阅读说明：本技术 一种磷酸酯胺盐的制备方法 (Preparation method of phosphate 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：本发明公开了一种磷酸酯胺盐的制备方法,包括：(a)：C1-C4短链一元醇与含磷氧化物酯化反应得到磷酸酯；(b)：(a)产物与烷基伯胺反应,即得到本产品。本发明设计合理,具有非常高的抗磨性和极压性,节能环保,并且与其他润滑油添加剂之间配伍性好,应用广泛。(The invention discloses a preparation method of phosphate amine salt, which comprises the following steps: (a) the method comprises the following steps Esterifying C1-C4 short-chain monohydric alcohol with phosphorus-containing oxide to obtain phosphate; (b) the method comprises the following steps (a) The product reacts with alkyl primary amine to obtain the product. The invention has reasonable design, very high abrasion resistance and extreme pressure property, energy saving and environmental protection, and has good compatibility with other lubricating oil additives and wide application.)

1. The preparation method of the phosphate amine salt is characterized by comprising the following steps:

s1: putting C1-C4 short-chain monohydric alcohol into a four-mouth bottle with a condensation reflux device, a thermometer and a sealed stirrer, and stirring for 5-10min by the sealed stirrer;

s2: putting phosphorus-containing oxides into four-mouth bottles in batches, and controlling the feeding temperature to be 0-30 ℃; after the feeding is finished, heating the four-mouth bottle to 60-80 ℃, and reacting for 3-3.5 h;

s3: and (3) adding alkyl primary amine into the four-mouth bottle in batches, controlling the feeding temperature to be 35-40 ℃, after the feeding is finished, heating the four-mouth bottle to 75-85 ℃, and reacting for 3-3.5 hours to obtain the product.

2. The method for preparing the amine salt of phosphoric acid ester according to claim 1, wherein the short-chain monohydric alcohol of C1-C4 in S1 is one of isopropanol or n-butanol.

3. The method according to claim 1, wherein the phosphorus-containing oxide in S2 is one of phosphorus pentoxide and phosphorus pentoxide containing low-viscosity refined oil.

4. The method according to claim 3, wherein the phosphorus pentoxide containing the refined oil with low viscosity is a mixture of white oil and phosphorus pentoxide.

5. The method according to claim 1, wherein the alkyl primary amine in S3 is a tertiary alkyl primary amine.

Technical Field

The invention relates to the technical field of petrochemical industry, in particular to a preparation method of phosphate amine salt.

Background

The equipment can not be operated with lubricating oil, the lubricating oil can not be operated with lubricating oil additives, the lubricating oil additives are the essence of various modern high-grade lubricating oils, currently, the lubricating oil additives are common production products in the petrochemical field, but the existing lubricating oil additives have the obvious defects of insufficient extreme pressure anti-wear property, large addition amount and poor performance stability in the preparation process, and therefore a preparation method of the phosphate amine salt is designed to solve the problems.

Disclosure of Invention

The invention aims to solve the existing problems, and provides a preparation method of phosphate amine salt, which has very high abrasion resistance and extreme pressure property, is energy-saving and environment-friendly, can be well compatible with other lubricating oil additives, and is widely applied.

In order to achieve the purpose, the invention adopts the following technical scheme:

a preparation method of phosphate amine salt comprises the following steps:

s1: putting C1-C4 short-chain monohydric alcohol into a four-mouth bottle with a condensation reflux device, a thermometer and a sealed stirrer, and stirring for 5-10min by the sealed stirrer;

s2: putting phosphorus-containing oxides into four-mouth bottles in batches, and controlling the feeding temperature to be 0-30 ℃; after the feeding is finished, heating the four-mouth bottle to 60-80 ℃, and reacting for 3-3.5 h;

s3: and (3) adding alkyl primary amine into the four-mouth bottle in batches, controlling the feeding temperature to be 35-40 ℃, after the feeding is finished, heating the four-mouth bottle to 75-85 ℃, and reacting for 3-3.5 hours to obtain the product.

Preferably, in the S1, the C1-C4 short-chain monohydric alcohol is one of isopropanol or n-butanol.

Preferably, in S2, the phosphorus-containing oxide is one of phosphorus pentoxide and phosphorus pentoxide containing a low-viscosity refined oil.

Preferably, the phosphorus pentoxide containing low-viscosity refined oil is formed by mixing white oil and phosphorus pentoxide.

Preferably, the alkyl primary amine is a tertiary alkyl primary amine or the like.

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

the invention has reasonable design, very high wear resistance and extreme pressure property, the extreme pressure property test (four-ball machine test) is shown in table 1, the invention is energy-saving and environment-friendly, and the invention has good compatibility with other lubricating oil additives and wide application.

TABLE 1

Detailed Description

The following will clearly and completely describe the technical solutions in the embodiments of the present invention, 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

The method comprises the following steps:

s1: putting 185g of isopropanol into a 1000ml four-mouth bottle with a condensing reflux device, a thermometer and a sealed stirrer, and uniformly stirring for 5min by the sealed stirrer after putting;

s2: 245g of phosphorus pentoxide (formed by mixing white oil and phosphorus pentoxide, wherein the mass of the phosphorus pentoxide is 142g, and the mass of the white oil is 103 g) containing low-viscosity refined oil is put into a four-mouth bottle in batches, and the feeding temperature is controlled to be less than 30 ℃; after the feeding is finished, heating the four-mouth bottle to 75-80 ℃, and reacting for 2 hours;

s3: 390g of tertiary alkyl primary amine is added into a four-mouth bottle in batches, the feeding temperature is controlled to be less than 50 ℃, after the feeding is finished, the temperature of the four-mouth bottle is raised to 75 ℃, and the reaction time is 3 hours, so that the product can be obtained.

Example 2

The method comprises the following steps:

s1: 226g of n-butanol is put into a 1000ml four-mouth bottle with a condensing reflux device, a thermometer and a sealed stirrer, and after the putting is finished, the mixture is uniformly stirred for 8min by the sealed stirrer;

s2: 216g of phosphorus pentoxide (formed by mixing white oil and phosphorus pentoxide and having a mass of 142g and 74 g) containing low-viscosity refined oil is put into a four-mouth bottle in batches, and the feeding temperature is controlled to be less than 30 ℃; after the feeding is finished, heating the four-mouth bottle to 60-65 ℃, and reacting for 3 hours;

s3: 380g of tertiary alkyl primary amine is added into the four-mouth bottle in batches, the feeding temperature is controlled to be less than 50 ℃, after the feeding is finished, the temperature of the four-mouth bottle is raised to 80 ℃, and the reaction time is 3 hours, so that the product can be obtained.

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.