CN109387600A - The measurement method of effective component in a kind of α olefin sulfonate product - Google Patents
The measurement method of effective component in a kind of α olefin sulfonate product Download PDFInfo
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- CN109387600A CN109387600A CN201811282876.4A CN201811282876A CN109387600A CN 109387600 A CN109387600 A CN 109387600A CN 201811282876 A CN201811282876 A CN 201811282876A CN 109387600 A CN109387600 A CN 109387600A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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Abstract
The measurement method of effective component in a kind of α olefin sulfonate product provided by the invention, comprising the following steps: weigh m grams of α olefin sulfonate product in beaker, distilled water is added and stirs to get test fluid；The quality for the phenolphthalein reagent that 1 drop mass fraction of test is 1% is a grams；N drop phenolphthalein reagent is added dropwise；The buret equipped with hydrochloric acid solution is taken to be titrated, the volume Vml of hydrochloric acid is added dropwise in record；250ml volumetric flask is taken, is weighed, quality is p grams, and liquid is transferred in 250ml volumetric flask, and volatile alcohol organic matters are added；250ml volumetric flask is placed in Rotary Evaporators, is dried；It takes out 250ml volumetric flask to be weighed, quality is q grams；Active constituent content γ=(q-p-0.0585V-0.01an)/m can be calculated according to formula.Measurement method of the invention carries out acid base titration test first with phenolphthalein reagent, and the content of sodium hydroxide, then carries out rotary evaporation test again in test product, and easy to operate for excluding interference of the sodium hydroxide to measurement result, accuracy of measurement is high.
Description
Technical field
The present invention relates to technical field of surfactant, and in particular to effective component in a kind of α olefin sulfonate product
Measurement method.
Background technique
α olefin sulfonate is a kind of white to yellow powder, and main component is that alkene shines base sulfonate, and a small amount of
Two xanthates etc..Biological degradability is good, and irritation is low, hypotoxicity.It is mainly made of sulfonation neutralisation, is surfactant,
It is mainly used as the detergent of foam class skin care item, is particularly suitable for manufacture acidic foam, strong detergency, foam is steady in the presence of grease
It is fixed, it is small to skin and eye irritation.
The sulfonating reaction as involved in the production technology of α olefin sulfonate, use oleum, sulfur trioxide etc. as
Sulfonating agent remains sulfonating agent in product in order to prevent, is generally needed to be added excessive sodium hydroxide as neutralization reagent, hydroxide
Sodium excessively will affect the measurement of effective component in α olefin sulfonate, therefore, in order to improve accuracy of measurement, need to exclude hydrogen-oxygen
Change the interference of sodium.
Summary of the invention
In view of the above problems, the present invention provides a kind of measurement method of effective component in α olefin sulfonate product, measurement
Accuracy is high.
To achieve the above object, the present invention solves by the following technical programs:
The measurement method of effective component in a kind of α olefin sulfonate product, comprising the following steps:
S1 weighs m grams of α olefin sulfonate product in 50ml beaker, stirs evenly after a small amount of distilled water is added, until completely molten
Solution, obtains test fluid；
The quality for the phenolphthalein reagent that 1 drop mass fraction of S2 test is 1% is a grams；
Test fluid is transferred in 50ml volumetric flask by S3, and 1% phenolphthalein reagent of n drop is added dropwise into test fluid, and n is more than or equal to 1
Integer, test fluid become red, and distilled water then is added into 50ml volumetric flask until water level reaches 1/5 position of graduation mark；
S4 takes the acid burette equipped with 1mol/l hydrochloric acid solution to be titrated, until the color of test fluid is become by red suddenly
Colourless, the volume Vml of hydrochloric acid is added dropwise in record；
S5 takes 250ml volumetric flask, weighs, and recording its quality is p grams, and the liquid in 50ml volumetric flask is fully transferred to 250ml
In volumetric flask, volatile alcohol organic matters are added, until liquid level reaches 1/3 position of 250ml volumetric flask graduation mark；
250ml volumetric flask is placed in Rotary Evaporators by S6, temperature is 50~60 DEG C, revolving speed is 30~40rpm condition backspin
Turn 15~30min of evaporation, until drying completely；
It after S7 is cooling, takes out 250ml volumetric flask and is weighed, recording its quality is q grams；
S8 can calculate active constituent content γ=(q-p-0.0585V-0.01an)/m according to formula.
Specifically, the α olefin sulfonate product is α-sodium olefin sulfonate product, α-olefin sulfonic acid potassium product, α-alkenyl
One of sulfonic acid calcium product, α-olefin sulfonic acid magnesium products.
Specifically, the pH value of the α olefin sulfonate product is greater than 7.
Specifically, n is equal to 2 in the step S3,2 1% phenolphthalein reagents of drop are added.
Specifically, the volatile alcohol organic matters are selected from ethyl alcohol, normal propyl alcohol, isobutanol, n-butanol, 2-methyl-1-butene
At least one of alcohol, isoamyl alcohol.
Specifically, the ratio of distilled water and volatile alcohol organic matters is 1:10 in 250ml volumetric flask in the step S5
~20.
The beneficial effects of the present invention are:
The first, the measurement method of effective component, carries out first with phenolphthalein reagent in α olefin sulfonate product provided by the invention
Acid base titration is tested, and the content of sodium hydroxide, then carries out rotary evaporation test, for excluding sodium hydroxide again in test product
Interference to measurement result, easy to operate, accuracy of measurement is high；
The second, traditional acid base titration test is individually carried out with rotary evaporation test, double sampling is needed, due to adopting twice
Sample is required to weigh, and can generate large error when weighing twice, individually be tested without same sample, due to stirring unequal original
The component content of cause, two groups of samples is different, is equally unfavorable for improving measurement accuracy, measurement method of the invention uses same survey
Two tests can be completed in test solution, easy to operate, and measurement accuracy is high.
Specific embodiment
In order to further appreciate that feature of the invention, technological means and specific purposes achieved, function, tie below
Closing specific embodiment, the present invention is described in further detail.
Embodiment 1
The measurement method of effective component in a kind of α-sodium olefin sulfonate product, comprising the following steps:
S1 weighs α-sodium olefin sulfonate product of 5 grams of pH values greater than 7 in 50ml beaker, stirs after a small amount of distilled water is added
It is even, until being completely dissolved, obtain test fluid；
The quality for the phenolphthalein reagent that 1 drop mass fraction of S2 test is 1% is 0.05 gram；
Test fluid is transferred in 50ml volumetric flask by S3, and 2 1% phenolphthalein reagents of drop are added dropwise into test fluid, since test fluid is in alkali
Property, phenolphthalein reagent chance alkali becomes red, distilled water then is added into 50ml volumetric flask until water level reaches 1/5 of graduation mark
It sets；
S4 takes the acid burette equipped with 1mol/l hydrochloric acid solution to be titrated, hydrochloric acid solution with it is residual in α-sodium olefin sulfonate product
Neutralization reaction occurs for the sodium hydroxide stayed, and when sodium hydroxide is reacted completely, until hydrochloric acid is gradually added dropwise, making test fluid is in acid
Property, the sour color of phenolphthalein reagent chance becomes colourless by red, records the volume 14ml that hydrochloric acid is added dropwise；
S5 takes 250ml volumetric flask, weighs, and recording its quality is 270 grams, and the liquid in 50ml volumetric flask is fully transferred to
In 250ml volumetric flask, ethyl alcohol is added, until liquid level reaches 1/3 position of 250ml volumetric flask graduation mark, at this time 250ml volumetric flask
The ratio of middle distilled water and volatile alcohol organic matters is 1:15；
250ml volumetric flask is placed in Rotary Evaporators by S6, rotary evaporation under the conditions of temperature is 60 DEG C, revolving speed is 35rpm
20min, until drying completely, second alcohol and water is vapored away during rotary evaporation, there is residual 250ml volumetric flask interior bottom portion after drying
Object is stayed, residue is effective component, the quality of sodium chloride and phenolphthalein；
It after S7 is cooling, takes out 250ml volumetric flask and is weighed, recording its quality is 274.8 grams；
S8 can calculate active constituent content γ=(274.8-270-0.0585 × 14-0.01 × 0.05 × 2)/5 according to formula
=79.6%.
Computing Principle in step S8 are as follows: the γ=(gross mass -250ml of 250ml volumetric flask and residue after rotary evaporation
After quality-acid base titration of volumetric flask in test fluid sodium chloride quality-addition phenolphthalein reagent quality)/sampling quality.
1 kind of embodiment of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but not
Limitations on the scope of the patent of the present invention therefore can be interpreted as.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (6)
1. the measurement method of effective component in a kind of α olefin sulfonate product, which comprises the following steps:
S1 weighs m grams of α olefin sulfonate product in 50ml beaker, stirs evenly after a small amount of distilled water is added, until completely molten
Solution, obtains test fluid；
The quality for the phenolphthalein reagent that 1 drop mass fraction of S2 test is 1% is a grams；
Test fluid is transferred in 50ml volumetric flask by S3, and 1% phenolphthalein reagent of n drop is added dropwise into test fluid, and n is more than or equal to 1
Integer, test fluid become red, and distilled water then is added into 50ml volumetric flask until water level reaches 1/5 position of graduation mark；
S4 takes the acid burette equipped with 1mol/l hydrochloric acid solution to be titrated, until the color of test fluid is become by red suddenly
Colourless, the volume Vml of hydrochloric acid is added dropwise in record；
S5 takes 250ml volumetric flask, weighs, and recording its quality is p grams, and the liquid in 50ml volumetric flask is fully transferred to 250ml
In volumetric flask, volatile alcohol organic matters are added, until liquid level reaches 1/3 position of 250ml volumetric flask graduation mark；
250ml volumetric flask is placed in Rotary Evaporators by S6, temperature is 50~60 DEG C, revolving speed is 30~40rpm condition backspin
Turn 15~30min of evaporation, until drying completely；
It after S7 is cooling, takes out 250ml volumetric flask and is weighed, recording its quality is q grams；
S8 can calculate active constituent content γ=(q-p-0.0585V-0.01an)/m according to formula.
2. the measurement method of effective component in a kind of α olefin sulfonate product according to claim 1, which is characterized in that
The α olefin sulfonate product is α-sodium olefin sulfonate product, α-olefin sulfonic acid potassium product, α-olefin sulfonic acid calcium product, α-alkene
One of base sulfonic acid magnesium products.
3. the measurement method of effective component in a kind of α olefin sulfonate product according to claim 1, which is characterized in that
The pH value of the α olefin sulfonate product is greater than 7.
4. the measurement method of effective component in a kind of α olefin sulfonate product according to claim 1, which is characterized in that
N is equal to 2 in the step S3, and 2 1% phenolphthalein reagents of drop are added.
5. the measurement method of effective component in a kind of α olefin sulfonate product according to claim 1, which is characterized in that
The volatile alcohol organic matters in ethyl alcohol, normal propyl alcohol, isobutanol, n-butanol, 2-methyl-1-butene alcohol, isoamyl alcohol extremely
Few one kind.
6. the measurement method of effective component in a kind of α olefin sulfonate product according to claim 1, which is characterized in that
The ratio of distilled water and volatile alcohol organic matters is 1:10~20 in 250ml volumetric flask in the step S5.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000128854A (en) * | 1998-10-23 | 2000-05-09 | Toagosei Co Ltd | Production of acrylamidoalkanesulfonic acid salt |
| CN1327979A (en) * | 2001-06-27 | 2001-12-26 | 秦立君 | Process for preparing petroleum sulfonate used in oil field |
| CN1800159A (en) * | 2004-12-30 | 2006-07-12 | 中国科学院理化技术研究所 | Narrow distillate alpha-olefin derived alkylbenzene sulfonate and its synthesis method and uses |
| CN101693678A (en) * | 2009-10-27 | 2010-04-14 | 南京工业大学 | Process for preparing alpha-sulfo fatty acid methyl ester sodium salt |
| CN102304069A (en) * | 2011-06-23 | 2012-01-04 | 东北石油大学 | Method for synthesizing saturated cardanol sulfonate surfactant for oil displacement |
| CN103265460A (en) * | 2013-06-13 | 2013-08-28 | 杨锌荣 | Alkyl diphenyl ether sulfonate and preparation method thereof |
| CN104829498A (en) * | 2015-03-16 | 2015-08-12 | 福建泰丰医药化工有限公司 | Preparation method of cocounut oil acyl-oxygen ethyl sulfonate |
-
2018
- 2018-10-31 CN CN201811282876.4A patent/CN109387600A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000128854A (en) * | 1998-10-23 | 2000-05-09 | Toagosei Co Ltd | Production of acrylamidoalkanesulfonic acid salt |
| CN1327979A (en) * | 2001-06-27 | 2001-12-26 | 秦立君 | Process for preparing petroleum sulfonate used in oil field |
| CN1800159A (en) * | 2004-12-30 | 2006-07-12 | 中国科学院理化技术研究所 | Narrow distillate alpha-olefin derived alkylbenzene sulfonate and its synthesis method and uses |
| CN101693678A (en) * | 2009-10-27 | 2010-04-14 | 南京工业大学 | Process for preparing alpha-sulfo fatty acid methyl ester sodium salt |
| CN102304069A (en) * | 2011-06-23 | 2012-01-04 | 东北石油大学 | Method for synthesizing saturated cardanol sulfonate surfactant for oil displacement |
| CN103265460A (en) * | 2013-06-13 | 2013-08-28 | 杨锌荣 | Alkyl diphenyl ether sulfonate and preparation method thereof |
| CN104829498A (en) * | 2015-03-16 | 2015-08-12 | 福建泰丰医药化工有限公司 | Preparation method of cocounut oil acyl-oxygen ethyl sulfonate |
Non-Patent Citations (1)
| Title |
|---|
| 张澄清等: "《石油和石油产品标准》", 31 December 1964 * |
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