CN111925574A - High-pressure sealing ring and preparation method thereof - Google Patents

Abstract

The invention discloses a high-pressure sealing ring and a preparation method thereof, wherein the high-pressure sealing ring comprises the following components: 100-120 parts of styrene butadiene rubber, 2-7 parts of reinforcing agent, 1.2-3.5 parts of vulcanizing agent, 0.6-1.9 parts of accelerator, 3-7 parts of anti-aging agent, 3-8 parts of zinc oxide and 0.6-1.6 parts of stearic acid; wherein the reinforcing agent is Al modified by p-dodecyl benzene sulfonyl₂O₃‑MgO‑TiO₂Solid solution. The invention provides a high-pressure sealing ring, which is prepared by adding Al into styrene butadiene rubber₂O₃‑MgO‑TiO₂Two treatment steps of solid solution structure treatment and p-dodecylbenzenesulfonyl group modification greatly promote Al₂O₃Improved while uniformly dispersed in styrene butadiene rubberThe fusion ability of the styrene butadiene rubber with natural rubber is improved, and the mechanical properties such as mechanics, strength and the like of the styrene butadiene rubber are obviously improved.

Description

High-pressure sealing ring and preparation method thereof

Technical Field

The invention belongs to the technical field of sealing ring manufacturing, and particularly relates to a high-pressure sealing ring and a preparation method thereof.

Background

Along with the development of economy and manufacturing technology in China, the use of high-pressure sealing equipment in main national economy industries such as national defense, chemical engineering, petroleum, coal, transportation, mechanical manufacturing and the like is increased day by day, higher requirements are put on sealing rings under high-pressure working conditions, and fluid or solid particles are prevented from leaking from adjacent joint surfaces and external impurities such as dust, moisture and the like are prevented from entering the interior of machine equipment.

The conventional rubber seal ring has the problems that: the pressure resistance is poor, the product surface static friction coefficient is high, and the like, so the service life is short, the sealing ring needs to be frequently replaced, time and labor are wasted, and the resource waste is also caused. Aiming at the problems of poor pressure resistance and changeability of the rubber sealing ring, a high-strength material is generally added; although the strength of the material can be improved, the elasticity of the material is reduced, the deformation coefficient is increased, and the service life of the sealing ring is directly influenced.

Nano Al₂O₃The composite material has the characteristics of high hardness, good dimensional stability and the like, and can be used for reinforcing and toughening various materials. However, nano Al₂O₃The reinforcing toughening rubber is a polar compound, and under the interaction of factors such as van der Waals force, electrostatic force, capillary force, self gravity and the like in a medium, particles are easy to agglomerate and are difficult to disperse in the process of compounding with a rubber material, so that the mechanical properties such as mechanics, strength and the like of the reinforcing toughening rubber product are not ideal.

Disclosure of Invention

The invention provides a formula of a high-pressure rubber sealing ring and a preparation method thereof, aiming at overcoming the defects in the prior art.

The invention provides a high-pressure sealing ring which comprises the following components in parts by mass: 100-120 parts of styrene butadiene rubber, 2-7 parts of reinforcing agent, 1.2-3.5 parts of vulcanizing agent, 0.6-1.9 parts of accelerator, 3-7 parts of anti-aging agent, 3-8 parts of zinc oxide and 0.6-1.6 parts of stearic acid.

The reinforcing agent is Al modified by p-dodecyl benzene sulfonyl₂O₃-MgO-TiO₂Solid solution.

P-dodecylbenzenesulfonyl modified Al₂O₃-MgO-TiO₂The preparation method of the solid solution strengthening agent comprises the following steps:

step 1: 50gAl is added₂O₃And 30g of MgO for wet ball milling for 5h, adding 20g of TiO2 for continuous wet ball milling for 3h to obtain Al₂O₃MgO and TiO₂A uniform mixture A of the three;

step 2: drying the mixture A obtained in the step 1 at 100 ℃ for 1h, sintering at 800-1000 ℃ for 3h, and finally grinding to obtain nanoscale Al₂O₃-MgO-TiO₂Solid solution powder B;

and step 3: adding 80g of solid solution powder B prepared in the step 2 into 100ml of H with the mass fraction of 5%₂O₂Filtering in water solution at room temperature under ultrasonic for 2h, repeating the above steps for 2 times, washing and drying to obtain Al₂O₃Al having a large number of hydroxyl groups on the surface₂O₃-MgO-TiO₂Solid solution powder C;

and 4, step 4: adding 50g of solid solution powder C obtained in the step 3 into a toluene solvent in which 35g of p-dodecylbenzenesulfonyl chloride is dissolved, dropwise adding 10g of triethylamine at 25 ℃ under stirring, continuously reacting for 1h after dropwise adding, filtering and drying to obtain p-dodecylbenzenesulfonyl modified Al₂O₃-MgO-TiO₂A solid solution strengthening agent.

The invention also provides a preparation method of the high-pressure sealing ring, which comprises the following steps:

step 1: placing styrene butadiene rubber into an open mill, plasticating raw rubber, controlling the temperature at 60-80 ℃ and plasticating time at 15min to obtain plasticated rubber.

Step 2: placing the plasticated rubber into an internal mixer, adding a reinforcing agent, a vulcanizing agent, an anti-aging agent, an accelerator, zinc oxide and stearic acid, and mixing to prepare mixed rubber, wherein the mixing temperature is controlled at 130-150 ℃, and the mixing time is 25 min.

And step 3: and vulcanizing the rubber compound in a vulcanizing machine at the vulcanizing temperature of 150-160 ℃, under the pressure of 20-30MPa for 15min, and finally performing compression molding to obtain the high-pressure sealing ring.

Compared with the prior art, the high-pressure sealing ring provided by the invention contains the styrene butadiene rubber which is an excellent elastomer and is very suitable for manufacturingA seal ring; nanometer aluminum oxide with high hardness and good dimensional stability is prepared into Al modified by p-dodecyl benzene sulfonyl₂O₃-MgO-TiO₂In the course of solid solution, Al₂O₃-MgO-TiO₂The solid solution structure reduces Al₂O₃Polarity, inhibiting the aggregation capability and improving the dispersibility; the introduced p-dodecyl benzene sulfonyl is a linear alkyl arene which has certain similarity with the chemical structure of styrene butadiene rubber and can further increase Al₂O₃The dispersibility and the compatibility with the natural rubber are increased. Two processing steps greatly promote Al₂O₃The styrene butadiene rubber is uniformly dispersed, the fusion capacity of the styrene butadiene rubber and natural rubber is improved, and the mechanical properties such as mechanics, strength and the like of the natural rubber are obviously improved. Therefore, p-dodecylbenzenesulfonyl group-modified Al is added₂O₃-MgO-TiO₂The seal ring of solid solution has excellent high pressure resistance.

Detailed Description

For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.

In the following examples and comparative examples, the vulcanizing agent was 4,4' -dithiodimorpholine; the accelerator is dibenzothiazyl disulfide; the anti-aging agent is anti-aging agent 4010.

Example 1

The formula of the high-pressure sealing ring comprises the following components in parts by mass: 100 parts of styrene butadiene rubber, 2 parts of reinforcing agent, 1.2 parts of vulcanizing agent, 0.6 part of accelerator, 3 parts of anti-aging agent, 3 parts of zinc oxide and 0.6 part of stearic acid.

The reinforcing agent is Al modified by p-dodecyl benzene sulfonyl₂O₃-MgO-TiO₂Solid solution.

P-dodecylbenzenesulfonyl modified Al₂O₃-MgO-TiO₂The preparation method of the solid solution strengthening agent comprises the following steps:

step 1: 50gAl is added₂O₃And 30g of MgO for wet ball milling for 5h, adding 20g of TiO2 for continuous wet ball milling for 3h to obtain Al₂O₃MgO and TiO₂A uniform mixture A of the three;

step 2: drying the mixture A obtained in the step 1 at 100 ℃ for 1h, sintering at 800 ℃ for 3h, and finally grinding into nanoscale Al₂O₃-MgO-TiO₂Solid solution powder B;

and step 3: adding 80g of solid solution powder B prepared in the step 2 into 100ml of H with the mass fraction of 5%₂O₂Filtering in water solution at room temperature under ultrasonic for 2h, repeating the above steps for 2 times, washing and drying to obtain Al₂O₃Al having a large number of hydroxyl groups on the surface₂O₃-MgO-TiO₂Solid solution powder C;

and 4, step 4: adding 50g of solid solution powder C obtained in the step 3 into a toluene solvent in which 35g of p-dodecylbenzenesulfonyl chloride is dissolved, dropwise adding 10g of triethylamine at 25 ℃ under stirring, continuously reacting for 1h after dropwise adding, filtering and drying to obtain p-dodecylbenzenesulfonyl modified Al₂O₃-MgO-TiO₂A solid solution strengthening agent.

A preparation method of a high-pressure sealing ring comprises the following steps:

step 1: placing styrene butadiene rubber into an open mill, plasticating raw rubber, controlling the temperature at 60 ℃ and the plasticating time at 15min to obtain plasticated rubber.

Step 2: placing the plasticated rubber into an internal mixer, adding a reinforcing agent, a vulcanizing agent, an anti-aging agent, an accelerator, zinc oxide and stearic acid, and mixing to prepare rubber compound, wherein the mixing temperature is controlled at 130 ℃, and the mixing time is 25 min.

And step 3: and (3) vulcanizing the rubber compound in a vulcanizing machine at the vulcanization temperature of 150 ℃, under the pressure of 20Mpa for 15min, and finally performing compression molding to obtain the high-pressure sealing ring.

Example 2

The formula of the high-pressure sealing ring comprises the following components in parts by mass: 110 parts of styrene butadiene rubber, 4.5 parts of reinforcing agent, 1.9 parts of vulcanizing agent, 1.3 parts of accelerator, 5 parts of anti-aging agent, 6 parts of zinc oxide and 1.1 parts of stearic acid.

The reinforcing agent is Al modified by p-dodecyl benzene sulfonyl₂O₃-MgO-TiO₂Solid solution.

P-dodecylbenzenesulfonyl modified Al₂O₃-MgO-TiO₂The preparation method of the solid solution strengthening agent comprises the following steps:

step 1: 50gAl is added₂O₃And 30g of MgO for wet ball milling for 5h, adding 20g of TiO2 for continuous wet ball milling for 3h to obtain Al₂O₃MgO and TiO₂A uniform mixture A of the three;

step 2: drying the mixture A obtained in the step 1 at 100 ℃ for 1h, sintering at 900 ℃ for 3h, and finally grinding into nanoscale Al₂O₃-MgO-TiO₂Solid solution powder B;

and step 3: adding 80g of solid solution powder B prepared in the step 2 into 100ml of H with the mass fraction of 5%₂O₂Filtering in water solution at room temperature under ultrasonic for 2h, repeating the above steps for 2 times, washing and drying to obtain Al₂O₃Al having a large number of hydroxyl groups on the surface₂O₃-MgO-TiO₂Solid solution powder C;

and 4, step 4: adding 50g of solid solution powder C obtained in the step 3 into a toluene solvent in which 35g of p-dodecylbenzenesulfonyl chloride is dissolved, dropwise adding 10g of triethylamine at 25 ℃ under stirring, continuously reacting for 1h after dropwise adding, filtering and drying to obtain p-dodecylbenzenesulfonyl modified Al₂O₃-MgO-TiO₂A solid solution strengthening agent.

A preparation method of a high-pressure sealing ring comprises the following steps:

step 1: placing styrene butadiene rubber into an open mill, plasticating raw rubber, controlling the temperature at 70 ℃ and the plasticating time at 15min to obtain plasticated rubber.

Step 2: placing the plasticated rubber into an internal mixer, adding a reinforcing agent, a vulcanizing agent, an anti-aging agent, an accelerator, zinc oxide and stearic acid, and mixing to prepare mixed rubber, wherein the mixing temperature is controlled at 140 ℃ and the mixing time is 25 min.

And step 3: and (3) putting the rubber compound into a vulcanizing machine for vulcanization, wherein the vulcanization temperature is 155 ℃, the pressure range is 25Mpa, the vulcanization time is 15min, and finally, carrying out compression molding to obtain the high-pressure sealing ring.

Example 3

The formula of the high-pressure sealing ring comprises the following components in parts by mass: 120 parts of styrene butadiene rubber, 7 parts of reinforcing agent, 3.5 parts of vulcanizing agent, 1.9 parts of accelerator, 7 parts of anti-aging agent, 8 parts of zinc oxide and 1.6 parts of stearic acid.

The reinforcing agent is Al modified by p-dodecyl benzene sulfonyl₂O₃-MgO-TiO₂Solid solution.

P-dodecylbenzenesulfonyl modified Al₂O₃-MgO-TiO₂The preparation method of the solid solution strengthening agent comprises the following steps:

step 1: 50gAl is added₂O₃And 30g of MgO for wet ball milling for 5h, adding 20g of TiO2 for continuous wet ball milling for 3h to obtain Al₂O₃MgO and TiO₂A uniform mixture A of the three;

step 2: drying the mixture A obtained in the step 1 at 100 ℃ for 1h, sintering at 1000 ℃ for 3h, and finally grinding into nanoscale Al₂O₃-MgO-TiO₂Solid solution powder B;

and step 3: adding 80g of solid solution powder B prepared in the step 2 into 100ml of H with the mass fraction of 5%₂O₂Filtering in water solution at room temperature under ultrasonic for 2h, repeating the above steps for 2 times, washing and drying to obtain Al₂O₃Al having a large number of hydroxyl groups on the surface₂O₃-MgO-TiO₂Solid solution powder C;

and 4, step 4: adding 50g of solid solution powder C obtained in the step 3 into a toluene solvent in which 35g of p-dodecylbenzenesulfonyl chloride is dissolved, dropwise adding 10g of triethylamine at 25 ℃ under stirring, continuously reacting for 1h after dropwise adding, filtering and drying to obtain p-dodecylbenzenesulfonyl modified Al₂O₃-MgO-TiO₂A solid solution strengthening agent.

A preparation method of a high-pressure sealing ring comprises the following steps:

step 1: placing styrene butadiene rubber into an open mill, plasticating raw rubber, controlling the temperature at 80 ℃, and plasticating time at 15min to obtain plasticated rubber.

Step 2: placing the plasticated rubber into an internal mixer, adding a reinforcing agent, a vulcanizing agent, an anti-aging agent, an accelerator, zinc oxide and stearic acid, and mixing to prepare rubber compound, wherein the mixing temperature is controlled at 150 ℃, and the mixing time is 25 min.

And step 3: and (3) putting the rubber compound into a vulcanizing machine for vulcanization, wherein the vulcanization temperature is 160 ℃, the pressure range is 30Mpa, the vulcanization time is 15min, and finally, carrying out compression molding to obtain the high-pressure sealing ring.

Comparative example 1

The formula of the high-pressure sealing ring comprises the following components in parts by mass: 110 parts of styrene butadiene rubber, 4.5 parts of reinforcing agent, 1.9 parts of vulcanizing agent, 1.3 parts of accelerator, 5 parts of anti-aging agent, 6 parts of zinc oxide and 1.1 parts of stearic acid.

The reinforcing agent is Al₂O₃-MgO-TiO₂A solid solution, the method of making comprising the steps of:

step 1: 50gAl is added₂O₃And 30g of MgO are subjected to wet ball milling for 5 hours, and 20g of TiO is added₂Carrying out wet ball milling for 3h to obtain Al₂O₃MgO and TiO₂A uniform mixture A of the three;

step 2: drying the mixture A obtained in the step 1 at 100 ℃ for 1h, sintering at 900 ℃ for 3h, and finally grinding into nanoscale Al₂O₃-MgO-TiO₂Solid solution powder;

a method for preparing a high-pressure seal ring, which comprises the same steps as example 2.

Comparative example 2

The formula of the high-pressure sealing ring comprises the following components in parts by mass: 110 parts of styrene butadiene rubber, 4.5 parts of reinforcing agent, 1.9 parts of vulcanizing agent, 1.3 parts of accelerator, 5 parts of anti-aging agent, 6 parts of zinc oxide and 1.1 parts of stearic acid.

The reinforcing agent is nano Al modified by p-dodecyl benzene sulfonyl₂O₃The preparation method comprises the following steps:

step 1: nano 80g of Al₂O₃Adding 100ml of H with the mass fraction of 5%₂O₂Filtering in water solution at room temperature under ultrasonic for 2h, repeating the above steps for 2 times, washing and drying to obtain nano Al with a large amount of hydroxyl on the surface₂O₃。

Step 2: 50g of nano Al with a large amount of hydroxyl on the surface obtained in the step 2₂O₃Adding into toluene dissolved with 35g of p-dodecylbenzene sulfonyl chloride, dropwise adding 10g of triethylamine at 25 ℃ under stirring, continuously reacting for 1h after dropwise adding, filtering and drying to obtain p-dodecylbenzene sulfonyl modified nano Al₂O₃A reinforcing agent.

A method for preparing a high-pressure seal ring, which comprises the same steps as example 2.

Comparative example 3

The formula of the high-pressure sealing ring comprises the following components in parts by mass: 110 parts of styrene butadiene rubber, 4.5 parts of reinforcing agent, 1.9 parts of vulcanizing agent, 1.3 parts of accelerator, 5 parts of anti-aging agent, 6 parts of zinc oxide and 1.1 parts of stearic acid.

The reinforcing agent is nano Al₂O₃。

A method for preparing a high-pressure seal ring, which comprises the same steps as example 2.

TABLE 1 compression resistance of seal rings in different embodiments

Detailed description of the preferred embodiments	Example 1	Example 2	Example 3	Comparative example 1	Comparative example 2	Comparative example 3
							Compressive strength (MPa)	45.33	46.16	45.71	40.69	39.77	37.05

As can be seen from Table 1, p-dodecylbenzenesulfonyl group is added to Al₂O₃The using effect after modification is not obvious, but the modification is carried out on Al₂O₃-MgO-TiO₂The use effect of the modified solid solution is very obvious.

Through Al₂O₃-MgO-TiO₂The solid solution and the dodecyl benzene sulfonyl are modified, and the Al is obviously increased₂O₃The dispersibility and compatibility in the styrene butadiene rubber obviously increase the mechanical properties such as mechanics, strength and the like of the composite rubber material, and the sealing ring made of the material has excellent high-pressure resistance.

Claims (4)

1. The high-pressure sealing ring is characterized by comprising the following components in parts by mass: 100-120 parts of styrene butadiene rubber, 2-7 parts of reinforcing agent, 1.2-3.5 parts of vulcanizing agent, 0.6-1.9 parts of accelerator, 3-7 parts of anti-aging agent, 3-8 parts of zinc oxide and 0.6-1.6 parts of stearic acid;

the reinforcing agent is Al modified by p-dodecyl benzene sulfonyl₂O₃-MgO-TiO₂Solid solution.

2. The high-pressure seal ring according to claim 1, comprising the following components in parts by mass: 110 parts of styrene butadiene rubber, 4.5 parts of reinforcing agent, 1.9 parts of vulcanizing agent, 1.3 parts of accelerator, 5 parts of anti-aging agent, 6 parts of zinc oxide and 1.1 parts of stearic acid.

3. The high-pressure seal ring according to claim 1, wherein the p-dodecylbenzenesulfonyl group-modified Al₂O₃-MgO-TiO₂The preparation method of the solid solution strengthening agent comprises the following steps:

step 1: 50gAl is added₂O₃And 30g of MgO for wet ball milling for 5h, adding 20g of TiO2 for continuous wet ball milling for 3h to obtain Al₂O₃MgO and TiO₂A uniform mixture A of the three;

step 2: drying the mixture A obtained in the step 1 at 100 ℃ for 1h, sintering at 800-1000 ℃ for 3h, and finally grinding to obtain nanoscale Al₂O₃-MgO-TiO₂Solid solution powder B;

and step 3: adding 80g of solid solution powder B prepared in the step 2 into 100ml of H with the mass fraction of 5%₂O₂Filtering in water solution at room temperature under ultrasonic for 2h, repeating the above steps for 2 times, washing and drying to obtain Al₂O₃Al having a large number of hydroxyl groups on the surface₂O₃-MgO-TiO₂Solid solution powder C;

and 4, step 4: adding 50g of solid solution powder C obtained in the step 3 into a toluene solvent in which 35g of p-dodecylbenzenesulfonyl chloride is dissolved, dropwise adding 10g of triethylamine at 25 ℃ under stirring, continuously reacting for 1h after dropwise adding, filtering and drying to obtain p-dodecylbenzenesulfonyl modified Al₂O₃-MgO-TiO₂A solid solution strengthening agent.

4. A method for manufacturing a high-pressure seal ring according to any one of claims 1 to 3, comprising the steps of:

step 1: placing styrene butadiene rubber in an open mill, plasticating raw rubber, controlling the temperature at 60-80 ℃, and plasticating for 15min to obtain plasticated rubber;

step 2: placing the plasticated rubber in an internal mixer, adding a reinforcing agent, a vulcanizing agent, an anti-aging agent, an accelerator, zinc oxide and stearic acid, and mixing to prepare mixed rubber, wherein the mixing temperature is controlled at 130-150 ℃, and the mixing time is 25 min;

and step 3: and vulcanizing the rubber compound in a vulcanizing machine at the vulcanizing temperature of 150-160 ℃, under the pressure of 20-30MPa for 15min, and finally performing compression molding to obtain the high-pressure sealing ring.