CN102527293B - Method for preparing lauryl ether phosphate ester - Google Patents
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Abstract
The invention relates to a method for preparing lauryl ether phosphate ester, which adopts a method of adding AEO3 and P2O5 in a process step by step, and adding phosphoric acid and MAP-L, so that content of monoester in products is increased, and the products can achieve requirements for standard color and luster without adding hydrogen peroxide. Irritation is reduced, foams are abundant, combination property is good, and the method can be applied to the fields of cosmetics including facial cleanser, hand cleanser, facial washer and the like.
Description
Technical field
The invention belongs to surfactant field, especially relate to a kind of preparation method of ether phosphate.
Background technology
Phosphate is one type very important in surfactant, because it is structurally similar to natural phospholipid with physiological effect, in skin, there is extraordinary compatibility, in and after salify the characteristic of existing general anion surfactant as water-soluble, emulsibility etc., also has certain dirt-removing power, but be unlikely to degreasing, the surfactant that belongs to mildness, be very suitable for the cleaning of skin, it has good antistatic behaviour, soft conditioning property, emulsifying dispersivity, its excitant is little, gentle, easily rinse, foam is abundant fine and smooth, wash rear smooth, be widely used in skin nursing products.Due to it, there is the characteristics such as good antistatic behaviour, emulsifying dispersivity, lubricated, acid-fast alkali-proof simultaneously, be widely used in chemical fibre, weaving, leather, plastics, papermaking, agricultural chemicals medicine and other fields.
Phosphate is by hydroxyl fatty alcohol or ether and phosphoric acid agent reaction generation phosphate monoester, dibasic acid esters, three esters and free phosphoric acid.According to the difference of phosphoric acid agent, preparation method is divided into again three kinds: polyphosphoric acid method, POCl3 method, phosphorus pentoxide method.Polyphosphoric acid method is used for making high phosphate monoester (> 90%), is mainly used in pharmaceutical industry; POCl3 is mainly used in the bisalkyl phosphate of high-load processed, is used in textile finish oil; Phosphorus pentoxide method, obtains monoester content in 70% left and right, and dibasic acid esters content, at the product of 20% left and right, is mainly used in the fields such as weaving and daily cleaning.
By phosphorus pentoxide legal system, obtaining phosphate has 70% monoesters and 20% dibasic acid esters, in and salify after monoesters dissolubility good, dibasic acid esters detergency is good, integrate possessed outstanding mild surfactant whole features, its application is also the most extensive, weaving, daily cleaning, skin nursing can be used.Due to the different qualities of monoesters and dibasic acid esters, prepare the dibasic acid esters of the high phosphate monoester of phosphate requirement and some, the height of monoester content has represented the quality of the application performance of phosphate, has also reflected the height of preparing phosphate level.With dodecyl alcohol phosphate processed and slightly different with the phosphate application of ether system, alkyl phosphate foam is abundant, fine and smooth, be generally used for skin nursing as in the opaque products such as mildy wash, mildy wash, and ether phosphate detergency is stronger than alkyl phosphate, generally be used in mildy wash, shower cream, hand cleanser, can be in transparent or semitransparent product, purposes is more wide in range than alkyl phosphate.With ether phosphate processed, compare alkyl phosphate color and luster and more easily deepen, technological requirement is wanted to tight relatively.The technique of existing domestic ether phosphate processed is: AEO3 is warmed up to 40 ℃ of left and right and adds catalyst phosphorous acid or ortho phosphorous acid, under strong stirring, substep adds P
2o
5, feed time, probably at 1 hour, is warmed up to 60-70 ℃ afterwards, reacts 4 hours, adds hydrogen peroxide decolouring after esterification completes.The deficiency of this method for making: P
2o
5easily caking, can not effectively utilize, and color and luster is dark, needs hydrogen peroxide bleaching, and this color stability to final products can be influential; Monoester content is low, and generally, between 40-60%, foam is few, and accessory substance is many, and excitant is high, and combination property is poor, seldom can be used on cosmetics.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of preparation method of lauryl ether phosphate ester, not only improved the content of monoesters in product, and do not need to add hydrogen peroxide and just can make product reach the requirement of standard color and luster, reduce excitant, foam is abundant, and good combination property is especially applicable to cosmetics and uses.
The technical solution used in the present invention is: a kind of preparation method of lauryl ether phosphate ester, described preparation method comprises the steps:
A. in reactor, add the phosphoric acid of the total inventory 45-55% of AEO3 (laureth) and 1-3%, be heated to 40-80 ℃, stir lower reaction 0.5-3 hour, total inventory of described AEO3 is 40-55%;
B. add the inferior sodium phosphate of 0.03-0.06% and the deionized water of 0.4-0.6%;
C. cool to below 45 ℃, add P
2o
5the 45-55% of total inventory, minute 4-15 time every minor tick 5-30 minute throwing P
2o
5, finish rear continuation at stirring reaction 1-5 hour below 45 ℃, described P
2o
5total inventory be 8-12%;
D. be heated to 50-80 ℃ of reaction 4-12 hour;
E. cool to 30-50 ℃, throw remaining AEO3, be then heated to 40-80 ℃ of reaction 0.5-3 hour;
F. cool to below 45 ℃, throw remaining P
2o
5, minute 4-15 time every minor tick 5-30 minute throwing P
2o
5, finish rear continuation at stirring reaction 1-5 hour below 45 ℃;
G. be heated to 50-80 ℃ of reaction 4-16 hour, obtain reactant mixture;
H. sample examination, the monoester content in reactant mixture being detected reaches 60% when above, adds the MAP-L (alkyl phosphate) of the 25-35% of molten condition, stirs, and obtains mixed liquor;
I. when mixeding liquid temperature is 50-85 ℃, add the solution being made into by alkali lye, the triethanolamine of 0.2-0.5% and the deionized water of 1-5% that the sheet alkali of 0.5-0.8% and the deionized water of 2-7% are made into, finish rear continuation reaction 1-5 hour, obtain described lauryl ether phosphate ester.
In A-I step, the percentage of described each reactant represents that the inventory of each reactant accounts for the mass percent of all reactant inventory summations.
The lauryl ether phosphate ester preparing by the method for the invention, it meets following technical target of the product as in the table below:
As the preparation method's of lauryl ether phosphate ester preferred version, described preparation method comprises the steps:
A. in reactor, add 25.58% AEO3 and 1.8% phosphoric acid, be heated to 70 ℃, stir lower reaction 2 hours;
B. add 0.05% inferior sodium phosphate and 0.5% deionized water;
C. cool to below 45 ℃, add 5.19% P
2o
5, minute 4 every minor ticks are thrown P for 20 minutes
2o
5, finish rear continuation stirring reaction below 45 ℃ 2 hours;
D. be heated to 70 ℃ of reactions 4 hours;
E. cool to 30-45 ℃, add 25.58% AEO3, be then heated to 70 ℃ of reactions 2 hours;
F. cool to below 45 ℃, add 5.19% P
2o
5, minute 4 every minor ticks are thrown P for 20 minutes
2o
5, finish rear continuation stirring reaction below 45 ℃ 2 hours;
G. be heated to 70 ℃ of reactions 6 hours, obtain reactant mixture;
H. sample examination, the monoester content in reactant mixture being detected reaches 60% when above, adds 27.2% MAP-L of molten condition, stirs, and obtains mixed liquor;
I. when mixeding liquid temperature is 60 ℃, add the deionized water of alkali lye that the sheet alkali with 5.4% deionized water and 0.54% is made into and 2.7% and the solution that 0.27% triethanolamine is made into, after finishing, at 67 ℃, continue reaction 1 hour, obtain described lauryl ether phosphate ester.
In A-I step, the percentage of described each reactant represents that the inventory of each reactant accounts for the mass percent of all reactant inventory summations.
Advantage and good effect that the present invention has are:
1. owing to having added phosphoric acid in reaction mass, adopt the method for stepwise reaction, monoester content in lauryl ether phosphate ester that the present invention obtains is improved significantly, reach more than 70%.
2. adopt substep to add AEO3 and P
2o
5method, make the surfactant generating have emulsification to the material newly adding, accelerated reaction speed, simultaneously P
2o
5rate of dispersion be also improved, be not easy caking, heat of reaction is discharged in time, product color is improved.
3. because product color is good, do not need to add hydrogen peroxide bleaching and just can reach requirement, avoided many troubles variable color as long in the finished product storage time of using hydrogen peroxide to bring, to the increase of application on human skin excitant etc.
4. in technique, add MAP-L, and by part phosphate and salify, this compounded technology has been applied in manufacturing process, product combination property is improved as spumescence, enriched properties of product.
5. product excitant reduces greatly, is widely used in the cosmetic fields such as mildy wash, hand cleanser, mildy wash.
The specific embodiment
Below in conjunction with three embodiment, the present invention is illustrated:
Embodiment mono-:
Technical process:
A. in reactor, add the AEO3 of 188kg and the phosphoric acid of 13.3kg, be heated to 70 ℃, stir lower reaction 2 hours;
B. add the inferior sodium phosphate of 0.4kg and the deionized water of 4kg;
C. cool to 45 ℃ of following also holding temperatures and be no more than 45 ℃, add the P of 38kg
2o
5, minute 4 every minor ticks are thrown P for 20 minutes
2o
5, finish rear continuation stirring reaction 2 hours at 45 ℃;
D. be heated to 70 ℃ of reactions 4 hours;
E. cool to 30-45 ℃, add the AEO3 of 188kg, be then heated to 70 ℃ of reactions 2 hours;
F. cool to below 45 ℃, throw the P of 38kg
2o
5, minute 4 every minor ticks are thrown P for 20 minutes
2o
5, finish rear continuation stirring reaction 2 hours at 45 ℃;
G. be heated to 70 ℃ of reactions 6 hours, obtain reactant mixture;
H. sample examination, records monoester content in reactant mixture and reaches 60% when above, adds the MAP-L of the 200kg of molten condition, stirs, and obtains mixed liquor;
I. when mixeding liquid temperature is 60 ℃, the solution that adds the alkali lye that is made into the deionized water of 40kg and the sheet alkali of 4kg and the deionized water of 20kg and the triethanolamine of 2kg to be made into continues reaction 1 hour at 67 ℃ after finishing, obtain product;
J. sample examination, recording solids content in product is 90.65%, monoester content is 73.2%, dibasic acid esters content is 5.78%, and phosphorus acid content is 5.21%, color and luster < 30, reached technical target of the product, packing discharging, resulting lauryl ether phosphate ester outward appearance is light yellow thick liquid, cooling is that micro-yellow approaches colourless body of paste afterwards.
Embodiment bis-:
Technical process:
A. in reactor, add the AEO3 of 32kg and the phosphoric acid of 3.75kg, be heated to 80 ℃, stir lower reaction 0.5 hour;
B. add the inferior sodium phosphate of 0.075kg and the deionized water of 0.75kg;
C. cool to 45 ℃ of following also holding temperatures and be no more than 45 ℃, add the P of 6.4kg
2o
5, minute 15 every minor ticks are thrown P for 5 minutes
2o
5, finish rear continuation stirring reaction 1 hour at 45 ℃;
D. be heated to 80 ℃ of reactions 4 hours;
E. cool to 30-45 ℃, add the AEO3 of 30kg, be then heated to 80 ℃ of reactions 0.5 hour;
F. cool to below 45 ℃, throw the P of 6.0kg
2o
5, minute 15 every minor ticks are thrown P for 5 minutes
2o
5, finish rear continuation stirring reaction 1 hour at 45 ℃;
G. be heated to 80 ℃ of reactions 4 hours, obtain reactant mixture;
H. sample examination, records monoester content in reactant mixture and reaches 60% when above, adds the MAP-L of the 33.8kg of molten condition, stirs, and obtains mixed liquor;
I. when mixeding liquid temperature is 80 ℃, the solution that adds the alkali lye that is made into the deionized water of 7.5kg and the sheet alkali of 0.75kg and the deionized water of 3.75kg and the triethanolamine of 0.375kg to be made into continues reaction 1 hour at 85 ℃ after finishing, obtain product;
J. sample examination, recording solids content in product is 89.83%, monoester content is 70.61%, dibasic acid esters content is 14.02%, and phosphorus acid content is 5.68%, color and luster < 30, reached technical target of the product, packing discharging, resulting lauryl ether phosphate ester outward appearance is light yellow thick liquid, cooling is that micro-yellow approaches colourless body of paste afterwards.
Embodiment tri-:
Technical process:
A. in reactor, add the AEO3 of 171kg and the phosphoric acid of 9.15kg, be heated to 70 ℃, stir lower reaction 3 hours;
B. add the inferior sodium phosphate of 0.26kg and the deionized water of 2.6kg;
C. cool to 45 ℃ of following also holding temperatures and be no more than 45 ℃, add the P of 47kg
2o
5, minute 4 every minor ticks are thrown P for 20 minutes
2o
5, finish rear continuation stirring reaction 4 hours at 45 ℃;
D. be heated to 70 ℃ of reactions 12 hours;
E. cool to 30-45 ℃, add the AEO3 of 171kg, be then heated to 70 ℃ of reactions 3 hours;
F. cool to below 45 ℃, throw the P of 46kg
2o
5, minute 4 every minor ticks are thrown P for 20 minutes
2o
5, finish rear continuation stirring reaction 4 hours at 45 ℃;
G. be heated to 50 ℃ of reactions 16 hours, obtain reactant mixture;
H. sample examination, records monoester content in reactant mixture and reaches 60% when above, adds the MAP-L of the 295kg of molten condition, stirs, and obtains mixed liquor;
I. when mixeding liquid temperature is 50 ℃, the solution that adds the alkali lye that is made into the deionized water of 68.3kg and the sheet alkali of 6.83kg and the deionized water of 34.1kg and the triethanolamine of 3.41kg to be made into continues reaction 1 hour at 55 ℃ after finishing, obtain product;
J. sample examination, recording solids content in product is 90.02%, monoester content is 72.15%, dibasic acid esters content is 8.24%, and phosphorus acid content is 5.04%, color and luster < 30, reached technical target of the product, packing discharging, resulting lauryl ether phosphate ester outward appearance is light yellow thick liquid, cooling is that micro-yellow approaches colourless body of paste afterwards.
Above three embodiment of the present invention are had been described in detail, but described content is only preferred embodiment of the present invention, can not be considered to for limiting practical range of the present invention.All equalization variations of doing according to the present patent application scope and improvement etc., within all should still belonging to patent covering scope of the present invention.
Claims (2)
1. a preparation method for lauryl ether phosphate ester, is characterized in that, described preparation method comprises the steps:
A. in reactor, add AEO
3total 45-55% of inventory and the phosphoric acid of 1-3%, be heated to 40-80 ℃, stirs lower reaction 0.5-3 hour, described AEO
3total inventory be 40-55%;
B. add the inferior sodium phosphate of 0.03-0.06% and the deionized water of 0.4-0.6%;
C. cool to below 45 ℃, add P
2o
5the P of the 45-55% of total inventory
2o
5, minute 4-15 time every minor tick 5-30 minute throwing P
2o
5, finish rear continuation at stirring reaction 1-5 hour below 45 ℃, described P
2o
5total inventory be 8-12%;
D. be heated to 50-80 ℃ of reaction 4-12 hour;
E. cool to 30-50 ℃, throw remaining AEO
3, be then heated to 40-80 ℃ of reaction 0.5-3 hour;
F. cool to below 45 ℃, throw remaining P
2o
5, minute 4-15 time every minor tick 5-30 minute throwing P
2o
5, finish rear continuation at stirring reaction 1-5 hour below 45 ℃;
G. be heated to 50-80 ℃ of reaction 4-16 hour, obtain reactant mixture;
H. sample examination, the monoester content in reactant mixture being detected reaches 60% when above, adds the MAP-L of the 25-35% of molten condition, stirs, and obtains mixed liquor;
I. when mixeding liquid temperature is 50-85 ℃, the solution that adds the alkali lye that is made into by the sheet alkali of 0.5-0.8% and the deionized water of 2-7% and the triethanolamine of 0.2-0.5% and the deionized water of 1-5% to be made into, finish rear continuation reaction 1-5 hour, obtain described lauryl ether phosphate ester;
In A-I step, the percentage of described each reactant represents that the inventory of each reactant accounts for the mass percent of all reactant inventory summations
Described AEO
3be laureth, described MAP-L is alkyl phosphate.
2. the preparation method of lauryl ether phosphate ester according to claim 1, is characterized in that, described preparation method comprises the steps:
A. in reactor, add 25.58% AEO
3phosphoric acid with 1.80%, is heated to 70 ℃, stirs lower reaction 2 hours;
B. add 0.05% inferior sodium phosphate and 0.5% deionized water;
C. cool to below 45 ℃, add 5.19% P
2o
5, minute 4 every minor ticks are thrown P for 20 minutes
2o
5, finish rear continuation stirring reaction below 45 ℃ 2 hours;
D. be heated to 70 ℃ of reactions 4 hours;
E. cool to 30-45 ℃, add 25.58% AEO
3, be then heated to 70 ℃ of reactions 2 hours;
F. cool to below 45 ℃, add 5.19% P
2o
5, minute 4 every minor ticks are thrown P for 20 minutes
2o
5, finish rear continuation stirring reaction below 45 ℃ 2 hours;
G. be heated to 70 ℃ of reactions 6 hours, obtain reactant mixture;
H. sample examination, the monoester content in reactant mixture being detected reaches 60% when above, adds 27.2% MAP-L of molten condition, stirs, and obtains mixed liquor;
I. when mixeding liquid temperature is 60 ℃, add the deionized water of alkali lye that the sheet alkali with 5.4% deionized water and 0.54% is made into and 2.7% and the solution that 0.27% triethanolamine is made into, after finishing, at 67 ℃, continue reaction 1 hour, obtain described lauryl ether phosphate ester;
In A-I step, the percentage of described each reactant represents that the inventory of each reactant accounts for the mass percent of all reactant inventory summations.
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