CN101838286A - Method and equipment for preparing fatty alcohol (ether) phosphate - Google Patents
Method and equipment for preparing fatty alcohol (ether) phosphate Download PDFInfo
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- CN101838286A CN101838286A CN 201010159509 CN201010159509A CN101838286A CN 101838286 A CN101838286 A CN 101838286A CN 201010159509 CN201010159509 CN 201010159509 CN 201010159509 A CN201010159509 A CN 201010159509A CN 101838286 A CN101838286 A CN 101838286A
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Abstract
The invention relates to a method and equipment for preparing fatty alcohol (ether) phosphate, and relates to a method and equipment for preparing fatty alcohol (or polyoxyalkylene fatty alcohol) phosphate with high purity and excellent color and luster. In the preparation process, a reactor with a stirrer is adopted; and the reactor is provided with one or two kinds of equipment of a homogenizer and a circulating pump outside the reactor. The method comprises the following preparation processes of: adding one material in fatty alcohol (ether) and a mixture or a phosphorus acylating agent totally or in parts, performing homogenization or high-speed stirring at a reaction temperature, and simultaneously, quantitatively adding the other material in the fatty alcohol (ether) and the mixture or the phosphorus acylating agent into the equipment continuously or in parts for quick homodisperse to prepare the fatty alcohol (ether) phosphate with high purity and white color and luster.
Description
Technical field:
The present invention relates to the manufacture method and the equipment of fatty alcohol (or polyoxy alkylidene Fatty Alcohol(C12-C14 and C12-C18)) phosphoric acid ester, specially refer to the manufacture method and the equipment of fatty alcohol (or the polyoxy alkylidene Fatty Alcohol(C12-C14 and C12-C18)) phosphoric acid ester of high purity, white shade.
Background technology:
Fatty alcohol (or polyoxy alkylidene Fatty Alcohol(C12-C14 and C12-C18)) phosphoric acid ester (being designated hereinafter simply as Fatty Alcohol(C12-C14 and C12-C18) (ether) phosphoric acid ester) is that a class is used anion surfactant very widely, and there are chemical fibre, weaving, leather, plastics, papermaking, washing composition and makeup etc. in the field that relates to.Multiple functional characteristics such as that this class tensio-active agent has is wetting, washing, solubilising, emulsification, lubricated, antirust, inhibition, dispersion, chelating, antistatic and biological degradability are good.
Fatty Alcohol(C12-C14 and C12-C18) (ether) phosphoric acid ester is to be made by the reaction of Fatty Alcohol(C12-C14 and C12-C18) or fatty alcohol-ether and phosphorylating agent.The kind of phosphorylating agent is a lot, and ortho-phosphoric acid, Vanadium Pentoxide in FLAKES, polyphosphoric acid, phosphorus trichloride, phosphorus oxychloride or their mixture are for example arranged.
In today that environment protection and safety in production more and more come into one's own, use strong pollution such as phosphorus trichloride, phosphorus oxychloride and highly toxic compound superseded day by day as the method for phosphorylating agent.Thus, normally used phosphorylating agent is main is exactly the single of ortho-phosphoric acid, Vanadium Pentoxide in FLAKES, this gang of polyphosphoric acid or their mixture.
Many reported in literature have been arranged and made Fatty Alcohol(C12-C14 and C12-C18) (ether) phosphoric acid ester by the reaction of the mixture more than a kind or 2 kinds in ortho-phosphoric acid, Vanadium Pentoxide in FLAKES, the polyphosphoric acid and Fatty Alcohol(C12-C14 and C12-C18) or alcohol ether.A large amount of patent reports only is that these methods are had various variation and improvement.
Japanese Patent (spy opens clear 55-064593) has disclosed the method for Vanadium Pentoxide in FLAKES and organic hydroxy compounds reaction, and its resultant is the almost equimolar mixture of phosphate monoester and phosphodiester, promptly so-called sesquialter phosphoric acid ester.
When Japanese Patent (special public clear 41-014416) has been put down in writing organic hydroxy compounds and Vanadium Pentoxide in FLAKES reaction manufacturing organophosphate, add the method that 0.5～3 mole of water adds Vanadium Pentoxide in FLAKES more earlier.
And for example Japanese Patent (special public clear 55-064593) has been put down in writing C
8～C
20Saturated or undersaturated Fatty Alcohol(C12-C14 and C12-C18) or alcohol ether and ortho-phosphoric acid under reduced pressure reacting by heating make Fatty Alcohol(C12-C14 and C12-C18) or pure ether phosphate.
There is following shortcoming in above-described the whole bag of tricks:
1) because ortho-phosphoric reactivity is low, reaction conversion ratio was not high when therefore list was with ortho-phosphoric acid, need at high temperature reach the water that will produce in the time of will being condensed into ester under the condition of high vacuum degree and boil off, and this will cause product color to be deepened.
2) Vanadium Pentoxide in FLAKES reactive behavior height, but owing to be solid, the reaction with Fatty Alcohol(C12-C14 and C12-C18) under reaction conditions is not a homogeneous reaction, with the reaction of longer carbochain Fatty Alcohol(C12-C14 and C12-C18) in the reaction solution thickness, make it can not disperse to participate in reaction well.Therefore, reaction conversion ratio is also not high, is difficult to Fatty Alcohol(C12-C14 and C12-C18) in the product (ether) phosphoric acid ester is controlled at high purity, and color and luster is deepened.
3) ortho-phosphoric acid, Vanadium Pentoxide in FLAKES, polyphosphoric acid are mixed into to mix phosphorylating agent be method relatively preferably, reactive behavior is also enough, and reaction solution also is homogeneous phase basically.But this mixes phosphorylating agent itself than thickness, adds in the popular response still and reacts, and still is difficult to control it and reacts well, causes product purity low, shade deviation.
Summary of the invention:
The technical problem to be solved in the present invention is to overcome deficiency of the prior art, proposes a kind of manufacture method and equipment of new Fatty Alcohol(C12-C14 and C12-C18) (ether) phosphoric acid ester, not only operates simple and easyly, and obtains Fatty Alcohol(C12-C14 and C12-C18) (ether) phosphoric acid ester of high purity, white shade.
The present invention is achieved by the following technical measures.The producing apparatus of Fatty Alcohol(C12-C14 and C12-C18) (ether) phosphoric acid ester comprises the top cover with material inlet, has the housing of reaction product relief outlet, and the heating jacket of hull outside, and agitator also comprise homogenizer.
The producing apparatus of Fatty Alcohol(C12-C14 and C12-C18) (ether) phosphoric acid ester also comprises still outer circulation pump.
The rotating speed of described agitator is 100～500rpm.(rpm: rotations per minute)
Described homogenizer places the inboard of housing.
Described homogenizer places the outside of housing, links to each other with top cover with pipeline.
Described homogenizer places the inboard of housing, links to each other with still outer circulation pump by pipeline.
The rotating speed of described homogenizer is 600～4500rpm.
The manufacture method of fatty alcohol (ether) phosphoric acid ester; be under temperature of reaction; with the mixture of phosphorylating agent and fatty alcohol (ether) or fatty alcohol (ether) mutually at regular time and quantity, step by step, mix equably; and material carried out quick homodisperse; impel reaction evenly to carry out, obtain fatty alcohol (ether) phosphoric acid ester.
In equipment, add the mixture of fatty alcohol (ether) or fatty alcohol (ether), and heat, under temperature of reaction, add phosphorylating agent at regular time and quantity, step by step, equably, above-mentioned material is carried out quick homodisperse, impel reaction evenly to carry out.
In equipment, add phosphorylating agent, and heat, under temperature of reaction, add the mixture of fatty alcohol (ether) or fatty alcohol (ether) at regular time and quantity, step by step, equably, above-mentioned material is carried out quick homodisperse, impel reaction evenly to carry out.
In equipment, add the mixture of part fatty alcohol (ether) or fatty alcohol (ether), and heat, under temperature of reaction, add the part phosphorylating agent at regular time and quantity, step by step, equably, above-mentioned material is carried out quick homodisperse, impel reaction evenly to carry out; Continue to add the mixture of part fatty alcohol (ether) or fatty alcohol (ether), add the part phosphorylating agent again, still material is carried out quick homodisperse, impel reaction evenly to carry out; Proceed successively, up to the end that feeds intake.
In equipment, add the part phosphorylating agent, and heat, under temperature of reaction, add the mixture of fatty alcohol (ether) or fatty alcohol (ether) at regular time and quantity, step by step, equably, above-mentioned material is carried out quick homodisperse, impel reaction evenly to carry out; Continue to add the part phosphorylating agent, add the mixture phosphorylating agent of part fatty alcohol (ether) or fatty alcohol (ether) again, still material is carried out quick homodisperse, impel reaction evenly to carry out; Proceed successively, up to the end that feeds intake.
In the process of feeding intake, the adding speed control that material is dropped in the back feed intake at every turn account for the total amount that feeds intake 5～100% between.
Described reaction product is the product of Fatty Alcohol(C12-C14 and C12-C18) (ether) phosphoric acid ester total content in the high purity more than 80%, white shade.
Preparation process has been used the reactor equipment that contains homogenizer in the still, the outer homogenizer of still or one or two or more kinds combination of agitator; once or gradation add earlier a kind of material among Fatty Alcohol(C12-C14 and C12-C18) (ether) and composition thereof or the phosphorylating agent; under temperature of reaction, open homogeneous or (reaching) stirring; simultaneously continuously or gradation with in the another kind of material dosing ground adding equipment among phosphorylating agent or Fatty Alcohol(C12-C14 and C12-C18) (ether) and composition thereof; carry out quick homodisperse, to obtain Fatty Alcohol(C12-C14 and C12-C18) (ether) phosphoric acid ester of high purity, white shade.
Described homogenizer, its principle of work is to rotate stably by rotor high-speed, form comprehensive kinetic energy effect such as high frequency, intensive centrifugal force, tangent to periphery speed, angle speed, under the stator effect, form combined effects such as shearing friction, centrifugal extruding, the collision of liquid stream, make immiscible or difficult mix two-phase or multiphase promptly, equably, fine and smooth ditch is to dispersion, homogeneous.Use in the present invention, the Fatty Alcohol(C12-C14 and C12-C18) (ether) that makes participation react contacts equably rapidly with phosphorylating agent and disperses exactly, thereby reaches the ideal reaction effect.
Described fatty alcohol can be known C in the industry
8～C
22Saturated or the unsaturated long chain aliphatic alcohol of straight or branched, Fatty Alcohol(C12-C14 and C12-C18), synthol or their mixture of natural origin, above raw material can be bought by commerce and obtain.
The polyoxyethylene that described polyoxy alkylidene Fatty Alcohol(C12-C14 and C12-C18) is above-mentioned Fatty Alcohol(C12-C14 and C12-C18) and (or) the polyoxypropylene affixture, and the mixture of these alcohol or alcohol ether, above raw material can be bought by commerce and obtain.
Described phosphorylating agent is known ortho-phosphoric acid in the industry, Vanadium Pentoxide in FLAKES, polyphosphoric acid etc. and their mixture, and above raw material can be bought by commerce and obtain.
After the present invention adopts abovementioned technology; when under homogeneous or high-speed stirring condition, adding to a kind of material dosing among Fatty Alcohol(C12-C14 and C12-C18) (ether) and composition thereof or the phosphorylating agent in the another kind of material equably; the moment of reaction can not make Fatty Alcohol(C12-C14 and C12-C18) (ether) or the excessive uneven situation of reaction that causes of phosphorylating agent partial concn; use above-mentioned conversion unit not only to make Fatty Alcohol(C12-C14 and C12-C18) (ether) phosphoric acid ester reaction conversion ratio quite high simultaneously; and speed of response is also very fast; reaction does not need material is heated for a long time; therefore avoid the too much by product that causes; the color and luster of reaction product can not deepened yet, thereby obtains Fatty Alcohol(C12-C14 and C12-C18) (ether) phosphoric acid ester in high purity white pool.
Description of drawings:
Accompanying drawing 2 is the embodiment of the invention 2 employed equipment synoptic diagram;
Accompanying drawing 3 is the embodiment of the invention 4 employed equipment synoptic diagram.
Among the figure: 1 is material inlet, and 2 is top cover, and 3 is housing, and 4 is product offtake, and 5 is heating jacket, and 6 is agitator, and 7 is homogenizer, and 8 is still outer circulation pump.
Embodiment:
The invention will be further described below in conjunction with drawings and Examples.
As shown in Figure 1, lauryl alcohol 150kg added by material inlet 1 have in the equipment of agitator 6 and clarifixator 7, utilize heating jacket 5, while stirring heat temperature raising to 40～45 ℃.Open clarifixator 7, rotating speed is controlled at 3000rpm, and Vanadium Pentoxide in FLAKES 30kg gradation is added, and per hour adds speed control in 30% of the whole amounts of Vanadium Pentoxide in FLAKES.Finish and be warming up to 100～105 ℃, continue reaction 3h.Under agitator stirs, be cooled to 50～55 ℃ of dischargings then, promptly get Tryfac 5573.The detection data are shown in Table 1.In the present embodiment, also can utilize the equipment shown in accompanying drawing 2 and the accompanying drawing 3 to produce.
As shown in Figure 1, lauryl alcohol 150kg added by material inlet 1 have in the equipment of agitator 6 and clarifixator 7, utilize heating jacket 5, while stirring heat temperature raising to 40～45 ℃.Open clarifixator 7, rotating speed is controlled at 3000rpm, and 30kg evenly adds with Vanadium Pentoxide in FLAKES, per hour adds speed control in 70% of the whole amounts of Vanadium Pentoxide in FLAKES.Finish and be warming up to 100～105 ℃, continue reaction 3h.Under agitator stirs, be cooled to 50～55 ℃ of dischargings then, promptly get Tryfac 5573.The detection data are shown in Table 1.In the present embodiment, also can utilize the equipment shown in accompanying drawing 2 and the accompanying drawing 3 to produce.
As shown in Figure 2, cetostearyl alcohol 150kg added by material inlet 1 have in the equipment of agitator 6, utilize heating jacket 5 heat temperature raising to 80～85 ℃ while stirring.Be open at the clarifixator 7 of equipment outside, the control rotating speed homogenizes the material in the equipment at 1500rpm by clarifixator 7; And will send back to again in the equipment through the material behind clarifixator 7 homogeneous by pipeline, simultaneously polyphosphoric acid 50kg is evenly added, per hour add speed control polyphosphoric acid all amount 70%.Be warming up to 135～140 ℃ after finishing, continue reaction 3h.Under agitation be cooled to 70～75 ℃ of dischargings then, promptly get the cetearyl phosphoric acid ester.The detection data are shown in Table 1.In the present embodiment, also can utilize the equipment shown in accompanying drawing 1 and the accompanying drawing 3 to produce.
As shown in Figure 1, hexadecanol 150kg is had in the equipment of agitator 6 and clarifixator 7 by material inlet 1 input, utilize heating jacket 5.Heat temperature raising to 80～85 ℃ while stirring.Open clarifixator 7, the control rotating speed is at 2500rpm, and (polyphosphoric acid: Vanadium Pentoxide in FLAKES=1: 3) 50kg evenly adds, and per hour adds speed control for mixing 25% of the whole amounts of phosphorylating agent with pre-configured.Finish and be warming up to 120～125 ℃, continue reaction 3h.Under common stirring, be cooled to 65～70 ℃ of dischargings then, promptly get the hexadecyl phosphoric acid ester.The detection data are shown in Table 1.In the present embodiment, also can utilize the equipment shown in accompanying drawing 2 and the accompanying drawing 3 to produce.
As shown in Figure 1, hexadecanol 150kg is had in the equipment of agitator 6 and clarifixator 7 by material inlet 1 input, utilize heating jacket 5 heat temperature raising to 80～85 ℃ while stirring.Open clarifixator 7, the control rotating speed is at 2500rpm, and (polyphosphoric acid: Vanadium Pentoxide in FLAKES=1: 3) 50kg evenly adds, and per hour adds speed control 100% hour for the whole amounts of mixing phosphorylating agent with pre-configured mixing phosphorylating agent.Finish and be warming up to 120～125 ℃, continue reaction 3h.Under agitation be cooled to 65～70 ℃ of dischargings then, promptly get the hexadecyl phosphoric acid ester.The detection data are shown in Table 1.In the present embodiment, also can utilize the equipment shown in accompanying drawing 2 and the accompanying drawing 3 to produce.
As shown in Figure 3, lauryl alcohol 3 (AEO3) 150kg is had in the equipment of agitator 6 and clarifixator 7 by material inlet 1 input, while stirring heat temperature raising to 45～50 ℃.Be open at the still outer circulation pump 8 of equipment outside; open clarifixator 7 simultaneously; the control rotating speed is at 2400rpm, and (polyphosphoric acid: Vanadium Pentoxide in FLAKES=1: 3) 15kg evenly adds, and per hour adds speed control for mixing 10% of the whole amounts of phosphorylating agent with pre-configured mixing phosphorylating agent.After material in the equipment homogenized by clarifixator 7 and will expect to send back to again in the equipment, finish simultaneously and be warming up to 95～100 ℃, continue to react 3h by still outer circulation pump 8 and pipeline.Under common stirring, be cooled to 45～50 ℃ of dischargings then, promptly get lauryl ether-3 phosphoric acid ester.The detection data are shown in Table 1.In the present embodiment, also can utilize the equipment shown in accompanying drawing 1 and the accompanying drawing 2 to produce.
(polyphosphoric acid: Vanadium Pentoxide in FLAKES=1: 3) 50kg evenly adds except phosphorylating agent being changed into the mixing phosphorylating agent; per hour add speed control for mixing 100% of the whole amounts of phosphorylating agent; and the rotating speed of control clarifixator 7 repeats embodiment 1 outside 2700rpm.Obtain Tryfac 5573.The detection data are shown in Table 1.In the present embodiment, also can utilize the equipment shown in accompanying drawing 2 and the accompanying drawing 3 to produce.
As shown in Figure 1, the mixture 75kg of lauryl alcohol 75kg and lauryl alcohol 2 and Semen Myristicae alcohol ether 2 dropped into by material inlet 1 have in the equipment of agitator 6 and clarifixator 7, utilize heating jacket 5, stir and 50～55 ℃ of heat temperature raisings.Open clarifixator 7, rotating speed is controlled at 800rpm, and (polyphosphoric acid: Vanadium Pentoxide in FLAKES=1: 3) 50kg evenly adds, and per hour adds speed control for mixing 30% of the whole amounts of phosphorylating agent with pre-configured mixing phosphorylating agent.Finish and be warming up to 100～105 ℃, continue reaction 3h.Under agitation be cooled to 50～55 ℃ of dischargings then, promptly get the mixed phosphate ester of lauryl alcohol and lauryl alcohol and tetradecyl alcohol mixed alcohol ether 2.The detection data are shown in Table 1.In the present embodiment, also can utilize the equipment shown in accompanying drawing 2 and the accompanying drawing 3 to produce.
Embodiment 9
As shown in Figure 1, hexadecanol 150kg is had in the equipment of agitator 6 and clarifixator 7 by material inlet 1 input, utilize heating jacket 5.Heat temperature raising to 80～85 ℃ while stirring.Open clarifixator 7, the control rotating speed is at 4500rpm, and 65kg evenly adds with ortho-phosphoric acid, per hour adds speed control in 50% of the whole amounts of ortho-phosphoric acid.Finish and be warming up to 120～125 ℃, continue reaction 3h.Under agitation be cooled to 75～80 ℃ of dischargings then, promptly get the hexadecyl phosphoric acid ester.The detection data are shown in Table 1.In the present embodiment, also can utilize the equipment shown in accompanying drawing 2 and the accompanying drawing 3 to produce.
Embodiment 10
As shown in Figure 1, (polyphosphoric acid: Vanadium Pentoxide in FLAKES=1: 3) 50kg has in the equipment of agitator 6 and clarifixator 7 by material inlet 1 input, utilizes heating jacket 5, while stirring heat temperature raising to 40～45 ℃ with pre-configured mixing phosphorylating agent.Open clarifixator 7, rotating speed is controlled at 3000rpm, and 150kg evenly adds with lauryl alcohol, per hour adds speed control in 50% of the whole amounts of lauryl alcohol.Finish and be warming up to 100～105 ℃, continue reaction 2.5h.Under agitation be cooled to 50～55 ℃ of dischargings then, be about to Tryfac 5573.The detection data are shown in Table 1.In the present embodiment, also can utilize the equipment shown in accompanying drawing 2 and the accompanying drawing 3 to produce.
Embodiment 11
As shown in Figure 1, ortho-phosphoric acid 30kg is had in the equipment of agitator 6 and clarifixator 7 by material inlet 1 input, utilize heating jacket 5, while stirring heat temperature raising to 60～65 ℃.Open clarifixator 7, rotating speed is controlled at 2000rpm, and 150kg lauryl alcohol-2 is evenly added, and per hour adds speed control in 100% of the whole amounts of lauryl alcohol-2.Finish and be warming up to 100～105 ℃, once more Vanadium Pentoxide in FLAKES 25kg is evenly added, per hour add speed control in 25% of the whole amounts of Vanadium Pentoxide in FLAKES.Finish and continue reaction 2h.Under common stirring, be cooled to 50～55 ℃ of dischargings then, be about to lauryl alcohol-2 phosphoric acid ester.The detection data are shown in Table 1.In the present embodiment, also can utilize the equipment shown in accompanying drawing 2 and the accompanying drawing 3 to produce.
Comparative example 1
Comparative example 2
Comparative example 3
Repeat embodiment 11, promptly evenly add, but do not use clarifixator, product lauryl ether 2 phosphoric acid ester that obtain by the order of well-established law with ortho-phosphoric acid-lauryl alcohol 2-Vanadium Pentoxide in FLAKES.The detection data are shown in Table 1.
Annotate 1: the group that the color and luster of product is made up of experimenter person 5 people is with the sensory testing---visual method, comply with following standard determination:
White: white and glossy; Amber; Pale brown look.With the most result of determination of 5 philtrums is foundation.Annotate 2: adopt 5% aqueous solution of potentiometric titration during the numerical value of the monoesters of product, diester and total ester to product
Carry out determination of acid value, press the content that the column count formula calculates monoesters, diester, both additions then are total ester contents.
X in the formula
1Be monoester content, X
2Be two ester contents, X
3Be free phosphoric acid content; C is the actual concentrations of titrating solution potassium hydroxide-ethanol solution, M
1Be the molecular weight of monoesters, M
2Be the molecular weight of diester, V
1, V
2And V
3Be respectively from beginning to be titrated to the milliliter number of first, second and third potassium hydroxide-ethanol solution that hop point consumes; M is a sample quality.
From table, can learn, use clarifixator especially to adopt the clarifixator of higher rotation speed, control suitable adding speed simultaneously, not only the product color and luster is white, Fatty Alcohol(C12-C14 and C12-C18) (ether) phosphate ester content is also high, and free phosphoric acid content has also significantly reduced, and has reached effect of the present invention.
Above-described only is the preferred embodiment for the present invention.Should be pointed out that for the person of ordinary skill of the art under the premise of not departing from the present invention, can also make some modification and improvement, these also should be considered as belonging to protection scope of the present invention.
Claims (14)
1. the producing apparatus of Fatty Alcohol(C12-C14 and C12-C18) (ether) phosphoric acid ester, comprise the have material inlet top cover (2) of (1), have the housing (3) of reaction product relief outlet (4), the heating jacket (5) in housing (3) outside, and agitator (6), it is characterized in that: also comprise homogenizer (7).
2. the producing apparatus of Fatty Alcohol(C12-C14 and C12-C18) according to claim 1 (ether) phosphoric acid ester is characterized in that: also comprise still outer circulation pump (8).
3. the producing apparatus of Fatty Alcohol(C12-C14 and C12-C18) according to claim 1 (ether) phosphoric acid ester is characterized in that: the rotating speed of described agitator (6) is 100～500rpm.(rpm: rotations per minute)
4. the producing apparatus of Fatty Alcohol(C12-C14 and C12-C18) according to claim 1 (ether) phosphoric acid ester is characterized in that: described homogenizer (7) places the inboard of housing (3).
5. the producing apparatus of Fatty Alcohol(C12-C14 and C12-C18) according to claim 1 (ether) phosphoric acid ester is characterized in that: described homogenizer (7) places the outside of housing (3), links to each other with top cover (2) with pipeline.
6. the producing apparatus of Fatty Alcohol(C12-C14 and C12-C18) according to claim 1 (ether) phosphoric acid ester is characterized in that: described homogenizer (7) places the inboard of housing (3), links to each other with still outer circulation pump (8) by pipeline.
7. the producing apparatus of Fatty Alcohol(C12-C14 and C12-C18) according to claim 1 (ether) phosphoric acid ester is characterized in that: the rotating speed of described homogenizer (7) is 600～4500rpm.
8. the manufacture method of fatty alcohol (ether) phosphoric acid ester; it is characterized in that: under temperature of reaction; with the mixture of phosphorylating agent and fatty alcohol (ether) or fatty alcohol (ether) mutually at regular time and quantity, step by step, mix equably; and material carried out quick homodisperse; impel reaction evenly to carry out, obtain fatty alcohol (or ether) phosphoric acid ester.
9. the manufacture method of fatty alcohol according to claim 1 (ether) phosphoric acid ester; it is characterized in that: in equipment; the mixture that adds fatty alcohol (ether) or fatty alcohol (ether); and heat; under temperature of reaction; add phosphorylating agent at regular time and quantity, step by step, equably, above-mentioned material is carried out quick homodisperse, impel reaction evenly to carry out.
10. the manufacture method of fatty alcohol according to claim 1 (ether) phosphoric acid ester; it is characterized in that: in equipment; add phosphorylating agent; and heat; under temperature of reaction; add the mixture of fatty alcohol (ether) or fatty alcohol (ether) at regular time and quantity, step by step, equably, above-mentioned material is carried out quick homodisperse, impel reaction evenly to carry out.
11. the manufacture method of fatty alcohol according to claim 1 (ether) phosphoric acid ester, it is characterized in that: in equipment, the mixture that adds part fatty alcohol (ether) or fatty alcohol (ether), and heat, under temperature of reaction, add the part phosphorylating agent at regular time and quantity, step by step, equably, above-mentioned material is carried out quick homodisperse, impel reaction evenly to carry out; Continue to add the mixture of part fatty alcohol (ether) or fatty alcohol (ether), add the part phosphorylating agent again, still material is carried out quick homodisperse, impel reaction evenly to carry out; Proceed with this, up to the end that feeds intake.
12. the manufacture method of fatty alcohol according to claim 1 (ether) phosphoric acid ester, it is characterized in that: in equipment, add the part phosphorylating agent, and heat, under temperature of reaction, add the mixture of fatty alcohol (ether) or fatty alcohol (ether) at regular time and quantity, step by step, equably, above-mentioned material is carried out quick homodisperse, impel reaction evenly to carry out; Continue to add the part phosphorylating agent, add the mixture phosphorylating agent of part fatty alcohol (ether) or fatty alcohol (ether) again, still material is carried out quick homodisperse, impel reaction evenly to carry out; Proceed with this, up to the end that feeds intake.
13. the manufacture method of fatty alcohol phosphoric acid ester according to claim 1 is characterized in that: the adding speed control that material is dropped in the back feed intake at every turn account for the total amount that feeds intake 5～100% between.
14. the manufacture method of Fatty Alcohol(C12-C14 and C12-C18) (ether) phosphoric acid ester, its feature exists: described reaction product is the product of Fatty Alcohol(C12-C14 and C12-C18) (ether) phosphoric acid ester total content in the high purity white pool more than 80%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103012469A (en) * | 2012-12-29 | 2013-04-03 | 山东科技大学 | Method for preparing high-carbon alkyl phosphate for cosmetics |
| CN103483375A (en) * | 2013-10-09 | 2014-01-01 | 广州潮徽化工科技有限公司 | High-carbon fatty alcohol phosphate ester emulsifier, and preparation method and application thereof |
| CN106317106A (en) * | 2015-06-18 | 2017-01-11 | 上海福岛化工科技发展有限公司 | Method for synthesizing phosphate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012469A (en) * | 2012-12-29 | 2013-04-03 | 山东科技大学 | Method for preparing high-carbon alkyl phosphate for cosmetics |
| CN103012469B (en) * | 2012-12-29 | 2015-10-28 | 山东科技大学 | The preparation method of high alkyl phosphate used for cosmetic |
| CN103483375A (en) * | 2013-10-09 | 2014-01-01 | 广州潮徽化工科技有限公司 | High-carbon fatty alcohol phosphate ester emulsifier, and preparation method and application thereof |
| CN103483375B (en) * | 2013-10-09 | 2016-03-16 | 广州潮徽化工科技有限公司 | A kind of high-carbon fatty alcohol phosphoric acid ester emulsifying agent and preparation method thereof and application |
| CN106317106A (en) * | 2015-06-18 | 2017-01-11 | 上海福岛化工科技发展有限公司 | Method for synthesizing phosphate |
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