阅读说明：本技术 一种减摩剂的制备方法 (Preparation method of friction reducer ) 是由 王勇 章晨 于 2020-11-17 设计创作，主要内容包括：本发明涉及减摩剂技术领域,特别是涉及一种减摩剂的制备方法。所述减摩剂的制备方法包括：将催化剂和溶胶电荷调节剂混合得到第一溶液；对所述第一溶液水浴加热；将硅源和有机溶剂混合得到第二溶液；将所述第二溶液加入第一溶液中,以使所述第二溶液与第一溶液反应第一预设时间,形成第三溶液；使用洗涤剂对所述第三溶液离心洗涤得到所述减摩剂,由于所述硅源本身具有耐高温、高压的特性,则制备的所述减摩剂可胜任高压、高温的环境。另外,通过上述方法制备的减摩剂的粒径可小于1微米,且具有单分散性。(The invention relates to the technical field of friction reducers, in particular to a preparation method of a friction reducer. The preparation method of the friction reducer comprises the following steps: mixing a catalyst and a sol charge regulator to obtain a first solution; heating the first solution in a water bath; mixing a silicon source and an organic solvent to obtain a second solution; adding the second solution into the first solution to enable the second solution to react with the first solution for a first preset time to form a third solution; and centrifugally washing the third solution by using a detergent to obtain the friction reducer, wherein the silicon source has the characteristics of high temperature resistance and high pressure resistance, so that the prepared friction reducer can be in high-pressure and high-temperature environments. In addition, the friction reducer prepared by the above method may have a particle size of less than 1 micron and have monodispersity.)

1. A method of preparing a friction reducer, comprising:

mixing a catalyst and a sol charge regulator to obtain a first solution;

heating the first solution in a water bath;

mixing a silicon source and an organic solvent to obtain a second solution;

adding the second solution into the first solution to enable the second solution to react with the first solution for a first preset time to form a third solution;

and centrifugally washing the third solution by using a detergent to obtain the friction reducer.

2. The method of claim 1, further comprising:

dispersing the friction reducer in a solution to obtain a friction reducer solution;

heating the friction reducer solution in water bath;

adding a silane coupling agent solution into the friction reducing agent solution to enable the silane coupling agent solution and the friction reducing agent solution to react for a second preset time;

adding styrene to the friction reducer solution;

adding an initiator into the friction reducer solution to obtain a modified friction reducer solution;

and centrifugally washing the modified friction reducer solution by using a detergent to obtain the modified friction reducer.

3. The production method according to claim 1, wherein the catalyst comprises aqueous ammonia having a concentration of 0.5 to 5 mol/L.

4. The method according to claim 1, wherein the sol charge control agent comprises potassium chloride, and the concentration of the potassium chloride is 0 to 20 mmol/L.

5. The method of claim 1, wherein the silicon source comprises ethyl orthosilicate.

6. The production method according to claim 1, wherein the organic solvent includes at least one of absolute ethanol and isopropyl alcohol.

7. The method according to claim 1, wherein the concentration of the second solution is 0.1 to 2 mol/L.

8. The method of claim 1, wherein the detergent comprises toluene.

9. The method of claim 1, wherein the first solution is heated in a water bath at a temperature of 30 to 80 ℃.

10. The method of claim 1, wherein the second solution is added to the first solution at a rate of 0.5-2 mL/min.

Technical Field

The embodiment of the invention relates to the technical field of friction reducers, in particular to a preparation method of a friction reducer.

Background

The friction exists in the places where the transmission system of automobiles and ships and the gear boxes of wind generating sets have mechanical transmission, and the application range of the friction reducing agent is very wide. Therefore, the use environment is complex and variable, and the requirements on the properties of temperature, pressure, medium and interface are variable. For example, in the gear box of a large wind turbine, there is a high pressure, high temperature environment between the friction surfaces of the gears.

However, in the process of implementing the embodiment of the present invention, the inventors of the present invention found that: the traditional nano particle friction reducing agent such as copper, tin and the like can not be qualified in high-pressure and high-temperature environments, so that an anti-friction agent capable of being qualified in high-pressure and high-temperature environments is urgently needed.

Disclosure of Invention

In view of the above problems, embodiments of the present invention provide a method of making a friction reducer that overcomes or at least partially solves the above problems.

According to an aspect of an embodiment of the present invention, there is provided a method of preparing a friction reducer, including: mixing a catalyst and a sol charge regulator to obtain a first solution; heating the first solution in a water bath; mixing a silicon source and an organic solvent to obtain a second solution; adding the second solution into the first solution to enable the second solution to react with the first solution for a first preset time to form a third solution; and centrifugally washing the third solution by using a detergent to obtain the friction reducer.

In an optional manner, the method further comprises: dispersing the friction reducer in a solution to obtain a friction reducer solution; heating the friction reducer solution in water bath; adding a silane coupling agent solution into the friction reducing agent solution to enable the silane coupling agent solution and the friction reducing agent solution to react for a second preset time; adding styrene to the friction reducer solution; adding an initiator into the friction reducer solution to obtain a modified friction reducer solution; and centrifugally washing the modified friction reducer solution by using a detergent to obtain the modified friction reducer.

In an optional mode, the catalyst comprises ammonia water, and the concentration of the ammonia water is 0.5-5 mol/L.

In an alternative mode, the sol charge regulator comprises potassium chloride, and the concentration of the potassium chloride is 0-20 mmol/L.

In an alternative form, the silicon source includes tetraethyl orthosilicate.

In an alternative form, the organic solvent includes at least one of absolute ethanol and isopropyl alcohol.

In an alternative mode, the concentration of the second solution is 0.1 to 2 mol/L.

In an alternative form, the detergent comprises toluene.

In an alternative form, the temperature of the water bath heating of the first solution is from 30 to 80 ℃.

In an alternative embodiment, the second solution is added to the first solution at a rate of 0.5 to 2 mL/min.

The embodiment of the invention has the beneficial effects that: different from the existing preparation method of the friction reducer, the preparation method of the friction reducer provided by the embodiment of the invention comprises the following steps: mixing a catalyst and a sol charge regulator to obtain a first solution; heating the first solution in a water bath; mixing a silicon source and an organic solvent to obtain a second solution; adding the second solution into the first solution to enable the second solution to react with the first solution for a first preset time to form a third solution; and centrifugally washing the third solution by using a detergent to obtain the friction reducer, wherein the silicon source has the characteristics of high temperature resistance and high pressure resistance, so that the prepared friction reducer can be in high-pressure and high-temperature environments. In addition, the friction reducer prepared by the above method may have a particle size of less than 1 micron and have monodispersity.

Drawings

One or more embodiments are illustrated by way of example in the accompanying drawings, which correspond to the figures in which like reference numerals refer to similar elements and which are not to scale unless otherwise specified.

FIG. 1 is a schematic flow diagram of a method of making a friction reducer according to an embodiment of the present invention;

FIG. 2 is a scanning electron micrograph of a friction reducer 1 provided by an embodiment of the present invention;

FIG. 3 is a scanning electron micrograph of a friction reducer 2 provided by an embodiment of the present invention;

FIG. 4 is a scanning electron micrograph of a friction reducer 3 provided by an embodiment of the present invention;

FIG. 5 is a scanning electron micrograph of a friction reducer 4 provided by an embodiment of the present invention;

FIG. 6 is a scanning electron micrograph of a friction reducer 5 provided by an embodiment of the present invention;

FIG. 7 is a schematic flow diagram of another method of making a friction reducer according to an embodiment of the present invention.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

Example one

Referring to fig. 1, fig. 1 is a schematic flow chart of a method for preparing a friction reducer according to an embodiment of the present invention. The preparation method of the friction reducer comprises the following steps:

and step S101, mixing the catalyst and the sol charge regulator to obtain a first solution.

The catalyst comprises ammonia water, and the concentration of the ammonia water is 0.5-5 mol/L.

And S102, heating the first solution in a water bath.

The temperature for heating the first solution in the water bath is 30-80 ℃.

In some embodiments, the first solution is placed in a three-necked flask and heated in a water bath with magnetic stirring at 30-80 ℃.

Step S103, mixing a silicon source and an organic solvent to obtain a second solution.

The silicon source comprises tetraethoxysilane.

The organic solvent includes at least one of absolute ethanol and isopropanol.

The concentration of the second solution is 0.1-2 mol/L.

And step S104, adding the second solution into the first solution to enable the second solution to react with the first solution for a first preset time to form a third solution.

The second solution is added to the first solution at a rate of 0.5-2 mL/min.

In some embodiments, the second solution is added to the first solution using a precision flow type peristaltic pump.

It should be noted that, the speed of adding the second solution into the first solution is more than 2mL/min, the prepared friction reducer is easy to agglomerate, thereby affecting the performance of the friction reducer.

The first preset time may be 12 hours.

And step S105, centrifugally washing the third solution by using a detergent to obtain the friction reducer.

The detergent comprises toluene.

The particle size of the prepared friction reducer can be adjusted by adjusting the concentration of the second solution of the catalyst, the sol charge control agent, and the silicon source in the organic solvent. The concentration of the catalyst increases and the particle size of the friction reducer decreases. The concentration of the second solution of the silicon source in the organic solvent is increased and the particle size of the friction reducer is increased. The concentration of the sol charge regulator is increased and the particle size of the friction reducer is reduced.

For the convenience of a reader to more intuitively and better understand the performance and the effect of the friction reducer prepared by the preparation method of the friction reducer, the friction reducer with the proportion of 5 different raw materials is obtained by using the preparation method of the friction reducer, and the 5 friction reducers are as follows:

the preparation process of the friction reducer 1 comprises (1) preparation of monodisperse friction reducer. Uniformly mixing 0.5mol/L ammonia water and 5mmol/L potassium chloride solution to obtain a first solution; uniformly mixing tetraethoxysilane and absolute ethyl alcohol to prepare a second solution of 0.1 mol/L; placing the first solution into a three-neck flask, and heating the first solution in a water bath while magnetically stirring at the temperature of 30 ℃; the second solution is placed in a distillation flask, a rubber hose is connected with a three-neck flask, and the second solution is injected into the first solution at the speed of 0.5mL/min by using a precision flow peristaltic pump; and fully reacting for 12 hours while stirring to form a third solution, and centrifugally washing the third solution by using a detergent to obtain the friction reducer 1.

The preparation process of the friction reducer 2 comprises the steps of uniformly mixing 5mol/L ammonia water and 5mmol/L potassium chloride solution to obtain a first solution; uniformly mixing tetraethoxysilane and absolute ethyl alcohol to prepare a second solution of 2 mol/L; placing the first solution into a three-neck flask, and heating the first solution in a water bath while magnetically stirring at the temperature of 30 ℃; the second solution is placed in a distillation flask, a rubber hose is connected with a three-neck flask, and the second solution is injected into the first solution at the speed of 2mL/min by using a precision flow peristaltic pump; and fully reacting for 12 hours while stirring to form a third solution, and centrifugally washing the third solution by using a detergent to obtain the friction reducer 2.

The preparation process of the friction reducer 3 comprises the steps of uniformly mixing 2mol/L ammonia water and 20mmol/L potassium chloride solution to obtain a first solution; uniformly mixing tetraethoxysilane and absolute ethyl alcohol to prepare a second solution of 1 mol/L; placing the first solution into a three-neck flask, and heating the first solution in a water bath while magnetically stirring at 80 ℃; the second solution is placed in a distillation flask, a rubber hose is connected with a three-neck flask, and the second solution is injected into the first solution at the speed of 1mL/min by using a precision flow peristaltic pump; and fully reacting for 12 hours while stirring to form a third solution, and centrifugally washing the third solution by using a detergent to obtain the friction reducer 3.

The preparation process of the friction reducer 4 comprises the steps of uniformly mixing 2mol/L ammonia water and 20mmol/L potassium chloride solution to obtain a first solution; uniformly mixing ethyl orthosilicate and isopropanol to prepare a second solution with the concentration of 1 mol/L; placing the first solution into a three-neck flask, and heating the first solution in a water bath while magnetically stirring at 80 ℃; the second solution is placed in a distillation flask, a rubber hose is connected with a three-neck flask, and the second solution is injected into the first solution at the speed of 1mL/min by using a precision flow peristaltic pump; and fully reacting for 12 hours while stirring to form a third solution, and centrifugally washing the third solution by using a detergent to obtain the friction reducer 4.

The preparation process of the friction reducer 5 comprises the steps of uniformly mixing 2mol/L ammonia water and 20mmol/L potassium chloride solution to obtain a first solution; uniformly mixing tetraethoxysilane and absolute ethyl alcohol to prepare a second solution of 1 mol/L; placing the first solution into a three-neck flask, and heating the first solution in a water bath while magnetically stirring at 80 ℃; the second solution is placed in a distillation flask, a rubber hose is connected with a three-neck flask, and the second solution is injected into the first solution at the speed of 1mL/min by using a precision flow peristaltic pump; and fully reacting for 12 hours while stirring to form a third solution, and centrifugally washing the third solution by using a detergent to obtain the friction reducer 5.

And respectively observing the antifriction agent 1, the antifriction agent 2, the antifriction agent 3, the antifriction agent 4 and the antifriction agent 5 by using a scanning electron microscope. A scanning electron micrograph of the friction reducer 1 is taken, see figure 2. A scanning electron micrograph of the friction reducer 2 is taken, see figure 3. A scanning electron micrograph of the friction reducer 3 is taken, see figure 4. A scanning electron micrograph of the friction reducer 4 is taken, see figure 5. A scanning electron micrograph of the friction reducer 5 is taken, see figure 6.

As can be seen from fig. 2 to 6, the particle size of the friction reducer obtained by the preparation method of the friction reducer of the present application is less than 1 micron, and the friction reducer has uniform particle size and monodispersity.

As can be seen from fig. 2 to 6, when the concentrations of the second solutions of the catalyst, the sol charge control agent, and the silicon source in the organic solvent are different during the preparation of the friction reducing agent, the particle sizes of the obtained friction reducing agent are different, that is, the particle sizes of the friction reducing agent can be adjusted by adjusting the concentrations of the second solutions of the catalyst, the sol charge control agent, and the silicon source in the organic solvent.

In the embodiment of the invention, a first solution is obtained by mixing a catalyst and a sol charge regulator; heating the first solution in a water bath; mixing a silicon source and an organic solvent to obtain a second solution; adding the second solution into the first solution to enable the second solution to react with the first solution for a first preset time to form a third solution; and centrifugally washing the third solution by using a detergent to obtain the friction reducer, wherein the silicon source has the characteristics of high temperature resistance and high pressure resistance, so that the prepared friction reducer can be in high-pressure and high-temperature environments. In addition, the friction reducer prepared by the above method may have a particle size of less than 1 micron and have monodispersity.

Example two

Referring to fig. 7, fig. 7 is a schematic flow chart of another friction reducer manufacturing method according to an embodiment of the present invention. The method comprises the following steps:

and step S101, mixing the catalyst and the sol charge regulator to obtain a first solution.

And S102, heating the first solution in a water bath.

Step S103, mixing a silicon source and an organic solvent to obtain a second solution.

And step S104, adding the second solution into the first solution to enable the second solution to react with the first solution for a first preset time to form a third solution.

And step S105, centrifugally washing the third solution by using a detergent to obtain the friction reducer.

And S106, dispersing the friction reducer in a solution to obtain a friction reducer solution.

The solution is deionized water.

In some embodiments, the friction reducer may be placed in the deionized water and dispersed using an emulsifier to provide a friction reducer solution.

And step S107, heating the friction reducer solution in a water bath.

Preferably, the temperature at which the friction reducer solution is heated in a water bath is 70 ℃.

And S108, adding a silane coupling agent solution into the friction reducing agent solution to enable the silane coupling agent solution and the friction reducing agent solution to react for a second preset time.

The silane coupling agent comprises at least one of KH550, KH560, KH570 and KH 858.

The second preset time is 1-5 h.

In some embodiments, the silane coupling agent solution is maintained at a constant temperature while reacting with the friction reducer solution.

Step S109, adding styrene to the friction reducer solution.

And step S110, adding an initiator into the antifriction agent solution to obtain a modified antifriction agent solution.

The initiator comprises one or more of azobisisobutyronitrile, benzoyl peroxide and ammonium persulfate.

And step S111, carrying out centrifugal washing on the modified antifriction agent solution by using a detergent to obtain the modified antifriction agent.

In the embodiment of the invention, the friction reducer solution is obtained by dispersing the friction reducer in the solution; heating the friction reducer solution in water bath; adding a silane coupling agent solution into the friction reducing agent solution to enable the silane coupling agent solution and the friction reducing agent solution to react for a second preset time; adding styrene to the friction reducer solution; adding an initiator into the friction reducer solution to obtain a modified friction reducer solution; and centrifugally washing the modified friction reducer solution by using a detergent to obtain the modified friction reducer. The modified friction reducer can be matched with base oil, and can increase the fusion property with a metal interface when being used.

It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.