CN115926461A - Temperature-resistant pressure-resistant sealing gasket for nuclear power plant and preparation method thereof - Google Patents

Temperature-resistant pressure-resistant sealing gasket for nuclear power plant and preparation method thereof Download PDF

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CN115926461A
CN115926461A CN202310246898.XA CN202310246898A CN115926461A CN 115926461 A CN115926461 A CN 115926461A CN 202310246898 A CN202310246898 A CN 202310246898A CN 115926461 A CN115926461 A CN 115926461A
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temperature
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power plant
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CN115926461B (en
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马琼秀
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Chengdu Junma Sealing Technology Co ltd
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Chengdu Junma Sealing Technology Co ltd
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    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00Energy generation of nuclear origin
    • Y02E30/30Nuclear fission reactors

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Abstract

The application relates to the field of sealing materials, and particularly discloses a temperature-resistant and pressure-resistant sealing gasket for a nuclear power plant and a preparation method thereof, wherein the temperature-resistant and pressure-resistant sealing gasket is composed of the following raw materials in percentage by weight: 47-60% of modified composite fiber particles, 20-35% of modified mineral filler, 3-5% of rubber, 1-2% of vulcanizing agent, 0.1-0.4% of lubricant, 0.5-1.2% of coupling agent and the balance of carbon black. The preparation method of the temperature-resistant pressure-resistant sealing gasket comprises the following steps: step one, preparing modified composite fiber particles and modified mineral fillers for later use; step two, fully and uniformly mixing the carbon black, the lubricant and the coupling agent according to the formula amount to obtain a mixed material; and step three, rolling and pressing the modified composite fiber particles, the modified mineral filler, the vulcanizing agent, the rubber and the mixed material according to the formula amount to form a sheet, and vulcanizing to obtain the temperature-resistant pressure-resistant sealing gasket. The sealing gasket prepared by the method has excellent high-temperature-resistant thermal stability and lower stress relaxation rate.

Description

Temperature-resistant pressure-resistant sealing gasket for nuclear power plant and preparation method thereof
Technical Field
The application relates to the field of sealing materials, in particular to a temperature-resistant pressure-resistant sealing gasket for a nuclear power plant and a preparation method thereof.
Background
With the vigorous development of the economy in China, the automobile industry, the ship industry, the petrochemical industry, the internal combustion engine industry, the nuclear power generation industry and the aerospace industry in China are developed rapidly at a rapid speed in the last decade. The sealing gasket is an indispensable important part in the industries, and the environmental protection problem, the safety problem and the application performance quality related to the development of the industries have lip and tooth dependence.
In a sealing system applied to nuclear power generation, high temperature and high pressure are common application working conditions, under some environments, the temperature often exceeds 350 ℃ (350 ℃), the pressure often exceeds 15MPa (15 MPa), and temperature and pressure fluctuation are accompanied, the tight combination property of the internal structure of a common sealing gasket is poor, when the sealing gasket is subjected to high-temperature change in the using process, the viscous strain in the sealing material brings a serious stress relaxation phenomenon, and the high-temperature and heat resistance stability of the sealing gasket is poor. Therefore, it is urgently needed to develop a sealing material which can meet the high-temperature resistant stability in a nuclear power generation system and has a low stress relaxation rate.
Disclosure of Invention
The application provides a temperature-resistant pressure-resistant sealing gasket for a nuclear power plant and a preparation method thereof, solves the problems of poor high-temperature-resistant thermal stability and high stress relaxation rate of a sealing material in a sealing system applied to nuclear power generation, can obviously improve the high-temperature-resistant thermal stability of the sealing gasket, and effectively reduces the stress relaxation rate of the sealing gasket.
In a first aspect, the application provides a temperature and pressure resistant sealing gasket for a nuclear power plant, which adopts the following technical scheme:
a temperature-resistant pressure-resistant sealing gasket for a nuclear power plant is composed of the following raw materials in percentage by weight: 47-60% of modified composite fiber particles, 20-35% of modified mineral filler, 3-5% of rubber, 1-2% of vulcanizing agent, 0.1-0.4% of lubricant, 0.5-1.2% of coupling agent and the balance of carbon black;
the modified composite fiber particles are prepared by the following steps:
step 1, uniformly dispersing composite fibers in polyoxyethylene ether and calcium source solution to prepare slurry with the solid content of 40-60%, adding excessive carbonate solution into the slurry while stirring to obtain a solid product, and filtering and drying the solid product to obtain a modified material;
step 2, carrying out spray granulation on the modified material and the binding liquid to prepare modified composite fiber particles; the bonding fluid includes an elastomeric acrylic emulsion and a liquid phosphite.
By adopting the technical scheme, the composite fibers are uniformly dispersed in the polyoxyethylene ether and calcium source solution, carbonate ions in the added carbonate solution are combined with calcium ions in the calcium source solution, the composite fibers are wrapped and precipitated in the stirring process, the uniformity of each component can be maintained in the stirring process, uniform modified materials are obtained, the modified materials are subjected to spray granulation with the binding liquid, modified composite fiber particles with excellent binding effect are obtained, the modified composite fiber particles can be used as a filler of a sealing material, a good toughening and reinforcing effect is achieved, the mechanical property of the sealing material is improved, the modified composite fiber particles can be tightly combined with each raw material component, the compactness of the internal structure of the sealing material is effectively improved, and the sealing property of the sealing material is further improved.
The elastic acrylic emulsion and the liquid phosphite ester are fully mixed to form the binding liquid in a compounding manner, the elastic acrylic emulsion has excellent elasticity and binding property, and can promote the combination of raw material components and improve the high-temperature heat resistance stability of the sealing material in a synergistic manner by being matched with the liquid phosphite ester, and meanwhile, the stress relaxation phenomenon caused by viscous strain in the sealing material can be reduced, and the stress relaxation rate of the sealing material is effectively reduced.
The lubricant is oxidized polyethylene wax, the coupling agent is a silane coupling agent, the oxidized polyethylene wax has excellent lubricity and dispersibility and has certain coupling property, the compatibility among the raw material components is effectively improved, so that the modified composite fiber particles and the modified mineral filler can be uniformly dispersed in the system, the interfacial compoundability among the raw material components is jointly improved under the synergistic action of the coupling agent, the raw material components can be tightly connected, the high-temperature resistance and heat stability of the product is improved in an auxiliary manner, the stress relaxation rate of the sealing gasket is reduced, and the quality of the sealing gasket is improved.
Preferably, the composite fiber is a polyimide fiber and/or an aramid fiber.
More preferably, the composite fiber is a mixture of a polyimide fiber and an aramid fiber.
By adopting the technical scheme, the polyimide fiber has high strength and high modulus and good heat-resistant stability, is compounded with the aramid fiber to form the composite fiber, forms modified composite fiber particles under specific conditions, can effectively improve the high-temperature-resistant thermal stability of the sealing material, simultaneously assists in reducing the stress relaxation phenomenon caused by viscous strain in the sealing material, and effectively reduces the stress relaxation rate of the sealing material.
Preferably, the rubber is nitrile rubber or styrene butadiene rubber.
By adopting the technical scheme, the selection of the components of the rubber is optimized, and the selected nitrile rubber or styrene butadiene rubber is unvulcanized rubber, wherein the acrylonitrile content in the nitrile rubber is 36-40%, and the grade of the styrene butadiene rubber is SBR-1500, so that the subsequent rolling and sheet forming are facilitated, the raw material components are tightly connected, and the comprehensive performance of the product is improved in an auxiliary manner.
Preferably, the weight ratio of the elastic acrylic emulsion to the liquid phosphite is (2-3.5) to (0.5-1.2).
By adopting the technical scheme, the dosage relationship between the elastic acrylic emulsion and the liquid phosphite ester is optimized, the hot processing performance of the raw materials is further improved, the high-temperature-resistant thermal stability of the product is improved, the stress relaxation rate of the sealing gasket is reduced, and the quality of the sealing gasket is improved.
Preferably, the calcium source solution is a calcium acetate solution or a calcium nitrate solution, and the carbonate solution is a sodium carbonate solution.
By adopting the technical scheme, the calcium acetate solution or the calcium nitrate solution can provide calcium ions, the sodium carbonate solution provides carbonate ions, the calcium acetate solution and the carbonate ions are combined to form calcium carbonate precipitates, the calcium carbonate precipitates are used as a filler to reinforce the sealing material, and the mechanical property of the sealing gasket is ensured.
Preferably, the modified mineral filler is prepared by: and (3) uniformly dispersing the composite mineral material in water, adding a treating agent, and carrying out vacuum segmented heating circulation reaction while stirring until a dry modified mineral filler is formed.
By adopting the technical scheme, the composite mineral material is modified by the treating agent, and the vacuum segmented heating circulation reaction is combined, so that the prepared modified mineral filler can effectively improve the high-temperature-resistant thermal stability of the sealing material, and meanwhile, the stress relaxation phenomenon caused by the viscous strain in the sealing material is reduced in an auxiliary manner, and the stress relaxation rate of the sealing material is effectively reduced.
Preferably, the treatment agent comprises dopamine, dihydroxyphenylalanine and bismaleimide.
Further preferably, the weight ratio of dopamine, dihydroxyphenylalanine and bismaleimide is (1-2.5): (1-2): (1.7-2.6).
Dopamine, dihydroxyphenylalanine and bismaleimide are compounded to form a treating agent to modify the composite mineral material, and the dopamine is combined with a catechol group in the dihydroxyphenylalanine to form a substance with excellent adhesion so as to be beneficial to forming tight connection among the raw material components; the bismaleimide has excellent heat resistance and electrical insulation, ensures that the sealing gasket still has good insulation performance when working at high temperature and high pressure, can improve the interface composite property between a composite mineral material and other raw materials under the coordination of the dopamine and the dihydroxyphenylalanine, assists in reducing the stress relaxation phenomenon caused by viscous strain in the sealing material, assists in reducing the stress relaxation rate of the sealing material, and can effectively improve the high temperature resistance stability of the product.
Preferably, the vacuum subsection temperature rise once circulation is as follows: setting the vacuum degree to be 15Pa +/-10 Pa; the step of temperature rise comprises the following steps: the temperature of the first stage is 20-40 ℃, and the first stage is kept for 5-10min; the second stage temperature is 45-70 deg.C, and is maintained for 10-20min; the temperature of the third section is 75-95 ℃, and the temperature is kept for 5-10min.
By adopting the technical scheme, the reaction condition of vacuum sectional heating circulation is optimized, and the reaction between the raw materials is promoted by adopting a sectional heating mode under a proper vacuum degree, so that the improvement on the modification effect of the composite mineral material is facilitated, and the comprehensive performance of the sealing material is further improved.
Preferably, the composite mineral material comprises at least two of bentonite, kaolin, attapulgite and silicon dioxide.
By adopting the technical scheme, the component selection of the composite mineral material is optimized, so that the formed sealing material has a uniform and compact internal structure, and the comprehensive quality of the product is good.
In a second aspect, the application provides a preparation method of a temperature-resistant and pressure-resistant sealing gasket for a nuclear power plant, which adopts the following technical scheme:
a preparation method of a temperature-resistant pressure-resistant sealing gasket for a nuclear power plant comprises the following steps:
step one, preparing modified composite fiber particles and modified mineral fillers for later use;
step two, fully and uniformly mixing the carbon black, the lubricant and the coupling agent according to the formula amount to obtain a mixed material;
and step three, rolling and pressing the modified composite fiber particles, the modified mineral filler, the vulcanizing agent, the rubber and the mixed material according to the formula amount to form a sheet, and vulcanizing to obtain the temperature-resistant pressure-resistant sealing gasket.
By adopting the technical scheme, the prepared sealing gasket has good high-temperature resistance and thermal stability, and the stress relaxation rate of the sealing gasket can be reduced, so that the sealing gasket can work in a sealing system applied to nuclear power generation for a long time.
In summary, the present application has the following beneficial effects:
1. through the matching of the modified composite fiber particles and the modified mineral filler, the modified composite fiber particles and the modified mineral filler can be used as the filler of the sealing material, have good toughening and reinforcing effects, improve the mechanical property of the sealing material, can be tightly combined with various raw material components, effectively improve the compactness of the internal structure of the sealing material, synergistically improve the high-temperature-resistant thermal stability of the sealing material, simultaneously reduce the stress relaxation phenomenon caused by viscous strain in the sealing material, and effectively reduce the stress relaxation rate of the sealing material.
2. The lubricant is oxidized polyethylene wax, the coupling agent is a silane coupling agent, the oxidized polyethylene wax has excellent lubricity and dispersibility and has certain coupling property, the compatibility among the raw material components is effectively improved, so that the modified composite fiber particles and the modified mineral filler can be uniformly dispersed in a system, the interfacial compoundability among the raw material components is jointly improved under the synergistic action of the coupling agent, the raw material components are favorably and tightly connected, the high-temperature heat resistance stability of the product is improved in an auxiliary manner, the stress relaxation rate of the sealing gasket is reduced, and the quality of the sealing gasket is improved.
Description of the preferred embodiment
The present application will be described in further detail with reference to examples.
The raw materials used in the application are common commercial raw materials, wherein the water absorption rate of the polyimide fiber is less than or equal to 2 percent, the length is 1-10mm, and the density is 1.44g/cm 3 (ii) a The length of the aramid fiber is 1-6mm, and the density is 1.42g/cm 3 (ii) a The particle size of the carbon black is 1700-1900 meshes; the particle size of the bentonite, the kaolin, the attapulgite and the silicon dioxide is 350-400 meshes; the liquid phosphite is trilauryl phosphite; the vulcanizing agent is sulfur.
Preparation example 1
The modified composite fiber particles are prepared by the following steps:
step 1, uniformly dispersing 2kg of polyimide fibers in 100g of nonylphenol polyoxyethylene ether and a 15% calcium acetate solution by mass to prepare a slurry with a solid content of 40%, adding an excessive 20% sodium carbonate solution by mass into the slurry under a stirring condition of 50r/min, reacting to obtain a solid product, filtering the solid product, and drying at 37 ℃ to obtain a modified material;
step 2, preparing modified composite fiber particles by spraying and granulating the modified material and the binding liquid with the weight ratio of 1.5; the binding liquid is elastic acrylic emulsion and liquid phosphite ester with the weight ratio of 2.
Preparation example 2
The modified composite fiber particles are prepared by the following steps:
step 1, uniformly dispersing 2kg of aramid fiber in 150g of nonylphenol polyoxyethylene ether and 15% of calcium nitrate solution by mass to prepare slurry with the solid content of 60%, adding excessive 20% of sodium carbonate solution by mass into the slurry under the stirring condition of 50r/min, reacting to obtain a solid product, filtering the solid product, and drying at 37 ℃ to prepare a modified material;
step 2, preparing modified composite fiber particles by spraying and granulating the modified material and the binding liquid with the weight ratio of 1.3; the binding liquid is elastic acrylic emulsion and liquid phosphite ester with the weight ratio of 3.5.
Preparation example 3
The difference from the preparation example 1 is that the composite fiber is 1.2kg of polyimide fiber and 0.8kg of aramid fiber, and the rest is the same as the preparation example 1.
Preparation example 4
The difference from preparation example 3 is that the binding liquid is an elastic acrylic emulsion and a liquid phosphite in a weight ratio of 2.9.
Preparation example 5
The modified composite fiber particles are prepared by the following steps:
step 1, uniformly dispersing 0.2kg of polyimide fibers and 1.8kg of aramid fibers in 15% by mass of calcium nitrate solution, adjusting the pH to 8-9 to prepare slurry with the solid content of 60%, adding 20% by mass of sodium carbonate solution into the slurry under the stirring condition of 50r/min, reacting to obtain a solid product, filtering the solid product and drying at 37 ℃ to prepare a modified material;
step 2, preparing modified composite fiber particles by spraying and granulating the modified material and the binding liquid in a weight ratio of 1; the binding liquid is elastic acrylic emulsion and liquid phosphite ester with the weight ratio of 0.9.
Preparation example 1
The modified mineral filler is prepared by the following steps: uniformly dispersing 1kg of bentonite and 1kg of kaolin into 4kg of water, adding 0.37kg of treating agent, stirring and carrying out vacuum segmented heating circulation reaction until a dry modified mineral filler is formed; the treating agent is a mixture of 0.1kg of dopamine, 0.1kg of dihydroxyphenylalanine and 0.17kg of bismaleimide;
the vacuum sectional heating once circulation is as follows: setting the vacuum degree to 5Pa; the segmented temperature rise comprises the following steps: the temperature of the first stage is raised to 20 ℃ and kept for 10min; the temperature of the second stage is raised to 45 ℃ and kept for 20min; the temperature in the third stage is raised to 75 ℃ and kept for 10min.
Preparation example two
The modified mineral filler is prepared by the following steps: uniformly dispersing 1.8kg of attapulgite and 1kg of silicon dioxide in 5kg of water, adding 0.71kg of treating agent, stirring and carrying out vacuum segmented heating circulation reaction until a dry modified mineral filler is formed; the treating agent is a mixture of 0.25kg of dopamine, 0.2kg of dihydroxyphenylalanine and 0.26kg of bismaleimide;
the vacuum sectional heating once circulation is as follows: setting the vacuum degree to 25Pa; the step of temperature rise comprises the following steps: the temperature of the first stage is raised to 40 ℃ and kept for 5min; the temperature of the second stage is raised to 70 ℃ and kept for 10min; the temperature in the third stage is raised to 95 ℃ and kept for 5min.
Preparation example three
The difference from the first preparation example is that the composite mineral material is 1kg of kaolin, 0.8kg of attapulgite and 1kg of silicon dioxide, and the treating agent is a mixture of 0.2kg of dopamine, 0.13kg of dihydroxyphenylalanine and 0.2kg of bismaleimide; the rest is the same as the first preparation example.
Preparation example four
The difference from the third preparation example is that the vacuum sectional heating once circulation is as follows: setting the vacuum degree to 15Pa; the step of temperature rise comprises the following steps: the temperature of the first stage is raised to 35 ℃ and kept for 10min; the temperature of the second stage is raised to 60 ℃ and kept for 15min; the temperature of the third section is raised to 90 ℃ and kept for 8min; the rest is the same as the preparation examples.
Preparation example five
The difference from the fourth preparation example is that the composite mineral material is 2kg of bentonite and 1.8kg of kaolin, and the treating agent is a mixture of 0.5kg of dopamine, 0.01kg of dihydroxyphenylalanine and 0.06kg of bismaleimide; the rest is the same as the fourth preparation example.
Examples
Example 1
The temperature-resistant pressure-resistant sealing gasket for the nuclear power plant comprises the following raw materials in percentage by weight: 4.7kg of modified composite fiber particles prepared in preparation example 1, 3.5kg of modified mineral filler prepared in preparation example one, 0.5kg of nitrile rubber, 0.1kg of vulcanizing agent, 0.01kg of oxidized polyethylene wax, 0.05kg of silane coupling agent and 1.14kg of carbon black;
the preparation method of the temperature-resistant pressure-resistant sealing gasket for the nuclear power plant comprises the following steps: fully and uniformly mixing carbon black, oxidized polyethylene wax and a silane coupling agent to obtain a mixed material; and rolling and pressing the modified composite fiber particles prepared in the preparation example 1, the modified mineral filler prepared in the preparation example, a vulcanizing agent, rubber and a mixed material into sheets, and vulcanizing to obtain the temperature-resistant and pressure-resistant sealing gasket.
Example 2
The difference from the embodiment 1 is that the temperature-resistant and pressure-resistant sealing gasket for the nuclear power plant is composed of the following raw materials in percentage by weight: 6kg of modified composite fiber particles prepared in preparation example 1, 2.5kg of modified mineral filler prepared in preparation example one, 0.3kg of styrene-butadiene rubber, 0.2kg of vulcanizing agent, 0.04kg of oxidized polyethylene wax, 0.12kg of silane coupling agent and 0.84kg of carbon black; the rest is the same as in example 1.
Example 3
The difference from the embodiment 1 is that the temperature-resistant and pressure-resistant sealing gasket for the nuclear power plant is composed of the following raw materials in percentage by weight: 5.4kg of modified composite fiber particles prepared in preparation example 1, 3kg of modified mineral filler prepared in preparation example one, 0.4kg of styrene-butadiene rubber, 0.12kg of vulcanizing agent, 0.04kg of oxidized polyethylene wax, 0.1kg of silane coupling agent and 0.94kg of carbon black; the rest is the same as in example 1.
Example 4
The difference from example 3 is that the modified composite fiber particles obtained in preparation example 2 were used, and the rest was the same as example 3.
Example 5
The difference from example 3 is that the modified composite fiber particles obtained in preparation example 3 were selected and the rest was the same as example 3.
Example 6
The difference from example 3 is that the modified composite fiber particles obtained in preparation example 4 were used, and the rest was the same as example 3.
Example 7
The difference from example 3 is that the modified composite fiber particles obtained in preparation example 5 were used, and the rest was the same as example 3.
Example 8
The difference from example 6 is that the modified mineral filler obtained in preparation two was used, and the rest was the same as example 6.
Example 9
The difference from example 6 is that the modified mineral filler obtained in preparation three was used, and the rest was the same as example 6.
Example 10
The difference from example 6 is that the modified mineral filler obtained in preparation example four was used, and the rest was the same as example 6.
Example 11
The difference from example 6 is that the modified mineral filler obtained in preparation example five was used, and the rest was the same as example 6.
Comparative example 1
The difference from example 10 is that the modified composite fiber particles were replaced with 3kg of polyimide fiber and 2.4kg of aramid fiber, and the rest was the same as example 10.
Comparative example 2
The difference from example 10 is that the modified composite fiber particles are a mixture of 1.3kg of polyimide fiber, 1kg of aramid fiber, 1.3kg of calcium carbonate, 0.9kg of elastic acrylic emulsion and 0.5kg of liquid phosphite, and the rest is the same as example 10.
Comparative example 3
The difference from example 10 is that the modified composite fiber particles were the same as example 10 except that the binder solution was a polyvinyl alcohol solution.
Comparative example 4
The difference from example 10 is that the modified mineral filler was replaced with 1kg of kaolin, 1kg of attapulgite and 1kg of silica, and the rest was the same as in example 10.
Comparative example 5
The difference from example 10 is that the modified mineral filler is the same as example 10 except that dopamine is not added to the treating agent.
Comparative example 6
The difference from example 10 is that in the modified mineral filler, no bismaleimide was added to the treatment agent, and the remainder was the same as in example 10.
The gaskets produced in examples 1-11 and comparative examples 1-6 were tested according to GB/T20671.5-2020, classification System for non-metallic gasket materials and test method part 5: the creep relaxation rate test method of the gasket material "was used to test the stress relaxation rate, and the results are shown in table 1.
The gaskets prepared in examples 1 to 11 and comparative examples 1 to 6 were subjected to a high temperature thermal cycling bench test in the following cycle steps: raising the temperature to 370 ℃, adding the internal pressure to 17MPa, maintaining for 20 minutes, regulating the temperature to 270 ℃ in 30 minutes, regulating the internal pressure to 15MPa, maintaining the temperature and the pressure for 20 minutes, regulating the temperature to 370 ℃ in 30 minutes, regulating the internal pressure to 17MPa, repeating the cycle test, and recording the cycle times when the test result is qualified as that the sample has no leakage or breakdown.
TABLE 1
Stress relaxation rate/%) High temperature heatNumber of cycles/number of cycles of the cycle bench test
Example 1 10 25
Example 2 10 24
Example 3 9 27
Example 4 9 26
Example 5 8 29
Example 6 6 30
Example 7 9 27
Example 8 7 31
Example 9 5 32
Example 10 5 33
Example 11 7 30
Comparative example 1 19 18
Comparative example 2 17 20
Comparative example 3 15 21
Comparative example 4 19 20
Comparative example 5 16 20
Comparative example 6 16 18
As can be seen by combining examples 1 to 11 with table 1, the gasket produced by the present application has excellent high temperature thermal stability, and can withstand up to 33 high temperature thermal cycles in a high temperature thermal cycle bench test, while having a low stress relaxation rate.
As can be seen by combining example 10 and comparative examples 1 to 3 with table 1, in comparative example 1, no specific modification treatment was performed on the composite fiber, and only the polyimide fiber and the aramid fiber were added to the system; the raw material components of the modified composite fiber particles are directly and simply mixed in the comparative example 2, the binding solution is replaced by the polyvinyl alcohol solution in the comparative example 3, the cycle times of the sealing gaskets prepared in the comparative examples 1-3 in a high-temperature thermal cycle test are obviously reduced, the high-temperature-resistant thermal stability of the sealing material is obviously reduced, and the sealing material is influenced by the viscosity strain in the sealing material, has high stress relaxation rate and poor product quality. The polyimide fiber has high strength and high modulus and good heat resistance stability, is compounded with aramid fiber to form composite fiber which is uniformly dispersed in a calcium source solution, carbonate ions in a carbonate solution added subsequently are combined with calcium ions in the calcium source solution, the composite fiber is wrapped, clamped and precipitated in the stirring process, the uniformity of each component can be maintained in the stirring process, a uniform modified material is obtained, and the modified material is subjected to spray granulation with a binding solution to obtain modified composite fiber particles with excellent binding effect.
Combining example 10 and comparative examples 4-6 with table 1, it can be seen that the composite mineral material was not modified in comparative example 4, the dopamine was absent from the treating agent in comparative example 5, the bismaleimide was absent from the treating agent in comparative example 6, and the sealing materials prepared in comparative examples 4-6 had poor high temperature thermal stability and high stress relaxation rate; the compound mineral material is modified by adopting a treating agent formed by compounding dopamine, dihydroxyphenylalanine and bismaleimide, and the dopamine is combined with a catechol group in the dihydroxyphenylalanine to form a substance with excellent adhesiveness, so that the raw material components can be tightly connected; the bismaleimide has excellent heat resistance and point insulation, ensures that the sealing gasket still has good insulation performance when working at high temperature and high pressure, can improve the interfacial recombination between a composite mineral material and other raw materials under the cooperation of the dopamine and the dihydroxyphenylalanine, assists in reducing the stress relaxation phenomenon caused by viscous strain in the sealing material, assists in reducing the stress relaxation rate of the sealing material, and simultaneously can effectively improve the high temperature resistance stability of the product.
The specific embodiments are only for explaining the present application and are not limiting to the present application, and those skilled in the art can make modifications to the embodiments without inventive contribution as required after reading the present specification, but all the embodiments are protected by patent law within the scope of the claims of the present application.

Claims (10)

1. A temperature-resistant pressure-resistant sealing gasket for a nuclear power plant is characterized by comprising the following raw materials in percentage by weight: 47-60% of modified composite fiber particles, 20-35% of modified mineral filler, 3-5% of rubber, 1-2% of vulcanizing agent, 0.1-0.4% of lubricant, 0.5-1.2% of coupling agent and the balance of carbon black;
the modified composite fiber particles are prepared by the following steps:
step 1, uniformly dispersing composite fibers in polyoxyethylene ether and calcium source solution to prepare slurry with the solid content of 40-60%, adding excessive carbonate solution into the slurry while stirring to obtain a solid product, and filtering and drying the solid product to obtain a modified material;
step 2, carrying out spray granulation on the modified material and the binding liquid to prepare modified composite fiber particles; the bonding fluid includes an elastomeric acrylic emulsion and a liquid phosphite.
2. The temperature and pressure resistant gasket for a nuclear power plant of claim 1, wherein: the composite fiber is polyimide fiber and/or aramid fiber.
3. The temperature and pressure resistant gasket for a nuclear power plant of claim 1, wherein: the rubber is nitrile rubber or styrene butadiene rubber.
4. The temperature and pressure resistant gasket for a nuclear power plant of claim 1, wherein: the weight ratio of the elastic acrylic emulsion to the liquid phosphite ester is (2-3.5) to (0.5-1.2).
5. The temperature and pressure resistant gasket for a nuclear power plant according to any one of claims 1 to 4, wherein: the calcium source solution is a calcium acetate solution or a calcium nitrate solution, and the carbonate solution is a sodium carbonate solution.
6. The temperature and pressure resistant gasket for a nuclear power plant of claim 1, wherein: the modified mineral filler is prepared by the following steps: and (3) uniformly dispersing the composite mineral material in water, adding a treating agent, and carrying out vacuum segmented heating circulation reaction while stirring until a dry modified mineral filler is formed.
7. The temperature and pressure resistant gasket for a nuclear power plant according to claim 6, wherein: the treatment agent comprises dopamine, dihydroxyphenylalanine and bismaleimide.
8. The temperature and pressure resistant gasket for a nuclear power plant according to claim 6, wherein: the vacuum sectional heating once circulation is as follows: setting the vacuum degree to be 15Pa +/-10 Pa; the step of temperature rise comprises the following steps: the temperature of the first stage is 20-40 ℃, and the first stage is kept for 5-10min; the second stage temperature is 45-70 deg.C, and is maintained for 10-20min; the temperature of the third stage is 75-95 ℃, and the temperature is kept for 5-10min.
9. The temperature and pressure resistant seal for a nuclear power plant according to any one of claims 6 to 8, characterized in that: the composite mineral material comprises at least two of bentonite, kaolin, attapulgite and silicon dioxide.
10. The method for preparing a temperature and pressure resistant sealing gasket for a nuclear power plant according to any one of claims 1 to 9, wherein: the method comprises the following steps:
step one, preparing modified composite fiber particles and modified mineral fillers for later use;
step two, fully and uniformly mixing the carbon black, the lubricant and the coupling agent according to the formula amount to obtain a mixed material;
and step three, rolling and pressing the modified composite fiber particles, the modified mineral filler, the vulcanizing agent, the rubber and the mixed material according to the formula amount to form a sheet, and vulcanizing to obtain the temperature-resistant pressure-resistant sealing gasket.
CN202310246898.XA 2023-03-15 2023-03-15 Temperature-resistant pressure-resistant sealing gasket for nuclear power plant and preparation method thereof Active CN115926461B (en)

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JP2006096859A (en) * 2004-09-29 2006-04-13 Sunstar Engineering Inc Sealing material composition
CN102976307A (en) * 2012-12-04 2013-03-20 北京化工大学 Carbon nano tube surface functionalization method
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