Perfluoroether elastomer composition with low viscosity as well as preparation method and application thereof

Abstract

The invention relates to the technical field of perfluoroether elastomer compositions, in particular to a perfluoroether elastomer composition with low viscosity as well as a preparation method and application thereof. The perfluoroether elastomer composition is prepared from the following raw materials in parts by weight: 90-110 parts of perfluoroether rubber and 0.5-2 parts of a cross-linking agent, and the cross-linking agent comprises a urea-containing compound and a derivative thereof. The perfluoroether elastomer composition provided by the invention has good mechanical properties and excellent high temperature resistance, can reduce the viscous force of the perfluoroether elastomer composition with metal after being heated and vulcanized, can be used in contact with metal materials, and is suitable for the technical fields of semiconductors and aerospace.

Description

Technical Field

[0001] The invention relates to the technical field of perfluoroether elastomer compositions, and in particular to a perfluoroether elastomer composition with low viscosity, a preparation method and an application thereof. Background Art

[0002] Perfluoroether rubber has good high temperature resistance, corrosion resistance and chemical resistance, so perfluoroether rubber is made into seals for use in semiconductor manufacturing equipment. In particular, when perfluoroether rubber with a vulcanization point monomer containing a nitrile group is used to make seals, it has excellent thermal stability, which can reduce downtime caused by seal failure and reduce maintenance costs. However, seals vulcanized from perfluoroether rubber with a vulcanization point monomer containing a nitrile group have high adhesion to metals. Therefore, when the parts of semiconductor manufacturing equipment are replaced, the seals are not easy to separate from the metal parts, which increases the maintenance time, causes longer downtime, and increases maintenance costs.

[0003] At present, 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane (BOAP) is used as a cross-linking agent in combination with perfluoroether rubber, but the use of BOAP as a vulcanizing agent cannot reduce the adhesion between the seals vulcanized by perfluoroether rubber and the metal; the Chinese patent with patent application number CN202311209829.8 provides a fluororubber composition and a preparation method thereof that can effectively reduce the adhesion to metal, and adopts a method of adding polytetrafluoroethylene micropowder and perfluororesin to the fluororubber to reduce the adhesion between the fluororubber composition and the metal; but the technical solution does not involve reducing the adhesion to the metal without adding other raw materials.

[0004] Therefore, providing a perfluoroether elastomer composition with low viscosity after heat vulcanization is a major technical problem that needs to be solved at present. Summary of the invention

[0005] The first aspect of the present invention provides a low-viscosity perfluoroether elastomer composition, wherein the raw materials for its preparation include, by weight, 90-110 parts of perfluoroether rubber and 0.5-2 parts of a crosslinking agent, wherein the crosslinking agent includes urea-containing compounds and derivatives thereof.

[0006] In one embodiment, the perfluoroether rubber is copolymerized with hexafluoropropylene, tetrafluoroethylene, perfluoroalkoxyalkyl vinyl ether or perfluoroalkyl vinyl ether as main monomers and a small amount of vulcanization site monomer; the vulcanization site monomer is a vulcanization site monomer containing a nitrile group (CN-CSM).

[0007] In one embodiment, the perfluoroether rubber is a commercially available product, and examples thereof include perfluoroether rubber PFE 194T produced by 3M Company.

[0008] In one embodiment, the functional groups in the urea-containing compound and its derivatives include one or more combinations of cycloalkyl, olefin, benzene ring, and alkane.

[0009] The inventors found during the experiment that while reducing the adhesion between the perfluoroether elastomer composition and the metal after heating and vulcanization, perfluoroether rubber products of different colors can also be obtained; and the color is obtained by a cross-linking agent, not by adding a masterbatch. The perfluoroether elastomer composition provided in the present application can obtain perfluoroether rubber products of different colors by heating and vulcanization under the premise of low metal ion content, meeting the needs of different processes; the possible reason is that the functional groups of the urea-containing compounds and their derivatives used in the present application include cycloalkyl, olefins, benzene rings, and alkanes, and the functional groups contained therein will cause the perfluoroether elastomer composition to display different colors in the visible light region after vulcanization.

[0010] In one embodiment, the crosslinking agent includes a combination of one or more of N-butyl urea, allyl urea, imidazolidinyl urea, and N-cyclohexyl urea.

[0011] In one embodiment, the cross-linking agent is N-butyl urea.

[0012] In one embodiment, the cross-linking agent is allyl urea.

[0013] In one embodiment, the cross-linking agent is imidazolidinyl urea.

[0014] In one embodiment, the cross-linking agent is N-cyclohexylurea.

[0015] In one embodiment, the cross-linking agent further comprises a diaminophenol compound.

[0016] In one embodiment, the diaminophenol compound is 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane.

[0017] In one embodiment, the crosslinking agent includes one or more of N-butyl urea, allyl urea, imidazolidinyl urea, N-cyclohexyl urea, and 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane.

[0018] In one embodiment, the crosslinking agent is a composition formed of N-butyl urea and 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane.

[0019] In one embodiment, the crosslinking agent is a composition formed of allyl urea and 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane.

[0020] In one embodiment, the crosslinking agent is a composition formed of imidazolidinyl urea and 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane.

[0021] In one embodiment, the crosslinking agent is a composition formed of N-cyclohexylurea and 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane.

[0022] In one embodiment, the mass ratio of the urea-containing compound and its derivatives to the diaminophenol compound is (1-2): (1-2).

[0023] In order to reduce the adhesion between the perfluoroether elastomer composition and the metal after heat vulcanization, the inventors found in the experimental process that when a diaminophenol compound is used in combination with a urea-containing compound and its derivatives as a crosslinking agent, especially when the mass ratio of the urea-containing compound and its derivatives to the diaminophenol compound is (1-2): (1-2), the crosslinking agent and the perfluoroether rubber are combined, especially when the perfluoroether rubber contains a nitrile-containing vulcanization site monomer, the adhesion between the obtained perfluoroether elastomer composition and the metal after heat vulcanization can be reduced.

[0024] A second aspect of the present invention provides a method for preparing a perfluoroether elastomer composition with low viscosity, comprising the following steps:

[0025] A crosslinking agent is added to the perfluoroether rubber to obtain a perfluoroether elastomer composition having low viscosity.

[0026] In one embodiment, the method for preparing the perfluoroether elastomer composition having low viscosity comprises the following steps:

[0027] Adjust the roller distance of the mixing mill to 1.0-1.5mm, add the perfluoroether rubber into the mixing mill, thin it 2-3 times and wrap the roller, after it is fully softened, adjust the roller distance of the mixing mill to 0.6-0.8mm, add the cross-linking agent, after the cross-linking agent is evenly mixed, adjust the roller distance to 0.2mm, and use the triangle wrapping method to thin it 5-10 times; adjust the roller distance of the mixing mill to 1.0mm, take out the sheet, and obtain the perfluoroether elastomer composition, which is parked for more than 12 hours for standby use.

[0028] In one embodiment, the method for preparing the perfluoroether elastomer composition having low viscosity comprises the following steps:

[0029] Adjust the roller distance of the mixing mill to 1.0 mm, add the perfluoroether rubber into the mixing mill, pass it through the mill twice and wrap it with a roller. After it is fully softened, adjust the roller distance of the mixing mill to 0.6 mm, add the cross-linking agent, and after the cross-linking agent is evenly mixed, adjust the roller distance to 0.2 mm, and pass it through the mill 7 times using the triangle wrapping method; adjust the roller distance of the mixing mill to 1.0 mm, take out the sheet, and obtain the perfluoroether elastomer composition, which is parked for more than 12 hours for use.

[0030] A third aspect of the present invention provides an application of a low-viscosity perfluoroether elastomer composition, wherein a vulcanized product formed by heating and vulcanizing the low-viscosity perfluoroether elastomer composition is applied to the fields of semiconductor and aerospace technology.

[0031] In one embodiment, the adhesion between the vulcanized product obtained by heating and vulcanizing the perfluoroether elastomer composition and the metal is less than 220N.

[0032] In one embodiment, the heating vulcanization includes one-stage heating vulcanization and two-stage heating vulcanization. The vulcanization pressure of the one-stage heating vulcanization is 10-20 MPa, the vulcanization temperature is 150-190° C., and the vulcanization time is 5-15 min.

[0033] In one embodiment, the vulcanization pressure of the one-stage heating vulcanization includes but is not limited to 10MPa, 11MPa, 12MPa, 13MPa, 14MPa, 15MPa, 16MPa, 17MPa, 18MPa, 19MPa, 20MPa; the vulcanization temperature includes but is not limited to 150°C, 155°C, 160°C, 165°C, 170°C, 175°C, 180°C, 185°C, 190°C; the vulcanization time includes but is not limited to 5min, 6min, 7min, 8min, 9min, 10min, 11min, 12min, 13min, 14min, 15min.

[0034] In one embodiment, the vulcanization temperature of the two-stage heating vulcanization is 280-300° C., and the vulcanization time is 20-30 hours.

[0035] In one embodiment, a perfluoroether elastomer composition is placed in a mold, and the mold is placed in a flat vulcanizer for one-stage heating and vulcanization to obtain a first-stage vulcanized product; after the first-stage vulcanized product is left for 6-12 hours, it is placed in an oven for two-stage heating and vulcanization, and the temperature is naturally reduced to 25°C to prepare a vulcanized product.

[0036] In one embodiment, the method for preparing a vulcanized product formed by heating and vulcanizing the perfluoroether elastomer composition comprises the following steps:

[0037] The perfluoroether elastomer composition is placed in a mold, and the mold is placed in a flat vulcanizer for one-stage heating vulcanization to obtain a one-stage vulcanized product, wherein the vulcanization pressure of the one-stage heating vulcanization is 15 MPa, the vulcanization temperature is 170°C, and the vulcanization time is 10 min; after the one-stage vulcanization product is parked for 10 hours, it is placed in an oven for two-stage heating vulcanization, wherein the vulcanization temperature of the two-stage heating vulcanization is 290°C, the vulcanization time is 24 hours, and the temperature is naturally lowered to 25°C to prepare a vulcanized product.

[0038] Beneficial Effects

[0039] 1. The perfluoroether elastomer composition provided in the present application has good mechanical properties and excellent high temperature resistance, and can meet the needs of more processes.

[0040] 2. The perfluoroether elastomer composition provided in the present application has a compression permanent deformation of less than or equal to 30 after heating and vulcanization, and can be used in working conditions such as high temperature compression.

[0041] 3. The perfluoroether elastomer composition provided in the present application can obtain perfluoroether rubber products of different colors by heating and vulcanization without using a masterbatch, while ensuring the low metal ion content of the vulcanized product, thereby meeting the use requirements of different processes.

[0042] 4. The perfluoroether elastomer composition provided in the present application has low adhesion to metals and is suitable for use in the fields of semiconductor and aerospace technology.

[0043] 5. In the present application, when urea-containing compounds and their derivatives are used as crosslinking agents, or when diaminophenol compounds are used in combination with urea-containing compounds and their derivatives as crosslinking agents, the adhesion between the perfluoroether elastomer composition and the metal after heating and vulcanization can be reduced to less than 220N. BRIEF DESCRIPTION OF THE DRAWINGS

[0044] Figure 1 Color state diagram of the sealing ring obtained after the perfluoroether elastomer composition provided in Examples 1-7 and Comparative Example 1 is heated and vulcanized.

[0045] Figure 2 This is the test standard content 1 of "Q / SXM 001-2022 Test method for adhesion of vulcanized rubber to metal under constant deformation".

[0046] Figure 3 This is the test standard content 2 of "Q / SXM 001-2022 Test method for adhesion of vulcanized rubber to metal under constant deformation".

[0047] Figure 4 This is the test standard content 3 of "Q / SXM 001-2022 Test method for adhesion of vulcanized rubber to metal under constant deformation".

[0048] Figure 5 This is the test standard content 4 of "Q / SXM 001-2022 Test method for adhesion of vulcanized rubber to metal under constant deformation". DETAILED DESCRIPTION

[0049] The purchase sources or models of the raw materials used in the following examples are shown in Table 1:

[0050] Table 1

[0051]

[0052] Example 1

[0053] In a first aspect, the present embodiment provides a low-viscosity perfluoroether elastomer composition, wherein the raw materials for preparing the perfluoroether elastomer composition include, by weight, 100 parts of perfluoroether rubber and 1.2 parts of a cross-linking agent.

[0054] The cross-linking agent is allyl urea.

[0055] The second aspect of this embodiment provides a method for preparing a perfluoroether elastomer composition with low viscosity, comprising the following steps:

[0056] Adjust the roller distance of the mixing mill to 1.0 mm, add the perfluoroether rubber into the mixing mill, pass it through the mill twice and wrap it with a roller. After it is fully softened, adjust the roller distance of the mixing mill to 0.6 mm, add the cross-linking agent, and after the cross-linking agent is evenly mixed, adjust the roller distance to 0.2 mm, and pass it through the mill 7 times using the triangle wrapping method; adjust the roller distance of the mixing mill to 1.0 mm, take out the sheet, and obtain the perfluoroether elastomer composition, which is parked for 12 hours for use.

[0057] A third aspect of this embodiment provides an application of a perfluoroether elastomer composition with low viscosity. The perfluoroether elastomer composition with low viscosity is subjected to heating and vulcanization to form a vulcanized product which is applied in the fields of semiconductor and aerospace technology.

[0058] The method for preparing a vulcanized product formed by heating and vulcanizing the perfluoroether elastomer composition comprises the following steps:

[0059] The perfluoroether elastomer composition is placed in a mold, and the mold is placed in a flat vulcanizer for one-stage heating vulcanization to obtain a one-stage vulcanized product, wherein the vulcanization pressure of the one-stage heating vulcanization is 15 MPa, the vulcanization temperature is 170°C, and the vulcanization time is 10 min; after the one-stage vulcanization product is parked for 10 hours, it is placed in an oven for two-stage heating vulcanization, wherein the vulcanization temperature of the two-stage heating vulcanization is 290°C, the vulcanization time is 24 hours, and the temperature is naturally lowered to 25°C to prepare a vulcanized product.

[0060] Example 2

[0061] In a first aspect, the present embodiment provides a low-viscosity perfluoroether elastomer composition, wherein the raw materials for preparing the perfluoroether elastomer composition include, by weight, 100 parts of perfluoroether rubber and 1.2 parts of a cross-linking agent.

[0062] The cross-linking agent is N-cyclohexylurea.

[0063] The second aspect of this embodiment provides a method for preparing a perfluoroether elastomer composition with low viscosity, comprising the following steps:

[0064] Adjust the roller distance of the mixing mill to 1.0 mm, add the perfluoroether rubber into the mixing mill, pass it through the mill twice and wrap it with a roller. After it is fully softened, adjust the roller distance of the mixing mill to 0.6 mm, add the cross-linking agent, and after the cross-linking agent is evenly mixed, adjust the roller distance to 0.2 mm, and pass it through the mill 7 times using the triangle wrapping method; adjust the roller distance of the mixing mill to 1.0 mm, take out the sheet, and obtain the perfluoroether elastomer composition, which is parked for 12 hours for use.

[0065] A third aspect of this embodiment provides an application of a perfluoroether elastomer composition with low viscosity. The perfluoroether elastomer composition with low viscosity is subjected to heating and vulcanization to form a vulcanized product which is applied in the fields of semiconductor and aerospace technology.

[0066] The method for preparing a vulcanized product formed by heating and vulcanizing the perfluoroether elastomer composition comprises the following steps:

[0067] The perfluoroether elastomer composition is placed in a mold, and the mold is placed in a flat vulcanizer for one-stage heating vulcanization to obtain a one-stage vulcanized product, wherein the vulcanization pressure of the one-stage heating vulcanization is 15 MPa, the vulcanization temperature is 170°C, and the vulcanization time is 10 min; after the one-stage vulcanization product is parked for 10 hours, it is placed in an oven for two-stage heating vulcanization, wherein the vulcanization temperature of the two-stage heating vulcanization is 290°C, the vulcanization time is 24 hours, and the temperature is naturally lowered to 25°C to prepare a vulcanized product.

[0068] Example 3

[0069] In a first aspect, the present embodiment provides a low-viscosity perfluoroether elastomer composition, wherein the raw materials for preparing the perfluoroether elastomer composition include, by weight, 100 parts of perfluoroether rubber and 1.2 parts of a cross-linking agent.

[0070] The cross-linking agent is imidazolidinyl urea.

[0071] The second aspect of this embodiment provides a method for preparing a perfluoroether elastomer composition with low viscosity, comprising the following steps:

[0072] Adjust the roller distance of the mixing mill to 1.0 mm, add the perfluoroether rubber into the mixing mill, pass it through the mill twice and wrap it with a roller. After it is fully softened, adjust the roller distance of the mixing mill to 0.6 mm, add the cross-linking agent, and after the cross-linking agent is evenly mixed, adjust the roller distance to 0.2 mm, and pass it through the mill 7 times using the triangle wrapping method; adjust the roller distance of the mixing mill to 1.0 mm, take out the sheet, and obtain the perfluoroether elastomer composition, which is parked for 12 hours for use.

[0073] A third aspect of this embodiment provides an application of a perfluoroether elastomer composition with low viscosity. The perfluoroether elastomer composition with low viscosity is subjected to heating and vulcanization to form a vulcanized product which is applied in the fields of semiconductor and aerospace technology.

[0074] The method for preparing a vulcanized product formed by heating and vulcanizing the perfluoroether elastomer composition comprises the following steps:

[0075] The perfluoroether elastomer composition is placed in a mold, and the mold is placed in a flat vulcanizer for one-stage heating vulcanization to obtain a one-stage vulcanized product, wherein the vulcanization pressure of the one-stage heating vulcanization is 15 MPa, the vulcanization temperature is 170°C, and the vulcanization time is 10 min; after the one-stage vulcanization product is parked for 10 hours, it is placed in an oven for two-stage heating vulcanization, wherein the vulcanization temperature of the two-stage heating vulcanization is 290°C, the vulcanization time is 24 hours, and the temperature is naturally lowered to 25°C to prepare a vulcanized product.

[0076] Example 4

[0077] In a first aspect, the present embodiment provides a low-viscosity perfluoroether elastomer composition, wherein the raw materials for preparing the perfluoroether elastomer composition include, by weight, 100 parts of perfluoroether rubber and 1.2 parts of a cross-linking agent.

[0078] The cross-linking agent is N-butyl urea.

[0079] The second aspect of this embodiment provides a method for preparing a perfluoroether elastomer composition with low viscosity, comprising the following steps:

[0080] Adjust the roller distance of the mixing mill to 1.0 mm, add the perfluoroether rubber into the mixing mill, pass it through the mill twice and wrap it with a roller. After it is fully softened, adjust the roller distance of the mixing mill to 0.6 mm, add the cross-linking agent, and after the cross-linking agent is evenly mixed, adjust the roller distance to 0.2 mm, and pass it through the mill 7 times using the triangle wrapping method; adjust the roller distance of the mixing mill to 1.0 mm, take out the sheet, and obtain the perfluoroether elastomer composition, which is parked for 12 hours for use.

[0081] A third aspect of this embodiment provides an application of a perfluoroether elastomer composition with low viscosity. The perfluoroether elastomer composition with low viscosity is subjected to heating and vulcanization to form a vulcanized product which is applied in the fields of semiconductor and aerospace technology.

[0082] The method for preparing a vulcanized product formed by heating and vulcanizing the perfluoroether elastomer composition comprises the following steps:

[0083] The perfluoroether elastomer composition is placed in a mold, and the mold is placed in a flat vulcanizer for one-stage heating vulcanization to obtain a one-stage vulcanized product, wherein the vulcanization pressure of the one-stage heating vulcanization is 15 MPa, the vulcanization temperature is 170°C, and the vulcanization time is 10 min; after the one-stage vulcanization product is parked for 10 hours, it is placed in an oven for two-stage heating vulcanization, wherein the vulcanization temperature of the two-stage heating vulcanization is 290°C, the vulcanization time is 24 hours, and the temperature is naturally lowered to 25°C to prepare a vulcanized product.

[0084] Example 5

[0085] In a first aspect, the present embodiment provides a low-viscosity perfluoroether elastomer composition, wherein the raw materials for preparing the perfluoroether elastomer composition include, by weight, 100 parts of perfluoroether rubber and 1.2 parts of a cross-linking agent.

[0086] The cross-linking agent is a composition of allyl urea and 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane, and the mass ratio of the allyl urea to the 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane is 1:2.

[0087] The second aspect of this embodiment provides a method for preparing a perfluoroether elastomer composition with low viscosity, comprising the following steps:

[0088] Adjust the roller distance of the mixing mill to 1.0 mm, add the perfluoroether rubber into the mixing mill, pass it through the mill twice and wrap it with a roller. After it is fully softened, adjust the roller distance of the mixing mill to 0.6 mm, add the cross-linking agent, and after the cross-linking agent is evenly mixed, adjust the roller distance to 0.2 mm, and pass it through the mill 7 times using the triangle wrapping method; adjust the roller distance of the mixing mill to 1.0 mm, take out the sheet, and obtain the perfluoroether elastomer composition, which is parked for 12 hours for use.

[0089] A third aspect of this embodiment provides an application of a perfluoroether elastomer composition with low viscosity. The perfluoroether elastomer composition with low viscosity is subjected to heating and vulcanization to form a vulcanized product which is applied in the fields of semiconductor and aerospace technology.

[0090] The method for preparing a vulcanized product formed by heating and vulcanizing the perfluoroether elastomer composition comprises the following steps:

[0091] The perfluoroether elastomer composition is placed in a mold, and the mold is placed in a flat vulcanizer for one-stage heating vulcanization to obtain a one-stage vulcanized product, wherein the vulcanization pressure of the one-stage heating vulcanization is 15 MPa, the vulcanization temperature is 170°C, and the vulcanization time is 10 min; after the one-stage vulcanization product is parked for 10 hours, it is placed in an oven for two-stage heating vulcanization, wherein the vulcanization temperature of the two-stage heating vulcanization is 290°C, the vulcanization time is 24 hours, and the temperature is naturally lowered to 25°C to prepare a vulcanized product.

[0092] Example 6

[0093] In a first aspect, the present embodiment provides a low-viscosity perfluoroether elastomer composition, wherein the raw materials for preparing the perfluoroether elastomer composition include, by weight, 100 parts of perfluoroether rubber and 1.2 parts of a cross-linking agent.

[0094] The cross-linking agent is a composition of N-butyl urea and 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane, and the mass ratio of the N-butyl urea to the 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane is 1:2.

[0095] The second aspect of this embodiment provides a method for preparing a perfluoroether elastomer composition with low viscosity, comprising the following steps:

[0096] Adjust the roller distance of the mixing mill to 1.0 mm, add the perfluoroether rubber into the mixing mill, pass it through the mill twice and wrap it with a roller. After it is fully softened, adjust the roller distance of the mixing mill to 0.6 mm, add the cross-linking agent, and after the cross-linking agent is evenly mixed, adjust the roller distance to 0.2 mm, and pass it through the mill 7 times using the triangle wrapping method; adjust the roller distance of the mixing mill to 1.0 mm, take out the sheet, and obtain the perfluoroether elastomer composition, which is parked for 12 hours for use.

[0097] A third aspect of this embodiment provides an application of a perfluoroether elastomer composition with low viscosity. The perfluoroether elastomer composition with low viscosity is subjected to heating and vulcanization to form a vulcanized product which is applied in the fields of semiconductor and aerospace technology.

[0098] The method for preparing a vulcanized product formed by heating and vulcanizing the perfluoroether elastomer composition comprises the following steps:

[0099] The perfluoroether elastomer composition is placed in a mold, and the mold is placed in a flat vulcanizer for one-stage heating vulcanization to obtain a one-stage vulcanized product, wherein the vulcanization pressure of the one-stage heating vulcanization is 15 MPa, the vulcanization temperature is 170°C, and the vulcanization time is 10 min; after the one-stage vulcanization product is parked for 10 hours, it is placed in an oven for two-stage heating vulcanization, wherein the vulcanization temperature of the two-stage heating vulcanization is 290°C, the vulcanization time is 24 hours, and the temperature is naturally lowered to 25°C to prepare a vulcanized product.

[0100] Example 7

[0101] In a first aspect, the present embodiment provides a low-viscosity perfluoroether elastomer composition, wherein the raw materials for preparing the perfluoroether elastomer composition include, by weight, 100 parts of perfluoroether rubber and 1.2 parts of a cross-linking agent.

[0102] The cross-linking agent is a composition of N-butyl urea and 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane, and the mass ratio of the N-butyl urea to the 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane is 2:1.

[0103] The second aspect of this embodiment provides a method for preparing a perfluoroether elastomer composition with low viscosity, comprising the following steps:

[0104] Adjust the roller distance of the mixing mill to 1.0 mm, add the perfluoroether rubber into the mixing mill, pass it through the mill twice and wrap it with a roller. After it is fully softened, adjust the roller distance of the mixing mill to 0.6 mm, add the cross-linking agent, and after the cross-linking agent is evenly mixed, adjust the roller distance to 0.2 mm, and pass it through the mill 7 times using the triangle wrapping method; adjust the roller distance of the mixing mill to 1.0 mm, take out the sheet, and obtain the perfluoroether elastomer composition, which is parked for 12 hours for use.

[0105] A third aspect of this embodiment provides an application of a perfluoroether elastomer composition with low viscosity. The perfluoroether elastomer composition with low viscosity is subjected to heating and vulcanization to form a vulcanized product which is applied in the fields of semiconductor and aerospace technology.

[0106] The method for preparing a vulcanized product formed by heating and vulcanizing the perfluoroether elastomer composition comprises the following steps:

[0107] The perfluoroether elastomer composition is placed in a mold, and the mold is placed in a flat vulcanizer for one-stage heating vulcanization to obtain a one-stage vulcanized product, wherein the vulcanization pressure of the one-stage heating vulcanization is 15 MPa, the vulcanization temperature is 170°C, and the vulcanization time is 10 min; after the one-stage vulcanization product is parked for 10 hours, it is placed in an oven for two-stage heating vulcanization, wherein the vulcanization temperature of the two-stage heating vulcanization is 290°C, the vulcanization time is 24 hours, and the temperature is naturally lowered to 25°C to prepare a vulcanized product.

[0108] Comparative Example 1

[0109] Comparative Example 1 provides a perfluoroether elastomer composition, and the specific implementation manner is the same as that of Example 1. The difference between Comparative Example 1 and Example 1 is that 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane is used as a crosslinking agent.

[0110] The vulcanized product formed by heating and vulcanizing the perfluoroether elastomer composition provided in Examples 1-7 and Comparative Example 1 is a sealing ring.

[0111] Performance Test:

[0112] (1) Color status:

[0113] Observe the color of the sealing ring obtained after the perfluoroether elastomer composition provided in Examples 1-7 and Comparative Example 1 is heated and vulcanized. The observation results are shown in Figure 1 .

[0114] (2) Vulcanization characteristic parameter test:

[0115] The perfluoroether elastomer compositions provided in Examples 1-7 and Comparative Example 1 were respectively tested for their vulcanization characteristic parameters in accordance with "GBT16584-1996 Determination of Vulcanization Characteristics of Rubber Using a Rotorless Vulcanizer". The vulcanization temperature in the rotorless vulcanizer was set to 180°C and the vulcanization time was set to 30 min. The vulcanization characteristic parameters included TS2, TC50, TC90, ML, and MH. The test results are shown in Table 2.

[0116] (3) Hardness test:

[0117] After the perfluoroether elastomer compositions provided in Examples 1-7 and Comparative Example 1 were heated and vulcanized, their Shore A hardness was measured in accordance with GBT 531.1-2008 Test method for indentation hardness of vulcanized rubber or thermoplastic rubber Part 1 - Shore hardness tester method (Shore hardness) standard. The test results are shown in Table 2.

[0118] (4) Tensile properties test:

[0119] After the perfluoroether elastomer compositions provided in Examples 1-7 and Comparative Example 1 were heated and vulcanized, their tensile strength, 100% modulus, and elongation at break were tested in accordance with GBT 528-2009 Determination of tensile stress-strain properties of vulcanized rubber or thermoplastic rubber. The test results are shown in Table 2.

[0120] (5) Compression set test:

[0121] After heating and vulcanization, the perfluoroether elastomer compositions provided in Examples 1-7 and Comparative Example 1 were tested for compression set at high temperature in accordance with GBT7759.1-2015 Determination of compression set of vulcanized rubber or thermoplastic rubber Part 1: At room temperature and high temperature conditions. The test results are shown in Table 2.

[0122] (6) Adhesion test:

[0123] The perfluoroether elastomer compositions provided in Examples 1-7 and Comparative Example 1 were heated and vulcanized, and then their adhesion to metal was tested in accordance with "Q / SXM001-2022 Test Method for Adhesion of Vulcanized Rubber to Metal under Constant Deformation". The test results are shown in Table 2.

[0124] Regarding the test standard "Q / SXM 001-2022 Test Method for Adhesion of Vulcanized Rubber to Metal under Constant Deformation" formulated for the applicant, the test content is as follows Figure 2-5 .

[0125] Table 2

[0126]

[0127]

[0128] It can be seen from the test results in Table 2 that when urea-containing compounds and their derivatives are used as cross-linking agents, or when diaminophenol compounds are used in combination with urea-containing compounds and their derivatives as cross-linking agents in the present application, the adhesion between the perfluoroether elastomer composition and the metal after heating and vulcanization can be reduced to less than 220N, and the perfluoroether elastomer composition can be used in contact with metal materials.

Claims

1. A perfluoroether elastomer composition with low viscosity, characterized in that: The raw materials for its preparation include, by weight: 90-110 parts of perfluoroether rubber and 0.5-2 parts of a crosslinking agent, wherein the crosslinking agent includes urea-containing compounds and derivatives thereof.

2. The perfluoroether elastomer composition with low viscosity according to claim 1, characterized in that The functional groups in the urea-containing compound and its derivatives include one or more combinations of cycloalkyl, olefin, benzene ring and alkane.

3. The perfluoroether elastomer composition with low viscosity according to claim 2, characterized in that The cross-linking agent includes one or more of N-butyl urea, allyl urea, imidazolidinyl urea and N-cyclohexyl urea.

4. The perfluoroether elastomer composition with low viscosity according to any one of claims 1 to 3, characterized in that: The cross-linking agent also includes diaminophenol compounds.

5. The perfluoroether elastomer composition with low viscosity according to claim 4, characterized in that The mass ratio of the urea-containing compound and its derivatives to the diaminophenol compound is (1-2): (1-2).

6. A method for preparing a perfluoroether elastomer composition with low viscosity as claimed in any one of claims 1 to 5, characterized in that: The following steps are involved: A crosslinking agent is added to the perfluoroether rubber to obtain a perfluoroether elastomer composition having low viscosity.

7. An application of the low-viscosity perfluoroether elastomer composition according to any one of claims 1 to 5, characterized in that: The vulcanized product formed by the low-viscosity perfluoroether elastomer composition after heating and vulcanization is applied to the semiconductor and aerospace technology fields.

8. The use of the perfluoroether elastomer composition with low viscosity as claimed in claim 7, characterized in that: The adhesion between the vulcanized product obtained by heating and vulcanizing the perfluoroether elastomer composition and the metal is less than 220N.

9. The use of the perfluoroether elastomer composition with low viscosity as claimed in claim 7, characterized in that: The heating vulcanization includes one-stage heating vulcanization and two-stage heating vulcanization. The vulcanization pressure of the one-stage heating vulcanization is 10-20 MPa, the vulcanization temperature is 150-190° C., and the vulcanization time is 5-15 min.

10. The use of the perfluoroether elastomer composition with low viscosity as claimed in claim 9, characterized in that: The vulcanization temperature of the second-stage heating vulcanization is 280-300°C.

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