Fatty alcohol polyether phosphate and preparation method thereof

By reacting fatty alcohol ethers with glucose via glycosylation followed by esterification with phosphorus pentoxide, a fatty alcohol polyether phosphate ester with excellent aluminum alloy corrosion inhibition and high emulsifying properties was prepared. This method solves the problem of insufficient protective performance of existing phosphate esters in harsh environments and realizes a low-cost and environmentally friendly preparation method.

CN121801071APending Publication Date: 2026-04-07深圳市如钦巴化学材料有限公司
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2026-01-20
Publication Date
2026-04-07

AI Technical Summary

Technical Problem

Existing phosphate esters offer limited protection for aluminum alloys in harsh corrosive environments, and traditional preparation methods require advanced equipment, are costly, and fail to meet environmental protection requirements.

Method used

Fatty alcohol ethers were used as initiators for phosphate molecules. After glycosylation with glucose, they were esterified with phosphorus pentoxide to prepare fatty alcohol polyether phosphate esters. This was a simple preparation method under normal pressure, which improved the corrosion inhibition and emulsification properties of aluminum alloys.

Benefits of technology

The prepared fatty alcohol polyether phosphate ester exhibits excellent aluminum alloy corrosion inhibition, lubrication extreme pressure, and high emulsification properties under normal pressure. Moreover, it is made from abundant raw materials, is easy and environmentally friendly to prepare, and has low cost.

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Abstract

The invention discloses fatty alcohol polyether phosphate and a preparation method thereof.The preparation method comprises the steps that firstly, glucose and fatty alcohol polyether are subjected to a glycosylation reaction, and glycosylated fatty alcohol polyether is obtained; and then, carrying out phosphate esterification on the glycosylated fatty alcohol polyether and phosphorus pentoxide to obtain monoester and diester of the glycosylated fatty alcohol polyether. According to different addition numbers of amine ether alkyl, EO, PO and sugar units, the performance of the finally obtained phosphate ester is adjusted from the molecular structure, and the obtained fatty alcohol polyether phosphate ester has better corrosion inhibition performance, lubricating extreme pressure performance and higher emulsifying performance on aluminum alloy on the basis of original fatty alcohol ether phosphate ester.
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Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of phosphate esters, and particularly relates to a novel fatty alcohol polyether phosphate ester and a preparation method thereof. BACKGROUND

[0002] Phosphate esters are a class of important organic compounds, which have a wide range of applications in many fields such as industry, agriculture, medicine, etc. Phosphate esters are important intermediates for many pesticides, which can be used to synthesize insecticides, fungicides and herbicides, etc. For example, trichlorfon, dimethoate and other common pesticides contain phosphate ester structures. Certain phosphate ester compounds have the function of regulating plant growth and can be used as plant growth regulators. They can promote the growth, development and flowering of plants, and improve the yield and quality of crops. Phosphate esters have emulsifying properties and can reduce the surface tension of liquids. This makes them widely used in detergents, emulsifiers, dispersants, etc. For example, alkyl phosphate esters can be used as anionic emulsifiers with good detergency, foaming and emulsifying properties. In metal working fluids, phosphate esters can be used as corrosion inhibitors to form a protective film on the metal surface, preventing metal corrosion and ensuring the smooth progress of aluminum alloy workpiece processing. Phosphate ester treatment can form an effective protective film under different aluminum alloy compositions and surface conditions, and has strong adaptability to factors such as aluminum alloy material and surface roughness. At the same time, the surface of the treated aluminum alloy can be subjected to subsequent processing such as coating and electroplating without affecting other processing processes.

[0003] Compared with traditional chromate treatment, phosphate ester treatment does not contain toxic hexavalent chromium ions, has less harm to the environment and human health, and meets environmental protection requirements. With the increasing strictness of environmental protection regulations, phosphate ester protection method has a broader application prospect.

[0004] Phosphate ester raw materials are relatively easy to obtain, and the treatment process is simple, without the need for complex equipment and high production costs. This makes phosphate ester protection of aluminum alloy have economic advantages in large-scale industrial production.

[0005] Patent application 201410673956.8 discloses a tall oil acid diethanolamide phosphate ester, whose chemical formula is as follows: or tall oil acid diethanolamide phosphate ester with single ester and double ester structures, respectively. Wherein R is a straight chain of C18 C24. In addition to being used for steel processing, the present application can also be used for aluminum alloy processing. Compared with existing tall oil acid diethanolamide borate esters, it has the advantages of strong extreme pressure, less rancidity of compounded liquid, low requirement for water quality for compounding, and wide application field, etc.

[0006] Although the phosphate ester on the market can protect the aluminum alloy to some extent, its protective performance is still limited. In severe corrosive environments, such as high humidity, strong acid and alkali, etc., the phosphate ester conversion film may be damaged, resulting in corrosion of the aluminum alloy. Therefore, it is urgent to synthesize a new type of phosphate ester with more efficient structure. SUMMARY

[0007] To solve the above problems, the primary purpose of the present application is to provide a fatty alcohol polyether phosphate and a preparation method thereof. In the molecular design, fatty alcohol ether is selected as the starting agent of the phosphate ester molecule. Glycosylation is carried out with glucose to obtain glycosylated fatty alcohol ether. Then, esterification reaction is carried out with phosphorus pentoxide. The obtained fatty alcohol polyether phosphate has better corrosion inhibition performance, lubricity and extreme pressure performance and higher emulsifying performance on the basis of the original fatty alcohol ether phosphate.

[0008] Another purpose of the present application is to provide a fatty alcohol polyether phosphate and a preparation method thereof. The main raw material is abundant in source, and the preparation method is simple, easy to operate and environmentally friendly. At the same time, the preparation method is carried out under normal pressure, which has low requirements for equipment production conditions and low cost.

[0009] To achieve the above purpose, the technical scheme of the present application is as follows.

[0010] A fatty alcohol polyether phosphate, comprising the following general formulae I and II:

[0011] Fatty alcohol polyether phosphate monoester of formula I

[0012] Fatty alcohol polyether phosphate diester of formula II

[0013] Wherein, R is a linear or branched saturated or unsaturated hydrocarbon group with C4-C18; EO is an ethylene oxide unit; a is a number from 1 to 20; PO is a propylene oxide unit; b is a number from 0 to 10; G is a sugar unit with 5 or 6 carbon atoms; and n is a number from 1 to 10.

[0014] When R is a linear or branched saturated or unsaturated hydrocarbon group with C4-C18; EO is an ethylene oxide unit; a is a number from 1 to 20; PO is a propylene oxide unit; b is a number from 0 to 10; G is a sugar unit with 5 or 6 carbon atoms; and n is a number from 1 to 10, the obtained product exhibits excellent aluminum alloy corrosion resistance and emulsifying ability, and the cutting fluid made therefrom has a long service life.

[0015] Further, the R is a C10-C18 straight chain or branched chain saturated or unsaturated hydrocarbon group; EO is an ethylene oxide unit; a is a number from 1 to 8; PO is a propylene oxide unit; b is a number from 0 to 5; G is a sugar unit of 5 or 6 carbon atoms; and n is a number from 1 to 4.

[0016] Further, the R is a C10-C18 straight chain or branched chain saturated or unsaturated hydrocarbon group; EO is an ethylene oxide unit; a is a number from 1 to 8; PO is a propylene oxide unit; b is a number from 0 to 5; G is a sugar unit of 5 or 6 carbon atoms; and n is a number from 1 to 4.

[0017] The present application selects a fatty alcohol ether as a starting agent of a phosphate ester molecule, performs glycosidation with glucose to obtain a glycosidation fatty alcohol ether, and then performs esterification reaction of the glycosidation fatty alcohol ether with diphosphorus pentoxide, so that the obtained product has better corrosion inhibition performance and higher emulsification performance on aluminum alloy.

[0018] The present application realizes a preparation method of a fatty alcohol polyether phosphate ester, first, performs glycosidation reaction of glucose and a fatty alcohol polyether to obtain a glycosidation fatty alcohol polyether; and then performs phosphate esterification of the glycosidation fatty alcohol polyether with diphosphorus pentoxide, and specifically includes the following steps:

[0019] Step (1), glycosidation reaction; glucose and a fatty alcohol ether are added into a reactor, glycosidation reaction is performed under the presence of an acid catalyst and vacuum conditions, after the reaction, unreacted sugar is removed by filtration or sedimentation to obtain a glycosidation modified alcohol ether, as shown in the following formula;

[0020]

[0021] Step (2), phosphate esterification reaction; the obtained glycosidation modified alcohol ether is placed into an experimental device provided with a stirrer, a thermometer, a water separator and a condenser tube, is inertized, and then is finally protected by inert gas, the condenser is opened, the temperature is raised to 40-80 DEG C for reaction, diphosphorus pentoxide is uniformly added in several times, the temperature rise of the reaction is controlled to be less than 5 DEG C, and a fatty alcohol polyether phosphate ester is obtained, as shown in the following formula:

[0022] .

[0023] The uniform addition in several times means that the diphosphorus pentoxide is evenly divided into several parts, and is added in several times corresponding to the several parts within the reaction time.

[0024] Further, in step (1), the glucose and the fatty alcohol ether are added into the reactor in a molar ratio of (1.20-12.00):1, glycosidation reaction is performed at 100-130 DEG C under the presence of an acid catalyst and the vacuum condition of a system pressure of 1-30 mHg.

[0025] Furthermore, the molar ratio of glucose to fatty alcohol polyether is (1.20~4.80):1; the fatty alcohol polyether is any one of isomeric decayl alcohol polyether, isomeric tridecayl alcohol polyether, and oleyl alcohol polyether.

[0026] Furthermore, the acid catalyst is either p-toluenesulfonic acid or dodecylbenzenesulfonic acid, and the amount of catalyst used is 0.2% to 0.5% of the total mass of glucose and alcohol ether. After the reaction, the temperature is lowered to 80 to 90°C, NaOH is added to neutralize to a pH of 8 to 9, and unreacted sugars are removed by filtration or sedimentation to obtain glycosylated modified alcohol ether.

[0027] Furthermore, the obtained glycosylated modified alcohol ether was placed in an experimental apparatus equipped with a stirrer, thermometer, water separator and condenser. The experimental apparatus was inertized three times. Finally, inert gas was introduced for protection, the condenser was turned on, and the temperature was raised to 40~80℃ for reaction. Phosphorus pentoxide was evenly divided into 8~10 portions and added in 8~10 portions over 6~10 hours. The reaction temperature was controlled to rise by less than 5℃. The esterification reaction was considered to be complete when the acid value no longer changed within half an hour.

[0028] Furthermore, in the phosphorylation reaction, the molar ratio of glycosylated modified alcohol ether to phosphorus pentoxide is: glycosylated modified alcohol ether: phosphorus pentoxide = (1~2):1.

[0029] Furthermore, the molar ratio of glycosylated modified alcohol ether to phosphorus pentoxide is (1.5~2):1. The resulting product exhibits excellent aluminum alloy corrosion resistance, lubrication under extreme pressure, and emulsification ability.

[0030] The inert gas is either nitrogen or argon.

[0031] Compared with the prior art, the beneficial effects of the present invention are:

[0032] In this invention, fatty alcohol ethers are selected as initiators for phosphate ester molecules in molecular design. Glycosylation with glucose yields glycosylated fatty alcohol ethers. Then, the glycosylated fatty alcohol ethers are esterified with phosphorus pentoxide. The resulting fatty alcohol polyether phosphate ester has better corrosion inhibition properties, lubrication extreme pressure properties, and higher emulsification properties for aluminum alloys.

[0033] Meanwhile, the main raw materials used in this invention are abundant, and the preparation method is simple, easy to operate, and environmentally friendly. The preparation method implemented in this invention is carried out under normal pressure, with low requirements for equipment production conditions and low cost. Detailed Implementation

[0034] To facilitate understanding of the present invention, a more comprehensive and detailed description of the invention will be provided below in conjunction with preferred embodiments. However, the scope of protection of the present invention is not limited to the specific embodiments described below. Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by those skilled in the art. The technical terms used herein are for the purpose of describing specific embodiments only and are not intended to limit the scope of protection of the present invention.

[0035] Example 1.

[0036] Step (1): Glucose and isomeric deca-ol ether (3EO) are added to the reactor at a molar ratio of 1.00:1. Under the presence of an acid catalyst and a vacuum condition with a system pressure of 1-30 mHg, a glycosylation reaction is carried out at 100-130°C. The amount of p-toluenesulfonic acid catalyst is 0.2%-0.5% of the total mass of glucose and alcohol ether. After reacting for 3-6 hours, the temperature is lowered to 80-90°C, and NaOH is added to neutralize to a pH of 8-9. Unreacted sugars are removed by filtration or sedimentation to obtain glycosylated modified alcohol ether.

[0037] The acid catalyst is p-toluenesulfonic acid.

[0038] Step (2): The obtained glycosylated modified alcohol ether was placed in an experimental apparatus equipped with a stirrer, thermometer, water separator, and condenser. The apparatus was inertized three times, and finally, nitrogen gas was introduced for protection. The condenser was turned on, and the temperature was raised to 40-80℃ for reaction. 0.4 mol of phosphorus pentoxide was evenly divided into 8-10 portions and added in 8-10 portions over 6-10 hours. The reaction temperature was controlled to rise by less than 5℃. The esterification reaction was considered complete when the acid value no longer changed within half an hour. The final product was tested to be 10% monoester and 66% diester.

[0039] The molar ratio of glycosylated modified alcohol ether to phosphorus pentoxide is 2.5:1. The resulting product exhibits general aluminum alloy corrosion resistance and emulsification ability.

[0040] Example 2.

[0041] Step (1): Glucose and isomeric deca-ol ether (3EO-1PO) are added to the reactor at a molar ratio of 1.20:1. Under the presence of an acid catalyst and a vacuum condition with a system pressure of 1~30 mHg, a glycosylation reaction is carried out at 100~130℃. The amount of p-toluenesulfonic acid catalyst is 0.2%~0.5% of the total mass of glucose and alcohol ether. After reacting for 3~6 hours, the temperature is lowered to 80~90℃, and NaOH is added to neutralize to a pH value of 8~9. Unreacted sugars are removed by filtration or sedimentation to obtain glycosylated modified alcohol ether.

[0042] The acid catalyst is p-toluenesulfonic acid.

[0043] In step (2), the obtained glycosylated modified alcohol ether was placed in an experimental apparatus equipped with a stirrer, thermometer, water separator, and condenser. The apparatus was inertized three times, and finally, nitrogen gas was introduced for protection. The condenser was turned on, and the temperature was raised to 40-80℃ for reaction. 0.5 mol of phosphorus pentoxide was evenly divided into 8-10 portions and added in 8-10 portions over 6-10 hours, controlling the temperature rise to be less than 5℃. The esterification reaction was considered complete when the acid value no longer changed within half an hour. The final product was tested to be 19% monoester and 78% diester.

[0044] The molar ratio of glycosylated modified alcohol ether to phosphorus pentoxide is 2:1. The resulting product exhibits excellent aluminum alloy etching and emulsification capabilities.

[0045] Example 3.

[0046] Step (1): Glucose and isomeric tridecyl alcohol ether (5EO) are added to the reactor at a molar ratio of 2.40:1. Under the presence of an acid catalyst and a vacuum condition with a system pressure of 1-30 mHg, a glycosylation reaction is carried out at 100-130°C. The amount of p-toluenesulfonic acid catalyst is 0.2%-0.5% of the total mass of glucose and alcohol ether. After reacting for 3-6 hours, the temperature is lowered to 80-90°C, and NaOH is added to neutralize to a pH of 8-9. Unreacted sugars are removed by filtration or sedimentation to obtain glycosylated modified alcohol ether.

[0047] The acid catalyst is dodecylbenzenesulfonic acid.

[0048] In step (2), the obtained glycosylated modified alcohol ether was placed in an experimental apparatus equipped with a stirrer, thermometer, water separator, and condenser. The apparatus was inertized three times, and finally, nitrogen gas was introduced for protection. The condenser was turned on, and the temperature was raised to 40-80℃ for reaction. 0.6 mol of phosphorus pentoxide was evenly divided into 8-10 portions and added in 8-10 portions over 6-10 hours, controlling the temperature rise to be less than 5℃. The esterification reaction was considered complete when the acid value no longer changed within half an hour. The final product was tested and found to contain 33% monoester and 65% diester.

[0049] The molar ratio of glycosylated modified alcohol ether to phosphorus pentoxide is 1.67:1. The resulting product exhibits excellent aluminum alloy etching and emulsification capabilities.

[0050] Example 4.

[0051] Step (1): Glucose and oleyl alcohol ether (3EO-3PO) are added to the reactor at a molar ratio of 7.20:1. Under the presence of an acid catalyst and a vacuum condition with a system pressure of 1~30mHg, a glycosylation reaction is carried out at 100~130℃. The amount of p-toluenesulfonic acid catalyst is 0.2%~0.5% of the total mass of glucose and alcohol ether. After reacting for 3~6 hours, the temperature is lowered to 80~90℃, and NaOH is added to neutralize to a pH value of 8~9. Unreacted sugars are removed by filtration or sedimentation to obtain glycosylated modified alcohol ether.

[0052] The acid catalyst is p-toluenesulfonic acid.

[0053] In step (2), the obtained glycosylated modified alcohol ether was placed in an experimental apparatus equipped with a stirrer, thermometer, water separator, and condenser. The apparatus was inertized three times, and finally, nitrogen gas was introduced for protection. The condenser was turned on, and the temperature was raised to 40-80℃ for reaction. 0.7 mol of phosphorus pentoxide was evenly divided into 8-10 portions and added in 8-10 portions over 6-10 hours. The temperature rise was controlled to be less than 5℃. The esterification reaction was considered complete when the acid value no longer changed within half an hour. The final product was tested to be 44% monoester and 54% diester.

[0054] The molar ratio of glycosylated modified alcohol ether to phosphorus pentoxide is 1.43:1. The resulting product exhibits excellent aluminum alloy etching and emulsification capabilities.

[0055] Example 5.

[0056] Step (1): Glucose and oleyl alcohol ether (3EO-3PO) are added to the reactor at a molar ratio of 7.20:1. Under the presence of an acid catalyst and a vacuum condition with a system pressure of 1~30mHg, a glycosylation reaction is carried out at 100~130℃. The amount of p-toluenesulfonic acid catalyst is 0.2%~0.5% of the total mass of glucose and alcohol ether. After reacting for 3~6 hours, the temperature is lowered to 80~90℃, and NaOH is added to neutralize to a pH value of 8~9. Unreacted sugars are removed by filtration or sedimentation to obtain glycosylated modified alcohol ether.

[0057] The acid catalyst is p-toluenesulfonic acid.

[0058] Step (2): The obtained glycosylated modified alcohol ether is placed in an experimental apparatus equipped with a stirrer, thermometer, water separator, and condenser. The apparatus is inertized three times, and finally nitrogen gas is introduced for protection. The condenser is turned on, and the temperature is raised to 40-80℃ for reaction. 0.9 mol of phosphorus pentoxide is evenly divided into 8-10 portions and added in 8-10 portions over 6-10 hours. The reaction temperature is controlled to rise by less than 5℃. The esterification reaction is considered complete when the acid value no longer changes within half an hour. The final product is tested to be 58% monoester and 38% diester (in specific embodiments, the final product ratio can only be a specific number, not a range).

[0059] The molar ratio of glycosylated modified alcohol ether to phosphorus pentoxide is 1.11:1 (please confirm this ratio). The resulting product exhibits excellent aluminum alloy etching and emulsification capabilities.

[0060] Test Example 1.

[0061] The samples prepared in Examples 1, 2, 3, 4, and 5, along with the control sample fatty alcohol ether phosphate, were formulated into metal cutting fluids according to the specifications. After dilution at a ratio of 1:20, the prepared test piece LY12 aluminum was completely immersed in the test fluid, covered with a glass cover, and transferred to a thermostat preheated to 55°C ± 2°C. The test was conducted continuously for the specified time. Then, the test piece was removed for inspection, according to the following standards:

[0062] Aluminum alloy:

[0063] Rust-free, with a pristine, new-looking finish (Grade A)

[0064] Slightly darkened, Grade B

[0065] Moderate darkening, grade C

[0066] Severe darkening, Grade D

[0067] The results are shown in Table 1 below.

[0068] Table 1

[0069]

[0070] As shown in Table 1, when the samples prepared in Examples 1, 2, 3, 4, and 5, and the control sample fatty alcohol ether phosphate were formulated into metal cutting fluids and diluted at a ratio of 1:20, the prepared test piece LY12 aluminum was completely immersed in the test solution, covered with a glass cover, and transferred to a thermostat that had been kept at 55°C ± 2°C. After continuous testing for the specified time, the fatty alcohol ether phosphate and the samples prepared in each example showed relatively better performance than the blank sample; the samples prepared in each example showed relatively superior performance than the control sample. In particular, the samples prepared in Examples 2, 3, and 4 showed significantly superior performance.

[0071] Test Example 2.

[0072] The samples and comparative samples of fatty alcohol ether phosphate obtained in Examples 1, 2, 3, 4 and 5 were formulated into metal cutting fluids according to the formulations in Table 2.

[0073] Table 2

[0074]

[0075] The prepared metal cutting fluid was diluted at a ratio of 1:20 and then tapped aluminum alloy holes using a tapping torque machine. The cutting fluid was circulated and sprayed onto the working surface using a magnetic pump. The tool life, tapping quality, and cutting fluid life were evaluated. The results of the lubrication extreme pressure and emulsification performance of the comparative example and fatty alcohol ether phosphate are shown in Table 3.

[0076] Table 3

[0077]

[0078] As can be seen from the table above, when the samples prepared in Examples 1, 2, 3, 4 and 5 and the comparative sample fatty alcohol ether phosphate were formulated into metal cutting fluids and diluted at a ratio of 1:20, the tool life, tapping quality and cutting fluid life were measured. The samples prepared in each example showed relatively better performance than the comparative sample. In particular, the sample prepared in Example 4 showed significantly better performance.

[0079] In summary, this invention selects fatty alcohol ethers as initiators for phosphate ester molecules in molecular design, obtains glycosylated fatty alcohol ethers by glycosylation with glucose, and then esterifies the glycosylated fatty alcohol ethers with phosphorus pentoxide. The resulting fatty alcohol polyether phosphate ester has better corrosion inhibition properties, lubrication extreme pressure properties and higher emulsification properties for aluminum alloys.

[0080] Meanwhile, the main raw materials used in this invention are abundant, and the preparation method is simple, easy to operate, and environmentally friendly. The preparation method implemented in this invention is carried out under normal pressure, with low requirements for equipment production conditions and low cost.

[0081] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A fatty alcohol polyether phosphate, characterized in that... The fatty alcohol polyether phosphate includes the following general formulas as shown in chemical structural formulas I and II: Formula I fatty alcohol polyether phosphate monoester Formula II fatty alcohol polyether phosphate diester Wherein, R is a straight-chain or branched saturated or unsaturated hydrocarbon group of C4 to C18; EO is an ethylene oxide unit; a is a number from 1 to 20; PO is an propylene oxide unit; b is a number from 0 to 10; G is a sugar unit with 5 or 6 carbon atoms; and n is a number from 1 to 10.

2. The fatty alcohol polyether phosphate ester as described in claim 1, characterized in that... R is a straight-chain or branched saturated or unsaturated hydrocarbon group of C10 to C18; EO is an ethylene oxide unit; a is a number from 1 to 8; PO is a propylene oxide unit; b is a number from 0 to 5; G is a sugar unit with 5 or 6 carbon atoms; n is a number from 1 to 4.

3. The fatty alcohol polyether phosphate ester as described in claim 2, characterized in that... R is a straight-chain or branched saturated or unsaturated hydrocarbon group of C12 to C18; EO is an ethylene oxide unit; a is a number from 1 to 5; PO is a propylene oxide unit; b is a number from 0 to 2; G is a sugar unit with 5 or 6 carbon atoms; n is a number from 1 to 2.

4. A method for preparing fatty alcohol polyether phosphate as described in claim 1, characterized in that... First, glucose and fatty alcohol polyether are subjected to a glycosylation reaction to obtain glycosylated fatty alcohol polyether; then, the glycosylated fatty alcohol polyether is phosphoric acid esterified with phosphorus pentoxide, specifically including the following steps: Step (1), glycosylation reaction: Glucose and fatty alcohol ether are added to the reactor and glycosylation reaction is carried out in the presence of acid catalyst and under vacuum conditions. After the reaction, unreacted sugar is removed by filtration or sedimentation to obtain glycosylated modified alcohol ether, as shown in the following formula. Step (2), phosphorylation reaction: The obtained glycosylated modified alcohol ether is placed in an experimental apparatus equipped with a stirrer, thermometer, water separator and condenser for inertization. Then, an inert gas is introduced for protection, the condenser is turned on, and the temperature is raised to 40~80℃ for reaction. Phosphorus pentoxide is added evenly in portions, and the reaction temperature rise is controlled to be less than 5℃ to obtain fatty alcohol polyether phosphate ester, as shown in the following formula: 。 5. The method for preparing fatty alcohol polyether phosphate as described in claim 4, characterized in that... In step (1), glucose and fatty alcohol ether are added to the reactor at a molar ratio of (1.20~12.00):1, and glycosylation reaction is carried out at 100~130℃ under vacuum conditions with an acid catalyst and a system pressure of 1~30mHg.

6. The method for preparing fatty alcohol polyether phosphate as described in claim 5, characterized in that... The molar ratio of glucose to fatty alcohol polyether is (1.20~4.80):1; the fatty alcohol polyether is any one of isomeric decayl alcohol polyether, isomeric tridecayl alcohol polyether, and oleyl alcohol polyether.

7. The method for preparing fatty alcohol polyether phosphate as described in claim 5, characterized in that... The acid catalyst is either p-toluenesulfonic acid or dodecylbenzenesulfonic acid. The amount of catalyst used is 0.2% to 0.5% of the total mass of glucose and alcohol ether. After the reaction, the temperature is lowered to 80 to 90°C, and NaOH is added to neutralize to a pH of 8 to 9. Unreacted sugars are removed by filtration or sedimentation to obtain glycosylated modified alcohol ether.

8. The method for preparing fatty alcohol polyether phosphate as described in claim 4, characterized in that... The obtained glycosylated modified alcohol ether was placed in an experimental apparatus equipped with a stirrer, thermometer, water separator and condenser. The experimental apparatus was inertized three times. Finally, inert gas was introduced for protection, the condenser was turned on, and the temperature was raised to 40~80℃ for reaction. Phosphorus pentoxide was evenly divided into 8~10 portions and added in 8~10 portions over 6~10 hours. The reaction temperature was controlled to rise by less than 5℃. The esterification reaction was considered to be complete when the acid value no longer changed within half an hour.

9. The method for preparing fatty alcohol polyether phosphate as described in claim 8, characterized in that... In the phosphorylation reaction, the molar ratio of glycosylated modified alcohol ether to phosphorus pentoxide is: glycosylated modified alcohol ether: phosphorus pentoxide = (1~2):

1.

10. The method for preparing fatty alcohol polyether phosphate as described in claim 9, characterized in that... The molar ratio of glycosylated modified alcohol ether to phosphorus pentoxide is (1.5~2):1, and the inert gas is either nitrogen or argon.

Citation Information

Patent Citations

  • Tall oil acid diacetyl amide phosphate ester, and preparation method thereof

    CN104530117A