CN103483375A - High-carbon fatty alcohol phosphate ester emulsifier, and preparation method and application thereof - Google Patents
High-carbon fatty alcohol phosphate ester emulsifier, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a high-carbon fatty alcohol phosphate ester emulsifier, and preparation method and application thereof The method comprises the steps of: first heating to completely dissolve C18-22 straight-chain alkyl fatty alcohol, adding a phosphorylation reagent, and homogenizing to obtain a disperse substance; well mixing the C18-22 straight-chain alkyl fatty alcohol, an anti-oxidant, a chelating agent and a catalyst, heating to 110-125 DEG C, and vacuumizing until complete dissolving of the straight-chain alkyl fatty alcohol to obtain a reactant; adding the disperse substance into the reactant and reacting under negative pressure; after the reaction, cooling to 60-75 DEG C, adding deionized water for hydrolysis, after hydrolysis adding 30 wt% of H2O2 for decoloration and insulating; then adding Na2HSO3 and insulating; cooling and discharging materials to obtain the high-carbon fatty alcohol phosphate ester emulsifier. The preparation method is environment-friendly, and the obtained emulsifier has good emulsification effect and can be widely applied to preparation of cosmetics.
Description
Technical field
The present invention relates to a kind of emulsifying agent, particularly a kind of high-carbon fatty alcohol phosphoric acid ester emulsifying agent and preparation method thereof and application.
Background technology
Alkyl phosphate is a kind of anion surfactant be comprised of phosphate diester, monoesters and non-ionic surface active thing.Because it has lower surface tension and the performances such as satisfactory stability, emulsifying property, dispersiveness, wettability, soil release performance and static resistance, and its performance approaches natural phosphates, easy degraded, low irritant, so its industry such as daily-use chemical industry, makeup, food, medicine, agricultural chemicals, synthetic materials that are widely used in weaving.China starts late to the research of phosphoric acid ester tensio-active agent, because phosphoric acid ester is applied in the specialty formula, makes various compounds in recent years, and its tempo is very fast, existing multiple phosphoric acid ester product.Action oriented research mainly concentrates on synthetic, purification and the formulating aspect of phosphoric acid ester product.At present, domestic fatty alcohol phosphate research mainly concentrates on middle low carbon fat alcohol phosphoric acid ester, the product of exploitation is used mainly as gentle, the low tensio-active agent stimulated, as Tryfac 5573 (1-isobutyl-3,5-dimethylhexylphosphoric acid) or lauryl alcohol phosphoric acid ester (EO=1,3,9 etc.), be applied in the products such as shampoo, body wash, cleansing milk.
Generally speaking, high-carbon fatty alcohol phosphoric acid ester (C >=18) is used mainly as emulsifying agent, and high-grade high-carbon fatty alcohol phosphoric acid ester emulsifying agent major part is monopolized by offshore company in the market, and price is higher.Homemade goods from kind, quality and quantity all with outer state-owned larger gap.High-quality high-carbon fatty alcohol phosphoric acid ester index is mainly reflected in content, free phosphoric acid content, unreacted nonionic thing, color and luster of single dibasic acid esters etc.Wherein, monoesters affects emulsifying property, water-soluble and static resistance; Dibasic acid esters impact is level and smooth, moistness, and therefore single, double ester must have rational collocation, could be on emulsification and skinfeel balance.In addition, free phosphoric acid, unreacted nonionic thing and color and luster are as far as possible low, do not affect follow-up formula.
The production method of middle low carbon fat alcohol (ether) phosphoric acid ester is set forth in more patent, as ZL201010159509.2, and ZL200710070153.3 etc.High-carbon fatty alcohol phosphoric acid ester preparation method is similar to middle low carbon fat alcohol phosphoric acid ester but be not quite similar, and is mainly that fusing point increases along with carbon chain lengths increases, and the high-carbon fatty alcohol reactive behavior reduces, and needs suitable catalyzer and solvent.The preparation method of the high alkyl phosphate of a kind of used for cosmetic is disclosed in the patent application that publication No. is CN103012469A; using eicosanol or behenyl alcohol is raw material; after phosphorylated; can obtain the phosphate mixture that can be good at being applied to makeup, its component is phosphate monoester, phosphate diester, free phosphoric acid, fatty alcohol.But some poisonous and hazardous solvents have been used in this patent application, as benzene or toluene, dimethylbenzene etc., these materials must thoroughly be removed by the mode of distillation in the production later stage, and environment, technique, equipment etc. are had relatively high expectations; If can not remove totally, HUMAN HEALTH is had to great harm; In addition, the phosphoric acid ester that this patent application obtains (monoesters+dibasic acid esters) content is lower, a little less than meaning that its emulsifying power, can not use as primary emulsion.
Summary of the invention
For the shortcoming and deficiency that overcome prior art, primary and foremost purpose of the present invention is to provide a kind of preparation method of high-carbon fatty alcohol phosphoric acid ester emulsifying agent.
Another object of the present invention is to provide the high-carbon fatty alcohol phosphoric acid ester obtained by above-mentioned preparation method emulsifying agent.
Another object of the present invention is to provide the application of described high-carbon fatty alcohol phosphoric acid ester emulsifying agent.
A further object of the present invention is to provide the cream frost that contains above-mentioned high-carbon fatty alcohol phosphoric acid ester emulsifying agent emulsion.
Purpose of the present invention is achieved through the following technical solutions: a kind of preparation method of high-carbon fatty alcohol phosphoric acid ester emulsifying agent comprises following steps:
(1) by C
18～22the straight chained alkyl fatty alcohol heats up while stirring; Work as C
18～22the straight chained alkyl fatty alcohol just dissolves fully, adds phosphorus esterification reagent, and homogeneous, obtain pre-dispersed thing, and the sealing froth breaking is stand-by;
(2) by C
18～22straight chained alkyl fatty alcohol, antioxidant, sequestrant and catalyzer mix, and are warming up to 110～125 ℃, treat C
18～22the straight chained alkyl fatty alcohol vacuumizes after dissolving fully, obtains reactant;
(3) pre-dispersed thing step (1) obtained joins in the reactant that step (2) obtains, and under condition of negative pressure, reacts;
(4) after reaction finishes, be cooled to 60～75 ℃, add deionized water to be hydrolyzed; Hydrolysis reaction adds the H that mass percent is 30% after finishing
2o
2decoloured, insulation;
(5) then add again Na
2hSO
3, insulation; Cooling discharge, obtain high-carbon fatty alcohol phosphoric acid ester emulsifying agent;
Wherein, the consumption of each raw material carries out proportioning by following mass ratio: C used in step (1)
18～22straight chained alkyl fatty alcohol: phosphorus esterification reagent: C used in step (2)
18～22straight chained alkyl fatty alcohol: antioxidant: sequestrant: catalyzer: the H of mass percent 30%
2o
2: Na
2hSO
3=40:20:60:0.05:0.05:0.5:(3～6): 2.8;
C described in step (1) and (2)
18～22the straight chained alkyl fatty alcohol is at least one in the carbonatoms straight chained alkyl fatty alcohol that is 18～22; Be preferably C
18fatty alcohol (stearyl alcohol), C
20fatty alcohol (eicosanol) and C
22at least one in fatty alcohol (behenyl alcohol);
The temperature of the intensification described in step (1), can be according to C
18～22the fusing point of straight chained alkyl fatty alcohol is controlled, and is warming up to C
18～22the straight chained alkyl fatty alcohol just dissolves fully;
Phosphorus esterification reagent described in step (1) is preferably P
2o
5, at least one in ortho-phosphoric acid, metaphosphoric acid and polyphosphoric acid;
Described polyphosphoric acid is preferably P
2o
5the polyphosphoric acid that equivalent is 85%;
The condition optimization of the homogeneous described in step (1) is: pressure-0.05～-0.1MPa under homogeneous 3～5min;
Antioxidant described in step (2) is preferably at least one in gsh, vitamins C, vitamin-E, 2,6 di tert butyl 4 methyl phenol (BHT), butylated hydroxy anisole (BHA), butylated hydroxytoluene, gallic acid and Tenox PG;
Sequestrant described in step (2) is preferably at least one in disodium ethylene diamine tetraacetate (EDTA-2Na), tetrasodium ethylenediamine tetraacetate (EDTA-4Na), sodium polyacrylate, etidronic acid and Etidronate disodium;
Catalyzer described in step (2) is preferably at least one in tosic acid, paratoluenesulfonic acid sodium salt, tosic acid potassium and paratoluenesulfonic acid ammonium salt;
The time vacuumized described in step (2) is preferably 15～30min;
The pre-dispersed thing that step (1) is obtained described in step (3) joins in the reactant that step (2) obtains and is preferably as follows and operated: the pre-dispersed thing that step (1) is obtained divides and joins for 4～6 times in the reactant that step (2) obtains, every minor tick 15～20min;
The condition optimization reacted under condition of negative pressure described in step (3) in-0.05～-react 5～8h under the 0.1MPa condition of negative pressure;
The consumption of the deionized water described in step (4) is preferably and is equivalent to the described C of step (1)
18～222/10～3/10 of straight chained alkyl fatty alcohol quality;
The time of the hydrolysis described in step (4) is preferably 1.5～3h;
The time of the insulation described in step (4) and (5) is preferably 30min;
A kind of high-carbon fatty alcohol phosphoric acid ester emulsifying agent, obtain by above-mentioned preparation method, that (carbonatoms is not less than 18 to the high-carbon fatty alcohol phosphate monoester, being preferably carbonatoms is 18～22), (carbonatoms is not less than 18 to the high-carbon fatty alcohol phosphate diester, being preferably carbonatoms is 18～22), unreacted nonionic thing, the mixture of free phosphoric acid and water, wherein, the total mass per-cent of high-carbon fatty alcohol phosphate monoester and high-carbon fatty alcohol phosphate diester is greater than>and 94%, the content of high-carbon fatty alcohol phosphate monoester>81% wherein, the content of high-carbon fatty alcohol phosphate diester<14%, free phosphoric acid and unreacted nonionic thing total mass per-cent<2%, the content mass percent of free phosphoric acid<1%, water is surplus, be preferably the content 81.8～83.8% of high-carbon fatty alcohol phosphate monoester, the content 11.5～13.8% of high-carbon fatty alcohol phosphate diester, the content 0.58～0.72% of free phosphoric acid, unreacted nonionic thing 0.57～0.8%,
The application of described high-carbon fatty alcohol phosphoric acid ester emulsifying agent in preparing makeup;
A kind of cream frost emulsion, contain above-mentioned high-carbon fatty alcohol phosphoric acid ester emulsifying agent;
Described cream frost emulsion, comprise the following composition of calculating by mass percentage: high-carbon fatty alcohol phosphoric acid ester emulsifying agent 0.5～2%, iso-octyl palmitate 2%, polydimethylsiloxane 2%, hexadeca-octadecyl alcohol 3%, 26# white oil 8%, glycerine 5%, xanthan gum 1%, propylene glycol 3%, trolamine 1.5%, disodium ethylene diamine tetraacetate 0.05%, 2,6 di tert butyl 4 methyl phenol 0.05%, extremely beautiful II0.1%;
Described cream frost emulsion also contains water, and water is surplus.
The present invention has following advantage and effect with respect to prior art:
(1) preparation method provided by the invention is friendly process, does not use poisonous, hazardous solvent, without " three wastes " discharge.
(2) to compare the difference of traditional method be that phosphorus esterification reagent is pre-dispersed in a part of reaction mass to preparation technology provided by the invention, avoids the local caking of phosphorus esterification reagent, the problem that level of response is inadequate.
(3) the high-carbon fatty alcohol phosphoric acid ester emulsifying agent lighter color obtained by preparation method provided by the invention, high-carbon fatty alcohol phosphoric acid ester monoesters and dibasic acid esters ratio are reasonable, have the well emulsify performance of monoesters and the sliding advantage of exquisiteness, silk of dibasic acid esters concurrently.Wherein, the total mass per-cent of high-carbon fatty alcohol phosphate monoester and high-carbon fatty alcohol phosphate diester is greater than>and 94%, the content of the content of high-carbon fatty alcohol phosphate monoester>81%, high-carbon fatty alcohol phosphate diester<14% wherein, free phosphoric acid and unreacted nonionic thing total mass per-cent<2%, the content mass percent of free phosphoric acid<1%; Because the content of product Free Phosphoric Acid is less than 1%, is applied in makeup and can damage skin;
(4) the high-carbon fatty alcohol phosphoric acid ester emulsifying agent that prepared by the present invention is used as emulsifying agent for cosmetic formulations, and emulsifying effectiveness is good; The emulsion obtained has good wettability and stability, and skinfeel is fine and smooth, silk is sliding.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
(1) by 60 mass parts C
18fatty alcohol (stearyl alcohol), 0.05 mass parts butylated hydroxy anisole (BHA), 0.05 mass parts EDTA-2Na and 0.5 mass parts tosic acid add in reactor A, stir and are warming up to 110 ℃, treat C
18fatty alcohol vacuumizes 30min after dissolving fully;
In reactor B, add 40 mass parts C
18fatty alcohol, stir and be warming up to C
18fatty alcohol just dissolves (temperature is 60 ℃), adds 20 mass parts by 10 mass parts P
2o
5with the phosphorylating agent that 10 mass parts ortho-phosphoric acid form, open homogeneous 5min under-0.05MPa, obtain pre-dispersed thing, the sealing froth breaking is stand-by;
By the pre-dispersed thing obtained in reactor B, divide and add rapidly for 4 times in reactor A, every minor tick 15min, after adding, reactor A maintains negative pressure-0.1MPa, continues reaction 5h.
(2) after step (1) reaction finishes, be cooled to 75 ℃.Add 12 mass parts deionized waters to be hydrolyzed, the time is 3h; Hydrolysis reaction adds the H that 3 mass parts concentration are mass percent 30% after finishing
2o
2, insulation 30min, then add 2.8 mass parts Na
2hSO
3, insulation 30min.Cooling discharge, obtain the lily C of outward appearance
18the fatty alcohol phosphate emulsifying agent.
The present invention adopts the content (detection method of following examples is with herein) of mono phosphoric acid ester, dibasic acid esters and free phosphoric acid in the potentiometric determination product.The method reference literature " Sun Yu, Zheng's women's headgear, Wang Bin. the research of analytical methods of high fatty alcohol phosphate ester [J]. Tianjin University of Technology's journal, 2007,26 (4): 25-27 ".Moisture content adopts oven drying method to measure.
The detected result obtained is as shown in table 1:
Table 1
| Index | Result (mass percent %) |
| C 18The fatty alcohol phosphate monoester | 83.24 |
| C 18The fatty alcohol phosphate diester | 13.60 |
| Free phosphoric acid | 0.58 |
| Unreacted nonionic thing | 0.80 |
| Moisture | Surplus |
Embodiment 2
(1) by 60 mass parts C
20fatty alcohol (eicosanol), 0.05 mass parts gallic acid, 0.05 mass parts etidronic acid and 0.5 mass parts paratoluenesulfonic acid sodium salt add in reactor A, stir and are warming up to 125 ℃, after the C20 fatty alcohol dissolves fully, vacuumize 15min;
In another reactor B, add 40 mass parts C
20fatty alcohol, stir and be warming up to C
20fatty alcohol just dissolves (temperature is 75 ℃), adds 20 mass parts by 8 mass parts P
2o
5with the phosphorylating agent that 12 mass parts metaphosphoric acids form, open homogeneous 3min under-0.1MPa, obtain pre-dispersed thing, the sealing froth breaking is stand-by;
By the pre-dispersed thing obtained in reactor B, divide and add rapidly for 5 times in reactor A, every minor tick 15min, after adding, reactor A maintains negative pressure-0.1MPa, continues reaction 8h;
(2) after step (1) reaction finishes, be cooled to 60 ℃.Add 10 mass parts deionized waters to be hydrolyzed, the time is 1.5h; Hydrolysis reaction adds the H that 6 mass parts concentration are mass percent 30% after finishing
2o
2, insulation 30min, then add 2.8 mass parts Na
2hSO
3, insulation 30min.Cooling discharge, obtain the lily C of outward appearance
20the fatty alcohol phosphate emulsifying agent.
Analytical results is as shown in table 2:
Table 2
| Index | Result (mass percent %) |
| C 20The fatty alcohol phosphate monoester | 83.76 |
| C 20The fatty alcohol phosphate diester | 11.52 |
| Free phosphoric acid | 0.66 |
| Unreacted nonionic thing | 0.65 |
| Moisture | Surplus |
Embodiment 3
(1) by 60 mass parts C
22straight chained alkyl fatty alcohol (behenyl alcohol), 0.05 mass parts BHA, 0.05 mass parts EDTA-2Na and 0.5 mass parts tosic acid potassium add in reactor A, stir and are warming up to 115 ℃, after the C22 fatty alcohol dissolves fully, vacuumize 20min;
In another reactor B, add 40 mass parts C
22fatty alcohol, stir and be warming up to C
22fatty alcohol just dissolves (temperature is 75 ℃), adds 20 mass parts by 12 mass parts P
2o
5with the phosphorylating agent that 8 mass parts ortho-phosphoric acid form, open homogeneous 4min under-0.08MPa, obtain pre-dispersed thing, the sealing froth breaking is stand-by;
By the pre-dispersed thing obtained in reactor B, divide and add rapidly for 5 times in reactor A, every minor tick 18min, after adding, reactor A maintains negative pressure-0.08MPa, continues reaction 6h;
(2) after step (1) reaction finishes, be cooled to 70 ℃.Add 10 mass parts deionized waters to be hydrolyzed, the time is 2h; Hydrolysis reaction adds the H that 3 mass parts concentration are mass percent 30% after finishing
2o
2, insulation 30min, then add 2.8 mass parts Na
2hSO
3, insulation 30min.Cooling discharge, obtain the lily C of outward appearance
22the fatty alcohol phosphate emulsifying agent.
Analytical results is as shown in table 3:
Table 3
| Index | Result (mass percent %) |
| C 22The fatty alcohol phosphate monoester | 81.80 |
| C 22The fatty alcohol phosphate diester | 13.77 |
| Free phosphoric acid | 0.72 |
| Unreacted nonionic thing | 0.57 |
| Moisture | Surplus |
Embodiment 4
(1) by 30 mass parts C
20fatty alcohol, 30 mass parts C
22fatty alcohol, 0.05 mass parts vitamin-E, 0.05 mass parts Etidronate disodium and 0.5 mass parts paratoluenesulfonic acid ammonium salt add in reactor A, stir and are warming up to 120 ℃, after fatty alcohol dissolves fully, vacuumize 30min;
In another reactor B, add 20 mass parts C
20fatty alcohol and 20 mass parts C
22fatty alcohol, stirring is warming up to fatty alcohol and just dissolves (temperature is 70 ℃), adds 20 mass parts by 15 mass parts P
2o
5with 5 mass parts polyphosphoric acid (P
2o
5equivalent 85%) phosphorylating agent that the phosphorylating agent formed forms, open homogeneous 3min under-0.05MPa, obtain pre-dispersed thing, and the sealing froth breaking is stand-by;
By the pre-dispersed thing obtained in reactor B, divide and add rapidly for 5 times in reactor A, every minor tick 20min, after adding, reactor A maintains negative pressure-0.05MPa, continues reaction 8h;
(2) after step (1) reaction finishes, be cooled to 70 ℃.Add 8 mass parts deionized waters to be hydrolyzed, the time is 2.5h; Hydrolysis reaction adds the H that 3 mass parts concentration are mass percent 30% after finishing
2o
2, insulation 30min, then add 2.8 mass parts Na
2hSO
3, insulation 30min.Cooling discharge, obtain the lily C of outward appearance
20fatty alcohol and C
22fatty alcohol mixes pure phosphoric acid ester emulsifying agent.Analytical results is as shown in table 4:
Table 4
| Index | Result (mass percent %) |
| C 20～22The fatty alcohol phosphate monoester | 82.13 |
| C 20～22The fatty alcohol phosphate diester | 12.78 |
| Free phosphoric acid | 0.62 |
| Unreacted nonionic thing | 0.76 |
| Moisture | Surplus |
Comparative Examples 1: according to traditional way, carry out the reinforced of embodiment 1
(1) by 100 mass parts C
18fatty alcohol (stearyl alcohol), 0.05 mass parts butylated hydroxy anisole (BHA), 0.05 mass parts EDTA-2Na and 0.5 mass parts tosic acid add in reactor A, stir and are warming up to 110 ℃, treat C
18fatty alcohol vacuumizes 30min after dissolving fully;
By 20 mass parts by 10 mass parts P
2o
5the phosphorylating agent formed with 10 mass parts ortho-phosphoric acid divides and adds rapidly for 4 times in reactor A, every minor tick 15min, and after adding, reactor A maintains negative pressure-0.1MPa, continues reaction 5h.
(2) after step (1) reaction finishes, be cooled to 75 ℃.Add 12 mass parts deionized waters to be hydrolyzed, the time is 3h; Hydrolysis reaction adds the H that 3 mass parts concentration are mass percent 30% after finishing
2o
2, insulation 30min, then add 2.8 mass parts Na
2hSO
3, insulation 30min.Cooling discharge, obtaining appearance color is lurid C
18the fatty alcohol phosphate emulsifying agent.Analytical results is as shown in table 5:
Table 5
| Index | Result (mass percent %) |
| C 18The fatty alcohol phosphate monoester | 72.34 |
| C 18The fatty alcohol phosphate diester | 8.52 |
| Free phosphoric acid | 3.25 |
| Unreacted nonionic thing | 12.02 |
| Moisture | Surplus |
From Comparative Examples 1, can find out; adopt traditional feed way unreacted nonionic thing content higher; phosphate monoester and dibasic acid esters total amount descend; and provided by the invention phosphorus esterification reagent is pre-dispersed in to the technique in a part of reaction mass, can avoid the local caking of phosphorus esterification reagent and the inadequate problem of level of response.
Application Example
Prepare cream frost emulsion (corresponding formula I～V successively) with the emulsifying agent of above-described embodiment 1～4 and Comparative Examples 1 preparation, reference formulation is as shown in table 6 below:
Table 6 reference formulation
(mass percent of each material of data representation in table)
Preparation technology:
(1) by high-carbon fatty alcohol phosphoric acid ester emulsifying agent, iso-octyl palmitate, polydimethylsiloxane, hexadeca-octadecyl alcohol, 26# white oil, ℃ fusing of 2,6 di tert butyl 4 methyl phenol heated and stirred to 80, stand-by as oil phase;
(2) by xanthan gum, glycerine, propylene glycol, disodium ethylene diamine tetraacetate and water heated and stirred to 85 ℃, stand-by as water;
(3) trolamine is added in water;
(4) oil phase is added rapidly in water to 3000r/min homogeneous 5min;
(5) be cooled to room temperature, add extremely beautiful II, stir, obtain cream frost emulsion.
Stability test:
(1) sensory testing: the proterties of visual inspection product sees if there is abnormal;
(2) oven test: sample is put into to the electro-heating standing-temperature cultivator 24h of (40 ± 1) ℃, recovered after room temperature to observe whether thinning, variable color is arranged, the phenomenons such as layering and changes in hardness, with the resistance toheat of judgement sample;
(3) low temperature resistant test: sample is put into to the refrigerator 24h of (5～-10) ℃, recovered after room temperature to observe whether thinning, variable color is arranged, the phenomenons such as layering and changes in hardness, with the cold tolerance of judgement sample;
(4) centrifugal test: sample is placed in to whizzer, with the speed test 30min of 3000r/min, observes separation, the layering situation of sample.
Test result is as shown in table 7:
Table 7 stability test result
Annotate: the emulsion that in the successively corresponding table 6 of emulsion I～V, formula I～V prepares
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (10)
1. the preparation method of a high-carbon fatty alcohol phosphoric acid ester emulsifying agent is characterized in that comprising following steps:
(1) by C
18～22the straight chained alkyl fatty alcohol heats up while stirring; Work as C
18～22the straight chained alkyl fatty alcohol just dissolves fully, adds phosphorus esterification reagent, and homogeneous, obtain pre-dispersed thing, and the sealing froth breaking is stand-by;
(2) by C
18～22straight chained alkyl fatty alcohol, antioxidant, sequestrant and catalyzer mix, and are warming up to 110～125 ℃, treat C
18～22the straight chained alkyl fatty alcohol vacuumizes after dissolving fully, obtains reactant;
(3) pre-dispersed thing step (1) obtained joins in the reactant that step (2) obtains, and under condition of negative pressure, reacts;
(4) after reaction finishes, be cooled to 60～75 ℃, add deionized water to be hydrolyzed; Hydrolysis reaction adds the H that mass percent is 30% after finishing
2o
2decoloured, insulation;
(5) then add again Na
2hSO
3, insulation; Cooling discharge, obtain high-carbon fatty alcohol phosphoric acid ester emulsifying agent;
Wherein, the consumption of each raw material carries out proportioning by following mass ratio: C used in step (1)
18～22straight chained alkyl fatty alcohol: phosphorus esterification reagent: C used in step (2)
18～22straight chained alkyl fatty alcohol: antioxidant: sequestrant: catalyzer: the H of mass percent 30%
2o
2: Na
2hSO
3=40:20:60:0.05:0.05:0.5:(3～6): 2.8.
2. the preparation method of high-carbon fatty alcohol phosphoric acid ester emulsifying agent according to claim 1, is characterized in that: the C described in step (1) and (2)
18～22the straight chained alkyl fatty alcohol is at least one in the carbonatoms straight chained alkyl fatty alcohol that is 18～22.
3. the preparation method of high-carbon fatty alcohol phosphoric acid ester emulsifying agent according to claim 2, is characterized in that: described C
18～22the straight chained alkyl fatty alcohol is C
18fatty alcohol, C
20fatty alcohol and C
22at least one in fatty alcohol.
4. the preparation method of high-carbon fatty alcohol phosphoric acid ester emulsifying agent according to claim 1, it is characterized in that: the phosphorus esterification reagent described in step (1) is P
2o
5, at least one in ortho-phosphoric acid, metaphosphoric acid and polyphosphoric acid;
Antioxidant described in step (2) is at least one in gsh, vitamins C, vitamin-E, 2,6 di tert butyl 4 methyl phenol, butylated hydroxy anisole, butylated hydroxytoluene, gallic acid and Tenox PG;
Sequestrant described in step (2) is at least one in disodium ethylene diamine tetraacetate, tetrasodium ethylenediamine tetraacetate, sodium polyacrylate, etidronic acid and Etidronate disodium;
Catalyzer described in step (2) is at least one in tosic acid, paratoluenesulfonic acid sodium salt, tosic acid potassium and paratoluenesulfonic acid ammonium salt.
5. the preparation method of high-carbon fatty alcohol phosphoric acid ester emulsifying agent according to claim 1, it is characterized in that: the condition of the homogeneous described in step (1) is: pressure-0.05～-0.1MPa under homogeneous 3～5min;
The time vacuumized described in step (2) is 15～30min;
The pre-dispersed thing that step (1) is obtained described in step (3) joins in the reactant that step (2) obtains as to be operated as follows: the pre-dispersed thing that step (1) is obtained divides and joins for 4～6 times in the reactant that step (2) obtains, every minor tick 15～20min;
The condition of reacting under condition of negative pressure described in step (3) in-0.05～-react 5～8h under the 0.1MPa condition of negative pressure;
The consumption of the deionized water described in step (4) is for being equivalent to the described C of step (1)
18～222/10～3/10 of straight chained alkyl fatty alcohol quality;
The time of the hydrolysis described in step (4) is 1.5～3h;
The time of the insulation described in step (4) and (5) is 30min.
6. a high-carbon fatty alcohol phosphoric acid ester emulsifying agent, by claim 1～5 any one, described preparation method obtains.
7. high-carbon fatty alcohol phosphoric acid ester emulsifying agent according to claim 6, is characterized in that: the mixture that is high-carbon fatty alcohol phosphate monoester, high-carbon fatty alcohol phosphate diester, unreacted nonionic thing, free phosphoric acid and water; Wherein, the total mass per-cent of high-carbon fatty alcohol phosphate monoester and high-carbon fatty alcohol phosphate diester is greater than>and 94%, the content of the content of high-carbon fatty alcohol phosphate monoester>81%, high-carbon fatty alcohol phosphate diester<14% wherein, free phosphoric acid and unreacted nonionic thing total mass per-cent<2%, the content mass percent of free phosphoric acid<1%.
8. the application of high-carbon fatty alcohol phosphoric acid ester emulsifying agent claimed in claim 6 in preparing makeup.
9. a cream frost emulsion, contain high-carbon fatty alcohol phosphoric acid ester emulsifying agent claimed in claim 6.
10. cream according to claim 9 frost emulsion, it is characterized in that comprising the following composition of calculating by mass percentage: high-carbon fatty alcohol phosphoric acid ester emulsifying agent 0.5～2%, iso-octyl palmitate 2%, polydimethylsiloxane 2%, hexadeca-octadecyl alcohol 3%, 26# white oil 8%, glycerine 5%, xanthan gum 1%, propylene glycol 3%, trolamine 1.5%, disodium ethylene diamine tetraacetate 0.05%, 2,6 di tert butyl 4 methyl phenol 0.05%, extremely beautiful II0.1%.
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|---|---|---|---|
| CN201310469754.7A CN103483375B (en) | 2013-10-09 | 2013-10-09 | A kind of high-carbon fatty alcohol phosphoric acid ester emulsifying agent and preparation method thereof and application |
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| CN107337689A (en) * | 2017-07-13 | 2017-11-10 | 中国日用化学工业研究院 | A kind of synthetic method of alkyl phosphate monoester |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107337689A (en) * | 2017-07-13 | 2017-11-10 | 中国日用化学工业研究院 | A kind of synthetic method of alkyl phosphate monoester |
| CN107337689B (en) * | 2017-07-13 | 2020-05-05 | 中国日用化学工业研究院 | Synthesis method of alkyl phosphate monoester |
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