阅读说明：本技术 一种酸式磷酸酯脂肪胺盐的制备方法 (Preparation method of acid phosphate fatty amine salt ) 是由 张媞 张强 杨语诗 潘玉秋 李雅娜 于 2021-08-24 设计创作，主要内容包括：本发明公开了一种酸式磷酸酯脂肪胺盐的制备方法,其特征包括以下方法：(a)：C5-C8脂肪醇与含磷氧化物酯化反应,得到酸性磷酸酯；(b)：于(a)产物中投入C12-C14烷基伯胺,胺化反应,得到终产物。本产品比不含氮的含磷化合物具有更高的承载能力、较好的防锈性能和长期储存稳定性；酸性磷酸脂肪铵盐由于空间位阻小,容易在摩擦表面形成吸附,具有好的极压抗磨性能；酸性磷酸酯由于具有良好的摩擦学性能,而且生产工艺简单,工业“三废”少,满足用户要求,填补市场空缺。(The invention discloses a preparation method of acid phosphate ester fatty amine salt, which is characterized by comprising the following steps: (a) the method comprises the following steps C5-C8 fatty alcohol and phosphorus-containing oxide are subjected to esterification reaction to obtain acidic phosphate; (b) the method comprises the following steps And (C) adding C12-C14 alkyl primary amine into the product (a), and carrying out amination reaction to obtain a final product. Compared with a nitrogen-free phosphorus-containing compound, the product has higher bearing capacity, better antirust performance and long-term storage stability; the acidic fatty ammonium phosphate salt is easy to form adsorption on the friction surface due to small steric hindrance, and has good extreme pressure anti-wear performance; the acidic phosphate ester has good tribological performance, simple production process and less industrial three wastes, meets the requirements of users and fills the market vacancy.)

1. The preparation method of the acid phosphate ester fatty amine salt is characterized by comprising the following steps of esterifying fatty alcohol and phosphorus-containing oxide, and aminating the esterified fatty alcohol and the phosphorus-containing oxide with alkyl primary amine.

2. The method of claim 1, wherein the fatty alcohol is C5-C8 fatty alcohol, such as primary and secondary primary alcohol, such as pentanol, hexanol, octanol, the phosphorus-containing oxide is phosphorus pentoxide, and the primary alkyl amine is C12-C14 primary alkyl amine, such as tertiary primary alkyl amine.

3. The method for preparing fatty amine acid phosphate according to claim 2, wherein the feeding manner is to batch feed phosphorus-containing oxide into C5-C8 fatty alcohol.

4. The method for preparing fatty amine acid phosphate according to claim 2, wherein the feeding temperature is 30-60 ℃ and the reaction temperature is controlled to 80-100 ℃ to obtain a transparent intermediate product.

5. The method of claim 2, wherein the C12-C14 alkyl primary amine is fed in portions into the intermediate product.

6. The method of claim 2, wherein the feed temperature is controlled to be <60 ℃.

7. The method for preparing fatty amine acid phosphate according to claim 2, wherein the reaction temperature is controlled at 85-90 ℃ after the feeding is finished, and the product is obtained.

Technical Field

The invention relates to the technical field of lubricating oil additives, in particular to a preparation method of acid phosphate ester fatty amine salt.

Background

In all mechanical equipment and transport tools, friction and abrasion exist between parts moving relatively, so that the equipment cannot operate flexibly due to light weight, and mechanical damage, lubricant consumption and service life reduction of the machinery are caused due to power loss. The use of a fluid lubricant, a lubricating oil, is an important method of widespread utility in order to ensure proper operation of machinery and vehicles, and to increase their useful life. Commercially available lubricating oils vary in their brands depending on the conditions and environment in which mechanical equipment and transportation are used, and in boundary lubrication, when a metal surface is subjected to only a moderate load, if an additive is adsorbed on the metal surface or strongly wears away from the metal surface, the additive is called an anti-wear additive. When the metal surface bears a high load, a large amount of metal surfaces are in direct contact to generate a large amount of heat, a film formed by an antiwear agent is damaged and does not play a role in protecting the metal surface any more, if an additive can generate a chemical reaction film by a chemical reaction with the metal surface to play a role in lubrication and prevent the metal surface from being scratched and even welded, the most harsh boundary lubrication is usually called extreme pressure lubrication, the additive is called an extreme pressure additive, the extreme pressure antiwear performance is an important service performance of industrial gear oil, the extreme pressure antiwear performance is realized mainly by adding the extreme pressure antiwear additive, and a formula and a preparation method of the fatty amine salt of acid phosphate ester are provided.

Disclosure of Invention

The invention aims to solve the problems in the prior art and provides a preparation method of acid phosphate fatty amine salt.

Firstly, C5-C8 fatty alcohol is put into a reaction kettle, phosphorus-containing oxide is added in batches under stirring at room temperature to obtain a transparent intermediate product, and C12-C14 alkyl primary amine is added in batches under controlled temperature to obtain the acid phosphate fatty amine salt.

Compared with the prior art, the invention has the beneficial effects that:

the fatty amine salt of the acidic phosphate ester (phosphorus nitrogen agent) obtained by the reaction of the acidic phosphate ester and the long-chain amine has higher bearing capacity, better antirust performance and long-term storage stability compared with a phosphorus-containing compound without nitrogen; the acidic fatty ammonium phosphate salt has good extreme pressure anti-wear performance because the steric hindrance is small and the absorption is easy to form on the friction surface; the acidic phosphate ester has good tribological performance, simple production process, less industrial three wastes and wide application prospect.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.

Example 1

Putting 88g of amyl alcohol into a reaction kettle with a condensation reflux device, a temperature control device and a sealed stirring device, stirring at room temperature, then putting 47g of phosphorus pentoxide in batches, controlling the feeding temperature to be 30 ℃, controlling the temperature to be 90 ℃ to react for 5 hours after the feeding is finished, obtaining light yellow transparent liquid, putting tertiary alkyl primary amine in batches under the condition that the temperature is lower than 60 ℃, and finishing the feeding. Controlling the temperature at 85 ℃ and reacting for 2 hours to obtain the product.

Example 2

102g of hexanol is put into a reaction kettle with a condensation reflux device, a temperature control device and a sealed stirring device, stirring is carried out at room temperature, 47g of phosphorus pentoxide is put into the reaction kettle in batches, the feeding temperature is controlled to be 45 ℃, the temperature is controlled to be 90 ℃ after feeding is finished, reaction is carried out for 4 hours, light yellow transparent liquid is obtained, tertiary alkyl primary amine is put into the reaction kettle in batches under the condition that the temperature is lower than 60 ℃, and feeding is finished. Controlling the temperature at 85 ℃ and reacting for 2 hours to obtain the product.

Example 3

130g of sec-octanol is put into a reaction kettle with a condensation reflux device, a temperature control device and a sealed stirring device, stirring is carried out at room temperature, 47g of phosphorus pentoxide is put into the reaction kettle in batches, the feeding temperature is controlled to be less than 50 ℃, after the feeding is finished, the temperature is controlled to be 90 ℃ to react for 4 hours, light yellow transparent liquid is obtained, tertiary alkyl primary amine is put into the reaction kettle in batches at the temperature of less than 60 ℃, and after the feeding is finished. Controlling the temperature at 85 ℃ and reacting for 2 hours to obtain the product.

Compared with the prior formula, the invention adopts the fatty amine salt of the acid phosphate ester, and the relative phosphate ester has stable structure, small acid value after hydrolysis test and no corrosion to copper sheets, so that the copper sheets can only have good wear resistance under light load and have poor extreme pressure wear resistance under heavy load; compared with a nitrogen-free phosphorus-containing compound, the phosphorus-nitrogen agent obtained by the reaction of the acidic phosphate and the long-chain amine has higher bearing capacity, better antirust performance and long-term storage stability, wherein hydroxyl is introduced into the molecular structure of the acidic phosphoric acid fatty amine salt, so that the oiliness of the additive can be improved, and the antifriction performance of the additive can be improved; the introduction of alkoxy can improve the hydrolytic stability of the additive; and different nitrogen-containing functional groups are introduced into the molecular structure, so that the extreme pressure antiwear property and the thermal stability of the additive can be improved.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.