CN112920607B - Sealing element for underwater equipment and preparation method thereof - Google Patents
Sealing element for underwater equipment and preparation method thereof Download PDFInfo
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- CN112920607B CN112920607B CN202110143104.8A CN202110143104A CN112920607B CN 112920607 B CN112920607 B CN 112920607B CN 202110143104 A CN202110143104 A CN 202110143104A CN 112920607 B CN112920607 B CN 112920607B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
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Abstract
The application discloses a sealing element for underwater equipment and a preparation method thereof, and relates to the technical field of sealing element materials. A sealing element for underwater equipment is mainly prepared from the following raw materials in parts by weight: 80-120 parts of silicon rubber, 1.8-3.5 parts of alpha-zinc hydroxypropionate, 3-10 parts of hydroxyl-terminated polybutylene, 3-9 parts of a curing agent, 4-5.5 parts of a vulcanizing agent and 14-20 parts of a filler. It has the advantage of good corrosion resistance. The preparation method comprises the following steps: kneading, vulcanization, and the like. The preparation method has the advantage of improving the corrosion resistance of the product.
Description
Technical Field
The application relates to the technical field of sealing element materials, in particular to a sealing element for underwater equipment and a preparation method thereof.
Background
Silicone rubbers are rubbers whose backbone is composed of alternating silicon and oxygen atoms to which two organic groups are usually attached. The silicone rubber has the advantages of excellent high and low temperature resistance, oil resistance and the like, and is widely used as a sealing element material in the fields of automobiles, medical treatment, underwater submarines, aerospace and the like. The sealing element for underwater equipment, especially for equipment working in seawater such as submarine and ocean measuring equipment, has higher requirement on the corrosion resistance of materials due to higher salt content in seawater.
At present, zinc oxide is added into a common silicon rubber sealing element for underwater equipment, the zinc oxide is used as a reinforcing agent and a vulcanization activator, and zinc ions in the zinc oxide and silicon rubber generate salt-resistant cross-linked bonds, so that the corrosion resistance of the sealing element is improved.
In view of the above-mentioned related technologies, the inventors believe that the greater density of zinc oxide, the lesser density of silicone rubber, and the greater density difference between zinc oxide and silicone rubber are detrimental to the uniform dispersion of zinc oxide in silicone rubber and to the better improvement of the corrosion resistance of silicone rubber seals for underwater equipment.
Disclosure of Invention
In order to improve the corrosion resistance of a silicon rubber sealing element for underwater equipment, the application provides a sealing element for the underwater equipment and a preparation method thereof.
In a first aspect, the present application provides a sealing member for an underwater device, which adopts the following technical scheme:
a sealing element for underwater equipment is mainly prepared from the following raw materials in parts by weight: 80-120 parts of silicon rubber, 1.8-3.5 parts of alpha-zinc hydroxypropionate, 3-10 parts of hydroxyl-terminated polybutylene, 3-9 parts of a curing agent, 4-5.5 parts of a vulcanizing agent and 14-20 parts of a filler.
By adopting the technical scheme, zinc oxide is replaced by the alpha-zinc hydroxypropionate, and the hydroxyl-terminated polydiene is added, so that the alpha-zinc hydroxypropionate and the hydroxyl-terminated polydiene have good compatibility, and the alpha-zinc hydroxypropionate is uniformly dispersed in the silicon rubber along with the hydroxyl-terminated polydiene in the vulcanization process, thereby being beneficial to the cross-linking reaction of zinc ions and the silicon rubber and being beneficial to better improving the mechanical property and the corrosion resistance of a sealing element product; under the combined action of the alpha-zinc hydroxypropionate and the hydroxyl-terminated polydibutene, the zinc ion has higher reactivity, can reduce the vulcanization temperature, is favorable for preventing the occurrence of a reversion phenomenon, and is favorable for better improving the tensile resistance and the corrosion resistance of a sealing element product.
Preferably, the sealing element is mainly prepared from the following raw materials in parts by weight: 95-105 parts of silicon rubber, 2.5-2.8 parts of alpha-zinc hydroxypropionate, 5.5-7.5 parts of hydroxyl-terminated polybutylene, 5.5-6.5 parts of curing agent, 4-5.5 parts of vulcanizing agent and 14-20 parts of filling material. More preferably, 100 parts of silicon rubber, 2.6 parts of alpha-zinc hydroxypropionate, 6.5 parts of hydroxyl-terminated polybutylene, 6 parts of curing agent, 4.8 parts of vulcanizing agent and 18 parts of filling material.
By adopting the technical scheme, the better raw material feeding proportion is used, the tensile resistance and the corrosion resistance of the product are favorably improved, the service life of the product is favorably prolonged, and the market popularization of the product is favorably realized.
Preferably, the curing agent is N-phenyl-gamma-aminopropyltrimethoxysilane.
By adopting the technical scheme, the N-phenyl-gamma-aminopropyl trimethoxy silane curing agent is used, and the N-phenyl-gamma-aminopropyl trimethoxy silane interacts with the hydroxyl-terminated polybutylene and the alpha-zinc hydroxypropionate, so that the vulcanization effect is improved, and the tensile resistance of the product is better improved.
Preferably, the vulcanizing agent is N, N' -m-phenylene bismaleimide.
By adopting the technical scheme, the proper vulcanizing agent is used and matched with the curing agent, so that the vulcanizing effect is favorably improved, and the mechanical property of the product is favorably improved.
Preferably, the filler is talcum powder, and the particle size of the talcum powder is not more than 20 microns.
By adopting the technical scheme, the talcum powder is used as the filler and filled in the silicon rubber, which is beneficial to better improving the hardness property and the mechanical property of the product.
Preferably, the raw material of the sealing element also comprises 1.5-3 parts by weight of 2-hydroxyethyl methacrylate phosphate.
By adopting the technical scheme, the 2-hydroxyethyl methacrylate phosphate is added, which is beneficial to improving the adhesive strength among the components of the product and better improving the mechanical property of the product.
Preferably, the raw material of the sealing element also comprises 0.5-2 parts by weight of amino modified silicone oil.
By adopting the technical scheme, the amino modified silicone oil is added, so that the product has proper flexibility, the corrosion resistance of the product is improved, the sealing effect of the sealing element product in use is improved, and the service life of the product is prolonged.
In a second aspect, the present application provides a method for preparing a sealing member for underwater equipment, which adopts the following technical scheme:
a preparation method of a sealing element for underwater equipment is characterized by comprising the following steps:
s1 mixing: taking raw materials of the sealing element, adding the raw materials into a mixing roll, and mixing for 15-25min to prepare base rubber;
s2 vulcanization: transferring the basic glue into a mold at 155 ℃ of 145-2The pressure vulcanization is carried out for 120 seconds and 240 seconds, and the sealing element for the underwater equipment is prepared.
By adopting the technical scheme, because the alpha-zinc hydroxypropionate and the hydroxyl-terminated polybutylene are added, the vulcanization speed is high, the vulcanization can be completed at a lower temperature, the phenomenon of reversion of vulcanization is prevented, and the tensile resistance and the corrosion resistance of a sealing element product are improved better.
In summary, the present application includes at least one of the following beneficial technical effects:
1. according to the method, zinc oxide is replaced by alpha-zinc hydroxypropionate, and the end hydroxyl polybutylene is added, the alpha-zinc hydroxypropionate and the end hydroxyl polybutylene have good compatibility, and in the vulcanization process, the alpha-zinc hydroxypropionate is uniformly dispersed in the silicon rubber along with the end hydroxyl polybutylene, so that the cross-linking reaction of zinc ions and the silicon rubber is facilitated, and the mechanical property and the corrosion resistance of a sealing element product are better improved; under the combined action of the alpha-zinc hydroxypropionate and the hydroxyl-terminated polydibutene, the zinc ion has higher reactivity, can reduce the vulcanization temperature, is favorable for preventing the occurrence of reversion phenomenon of vulcanization, and is favorable for better improving the tensile resistance and the corrosion resistance of a sealing element product;
2. due to the low vulcanization temperature and no need of secondary vulcanization at high temperature for a long time, the method is beneficial to reducing energy consumption and reducing process cost; compared with zinc oxide, the alpha-zinc hydroxypropionate has low zinc content, is beneficial to reducing zinc emission, reducing heavy metal pollution and improving the environmental protection performance of products;
3. according to the preparation method, 2-hydroxyethyl methacrylate phosphate, amino modified silicone oil and proper curing agent and vulcanizing agent are added, so that the tensile resistance and the corrosion resistance of the product are improved better, the service life of the product is prolonged, and the product market popularization is facilitated.
Detailed Description
The inventor finds that in the process of preparing the silicon rubber sealing element for the underwater equipment by using the zinc oxide as the reinforcing agent, the zinc oxide has high density, the density difference between the zinc oxide and the silicon rubber is large, zinc ions are not favorably uniformly dispersed in the silicon rubber, the zinc ions are not favorably subjected to a crosslinking reaction with the silicon rubber, and the tensile property and the corrosion resistance of the silicon rubber sealing element for the underwater equipment are not favorably improved. Based on the above technical background, the present application provides a technical solution for improving the corrosion resistance of a product, which is specifically described in the following detailed description. In the actual production process, sealing element products with different sizes and shapes can be produced according to requirements.
The raw materials referred to in the present application are all commercially available, and the type and source of the raw materials are shown in table 1.
TABLE 1 Specification, type and origin of the raw materials
Examples
Example 1: the sealing element for the underwater equipment is prepared by the following method, and comprises the following steps:
s1 mixing: 100kg of silicon rubber is taken, 2.6kg of alpha-zinc hydroxypropionate, 6.5kg of hydroxyl-terminated polybutylene, 6kg of N-phenyl-gamma-aminopropyltrimethoxysilane curing agent, 4.8kg of N, N' -m-phenylene bismaleimide vulcanizing agent and 18kg of talcum powder are added, mixed uniformly, added into a mixing roll and mixed for 20min at the rotating speed of 10 r/min, and the base rubber is prepared.
S2 vulcanization: spreading the base rubber, cutting into desired size, transferring into injection molding machine containing mold, and processing at 150 deg.C under 160kg/cm2The pressure of (2) was cured for 180 seconds to produce several seals for underwater equipment with dimensions of 400mm x 200mm x 4 mm.
Example 2
Example 2 differs from example 1 in that 2.8kg of 2-hydroxyethyl methacrylate phosphate was added to example 2, all the other things remaining the same as example 1.
Example 3
Example 3 differs from example 2 in that example 3 added 1.2kg of amino-modified silicone oil in step S1, and otherwise remains the same as example 2.
Examples 4 to 13
Examples 4 to 13 are different from example 3 in the addition amount of each raw material of examples 4 to 13, and the addition amount of each raw material of examples 4 to 8 is shown in Table 2, and the addition amount of each raw material of examples 9 to 13 is shown in Table 3.
TABLE 2 addition amounts of the respective raw materials of examples 4 to 8
TABLE 4 addition amount of each raw material of examples 9 to 13
Examples 14 to 17
Examples 14-17 differ from example 3 in that the process parameters for each step of examples 14-17 are different and are otherwise identical to example 3, and the process parameters for each step of examples 14-17 are shown in Table 4.
TABLE 4 parameters in the various steps of examples 14-17
Comparative example
Comparative example 1
Comparative example 1 differs from example 1 in that comparative example 1 does not contain zinc alpha-hydroxypropionate, all the other things remaining in accordance with example 1.
Comparative example 2
Comparative example 2 differs from example 1 in that comparative example 2 does not have the hydroxyl terminated polydibutene added, and otherwise remains the same as example 1.
Comparative example 3
Comparative example 3 is different from comparative example 2 in that comparative example 3 replaces zinc alpha-hydroxypropionate with zinc oxide of equal mass (jinxin powder technology ltd, high grade, purity 99.7% of Dongguan), and the rest is in accordance with comparative example 2.
Comparative example 4
Comparative example 4 differs from comparative example 3 in that comparative example 4 increased the cure temperature from 150 c to 180 c, all else being consistent with comparative example 3.
Performance detection
1. Tensile strength: with reference to GBT528-2009 determination of tensile stress strain properties of vulcanized rubber or thermoplastic rubber, the required test pieces were prepared in the vulcanization step, and tensile strength tests were performed, with the test results as shown in table 5.
2. Liquid resistant tensile strength loss rate: with reference to GBT1690-2006 "methods for testing liquid resistance of vulcanized rubber or thermoplastic rubber", reference is made to the ingredient preparation test liquid disclosed in the oxide-containing standard simulation liquid 2 in the reference liquid in appendix a, and the test results are shown in table 5 after immersion for 7 days.
TABLE 5 comparison table of product performance test results of different sealing parts
Compared with the example 1, the comparative example 1 does not add the alpha-zinc hydroxypropionate, does not add the crosslinking accelerator containing zinc ions, and the prepared sealing element product has low tensile strength and poor mechanical property, is not beneficial to prolonging the service life of the product and is not beneficial to market popularization of the product. The comparative example 2 is added with the alpha-zinc hydroxypropionate, and the end hydroxyl polydibutene is not added, so that the alpha-zinc hydroxypropionate and the silicon rubber are not convenient to have better cross-linking reaction, and the tensile strength of the prepared sealing element product is improved, but the loss rate of the liquid-resistant tensile strength is higher, and the corrosion resistance is not good. Comparative example 3 zinc oxide was used instead of zinc alpha-hydroxypropionate, which has a higher density, and is not conducive to uniform dispersion of zinc oxide in silicone rubber, which is not conducive to better crosslinking reaction, and the resulting sealing member product has slightly improved tensile properties and increased loss rate of liquid-resistant tensile strength. Comparative example 4 on the basis of comparative example 3, the vulcanization temperature is increased, the crosslinking speed is accelerated, the tensile property is obviously improved, but the loss rate of the liquid-resistant tensile strength is increased, and the corrosion resistance is poor.
Comparing the experimental results of the example 1 and the comparative examples 1 to 4, it can be seen that, in the process of preparing the sealing element, zinc oxide is replaced by alpha-hydroxypropionate, and hydroxyl-terminated polydibutene is added, the alpha-hydroxypropionate and the hydroxyl-terminated polydibutene have good compatibility, and in the vulcanization process, the alpha-hydroxypropionate is uniformly dispersed in the silicone rubber along with the hydroxyl-terminated polydibutene, which is beneficial to the cross-linking reaction between zinc ions and the silicone rubber, and is beneficial to better improving the mechanical property and the corrosion resistance of the sealing element product. Under the combined action of the alpha-zinc hydroxypropionate and the hydroxyl-terminated polydibutene, the zinc ion has higher reactivity, can reduce the vulcanization temperature, is favorable for preventing the occurrence of a reversion phenomenon, and is favorable for better improving the tensile resistance and the corrosion resistance of a sealing element product. Meanwhile, because the vulcanization temperature is low, secondary vulcanization at high temperature for a long time is not needed, the energy consumption is reduced, and the process cost is reduced. Compared with zinc oxide, the alpha-zinc hydroxypropionate has low zinc content, is beneficial to reducing zinc emission, reducing heavy metal pollution and improving the environmental protection performance of products. The sealing element product prepared in the embodiment 1 has excellent tensile resistance and corrosion resistance, is beneficial to prolonging the service life of the product, and is beneficial to market popularization of the product.
The experimental results of comparative example 1 and example 2 show that the addition of 2-hydroxyethyl methacrylate phosphate in example 2 helps to improve the adhesion strength between the components in the seal and produces a seal product with better tensile resistance. Comparing the experimental results of example 2 and example 3, example 3 adds amino-modified silicone oil, which helps to improve the corrosion resistance of the product.
Compared with example 3, the addition amount of each raw material in examples 4-13 is different, wherein in examples 4-7, proper raw material feeding proportion is not used, and the tensile property of the prepared product is fluctuated; in the examples 8-11, the prepared product has excellent tensile resistance and corrosion resistance by using a better raw material feeding ratio; in examples 12 to 13, the best raw material feeding ratio is used, and the prepared sealing element product has excellent tensile resistance and corrosion resistance, so that the service life of the product is prolonged, and the market popularization of the product is facilitated.
Compared with example 3, the process parameters of the steps of examples 14 to 17 are different; wherein the vulcanization temperature in step S2 of example 14 is relatively high, the vulcanization temperature in example 14 is equivalent to the common vulcanization temperature of a zinc oxide system, and the tensile resistance of the prepared sealing element product is not obviously changed, but the corrosion resistance is reduced; therefore, in the preparation method for preparing the sealing element disclosed by the application, due to the fact that the alpha-zinc hydroxypropionate and the hydroxyl-terminated polydibutene are added simultaneously, vulcanization is not required to be carried out at high temperature, the vulcanization temperature is reduced, and the reduction of energy consumption is facilitated. The examples 15-17 select suitable process parameters, and the prepared sealing element products have excellent tensile resistance and corrosion resistance, are beneficial to prolonging the service life of the products, and are beneficial to market popularization of the products.
The embodiments of the present invention are preferred embodiments of the present application, and the scope of protection of the present application is not limited by the embodiments, so: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (8)
1. The sealing element for the underwater equipment is characterized by being mainly prepared from the following raw materials in parts by weight: 80-120 parts of silicon rubber, 1.8-3.5 parts of alpha-zinc hydroxypropionate, 3-10 parts of hydroxyl-terminated polybutylene, 3-9 parts of a curing agent, 4-5.5 parts of a vulcanizing agent and 14-20 parts of a filler.
2. The sealing member for underwater equipment according to claim 1, which is mainly prepared from the following raw materials in parts by weight: 95-105 parts of silicon rubber, 2.5-2.8 parts of alpha-zinc hydroxypropionate, 5.5-7.5 parts of hydroxyl-terminated polybutylene, 5.5-6.5 parts of curing agent, 4-5.5 parts of vulcanizing agent and 14-20 parts of filling material.
3. A seal for subsea equipment according to claim 1, characterized in that: the curing agent is N-phenyl-gamma-aminopropyl trimethoxy silane.
4. A seal for subsea equipment according to claim 1, characterized in that: the vulcanizing agent is N, N' -m-phenylene bismaleimide.
5. A seal for subsea equipment according to claim 1, characterized in that: the filler is talcum powder, and the particle size of the talcum powder is not more than 20 microns.
6. A seal for subsea equipment according to claim 1, characterized in that: the raw material of the sealing element also comprises 1.5-3 parts by weight of 2-hydroxyethyl methacrylate phosphate.
7. A seal for underwater equipment according to any of claims 1 to 6, characterized in that: the raw material of the sealing element also comprises 0.5-2 parts by weight of amino modified silicone oil.
8. A method of making a seal for underwater equipment according to any of claims 1 to 7, comprising the steps of:
s1 mixing: taking raw materials of the sealing element, adding the raw materials into a mixing roll, and mixing for 15-25min to prepare base rubber;
s2 vulcanization: transferring the basic glue into a mold at 155 ℃ of 145-2The pressure vulcanization is carried out for 120 seconds and 240 seconds, and the sealing element for the underwater equipment is prepared.
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| JPH08333507A (en) * | 1995-06-07 | 1996-12-17 | Shin Etsu Chem Co Ltd | Modified biodegradable polymer composition |
| US6255397B1 (en) * | 1999-09-10 | 2001-07-03 | The Goodyear Tire & Rubber Company | Rubber composition containing hydroxyl terminated liquid polymer and tire with sidewall thereof |
| JP2010155967A (en) * | 2009-07-31 | 2010-07-15 | Daiso Co Ltd | Filler for rubber and rubber composition |
| CN102614516A (en) * | 2012-04-25 | 2012-08-01 | 黑龙江大学 | Method for preparing odor-masking zinc lactate powder |
| CN105199153B (en) * | 2014-05-30 | 2018-03-13 | 比亚迪股份有限公司 | A kind of yielding rubber and preparation method thereof and automobile-used yielding rubber part |
| CN106633234A (en) * | 2016-11-24 | 2017-05-10 | 安徽美腾特种电缆材料有限公司 | Anti-aging seal ring rubber material and preparation method thereof |
| CN108059827A (en) * | 2017-11-26 | 2018-05-22 | 天长市荣盛有机硅科技有限公司 | A kind of high-intensity and high-tenacity modified silicon rubber material |
| CN111154265B (en) * | 2020-01-17 | 2022-08-12 | 沈阳化工大学 | A kind of silicone rubber/polybutylene succinate non-petroleum based thermoplastic vulcanizate and preparation method thereof |
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