic solvents such as butanone bigger owing to will extract or the processing of stripping oil content.
3. the present invention is applied to microwave reaction the saponification of emulsion, utilize the non-of microwave reaction to thermal effect, realized in water-organic solvent mixes mutually, carrying out saponification fast, shortened the time of saponification greatly, also improved the efficient of saponification.
In a word, the present invention compared with prior art, omitted determination step greatly, shortened analysis time (the whole mensuration process of the present invention only needs half an hour), practical, and measurement result (can guarantee that saponification reacts completely at short notice, guarantee the error at measurment that measurement result can not exclusively not cause because of saponification accurately and reliably; Reduce artificial error at measurment by reducing determination step; And, eliminated the manual titration) because the error that indicator brings by adopting the nonaqueous phase automatic potentiometric titration.
Embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment one: a kind of assay method of cold rolling unit emulsion saponification number, and its concrete operations step is as follows:
One, prepares reagent and instrument
Hydrochloric acid (analyzing pure); Butanone (analyzing pure); Ethanol (analyzing pure); Potassium hydroxide (analyzing pure); Gu part instrument (solid part of at present commercially available instrument all can satisfy accuracy must reach 0.001% and above requirement); Microwave reactor; Automatical potentiometric titrimeter.
Two, sample is handled
Accurately take by weighing emulsion 10g to microwave sample jar, add 10ml potassium hydroxide/alcohol mixed solution (wherein concentration of potassium hydroxide is formulated as identical with the concentration of used hydrochloric acid) and 10ml butanone as reaction medium, carry out the microwave saponification with the instrument working routine that configures in microwave reactor, specifically: the microwave reaction program is 550W (4 minutes)-0W (1 minute)-550W (2 minutes).
Three, sample is measured
1, the mensuration of concentration of emulsion used
Pipette the about 5g of emulsion, accurately measure the concentration of oil in the emulsion with solid part instrument.
2, the mensuration of emulsion saponification number
Will be through the sample of microwave saponification, under well-beaten situation, (the instrument condition of work of automatical potentiometric titrimeter comprises: the titration end-point control mode under the selected instrument condition of work using on the automatical potentiometric titrimeter, the titration end-point judgment mode, the condition that titration end-point criterion etc. can be set in automatical potentiometric titrimeter), with non-water soda acid electrode is indicator electrode, carries out automatic potentiometric titration with the hydrochloric acid of known accurate concentration.Hydrochloric acid content that titration is consumed and concentration of emulsion used can directly obtain the emulsion saponification number by the calculating of following formula:
Emulsion saponification number=[volume (the ml) * concentration of potassium hydroxide (mol/l) of the potassium hydroxide that the molecular weight of potassium hydroxide (56.1g/mol) * saponification consumes]/[emulsion sampling amount (g) * emulsion oil content content (%)].
Embodiment two: a kind of assay method of five frame connection rolling machine group emulsion saponification number, and its concrete operations step is as follows:
One, prepares reagent and instrument
Hydrochloric acid (analyzing pure); Butanone (analyzing pure); Ethanol (analyzing pure); Potassium hydroxide (analyzing pure); Gu part instrument (solid part of at present commercially available instrument all can satisfy accuracy must reach 0.001% and above requirement); Microwave reactor; Automatical potentiometric titrimeter.
Two, sample is handled
Accurately take by weighing emulsion 10g to microwave sample jar, add 8ml potassium hydroxide/alcohol mixed solution and 8ml butanone as reaction medium, carry out the microwave saponification with the instrument working routine that configures in microwave reactor, concrete operations are: the microwave reaction program is 550W (5 minutes)-0W (2 minutes)-550W (2 minutes).
Three, sample is measured
1, the mensuration of concentration of emulsion used
Pipette the about 10g of emulsion, accurately measure the concentration of oil in the emulsion with solid part instrument.
2, the mensuration of emulsion saponification number
Will be through the sample of microwave saponification, under well-beaten situation, on the automatical potentiometric titrimeter with selected instrument condition of work under, be indicator electrode with non-water soda acid electrode, carry out automatic potentiometric titration with the hydrochloric acid of known accurate concentration.Hydrochloric acid content that titration is consumed and concentration of emulsion used can directly obtain the emulsion saponification number by the calculating of following formula:
Emulsion saponification number=[volume (the ml) * concentration of potassium hydroxide (mol/l) of the potassium hydroxide that the molecular weight of potassium hydroxide (56.1g/mol) * saponification consumes]/[emulsion sampling amount (g) * emulsion oil content content (%)].
Embodiment three: a kind of assay method of cold rolling unit emulsion saponification number, and its concrete operations step is as follows:
One, prepares reagent and instrument
Hydrochloric acid (analyzing pure); Butanone (analyzing pure); Ethanol (analyzing pure); Potassium hydroxide (analyzing pure); Gu part instrument (solid part of at present commercially available instrument all can satisfy accuracy must reach 0.001% and above requirement); Microwave reactor; Automatical potentiometric titrimeter.
Two, sample is handled
Accurately take by weighing emulsion 10g to microwave sample jar, add 12ml potassium hydroxide/alcohol mixed solution and 12ml butanone, in microwave reactor, carry out the microwave saponification with the instrument working routine that configures as reaction medium.Specifically: the microwave reaction program is 550W (3 minutes)-0W (1 minute)-550W (3 minutes).
Three, sample is measured
1, the mensuration of concentration of emulsion used
Pipette the about 5g of emulsion, accurately measure the concentration of oil in the emulsion with solid part instrument.
2, the mensuration of emulsion saponification number
Will be through the sample of microwave saponification, under well-beaten situation, on the automatical potentiometric titrimeter with selected instrument condition of work under, be indicator electrode with non-water soda acid electrode, carry out automatic potentiometric titration with the hydrochloric acid of known accurate concentration.Hydrochloric acid content that titration is consumed and concentration of emulsion used can directly obtain the emulsion saponification number by the calculating of following formula:
Emulsion saponification number=[volume (the ml) * concentration of potassium hydroxide (mol/l) of the potassium hydroxide that the molecular weight of potassium hydroxide (56.1g/mol) * saponification consumes]/[emulsion sampling amount (g) * emulsion oil content content (%)].
Need to prove, add an amount of butanone solvent and be because saponification of the present invention is to carry out in oil water mixture, therefore need to add an amount of butanone as reaction medium so that saponification carry out more smoothly.In the microwave saponification, the setting of microwave reaction program is suitable, and microwave reaction can rapid reaction be finished, and prevents again owing to react that the sealable tank internal pressure is excessive, and explosion takes place.Non-water soda acid electrode can improve the precision that automatic potentiometric titration is measured, this is because this acid base neutralization titration occurs in the mixed solution of water one butanone, ethanol, therefore the response speed of general soda acid electrode and the selectivity of electrode all have certain influence to measurement result, therefore use non-water soda acid electrode can obtain more accurate test findings.
Claims (2)
1. the rapid assay methods of an emulsion saponification number, with emulsion directly and the excessive hydrogen kali microwave saponification takes place in ethanol and butanone medium, be indicator electrode with non-water soda acid electrode then, carry out automatic potentiometric titration, record the oil content content of this emulsion simultaneously with solid part instrument or Moisture Meter, by calculating the saponification number that can record this emulsion.
2. the rapid assay methods of a kind of emulsion saponification number according to claim 1 comprises the steps:
1) use solid part instrument or Moisture Meter accurately to measure the oil content content of emulsion;
2) quantitatively take by weighing emulsion to the sealable tank of microwave reactor, add excessive potassium hydroxide-ethanolic solution, add butanone solvent again with potassium hydroxide-ethanolic solution equal volume amounts;
3) opening microwave reactor makes saponification complete;
4) reaction mixture is an indicator electrode with non-water soda acid electrode, carries out automatic potentiometric titration;
5) the emulsion saponification number calculates according to following formula, and unit is mg potassium hydroxide/g: emulsion saponification number=(the volume ml * concentration of potassium hydroxide mol/l of the potassium hydroxide that the molecular weight 56.1g/mol of potassium hydroxide * saponification consumes)/(emulsion sampling amount g * emulsion oil content content %).3. the rapid assay methods of a kind of emulsion saponification number according to claim 1 comprises the steps:
1) use solid part instrument or Moisture Meter accurately to measure the oil content content of emulsion;
2) quantitatively take by weighing emulsion to the sealable tank of microwave reactor, add excessive potassium hydroxide-ethanolic solution, add butanone solvent again,
The ratio of the gram number of gram number that butanone adds and emulsion sampling is controlled at: emulsion: butanone=1:0.8～1.2;
3) opening microwave reactor makes saponification complete;
4) reaction mixture is an indicator electrode with non-water soda acid electrode, carries out automatic potentiometric titration;
5) the emulsion saponification number calculates according to following formula, and unit is mg potassium hydroxide/g: emulsion saponification number=(the volume ml * concentration of potassium hydroxide mol/l of the potassium hydroxide that the molecular weight 56.1g/mol of potassium hydroxide * saponification consumes)/(emulsion sampling amount g * emulsion oil content content %).4. according to the rapid assay methods of claim 2 or 3 described a kind of emulsion saponification numbers, it is characterized in that, in above-mentioned steps 3) in, the opening program of microwave reactor is: heating earlier 3～5 minutes, heated again 2～3 minutes after static 1～2 minute.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100251607A CN100520399C (en) | 2006-03-28 | 2006-03-28 | Fast measuring process of saponfication value of emulsion |
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| CNB2006100251607A CN100520399C (en) | 2006-03-28 | 2006-03-28 | Fast measuring process of saponfication value of emulsion |
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| CN100520399C true CN100520399C (en) | 2009-07-29 |
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| CN112697784A (en) * | 2020-12-14 | 2021-04-23 | 山东一诺威新材料有限公司 | Method for measuring grease content in polyether polyol |
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Non-Patent Citations (4)
| Title |
|---|
| 油脂皂化值、酸值等在油脂化工中的应用. 邢长洪.泸天化科技，第4期. 2000 |
| 油脂皂化值、酸值等在油脂化工中的应用. 邢长洪.泸天化科技，第4期. 2000 * |
| 电导滴定法测定深色油脂皂化值的研究. 王怀智等.粮食科技与经济，第1期. 2001 |
| 电导滴定法测定深色油脂皂化值的研究. 王怀智等.粮食科技与经济，第1期. 2001 * |
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