CN104829498B - A kind of preparation method of cocos nucifera oil acyloxyethyl sulfonate - Google Patents
A kind of preparation method of cocos nucifera oil acyloxyethyl sulfonate Download PDFInfo
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Abstract
The invention discloses a kind of cocos nucifera oil acyloxyethyl sulfonate product and preparation method thereof, it is characterised in that the method includes: by cocos nucifera oil acid esters, hydroxyethylsulfonic acid., the mixing of optional solvent, be heated to reflux, stirring reaction；The lower distillation of stirring removes the liquid in reaction system；Under stirring, reaction system is lowered the temperature, add alkali regulation pH value；Reaction system is lowered the temperature, separates out solid and be described cocos nucifera oil acyloxyethyl sulfonate；The preparation method desired reaction temperature of the cocos nucifera oil acyloxyethyl sulfonate that the present invention provides is low, response speed is fast, energy consumption is low, react more complete, the cocos nucifera oil acyloxyethyl sulfonate product prepared according to the method for the invention is color properties good, and the content of wherein cocos nucifera oil acyloxyethyl sulfonate is high, and the content of free fatty is low, product quality is high, is widely used.
Description
Technical field
The present invention relates to the synthesis technique of the anion surfactant of fatty acid derived,
It is specifically related to the preparation method of a kind of cocos nucifera oil acyloxyethyl sulfonate.
Background technology
Surfactant refers to have fixing hydrophilic and oleophilic group, on the surface of solution
Can align, and the material that surface tension is remarkably decreased can be made, be typically parent
Water and the organic amphiprotic molecule of hydrophobic group, dissolve in organic solution and aqueous solution；Parent
Water base group is usually carboxyl, sulfonic group, amino, hydroxyl and salt isopolarity group thereof,
Hydrophobic group is usually the non-polar groups such as chain hydrocarbon；Based on its construction features, live in surface
Property agent have moistening, emulsifying, bubble, wash, the several functions such as surface modification, make
Extensively apply, such as individual in detergents and cosmetic and other multiple industry for performance additive
And family's washing product production, metal process, industry cleaning link, oil exploitation, pesticide
Produce etc..
Fat acyl-oxygen ethyl sulfonate is a kind of conventional surfactant, and its chemistry is logical
Formula is RCOOCH2CH2SO3M, wherein R be carbon number be the alkyl of 9～17, M
For Na, NH4Deng monovalent cation, at present use cheap, be easy to get, reproducible
Natural oil is raw material preparation fat acyl-oxygen ethyl sulfonate.
Oleum Cocois is a kind of natural oil extracting from Cortex cocois radicis and obtaining, and its hydrolysis obtains
Coconut oil be the mixture containing multiple fatty acid, coconut oil be widely used in preparation
Kinds of surface activating agent, the anion surfactant cocos nucifera oil acyl that wherein coconut oil is derivative
Oxygen ethyl sulfonate has that resistance to hard water is strong, pH stability high, good moldability and life
The multiple superperformances such as thing degradability is good, are particularly well-suited to the formula for a product such as soaps.
In prior art the preparation of cocos nucifera oil acyloxyethyl sulfonate mainly use coconut oil with
Isethionate is raw material, adds suitable catalyst, under the conditions of heating under reduced pressure
Carrying out, its defect is that coconut oil can not be miscible with isethionate, reacts for biphase
Reaction, it is impossible to carrying out completely, conversion ratio is below 80%, does not participates in reaction in product
Free fatty impurity content high；Response time is long, usually more than 24 hours；Instead
Answer temperature high, generally 180～250 DEG C；Anion active material cocos nucifera oil acyl in product
The content of oxygen ethyl sulfonate is low, and generally less than 80%；Product color is poor, face
Color depth, for dark-brown or black.
Above-mentioned condition based on prior art, the present inventor is to cocos nucifera oil acyloxyethyl sulfonic acid
The synthesis technique of salt is studied, it is therefore an objective to offer one is easy and simple to handle, reaction is complete,
Reaction rate is fast, temperature is low, activity substance content is high in product, impurity content is low,
The preparation method of the cocos nucifera oil acyloxyethyl sulfonate that product color is good.
Summary of the invention
In order to overcome the problems referred to above, the present inventor's system to cocos nucifera oil acyloxyethyl sulfonate
Preparation Method has carried out studying with keen determination, found that: by selecting suitable reaction raw materials
And control suitable reaction condition and operating procedure, it is possible at a lower temperature easy,
Preparing cocos nucifera oil acyloxyethyl sulfonate rapidly, reaction is carried out completely and product color
Property good, in product, cocos nucifera oil acyloxyethyl sulfonate content is high, and free fatty acid content is low.
It is an object of the invention to provide following aspect:
(1) preparation method of a kind of cocos nucifera oil acyloxyethyl sulfonate, it is characterised in that
The method includes:
Step 1), by cocos nucifera oil acid esters, hydroxyethylsulfonic acid., the mixing of optional solvent, add
Hot reflux, stirring reaction；
Step 2), the lower distillation of stirring removes step 1) described in liquid in reaction system；
Step 3), by step 2 under stirring) described in reaction system cooling, add alkali adjust
Joint pH value；
Step 4), by step 3) described in reaction system cooling, separate out solid be institute
State cocos nucifera oil acyloxyethyl sulfonate.
(2) a kind of cocos nucifera oil acyloxyethyl sulfonate product, it is characterised in that described product
Product use the preparation method of the cocos nucifera oil acyloxyethyl sulfonate as described in above-mentioned (1) to prepare
Form.
The present invention described in detail below.
According to the present invention, it is provided that the preparation method of a kind of cocos nucifera oil acyloxyethyl sulfonate,
The method comprises the following steps:
Step 1), by cocos nucifera oil acid esters, hydroxyethylsulfonic acid., the mixing of optional solvent, add
Hot reflux, stirring reaction.
In a preferred embodiment in accordance with the present invention, cocos nucifera oil acid esters and ethoxy are used
Sulfonic acid is that cocos nucifera oil acyloxyethyl sulfonate prepared by raw material, and raw material is miscible, for single-phase instead
Should, reaction temperature is low, and response speed is fast, and reaction is completely.
In a preferred embodiment in accordance with the present invention, step 1) described in cocos nucifera oil acid esters
The Ester formed with alcohols for coconut oil, preferably coconut acid methylester, coconut oil second
Ester or coconut oil propyl ester.Described coconut oil is the natural oil Cortex cocois radicis extracted from Cortex cocois radicis
Oil through hydrolysis obtain or synthetic, for mixture containing multiple fatty acid,
The anion surfactant cocos nucifera oil acyloxyethyl sulfonate derived by coconut oil extensively should
For preparing multiple product.Raw material is easy to get, low price.Cocos nucifera oil acid esters and ethoxy
The most lower boiling methanol of by-product, ethanol or the propanol that sulfonic acid reaction generates, can be
It is distilled off under lower temperature, promotes that forward reaction is carried out so that react more complete.
In a preferred embodiment in accordance with the present invention, step 1) described in solvent permissible
Being alcohols solvent, preferably methanol, ethanol or propanol, to cocos nucifera oil acid esters and ethoxy
The dissolubility of sulfonic acid is all preferable, and low price, and boiling point is low, it is easy to be distilled off,
To improve the concentration of raw material in reaction system, accelerate reaction rate.
In a preferred embodiment in accordance with the present invention, step 1) in when described coconut oil
When ester is coconut acid methylester, described solvent is preferably ethanol or propanol；When described cocos nucifera oil
When acid esters is coconut oil ethyl ester, described solvent is preferably methanol or propanol；When described coconut palm
When oleate is coconut oil propyl ester, described solvent is preferably methanol or ethanol so that anti-
The by-product alcohol that should generate is different from the solvent in reaction system, the existence of solvent not shadow
Ring reaction forward to carry out.
In a preferred embodiment in accordance with the present invention, step 1) described in react and also may be used
To carry out in the case of solvent-free.Owing to cocos nucifera oil acid esters and hydroxyethylsulfonic acid. are miscible,
And be also beneficial to reaction forward in the absence of solvent and carry out, reaction carries out process
The alcohols material of middle generation serves as solvent to a certain extent also can promote reaction further.
In a preferred embodiment in accordance with the present invention, step 1) described in cocos nucifera oil acid esters
It is 1.05:1～1.2:1 with the mol ratio of hydroxyethylsulfonic acid., cocos nucifera oil acid esters excess so that hydroxyl
Ethylsulfonic acid fully reacts；Described hydroxyethylsulfonic acid. with the mol ratio of solvent is
1:1.6～1:3.5 so that cocos nucifera oil acid esters and hydroxyethylsulfonic acid. preferably dissolve, and concentration
Higher, improve reaction rate.
In a preferred embodiment in accordance with the present invention, step 1) described in be heated to reflux
Temperature is 70～130 DEG C, preferably 80～125 DEG C, more preferably 110～120 DEG C, makes
Must react and carry out with faster rate, reduce under high temperature unsaturated group in cocos nucifera oil acid esters simultaneously
Group is oxidized and causes impurity in product to increase and deepens with product colour.
In a preferred embodiment in accordance with the present invention, step 1) described in stirring reaction
Time is 0.5～5 hour, preferably 1～4.5 hour, more preferably 2～4 hours, at this
In the section time, reaction is carried out with faster rate, after such time, along with reactant
In system, reactant concentration is gradually lowered, and production concentration gradually rises, and by-product alcohol is to instead
The inhibitory action answering forward to carry out is gradually obvious, and reaction rate slows down gradually.
Step 2), the lower distillation of stirring removes step 1) described in liquid in reaction system.
In a preferred embodiment in accordance with the present invention, step 2) described in vapo(u)rizing temperature
Higher than solvent and the boiling point of by-product alcohol, it is 70～130 DEG C, preferably 80～125 DEG C,
More preferably 110～120 DEG C, to remove the by-product alcohol in reaction system, promote reaction
Forward is carried out, and reaction is more complete, removes the solvent in reaction system simultaneously, increases
Reactant concentration, improves reaction rate.
In a preferred embodiment in accordance with the present invention, step 2) described in distillation time
It is 1～6 hour, preferably 2～5 hours, more preferably 3～4 hours, is ensureing reaction
Solvent and by-product alcohol are completely removed the most simultaneously.Therefore distillation proceeds to
Till no liquid steams.
Step 3), by step 2 under stirring) described in reaction system cooling, add alkali adjust
Joint pH value.
In a preferred embodiment in accordance with the present invention, step 3) described in alkali can be
Conventional inorganic base, for example, alkali metal or alkaline earth metal hydroxide, carbonate or
Bicarbonate, for example, sodium hydroxide, sodium carbonate, sodium bicarbonate, potassium hydroxide,
Potassium carbonate, potassium bicarbonate, it is also possible to be ammonia or ammonia, preferably sodium hydroxide,
Sodium carbonate or sodium bicarbonate, for and step 2) in the cocos nucifera oil acyloxyethyl sulfonic acid that obtains
Reaction generates cocos nucifera oil acyloxyethyl sulfonate, low price, and does not introduce other impact
The impurity of product quality.
In a preferred embodiment in accordance with the present invention, step 3) in by described reactant
System is cooled to 70～85 DEG C, stopped reaction, and to maintain reaction system be liquid, it is simple to
Cocos nucifera oil acyloxyethyl sulfonic acid and alkali reaction.
In a preferred embodiment in accordance with the present invention, step 3) middle addition alkali regulation pH
Value to faintly acid, such as regulation pH value to less than 7, preferably regulation pH value to 5～6.5,
Thus by step 2) in the cocos nucifera oil acyloxyethyl sulfonic acid that obtains be completely converted into cocos nucifera oil acyl-oxygen
Ethyl sulfonate.
Step 4), by step 3) described in reaction system cooling, separate out solid be institute
State cocos nucifera oil acyloxyethyl sulfonate.
In a preferred embodiment in accordance with the present invention, step 4) described in cocos nucifera oil acyl-oxygen
Ethyl sulfonate is sodium coconut acyloxyethanesulfonate, cocos nucifera oil acyloxyethyl potassium sulfonate or coconut palm
Oleoyl oxygen ethylsulfonic acid ammonia, preferably sodium coconut acyloxyethanesulfonate, according to step 3)
The different alkali of middle selection obtains different cocos nucifera oil acyloxyethyl sulfonate, wherein cocos nucifera oil acyl
Oxygen ethylsulfonic acid sodium is the most commonly used, and production cost is low.
In a preferred embodiment in accordance with the present invention, in step 3) after stop stirring,
In step 4) in described reaction system is cooled to 22～28 DEG C so that cocos nucifera oil acyl-oxygen second
The cooling of base sulfonate separates out, and i.e. obtains described product, simplifies post-processing operation.
In a preferred embodiment in accordance with the present invention, step 1), step 2), step 3)
With step 4) described in reaction all decompression distillation reactor in carry out, it is simple to reacting
During control temperature remove solvent and by-product alcohol, promote that reaction forward is carried out,
Improve reaction rate.
According to the present invention, it is provided that a kind of cocos nucifera oil acyloxyethyl sulfonate product, its feature
Being, described product uses the preparation method of above-mentioned cocos nucifera oil acyloxyethyl sulfonate to prepare
Form.
In a preferred embodiment in accordance with the present invention, described cocos nucifera oil acyloxyethyl sulfonic acid
The colourity of product salt be not more than 30 black once, preferably no greater than 25 black once, the most not quite
In 20 black once, color properties good, of light color, for faint yellow, be widely used, the suitableeest
The manufacturing for domestic chemical products such as liquid detergent, soaps etc..
In a preferred embodiment in accordance with the present invention, at described cocos nucifera oil acyloxyethyl sulphur
In hydrochlorate product, the mass fraction of anion active material cocos nucifera oil acyloxyethyl sulfonate is not
Less than 95%, the cocos nucifera oil acyloxyethyl sulphur prepared far above other method in prior art
Hydrochlorate product, quality is higher, better quality.
In a preferred embodiment in accordance with the present invention, at described cocos nucifera oil acyloxyethyl sulphur
In hydrochlorate product, the mass fraction of impurity free fatty acid is not more than 0.6%, the most not quite
In 0.55%, more preferably no more than 0.5%, impurity content is low, and product quality is high.
The present invention is had the advantage that to include:
(1) preparation method of the cocos nucifera oil acyloxyethyl sulfonate that the present invention provides is with cocos nucifera oil
Acid esters and hydroxyethylsulfonic acid. are raw material, use two-step method to prepare cocos nucifera oil acyloxyethyl sulfonic acid
Salt, the most first prepares cocos nucifera oil acyloxyethyl sulfonic acid, then obtains described cocos nucifera oil acyl with alkali reaction
Oxygen ethyl sulfonate, reaction raw materials is miscible, for homogeneous reaction, desired reaction temperature
Low, energy consumption is low, and reaction is more complete；
(2) preparation method of the cocos nucifera oil acyloxyethyl sulfonate that the present invention provides is in reaction
When proceeding to a certain degree, distillation removes the by-product alcohol in reaction system, promotes reaction
Forward is carried out so that react more complete；
(3) preparation method of the cocos nucifera oil acyloxyethyl sulfonate that the present invention provides is in reaction
When proceeding to a certain degree, distillation removes the solvent in reaction system, increases reactant dense
Degree, thus improve reaction rate；
(4) anti-needed for the preparation method of the cocos nucifera oil acyloxyethyl sulfonate that the present invention provides
Answering temperature low, the time is short, and under minimizing high temperature, in cocos nucifera oil acid esters, unsaturated group is oxidized
And cause impurity in product to increase with product colour and deepen so that the quality of product is higher；
(5) the cocos nucifera oil acyloxyethyl sulfonate product that the present invention provides is color properties good, and
In product, the content of cocos nucifera oil acyloxyethyl sulfonate is high, and the content of free fatty is low,
Good product quality, is widely used.
Detailed description of the invention
Below by experimental example and embodiment, the present invention is described in more detail.Pass through
These explanations, the features and advantages of the invention will become more apparent from clearly.
Experimental example
The colourity inspection of experimental example 1 product
Platinum-cobalt colorimetry
(1) preparation standard colorimetric mother solution (500 black Zeng Danwei)
Accurately weigh 1.000g cobalt chloride hexahydrate and 1.245g potassium chloroplatinate in beaker
In, after water dissolution, move in 1000mL volumetric flask, add 100mL hydrochloric acid,
It is diluted with water to scale, shakes up, obtain standard colorimetric mother solution.
(2) preparation standard platinum-cobalt comparative solution
In the two pool-size bottles of 10 500mL and 14 250mL, it is separately added into table
The standard colorimetric mother solution of volume shown in 1, is diluted with water to scale, shakes up, obtain standard
Platinum-cobalt comparative solution.
The formula of table 1. standard platinum-cobalt comparative solution and colourity
(3) colourity of product is measured
Cocos nucifera oil acyloxyethyl prepared by the present invention is injected in a 100mL color comparison tube
Sodium sulfonate product, fills to groove；In the 100mL color comparison tube that another is identical
Inject the standard platinum-cobalt comparative solution with color similar with the said goods, fill to quarter
At line.The color of comparative product and standard platinum-cobalt comparative solution, during colorimetric at daylight or
Just to white background under daylight lamp irradiation, observe from top to bottom, it is to avoid side is observed,
Determine immediate color.
(4) expression of measurement result
The color of product with the standard platinum-cobalt comparative solution closest to product black once
(platinum-cobalt) color unit represents.Color and any standard platinum-cobalt pair such as fruit product
More inconsistent than solution, then according to estimating a close platinum-cobalt colourity, and retouch
State the color observed.
The Content Test of anion active material in experimental example 2 product
Methylene blue indicator method
(1) preparation lauryl sulfate sodium standard solution
It is about the moon of 0.004mol/L with reference to method compound concentration described in GB 5173-l985
It is also demarcated by osmanthus base sodium sulfate standard solution, is calculated its actual concentrations.
(2) preparation methylene blue solution
0.1g methylene blue is dissolved in 50mL water, is diluted to l00mL, draw
The above-mentioned solution of 30mL in 1000mL volumetric flask, add 6.8mL concentrated sulphuric acid and 50g without
Aqueous sodium persulfate, is diluted with water to scale, obtains methylene blue solution after dissolving.
(3) preparation dodecyl dimethyl benzyl ammonium bromide standard solution (cation mark
Quasi-solution)
Accurately weigh 1.42～1.46g100% bromo geramines (accurately to 0.0002g), molten
Yu Shuizhong, is transferred in l000mL volumetric flask, is diluted with water to scale, obtains concentration
It is about the dodecyl dimethyl benzyl ammonium bromide standard solution of 0.004mol/L.
(4) cation standard solution is demarcated
Draw 25mL lauryl sulfate sodium standard solution and fill in graduated cylinder in 100mL tool,
Add l0mL water, 25mL methylene blue solution and 15mL chloroform, after shaking up, use
Cation standard solution titrates, and first adds 2mL, and shaking uniformly, is placed 2min and treated biphase
Separate.Continuously add cation standard solution, each 2mL, after adding all every time
Shake and stand, until blue beginning stably occurs in aqueous phase, reduce cation
Standard solution adds speed, is finally down to each 1, with white board as background, biphase
Color is all titration end-point mutually.
It is calculated as follows the actual concentrations of cation standard solution:
Wherein, c1The actual concentrations of lauryl sulfate sodium standard solution, mol/L；
c2The actual concentrations of cation standard solution, mol/L；
V2Titration consumes the volume of cation standard solution, mL.
(5) titration product solution and blank solution
Accurately weigh cocos nucifera oil acyloxyethyl sulfonate product prepared by the lg present invention (accurately
To 0.001g) in beaker, add water heating for dissolving, it is transferred in 500mL volumetric flask,
It is diluted to scale.Draw the above-mentioned solution of 25mL and fill in graduated cylinder in 100mL tool, add
L0mL water, 25mL methylene blue solution and 15mL chloroform, after shaking up, with sun from
Substandard solution titrates, and first adds 2mL, and shaking uniformly, is placed 2min and treated two-phase laminated flow.
Continuously add cation standard solution, each 2mL, all shake also every time after adding
Stand, until blue beginning stably occurs in aqueous phase, reduce cation standard molten
Liquid adds speed, is finally down to each 1, with white board as background, and biphase color phase
It is all titration end-point.
Drawing 25mL water replaces 25mL product solution to do sky according to above-mentioned titration method
White test.
It is calculated as follows the mass fraction of anion active material in product:
Wherein, X1The mass fraction of anion active material, % in product；
c2The actual concentrations of cation standard solution, mol/L；
V3Product titration consumes the volume of cation standard solution, mL；
V0Blank titration consumes the volume of cation standard solution, mL；
The average molar mass of anion active material, g/mol in M product；
m1The quality of product, g.
The Content Test of free fatty in experimental example 3 product
Accurately weigh cocos nucifera oil acyloxyethyl sulfonate product prepared by the 5g present invention (accurately
To 0.01g) in 250mL conical flask, add 95% neutral alcohol (being not less than 20 DEG C)
50mL, shake well 10min, filter, and with 95% neutral alcohol (being not less than 20 DEG C)
45mL washs in three times, is filtered dry, and collects filtrate and washing liquid, with phenolphthalein indicator 5,
Being titrated to solution with standard solution of sodium hydroxide is blush, keeps 30s colour-fast i.e.
For titration end-point.
It is calculated as follows the mass fraction of free fatty in product:
Wherein, c3The concentration of standard solution of sodium hydroxide, mol/L；
V4Titration consumes the volume of standard solution of sodium hydroxide, mL；
m2The quality of product, g；
0.271 is the sodium hydroxide standard of 1.00mol/L with 1.00mL concentration
The stearic quality that solution is suitable, g.
Embodiment
Embodiment 1
Coconut acid methylester 245g, hydroxyethylsulfonic acid. is added in decompression distillation reactor
126g, methanol 100g, stirring and evenly mixing, 110 DEG C are heated to reflux 3 hours, 110 DEG C of steamings
Evaporate the methanol removing in reaction system 3 hours, steam to no liquid, reactant liquor is lowered the temperature
To 80 DEG C, add sodium hydroxide 35～45g and regulate pH to 6, reactant liquor is cooled to
25 DEG C, separate out a large amount of solid, dry, i.e. obtain sodium coconut acyloxyethanesulfonate product.
Measure the colourity of product according to method described in experimental example 1, result shows, embodiment
The colourity of 1 products obtained therefrom be 20 black once.
Sodium coconut acyloxyethanesulfonate in product is measured according to method described in experimental example 2
Content, result shows, the matter of sodium coconut acyloxyethanesulfonate in embodiment 1 products obtained therefrom
Amount mark is 96.3%.
The content of free fatty, result in product is measured according to method described in experimental example 3
Display, in embodiment 1 products obtained therefrom, the mass fraction of free fatty is 0.5%.
Embodiment 2
Coconut acid methylester 245g, hydroxyethylsulfonic acid. is added in decompression distillation reactor
126g, ethanol 100g, stirring and evenly mixing, 115 DEG C are heated to reflux 3.5 hours, 115 DEG C
Distill the methanol and ethanol removed in reaction system for 3.5 hours, steam to no liquid, will
Reactant liquor is cooled to 80 DEG C, adds sodium hydroxide 35～45g and regulates pH to 6, will reaction
Liquid is cooled to 25 DEG C, separates out a large amount of solid, dries, i.e. obtains cocos nucifera oil acyloxyethyl sulphur
Acid sodium product.
Measure the colourity of product according to method described in experimental example 1, result shows, embodiment
The colourity of 2 products obtained therefroms be 20 black once.
Sodium coconut acyloxyethanesulfonate in product is measured according to method described in experimental example 2
Content, result shows, the matter of sodium coconut acyloxyethanesulfonate in embodiment 2 products obtained therefrom
Amount mark is 97.7%.
The content of free fatty, result in product is measured according to method described in experimental example 3
Display, in embodiment 2 products obtained therefrom, the mass fraction of free fatty is 0.2%.
Embodiment 3
Coconut oil ethyl ester 260g, hydroxyethylsulfonic acid. is added in decompression distillation reactor
126g, ethanol 100g, stirring and evenly mixing, 115 DEG C are heated to reflux 4 hours, 115 DEG C of steamings
Evaporate the ethanol removing in reaction system 4 hours, steam to no liquid, reactant liquor is lowered the temperature
To 80 DEG C, add sodium hydroxide 35～45g and regulate pH to 6, reactant liquor is cooled to
25 DEG C, separate out a large amount of solid, dry, i.e. obtain sodium coconut acyloxyethanesulfonate product.
Measure the colourity of product according to method described in experimental example 1, result shows, embodiment
The colourity of 3 products obtained therefroms be 20 black once.
Sodium coconut acyloxyethanesulfonate in product is measured according to method described in experimental example 2
Content, result shows, the matter of sodium coconut acyloxyethanesulfonate in embodiment 3 products obtained therefrom
Amount mark is 95.9%.
The content of free fatty, result in product is measured according to method described in experimental example 3
Display, in embodiment 3 products obtained therefrom, the mass fraction of free fatty is 0.3%.
Embodiment 4
Coconut oil propyl ester 274g, hydroxyethylsulfonic acid. is added in decompression distillation reactor
126g, propanol 100g, stirring and evenly mixing, 120 DEG C are heated to reflux 4 hours, 120 DEG C of steamings
Evaporate the propanol removing in reaction system 4 hours, steam to no liquid, reactant liquor is lowered the temperature
To 80 DEG C, add sodium hydroxide 35～45g and regulate pH to 6, reactant liquor is cooled to
25 DEG C, separate out a large amount of solid, dry, i.e. obtain sodium coconut acyloxyethanesulfonate product.
Measure the colourity of product according to method described in experimental example 1, result shows, embodiment
The colourity of 4 products obtained therefroms be 20 black once.
Sodium coconut acyloxyethanesulfonate in product is measured according to method described in experimental example 2
Content, result shows, the matter of sodium coconut acyloxyethanesulfonate in embodiment 4 products obtained therefrom
Amount mark is 96.2%.
The content of free fatty, result in product is measured according to method described in experimental example 3
Display, in embodiment 4 products obtained therefrom, the mass fraction of free fatty is 0.4%.
Above in association with preferred implementation, experimental example and embodiment, the present invention is carried out
Describe in detail.But it is to be understood that, these detailed description of the invention are only to this
Bright illustrative explanations, does not constitute any restriction to protection scope of the present invention.?
In the case of spirit and scope of the present invention, can be in the technology of the present invention
Holding and embodiment carries out various improvement, equivalencing or modification, these each fall within
In protection scope of the present invention.Protection scope of the present invention is as the criterion with claims.
Claims (12)
1. the preparation method of a cocos nucifera oil acyloxyethyl sulfonate, it is characterised in that should
Method includes:
Step 1), by cocos nucifera oil acid esters, hydroxyethylsulfonic acid., the mixing of optional solvent, add
Hot reflux, stirring reaction；
Step 2), the lower distillation of stirring removes step 1) described in liquid in reaction system；
Step 3), by step 2 under stirring) described in reaction system cooling, add alkali adjust
Joint pH value；
Step 4), by step 3) described in reaction system cooling, separate out solid be institute
State cocos nucifera oil acyloxyethyl sulfonate.
The preparation side of cocos nucifera oil acyloxyethyl sulfonate the most according to claim 1
Method, it is characterised in that
Step 1) described in cocos nucifera oil acid esters be coconut acid methylester, coconut oil ethyl ester or cocos nucifera oil
Propyl propionate, and/or
Step 1) described in solvent be methanol, ethanol or propanol.
The preparation side of cocos nucifera oil acyloxyethyl sulfonate the most according to claim 1
Method, it is characterised in that
Step 1) in when described cocos nucifera oil acid esters is coconut acid methylester, described solvent is second
Alcohol or propanol；When described cocos nucifera oil acid esters is coconut oil ethyl ester, described solvent is methanol
Or propanol；When described cocos nucifera oil acid esters is coconut oil propyl ester, described solvent be methanol or
Ethanol.
The preparation side of cocos nucifera oil acyloxyethyl sulfonate the most according to claim 1
Method, it is characterised in that
Step 1) described in the mol ratio of cocos nucifera oil acid esters and hydroxyethylsulfonic acid. be 1.05:1～1.
2:1, described hydroxyethylsulfonic acid. is 1:1.6～1:3.5 with the mol ratio of solvent, and/or
Step 1) described in be heated to reflux temperature be 70～130 DEG C, and/or
Step 1) described in stir the response time be 0.5～5 hour.
The preparation side of cocos nucifera oil acyloxyethyl sulfonate the most according to claim 4
Method, it is characterised in that
Step 1) described in be heated to reflux temperature be 110～120 DEG C, and/or
Step 1) described in stir the response time be 2～4 hours.
6. according to the cocos nucifera oil acyloxyethyl sulfonate one of claim 1 to 5 Suo Shu
Preparation method, it is characterised in that
Step 2) described in vapo(u)rizing temperature be 70～130 DEG C, and/or
Step 2) described in distillation time be 1～6 hour.
The preparation side of cocos nucifera oil acyloxyethyl sulfonate the most according to claim 6
Method, it is characterised in that
Step 2) described in vapo(u)rizing temperature be 110～120 DEG C, and/or
Step 2) described in distillation time be 3～4 hours.
8. according to the cocos nucifera oil acyloxyethyl sulfonate one of claim 1 to 5 Suo Shu
Preparation method, it is characterised in that
Step 3) described in alkali be sodium hydroxide, sodium carbonate, sodium bicarbonate, hydroxide
Potassium, potassium carbonate, potassium bicarbonate, ammonia or ammonia, and/or
Step 3) in described reaction system is cooled to 70～85 DEG C, and/or
Step 3) in add alkali regulation pH value to 5～6.5.
The preparation side of cocos nucifera oil acyloxyethyl sulfonate the most according to claim 8
Method, it is characterised in that
Step 3) described in alkali be sodium hydroxide, sodium carbonate or sodium bicarbonate.
10. according to the cocos nucifera oil acyloxyethyl sulfonate one of claim 1 to 5 Suo Shu
Preparation method, it is characterised in that
Step 4) described in cocos nucifera oil acyloxyethyl sulfonate be cocos nucifera oil acyloxyethyl sulfonic acid
Sodium, cocos nucifera oil acyloxyethyl potassium sulfonate or cocos nucifera oil acyloxyethyl sulfonic acid ammonia, and/or
Step 4) in described reaction system is cooled to 22～28 DEG C.
The preparation side of 11. cocos nucifera oil acyloxyethyl sulfonate according to claim 10
Method, it is characterised in that
Step 4) described in cocos nucifera oil acyloxyethyl sulfonate be cocos nucifera oil acyloxyethyl sulfonic acid
Sodium.
12. according to the cocos nucifera oil acyloxyethyl sulfonate one of claim 1 to 5 Suo Shu
Preparation method, it is characterised in that step 1), step 2), step 3) and step 4)
Described in reaction all carry out reducing pressure in distillation reactor.
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