CN102839899B - Nuclear radiation resistant non-marking rubber product for sealing nuclear island and preparation method thereof - Google Patents
Nuclear radiation resistant non-marking rubber product for sealing nuclear island and preparation method thereof Download PDFInfo
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- CN102839899B CN102839899B CN201210339328.7A CN201210339328A CN102839899B CN 102839899 B CN102839899 B CN 102839899B CN 201210339328 A CN201210339328 A CN 201210339328A CN 102839899 B CN102839899 B CN 102839899B
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Abstract
The invention discloses a nuclear radiation resistant non-marking rubber product for sealing a nuclear island, which is prepared from a main material and a joint material, wherein the main material is prepared from the following materials in part by weight: 100 parts of ethylene propylene diene monomer, 4 to 8 parts of active agent, 1 to 5 parts of vulcanizing agent, 1 to 5 parts of accelerator, 0.5 to 3 parts of anti-aging agent and 15 to 35 parts of complex; and the joint material is prepared from the following materials in part by weight: 100 parts of ethylene propylene diene monomer, 3 to 7 parts of active agent, 1 to 4 parts of vulcanizing agent, 1 to 4 parts of accelerator, 0 to 1 part of scorch retarder, 3 to 7 parts of inert filler, 1 to 5 parts of anti-aging agent and 15 to 35 parts of complex. In addition, the invention further provides a method for preparing the non-marking rubber product. No marks visible to naked eyes remains at the joint of the non-marking rubber product, the convex and concave defects in the joint and in a non-joint position are within the specified limit of tolerance, and the tensile strength and the elongation at break in the joint and in the non-joint position are the same, so that the application requirement of sealing the nuclear island is satisfied.
Description
Technical field
The invention belongs to nuclear island technical field of sealing technology, be specifically related to a kind of nuclear island sealing seamless rubber item of resistance to nuclear radiation and preparation method thereof.
Background technology
After Fukushima, Japan nuclear incident, raising and perfect has been carried out in seal request and the design of the mankind to nuclear island.Under accident conditions, nuclear island is in high temperature, high pressure, high radiation environment.And prevent nuclear leakage and pollutant atmosphere, depend primarily on the various doors (personnel, equipment gate etc.) of sealing nuclear island, and these sealing depends primarily on high-quality rubber item.Therefore, the quality of rubber item is most important to the sealing function under normal operation and accident conditions.Because personnel, equipment gate are larger, countries in the world all do not have main equipment or the disposable vulcanized rubber article of producing of mould at present, and the method that all adopts joint is docked into as a whole rubber item (finished product) by vulcanized rubber through secondary.
Rubber belongs to macromolecular material, and before uncured, macromole is in chain-like structure (there is no use value), and after over cure, macromole becomes reticulated structure, and has given certain elasticity and physicals, makes it have use value.Vulcanizing popular saying is under certain pressure, temperature, time conditions, realizes macromolecular material and becomes cancellated process by chain-like structure.And the speed of sulfidation or the length of time, except pressure, temperature, depend in vulcanized rubber formula the factors such as vulcanizing agent, promotor (also can be understood as catalyzer), anti-aging agent, scorch retarder (being also vulcanization retardant).Traditional vulcanized joint method is by two or two method that vulcanized rubber secondary docks or couples together, the method is between vulcanized rubber, to have added unvulcanized rubber at two, realizes and connect or claim secondary crosslinking under certain pressure, temperature, time conditions.The shortcoming of this method is: one, vulcanized rubber becomes netted process from chain, and change has occurred rubber profile, and main manifestations is contraction, the shrinking percentage it has often been said exactly.And shrinkage ratio is larger, generally between 2%～3%, different due to vulcanized rubber and unvulcanized rubber shrinking percentage while so just having caused secondary joint, form obvious convex-concave lapping defect (wherein by the vulcanized rubber of joint owing to shrinking little or not shrinking geometrical shape and change the little or convex epirelief that do not changed; And have greatly indenture in the unvulcanized rubber shrinking percentage of two joints); Two, the physicals of joint (tensile strength, elongation rate of tensile failure, compression set etc.) is larger with non-joint difference.In general industry environment, can use, but have major safety risks in nuclear island environment.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, and the nuclear island sealing resistance to nuclear radiation seamless rubber item of a kind of joint without naked eyes visible marks is provided.This Yu Fei joint, goods joint convex-concave defect is in the tolerance zone of defined; Yu Fei joint, joint tensile strength, elongation rate of tensile failure equates, meets the application requiring of nuclear island sealing.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of nuclear island seals with the seamless rubber item of resistance to nuclear radiation, it is characterized in that, is made up of main material and joint material; Described main material is made up of the raw material of following weight part: 100 parts of terpolymer EP rubbers, 4-8 parts of promoting agents, 1-5 parts of vulcanizing agents, 1-5 parts of promotor, 0.5-3 parts, anti-aging agent, 15-35 parts of title complexs, wherein promoting agent is zinc oxide and/or stearic acid, vulcanizing agent is dicumyl peroxide and/or resol, promotor is one or more in promotor TAIC, captax and accelerant B Z, anti-aging agent is anti-aging agent RD and/or antioxidant MB, and title complex is one or more in paraffin oil, carbon black and cerium dioxide;
Described joint material is made up of the raw material of following weight part: 100 parts of terpolymer EP rubbers, 3-7 parts of promoting agents, 1-4 parts of vulcanizing agents, 1-4 parts of promotor, 0-1 part of scorch retarder, 3-7 parts of inert fillers, 1-5 parts, anti-aging agent, 15-35 parts of title complexs, wherein promoting agent is zinc oxide and/or stearic acid, and vulcanizing agent is dicumyl peroxide and/or resol, and promotor is promotor TAIC and/or rubber leveler 40MSF, scorch retarder is Whitfield's ointment and/or Tetra hydro Phthalic anhydride, and inert filler is with SiO
2for the acid title complex of carrier, anti-aging agent is one or more in antioxidant 4010NA, anti-aging agent RD and antioxidant MB, and title complex is one or more in paraffin oil, carbon black and cerium dioxide; Described with SiO
2for the acid title complex of carrier is made up of following methods: by SiO
2, terpine resin and mix according to 10: 1～3: 1～3 mass ratio containing the resol of 2wt%～6wt% boron that to be placed on temperature be stirring reaction 20min～40min in the reactor of 70 DEG C～80 DEG C, then vacuum hydro-extraction 3h～5h, obtains with SiO
2for the acid title complex of carrier.
Above-mentioned a kind of nuclear island seamless rubber item of resistance to nuclear radiation for sealing, described main material is made up of the raw material of following weight part: 100 parts of terpolymer EP rubbers, 5-7 parts of promoting agents, 2-4 parts of vulcanizing agents, 2-4 parts of promotor, 1-2 parts, anti-aging agent, 20-30 parts of title complexs; Described joint material is made up of the raw material of following weight part: 100 parts of terpolymer EP rubbers, 4-6 parts of promoting agents, 2-3 parts of vulcanizing agents, 2-3 parts of promotor, 0.3-0.7 part of scorch retarder, 4-6 parts of inert fillers, 2-4 parts, anti-aging agent, 20-30 parts of title complexs.
Above-mentioned a kind of nuclear island seamless rubber item of resistance to nuclear radiation for sealing, described main material is made up of the raw material of following weight part: 100 parts of terpolymer EP rubbers, 6 parts of promoting agents, 3 parts of vulcanizing agents, 3 parts of promotor, 1.5 parts, anti-aging agent, 25 parts of title complexs; Described joint material is made up of the raw material of following weight part: 100 parts of terpolymer EP rubbers, 5 parts of promoting agents, 2.5 parts of vulcanizing agents, 2.5 parts of promotor, 0.5 part of scorch retarder, 5 parts of inert fillers, 3 parts, anti-aging agent, 25 parts of title complexs.
The present invention also provides a kind of method of preparing the above-mentioned nuclear island sealing seamless rubber item of resistance to nuclear radiation, it is characterized in that, the method comprises the following steps:
Step 1, that terpolymer EP rubber, promoting agent, vulcanizing agent, promotor, anti-aging agent and title complex are placed in to opening rubber mixing machine by proportioning is mixing evenly, obtains main material;
Step 2, that terpolymer EP rubber, promoting agent, vulcanizing agent, promotor, scorch retarder, inert filler, anti-aging agent and title complex are placed in to opening rubber mixing machine by proportioning is mixing evenly, obtains joint material;
Step 3, shape and size selection mould according to nuclear island to be prepared sealing with the seamless rubber item of resistance to nuclear radiation, first main material described in step 1 is filled in mould, then joint material described in step 2 is filled in mould and described joint material is arranged in the two ends of mould main material, adopt vulcanizing press to vulcanize the mould that fills main material and joint material, after the demoulding, obtain work in-process; In described sulfidation, controlling sulfide stress is 10MPa～14MPa, and curing temperature is 150 DEG C～170 DEG C, and curing time is 10min～30min;
Step 4, work in-process described in multiple step 3 are spliced by the shape and size of the seamless rubber item of resistance to nuclear radiation according to nuclear island to be prepared sealing, then spliced joint is vulcanized, obtain the nuclear island sealing seamless rubber item of resistance to nuclear radiation; In described sulfidation, controlling sulfide stress is 10MPa～14MPa, and curing temperature is 150 DEG C～170 DEG C, and curing time is 10min～30min.
Above-mentioned method, curing temperature described in step 3 is 160 DEG C, curing time is 20min.
Above-mentioned method, curing temperature described in step 4 is 160 DEG C, curing time is 20min.
Described weight part can be gram, two, jin, kilogram, Dun Deng weight metering unit.
The present invention compared with prior art has the following advantages:
1, the rate of crosslinking of vulcanized rubber depends on temperature and time under pressure permanence condition, according to Arrhenius figure, temperature and time is defined as to 10 DEG C of the every risings of temperature, vulcanized rubber time shorten half at rubber industry.And be immutable at the pressure of actual production middle plateform vulcanizer, be the prerequisite of guaranteeing extrudate density; Temperature is variable, is difficult for realizing but limited by equipment and production efficiency.Therefore, only have vulcanizing agent in formula, promotor, anti-aging agent, scorch retarder and inert filler etc. to change, could change chemical reaction rate is vulcanization crosslinking speed.The present invention is based on this theory, to nuclear island, sealing improves and optimizes with main material and the joint material formula of the seamless rubber item of resistance to nuclear radiation, makes main material different from the vulcanization crosslinking speed of joint material.
2, formula of the present invention, at pressure, under temperature-resistant condition, can realize seamlessization of secondary joint, main material has reached sulfurizing point in primary vulcanization process, and joint material in primary vulcanization process in half cross-linked state, in the time vulcanizing for the second time, just reach sulfurizing point, so both can ensure the consistence of joint material shrinking percentage, avoid the joint convex-concave defect of bringing because shrinking difference, also can guarantee that main material and joint material are fully effectively crosslinked, having realized Yu Fei joint, joint physicals equates, eliminate the drawback of joint poor properties.
3, adopt nuclear island prepared by formula of the present invention and method to seal with the seamless rubber item of resistance to nuclear radiation joint without naked eyes visible marks, measure with vernier calliper, Yu Fei joint, joint convex-concave defect in the tolerance zone of defined (taking Φ 15 sections as example tolerance regulation ± 0.1mm, higher than GB GB/T3672.1-2002 regulation ± 0.15mm) actual joint convex-concave defect is zero tolerance, visual without vestige; Yu Fei joint, joint tensile strength, elongation rate of tensile failure equate, 55 degree levels: tensile strength >=7MPa, elongation rate of tensile failure >=450%; 75 degree level: tensile strength >=12MPa, elongation rate of tensile failure >=400%, meets the application requiring that nuclear island seals.
Below in conjunction with drawings and Examples, technical scheme of the present invention is described in further detail.
Brief description of the drawings
Fig. 1 is that nuclear island prepared by the embodiment of the present invention 1 seals the structural representation with the seamless rubber item of resistance to nuclear radiation.
Fig. 2 is the A-A cutaway view Amplified image of Fig. 1.
Fig. 3 is that nuclear island prepared by the embodiment of the present invention 3 seals the structural representation with the seamless rubber item of resistance to nuclear radiation.
Fig. 4 is the B-B cutaway view Amplified image of Fig. 3.
Fig. 5 is that nuclear island prepared by the embodiment of the present invention 5 seals the structural representation with the seamless rubber item of resistance to nuclear radiation.
Fig. 6 is the C-C cutaway view Amplified image of Fig. 5.
Description of reference numerals:
1-main material; 2-joint material.
Embodiment
Embodiment 1
The present embodiment nuclear island is the seamless rubber item of resistance to nuclear radiation for sealing, is made up of main material and joint material sulfuration; Described main material is made up of following raw material: terpolymer EP rubber 100kg, promoting agent 8kg, vulcanizing agent 1kg, promotor 5kg, anti-aging agent 0.5kg, title complex 35kg, wherein promoting agent is zinc oxide, and vulcanizing agent is dicumyl peroxide, and promotor is promotor TAIC, anti-aging agent is anti-aging agent RD, and title complex is paraffin oil;
Described joint material is made up of following raw material: terpolymer EP rubber 100kg, promoting agent 3kg, vulcanizing agent 1kg, promotor 1kg, inert filler 3kg, anti-aging agent 1kg, title complex 35kg, wherein promoting agent is zinc oxide, vulcanizing agent is dicumyl peroxide, promotor is promotor TAIC, and inert filler is with SiO
2for the acid title complex of carrier, anti-aging agent is antioxidant 4010NA, and title complex is paraffin oil; Described with SiO
2for the acid title complex of carrier is made up of following methods: by SiO
2, terpine resin and mix according to the mass ratio of 10: 1: 3 containing the resol of 2wt% boron that to be placed on temperature be stirring reaction 40min in the reactor of 70 DEG C, then vacuum hydro-extraction 5h, obtains with SiO
2for the acid title complex of carrier.
The nuclear island sealing of the present embodiment by the preparation method of the seamless rubber item of resistance to nuclear radiation is:
Step 1, that terpolymer EP rubber, promoting agent, vulcanizing agent, promotor, anti-aging agent and title complex are placed in to opening rubber mixing machine by proportioning is mixing evenly, obtains main material;
Step 2, that terpolymer EP rubber, promoting agent, vulcanizing agent, promotor, inert filler, anti-aging agent and title complex are placed in to opening rubber mixing machine by proportioning is mixing evenly, obtains joint material;
Step 3, be the mould of " O " shape according to nuclear island to be prepared sealing with shape (as depicted in figs. 1 and 2) and the size Selection cross section of the seamless rubber item of resistance to nuclear radiation, first main material 1 described in step 1 is filled in mould, then joint material 2 described in step 2 is filled in mould and described joint material 2 is arranged in the two ends of mould main material 1, adopt vulcanizing press to vulcanize the mould that fills main material 1 and joint material 2, after the demoulding, obtain work in-process; In described sulfidation, controlling sulfide stress is 10MPa, and curing temperature is 170 DEG C, and curing time is 10min;
Step 4, work in-process described in multiple step 3 are spliced into the shape of the nuclear island to be prepared sealing seamless rubber item of resistance to nuclear radiation, then spliced joint are vulcanized, obtain nuclear island and seal with the seamless rubber item of resistance to nuclear radiation; In described sulfidation, controlling sulfide stress is 10MPa, and curing temperature is 170 DEG C, and curing time is 10min.
Nuclear island prepared by the present embodiment seals with the seamless rubber item of resistance to nuclear radiation joint without naked eyes visible marks, measure with vernier calliper, Yu Fei joint, joint convex-concave defect in the tolerance zone of defined (taking Φ 15 sections as example tolerance regulation ± 0.1mm, specify higher than GB GB/T3672.1-2002 ± 0.15mm), actual joint convex-concave defect is zero tolerance, visual without vestige; Yu Fei joint, joint tensile strength, elongation rate of tensile failure equate, 55 degree levels: tensile strength >=7MPa, elongation rate of tensile failure >=450%; 75 degree level: tensile strength >=12MPa, elongation rate of tensile failure >=400%, meets the application requiring that nuclear island seals.
Embodiment 2
The present embodiment is identical with embodiment 1, wherein difference is: the promoting agent in main material is stearic acid or zinc oxide and stearic acid, vulcanizing agent is resol or dicumyl peroxide and resol, promotor is captax or accelerant B Z, or be two or three in promotor TAIC, captax and accelerant B Z, anti-aging agent is antioxidant MB or anti-aging agent RD and antioxidant MB, title complex is carbon black or cerium dioxide, or is two or three in paraffin oil, carbon black and cerium dioxide; Promoting agent in joint material is stearic acid or zinc oxide and stearic acid, vulcanizing agent is resol or dicumyl peroxide and resol, promotor is rubber leveler 40MSF or promotor TAIC and rubber leveler 40MSF, anti-aging agent is anti-aging agent RD or antioxidant MB, or be two or three in antioxidant 4010NA, anti-aging agent RD and antioxidant MB, title complex is carbon black or cerium dioxide, or is two or three in paraffin oil, carbon black and cerium dioxide.
Nuclear island prepared by the present embodiment seals with the seamless rubber item of resistance to nuclear radiation joint without naked eyes visible marks, measure with vernier calliper, Yu Fei joint, joint convex-concave defect in the tolerance zone of defined (taking Φ 15 sections as example tolerance regulation ± 0.1mm, higher than GB GB/T3672.1-2002 regulation ± 0.15mm) actual joint convex-concave defect is zero tolerance, visual without vestige; Yu Fei joint, joint tensile strength, elongation rate of tensile failure equate, 55 degree levels: tensile strength >=7MPa, elongation rate of tensile failure >=450%; 75 degree level: tensile strength >=12MPa, elongation rate of tensile failure >=400%, meets the application requiring that nuclear island seals.
Embodiment 3
The present embodiment nuclear island is the seamless rubber item of resistance to nuclear radiation for sealing, is made up of main material and joint material sulfuration; Described main material is made up of following raw material: terpolymer EP rubber 100g, promoting agent 4g, vulcanizing agent 5g, promotor 1g, anti-aging agent 3g, title complex 15g, wherein promoting agent is stearic acid, vulcanizing agent is resol, promotor is accelerant B Z, and anti-aging agent is antioxidant MB, and title complex is cerium dioxide;
Described joint material is made up of following raw material: terpolymer EP rubber 100g, promoting agent 7g, vulcanizing agent 4g, promotor 4g, scorch retarder 1g, inert filler 7g, anti-aging agent 5g, title complex 15g, wherein promoting agent is stearic acid, and vulcanizing agent is resol, and promotor is rubber leveler 40MSF, scorch retarder is Tetra hydro Phthalic anhydride, and inert filler is with SiO
2for the acid title complex of carrier, anti-aging agent is antioxidant MB, and title complex is cerium dioxide; Described with SiO
2for the acid title complex of carrier is made up of following methods: by SiO
2, terpine resin and mix according to the mass ratio of 10: 2: 2 containing the resol of 6wt% boron that to be placed on temperature be stirring reaction 20min in the reactor of 80 DEG C, then vacuum hydro-extraction 3h, obtains with SiO
2for the acid title complex of carrier.
The nuclear island sealing of the present embodiment by the preparation method of the seamless rubber item of resistance to nuclear radiation is:
Step 1, that terpolymer EP rubber, promoting agent, vulcanizing agent, promotor, anti-aging agent and title complex are placed in to opening rubber mixing machine by proportioning is mixing evenly, obtains main material;
Step 2, that terpolymer EP rubber, promoting agent, vulcanizing agent, promotor, scorch retarder, inert filler, anti-aging agent and title complex are placed in to opening rubber mixing machine by proportioning is mixing evenly, obtains joint material;
Step 3, be the mould of flower bud shape according to nuclear island to be prepared sealing with shape (as shown in Figure 3 and Figure 4) and the size Selection cross section of the seamless rubber item of resistance to nuclear radiation, first main material 1 described in step 1 is filled in mould, then joint material 2 described in step 2 is filled in mould and described joint material 2 is arranged in the two ends of mould main material 1, adopt vulcanizing press to vulcanize the mould that fills main material 1 and joint material 2, after the demoulding, obtain work in-process; In described sulfidation, controlling sulfide stress is 14MPa, and curing temperature is 150 DEG C, and curing time is 30min;
Step 4, work in-process described in multiple step 3 are spliced by the shape and size of the seamless rubber item of resistance to nuclear radiation according to nuclear island to be prepared sealing, then spliced joint is vulcanized, obtain the nuclear island sealing seamless rubber item of resistance to nuclear radiation; In described sulfidation, controlling sulfide stress is 14MPa, and curing temperature is 150 DEG C, and curing time is 30min.
Nuclear island prepared by the present embodiment seals with the seamless rubber item of resistance to nuclear radiation joint without naked eyes visible marks, measure with vernier calliper, Yu Fei joint, joint convex-concave defect in the tolerance zone of defined (taking Φ 15 sections as example tolerance regulation ± 0.1mm, higher than GB GB/T3672.1-2002 regulation ± 0.15mm) actual joint convex-concave defect is zero tolerance, visual without vestige; Yu Fei joint, joint tensile strength, elongation rate of tensile failure equate, 55 degree levels: tensile strength >=7MPa, elongation rate of tensile failure >=450%; 75 degree level: tensile strength >=12MPa, elongation rate of tensile failure >=400%, meets the application requiring that nuclear island seals.
Embodiment 4
The present embodiment is identical with embodiment 3, wherein difference is: the promoting agent in main material is zinc oxide or zinc oxide and stearic acid, vulcanizing agent is dicumyl peroxide or dicumyl peroxide and resol, promotor is promotor TAIC or captax, or be two or three in promotor TAIC, captax and accelerant B Z, anti-aging agent is anti-aging agent RD or anti-aging agent RD and antioxidant MB, title complex is paraffin oil or carbon black, or is two or three in paraffin oil, carbon black and cerium dioxide; Promoting agent in joint material is zinc oxide or zinc oxide and stearic acid, vulcanizing agent is dicumyl peroxide or dicumyl peroxide and resol, promotor is promotor TAIC or promotor TAIC and rubber leveler 40MSF, scorch retarder is Whitfield's ointment or Whitfield's ointment and Tetra hydro Phthalic anhydride, anti-aging agent is anti-aging agent RD or antioxidant 4010NA, or be two or three in antioxidant 4010NA, anti-aging agent RD and antioxidant MB, title complex is carbon black or paraffin oil, or is two or three in paraffin oil, carbon black and cerium dioxide.
Nuclear island prepared by the present embodiment seals with the seamless rubber item of resistance to nuclear radiation joint without naked eyes visible marks, measure with vernier calliper, Yu Fei joint, joint convex-concave defect in the tolerance zone of defined (taking Φ 15 sections as example tolerance regulation ± 0.1mm, higher than GB GB/T3672.1-2002 regulation ± 0.15mm) actual joint convex-concave defect is zero tolerance, visual without vestige; Yu Fei joint, joint tensile strength, elongation rate of tensile failure equate, 55 degree levels: tensile strength >=7MPa, elongation rate of tensile failure >=450%; 75 degree level: tensile strength >=12MPa, elongation rate of tensile failure >=400%, meets the application requiring that nuclear island seals.
Embodiment 5
The present embodiment nuclear island is the seamless rubber item of resistance to nuclear radiation for sealing, is made up of main material and joint material sulfuration; Described main material is made up of following raw material: terpolymer EP rubber 100kg, promoting agent 7kg, vulcanizing agent 2kg, promotor 2kg part, anti-aging agent 1kg, title complex 20kg, wherein promoting agent is zinc oxide and stearic acid (mass ratio 4: 3), and vulcanizing agent is resol, and promotor is captax and accelerant B Z(mass ratio 1: 1), anti-aging agent is antioxidant MB, and title complex is carbon black and cerium dioxide (mass ratio 1: 1);
Described joint material is made up of following raw material: terpolymer EP rubber 100kg, promoting agent 6kg, vulcanizing agent 3kg, promotor 2kg, scorch retarder 0.7kg, inert filler 6kg, anti-aging agent 4kg, title complex 30kg, wherein promoting agent is stearic acid, and vulcanizing agent is dicumyl peroxide and resol (mass ratio 1: 2), and promotor is promotor TAIC and rubber leveler 40MSF(mass ratio 1: 1), scorch retarder is Whitfield's ointment and Tetra hydro Phthalic anhydride (mass ratio 3: 4), and inert filler is with SiO
2for the acid title complex of carrier, anti-aging agent is antioxidant 4010NA and anti-aging agent RD (mass ratio 1: 1), and title complex is paraffin oil and carbon black (mass ratio 2: 1); Described with SiO
2for the acid title complex of carrier is made up of following methods: by SiO
2, terpine resin and mix according to the mass ratio of 10: 3: 2 containing the resol of 5wt% boron that to be placed on temperature be stirring reaction 30min in the reactor of 80 DEG C, then vacuum hydro-extraction 5h, obtains with SiO
2for the acid title complex of carrier.
The nuclear island sealing of the present embodiment by the preparation method of the seamless rubber item of resistance to nuclear radiation is:
Step 1, that terpolymer EP rubber, promoting agent, vulcanizing agent, promotor, anti-aging agent and title complex are placed in to opening rubber mixing machine by proportioning is mixing evenly, obtains main material;
Step 2, that terpolymer EP rubber, promoting agent, vulcanizing agent, promotor, scorch retarder, inert filler, anti-aging agent and title complex are placed in to opening rubber mixing machine by proportioning is mixing evenly, obtains joint material;
Step 3, be special-shaped mould according to nuclear island to be prepared sealing with shape (as shown in Figure 5 and Figure 6) and the size Selection cross section of the seamless rubber item of resistance to nuclear radiation, first main material 1 described in step 1 is filled in mould, then joint material 2 described in step 2 is filled in mould and described joint material 2 is arranged in the two ends of mould main material 1, adopt vulcanizing press to vulcanize the mould that fills main material 1 and joint material 2, after the demoulding, obtain work in-process; In described sulfidation, controlling sulfide stress is 13MPa, and curing temperature is 150 DEG C, and curing time is 30min;
Step 4, work in-process described in multiple step 3 are spliced by the shape and size of the seamless rubber item of resistance to nuclear radiation according to nuclear island to be prepared sealing, then spliced joint is vulcanized, obtain the nuclear island sealing seamless rubber item of resistance to nuclear radiation; In described sulfidation, controlling sulfide stress is 13MPa, and curing temperature is 150 DEG C, and curing time is 30min.
Nuclear island prepared by the present embodiment seals with the seamless rubber item of resistance to nuclear radiation joint without naked eyes visible marks, measure with vernier calliper, Yu Fei joint, joint convex-concave defect in the tolerance zone of defined (taking Φ 15 sections as example tolerance regulation ± 0.1mm, higher than GB GB/T3672.1-2002 regulation ± 0.15mm) actual joint convex-concave defect is zero tolerance, visual without vestige; Yu Fei joint, joint tensile strength, elongation rate of tensile failure equate, 55 degree levels: tensile strength >=7MPa, elongation rate of tensile failure >=450%; 75 degree level: tensile strength >=12MPa, elongation rate of tensile failure >=400%, meets the application requiring that nuclear island seals.
Embodiment 6
The present embodiment is identical with embodiment 5, wherein difference is: the promoting agent in main material is zinc oxide or stearic acid, vulcanizing agent is dicumyl peroxide or dicumyl peroxide and resol, promotor is promotor TAIC, a kind of in captax and accelerant B Z or three kinds, or be promotor TAIC and captax, or be promotor TAIC and accelerant B Z, anti-aging agent is anti-aging agent RD or anti-aging agent RD and antioxidant MB, title complex is paraffin oil, a kind of in carbon black and cerium dioxide or three kinds, or be paraffin oil and carbon black, or be paraffin oil and cerium dioxide, promoting agent in joint material is zinc oxide or zinc oxide and stearic acid, vulcanizing agent is dicumyl peroxide or resol, promotor is promotor TAIC or rubber leveler 40MSF, scorch retarder is Whitfield's ointment or Tetra hydro Phthalic anhydride, anti-aging agent is a kind of in antioxidant 4010NA, anti-aging agent RD and antioxidant MB or three kinds, or be antioxidant 4010NA and antioxidant MB, or be anti-aging agent RD and antioxidant MB, title complex is a kind of in paraffin oil, carbon black and cerium dioxide or three kinds, or be paraffin oil and cerium dioxide, or be carbon black and cerium dioxide.
Nuclear island prepared by the present embodiment seals with the seamless rubber item of resistance to nuclear radiation joint without naked eyes visible marks, measure with vernier calliper, Yu Fei joint, joint convex-concave defect in the tolerance zone of defined (taking Φ 15 sections as example tolerance regulation ± 0.1mm, higher than GB GB/T3672.1-2002 regulation ± 0.15mm) actual joint convex-concave defect is zero tolerance, visual without vestige; Yu Fei joint, joint tensile strength, elongation rate of tensile failure equate, 55 degree levels: tensile strength >=7MPa, elongation rate of tensile failure >=450%; 75 degree level: tensile strength >=12MPa, elongation rate of tensile failure >=400%, meets the application requiring that nuclear island seals.
Embodiment 7
The present embodiment nuclear island is the seamless rubber item of resistance to nuclear radiation for sealing, is made up of main material and joint material sulfuration; Described main material is made up of following raw material: terpolymer EP rubber 100kg, promoting agent 6kg, vulcanizing agent 3kg, promotor 3kg, anti-aging agent 1.5kg, title complex 25kg, wherein promoting agent is zinc oxide and stearic acid (mass ratio 1: 1), vulcanizing agent is dicumyl peroxide and resol (mass ratio 2: 1), promotor is promotor TAIC, captax and accelerant B Z(mass ratio 2: 2: 1), anti-aging agent is anti-aging agent RD and antioxidant MB (mass ratio 1: 2), and title complex is paraffin oil, carbon black and cerium dioxide (mass ratio 1: 2: 2);
Described joint material is made up of following raw material: terpolymer EP rubber 100kg, promoting agent 5kg, vulcanizing agent 2.5kg, promotor 2.5kg, scorch retarder 0.5kg, inert filler 5kg, anti-aging agent 3kg, title complex 25kg, wherein promoting agent is zinc oxide and stearic acid (mass ratio 3: 2), and vulcanizing agent is dicumyl peroxide and resol (mass ratio 1: 1), and promotor is promotor TAIC and rubber leveler 40MSF(mass ratio 3: 2), scorch retarder is Whitfield's ointment and Tetra hydro Phthalic anhydride (mass ratio 1: 1), and inert filler is with SiO
2for the acid title complex of carrier, anti-aging agent is antioxidant 4010NA, anti-aging agent RD and antioxidant MB (mass ratio 1: 1: 1), and title complex is paraffin oil, carbon black and cerium dioxide (mass ratio 2: 2: 1); Described with SiO
2for the acid title complex of carrier is made up of following methods: by SiO
2, terpine resin and mix according to the mass ratio of 10: 1: 1 containing the resol of 4wt% boron that to be placed on temperature be stirring reaction 30min in the reactor of 75 DEG C, then vacuum hydro-extraction 4h, obtains with SiO
2for the acid title complex of carrier.
The nuclear island sealing of the present embodiment by the preparation method of the seamless rubber item of resistance to nuclear radiation is:
Step 1, that terpolymer EP rubber, promoting agent, vulcanizing agent, promotor, anti-aging agent and title complex are placed in to opening rubber mixing machine by proportioning is mixing evenly, obtains main material;
Step 2, that terpolymer EP rubber, promoting agent, vulcanizing agent, promotor, scorch retarder, inert filler, anti-aging agent and title complex are placed in to opening rubber mixing machine by proportioning is mixing evenly, obtains joint material;
Step 3, shape and size selection mould according to nuclear island to be prepared sealing with the seamless rubber item of resistance to nuclear radiation, first main material described in step 1 is filled in mould, then joint material described in step 2 is filled in mould and described joint material is arranged in the two ends of mould main material, adopt vulcanizing press to vulcanize the mould that fills main material and joint material, after the demoulding, obtain work in-process; In described sulfidation, controlling sulfide stress is 12MPa, and curing temperature is 160 DEG C, and curing time is 20min;
Step 4, work in-process described in multiple step 3 are spliced by the shape and size of the seamless rubber item of resistance to nuclear radiation according to nuclear island to be prepared sealing, then spliced joint is vulcanized, obtain the nuclear island sealing seamless rubber item of resistance to nuclear radiation; In described sulfidation, controlling sulfide stress is 12MPa, and curing temperature is 160 DEG C, and curing time is 20min.
Nuclear island prepared by the present embodiment seals with the seamless rubber item of resistance to nuclear radiation joint without naked eyes visible marks, measure with vernier calliper, Yu Fei joint, joint convex-concave defect in the tolerance zone of defined (taking Φ 15 sections as example tolerance regulation ± 0.1mm, higher than GB GB/T3672.1-2002 regulation ± 0.15mm) actual joint convex-concave defect is zero tolerance, visual without vestige; Yu Fei joint, joint tensile strength, elongation rate of tensile failure equate, 55 degree levels: tensile strength >=7MPa, elongation rate of tensile failure >=450%; 75 degree level: tensile strength >=12MPa, elongation rate of tensile failure >=400%, meets the application requiring that nuclear island seals.
Embodiment 8
The present embodiment is identical with embodiment 7, wherein difference is: the promoting agent in main material is zinc oxide or stearic acid, vulcanizing agent is dicumyl peroxide or resol, promotor is one or both in promotor TAIC, captax and accelerant B Z, anti-aging agent is anti-aging agent RD or antioxidant MB, and title complex is one or both in paraffin oil, carbon black and cerium dioxide; Promoting agent in joint material is zinc oxide or stearic acid, vulcanizing agent is dicumyl peroxide or resol, promotor is promotor TAIC or rubber leveler 40MSF, scorch retarder is Whitfield's ointment or Tetra hydro Phthalic anhydride, anti-aging agent is one or both in antioxidant 4010NA, anti-aging agent RD and antioxidant MB, and title complex is one or both in paraffin oil, carbon black and cerium dioxide.
Nuclear island prepared by the present embodiment seals with the seamless rubber item of resistance to nuclear radiation joint without naked eyes visible marks, measure with vernier calliper, Yu Fei joint, joint convex-concave defect in the tolerance zone of defined (taking Φ 15 sections as example tolerance regulation ± 0.1mm, higher than GB GB/T3672.1-2002 regulation ± 0.15mm) actual joint convex-concave defect is zero tolerance, visual without vestige; Yu Fei joint, joint tensile strength, elongation rate of tensile failure equate, 55 degree levels: tensile strength >=7MPa, elongation rate of tensile failure >=450%; 75 degree level: tensile strength >=12MPa, elongation rate of tensile failure >=400%, meets the application requiring that nuclear island seals.
Embodiment 9
The present embodiment nuclear island is the seamless rubber item of resistance to nuclear radiation for sealing, is made up of main material and joint material sulfuration; Described main material is made up of following raw material: terpolymer EP rubber 100kg, promoting agent 5kg, vulcanizing agent 4kg, promotor 4kg, anti-aging agent 2kg, title complex 30kg, wherein promoting agent is zinc oxide and stearic acid (mass ratio 2: 3), and vulcanizing agent is resol, and promotor is captax and accelerant B Z(mass ratio 1: 3), anti-aging agent is antioxidant MB, and title complex is carbon black and cerium dioxide (mass ratio 2: 1);
Described joint material is made up of following raw material: terpolymer EP rubber 100kg, promoting agent 4kg, vulcanizing agent 2kg, promotor 3kg, scorch retarder 0.3kg, inert filler 4kg, anti-aging agent 2kg, title complex 20kg, wherein promoting agent is zinc oxide and stearic acid (mass ratio 1: 1), and vulcanizing agent is dicumyl peroxide and resol (mass ratio 1: 1), and promotor is promotor TAIC and rubber leveler 40MSF(mass ratio 1: 2), scorch retarder is Whitfield's ointment and Tetra hydro Phthalic anhydride (mass ratio 2: 1), and inert filler is with SiO
2for the acid title complex of carrier, anti-aging agent is antioxidant 4010NA, anti-aging agent RD and antioxidant MB (mass ratio 1: 1: 2), and title complex is paraffin oil, carbon black and cerium dioxide (mass ratio 1: 2: 1); Described with SiO
2for the acid title complex of carrier is made up of following methods: by SiO
2, terpine resin and mix according to the mass ratio of 10: 1: 1 containing the resol of 4wt% boron that to be placed on temperature be stirring reaction 30min in the reactor of 75 DEG C, then vacuum hydro-extraction 4h, obtains with SiO
2for the acid title complex of carrier.
The nuclear island sealing of the present embodiment by the preparation method of the seamless rubber item of resistance to nuclear radiation is:
Step 1, that terpolymer EP rubber, promoting agent, vulcanizing agent, promotor, anti-aging agent and title complex are placed in to opening rubber mixing machine by proportioning is mixing evenly, obtains main material;
Step 2, that terpolymer EP rubber, promoting agent, vulcanizing agent, promotor, scorch retarder, inert filler, anti-aging agent and title complex are placed in to opening rubber mixing machine by proportioning is mixing evenly, obtains joint material;
Step 3, shape and size selection mould according to nuclear island to be prepared sealing with the seamless rubber item of resistance to nuclear radiation, first main material described in step 1 is filled in mould, then joint material described in step 2 is filled in mould and described joint material is arranged in the two ends of mould main material, adopt vulcanizing press to vulcanize the mould that fills main material and joint material, after the demoulding, obtain work in-process; In described sulfidation, controlling sulfide stress is 12MPa, and curing temperature is 160 DEG C, and curing time is 20min;
Step 4, work in-process described in multiple step 3 are spliced by the shape and size of the seamless rubber item of resistance to nuclear radiation according to nuclear island to be prepared sealing, then spliced joint is vulcanized, obtain the nuclear island sealing seamless rubber item of resistance to nuclear radiation; In described sulfidation, controlling sulfide stress is 12MPa, and curing temperature is 160 DEG C, and curing time is 20min.
Nuclear island prepared by the present embodiment seals with the seamless rubber item of resistance to nuclear radiation joint without naked eyes visible marks, measure with vernier calliper, Yu Fei joint, joint convex-concave defect in the tolerance zone of defined (taking Φ 15 sections as example tolerance regulation ± 0.1mm, higher than GB GB/T3672.1-2002 regulation ± 0.15mm) actual joint convex-concave defect is zero tolerance, visual without vestige; Yu Fei joint, joint tensile strength, elongation rate of tensile failure equate, 55 degree levels: tensile strength >=7MPa, elongation rate of tensile failure >=450%; 75 degree level: tensile strength >=12MPa, elongation rate of tensile failure >=400%, meets the application requiring that nuclear island seals.
Embodiment 10
The present embodiment is identical with embodiment 9, wherein difference is: the promoting agent in main material is zinc oxide or stearic acid, vulcanizing agent is dicumyl peroxide or dicumyl peroxide and resol, promotor is promotor TAIC, a kind of in captax and accelerant B Z or three kinds, or be promotor TAIC and captax, or be promotor TAIC and accelerant B Z, anti-aging agent is anti-aging agent RD or anti-aging agent RD and antioxidant MB, title complex is paraffin oil, a kind of in carbon black and cerium dioxide or three kinds, or be paraffin oil and carbon black, or be paraffin oil and cerium dioxide, promoting agent in joint material is zinc oxide or stearic acid, vulcanizing agent is dicumyl peroxide or resol, promotor is promotor TAIC or rubber leveler 40MSF, scorch retarder is Whitfield's ointment or Tetra hydro Phthalic anhydride, anti-aging agent is one or both in antioxidant 4010NA, anti-aging agent RD and antioxidant MB, and title complex is one or both in paraffin oil, carbon black and cerium dioxide.。
Nuclear island prepared by the present embodiment seals with the seamless rubber item of resistance to nuclear radiation joint without naked eyes visible marks, measure with vernier calliper, Yu Fei joint, joint convex-concave defect in the tolerance zone of defined (taking Φ 15 sections as example tolerance regulation ± 0.1mm, higher than GB GB/T3672.1-2002 regulation ± 0.15mm) actual joint convex-concave defect is zero tolerance, visual without vestige; Yu Fei joint, joint tensile strength, elongation rate of tensile failure equate, 55 degree levels: tensile strength >=7MPa, elongation rate of tensile failure >=450%; 75 degree level: tensile strength >=12MPa, elongation rate of tensile failure >=400%, meets the application requiring that nuclear island seals.
The above; it is only preferred embodiment of the present invention; not the present invention is done to any restriction, every any simple modification of above embodiment being done according to invention technical spirit, change and equivalent structure change, and all still belong in the protection domain of technical solution of the present invention.
Claims (6)
1. nuclear island seals with the seamless rubber item of resistance to nuclear radiation, it is characterized in that, is made up of main material and joint material; Described main material is made up of the raw material of following weight part: 100 parts of terpolymer EP rubbers, 4-8 parts of promoting agents, 1-5 parts of vulcanizing agents, 1-5 parts of promotor, 0.5-3 parts, anti-aging agent, 15-35 parts of title complexs, wherein promoting agent is zinc oxide and/or stearic acid, vulcanizing agent is dicumyl peroxide and/or resol, promotor is one or more in promotor TAIC, captax and accelerant B Z, anti-aging agent is anti-aging agent RD and/or antioxidant MB, and title complex is one or more in paraffin oil, carbon black and cerium dioxide;
Described joint material is made up of the raw material of following weight part: 100 parts of terpolymer EP rubbers, 3-7 parts of promoting agents, 1-4 parts of vulcanizing agents, 1-4 parts of promotor, 0-1 part of scorch retarder, 3-7 parts of inert fillers, 1-5 parts, anti-aging agent, 15-35 parts of title complexs, wherein promoting agent is zinc oxide and/or stearic acid, vulcanizing agent is dicumyl peroxide and/or resol, promotor is promotor TAIC and/or rubber leveler 40MSF, scorch retarder is Whitfield's ointment and/or Tetra hydro Phthalic anhydride, inert filler is the acid title complex taking SiO2 as carrier, anti-aging agent is antioxidant 4010NA, one or more in anti-aging agent RD and antioxidant MB, title complex is paraffin oil, one or more in carbon black and cerium dioxide, described with SiO
2for the acid title complex of carrier is made up of following methods: by SiO
2, terpine resin and mix according to 10: 1～3: 1～3 mass ratio containing the resol of 2wt%～6wt% boron that to be placed on temperature be stirring reaction 20min～40min in the reactor of 70 DEG C～80 DEG C, then vacuum hydro-extraction 3h～5h, obtains with SiO
2for the acid title complex of carrier.
2. a kind of nuclear island according to claim 1 seamless rubber item of resistance to nuclear radiation for sealing, it is characterized in that, described main material is made up of the raw material of following weight part: 100 parts of terpolymer EP rubbers, 5-7 parts of promoting agents, 2-4 parts of vulcanizing agents, 2-4 parts of promotor, 1-2 parts, anti-aging agent, 20-30 parts of title complexs; Described joint material is made up of the raw material of following weight part: 100 parts of terpolymer EP rubbers, 4-6 parts of promoting agents, 2-3 parts of vulcanizing agents, 2-3 parts of promotor, 0.3-0.7 part of scorch retarder, 4-6 parts of inert fillers, 2-4 parts, anti-aging agent, 20-30 parts of title complexs.
3. a kind of nuclear island according to claim 2 seals with the seamless rubber item of resistance to nuclear radiation, it is characterized in that, described main material is made up of the raw material of following weight part: 100 parts of terpolymer EP rubbers, 6 parts of promoting agents, 3 parts of vulcanizing agents, 3 parts of promotor, 1.5 parts, anti-aging agent, 25 parts of title complexs; Described joint material is made up of the raw material of following weight part: 100 parts of terpolymer EP rubbers, 5 parts of promoting agents, 2.5 parts of vulcanizing agents, 2.5 parts of promotor, 0.5 part of scorch retarder, 5 parts of inert fillers, 3 parts, anti-aging agent, 25 parts of title complexs.
4. a method of preparing the nuclear island sealing seamless rubber item of resistance to nuclear radiation as described in claim 1,2 or 3, is characterized in that, the method comprises the following steps:
Step 1, that terpolymer EP rubber, promoting agent, vulcanizing agent, promotor, anti-aging agent and title complex are placed in to opening rubber mixing machine by proportioning is mixing evenly, obtains main material;
Step 2, that terpolymer EP rubber, promoting agent, vulcanizing agent, promotor, scorch retarder, inert filler, anti-aging agent and title complex are placed in to opening rubber mixing machine by proportioning is mixing evenly, obtains joint material;
Step 3, shape and size selection mould according to nuclear island to be prepared sealing with the seamless rubber item of resistance to nuclear radiation, first main material described in step 1 is filled in mould, then joint material described in step 2 is filled in mould and described joint material is arranged in the two ends of mould main material, adopt vulcanizing press to vulcanize the mould that fills main material and joint material, after the demoulding, obtain work in-process; In described sulfidation, controlling sulfide stress is 10MPa～14MPa, and curing temperature is 150 DEG C～170 DEG C, and curing time is 10min～30min;
Step 4, work in-process described in multiple step 3 are spliced by the shape and size of the seamless rubber item of resistance to nuclear radiation according to nuclear island to be prepared sealing, then spliced joint is vulcanized, obtain the nuclear island sealing seamless rubber item of resistance to nuclear radiation; In described sulfidation, controlling sulfide stress is 10MPa～14MPa, and curing temperature is 150 DEG C～170 DEG C, and curing time is 10min～30min.
5. the method for preparing the nuclear island sealing seamless rubber item of resistance to nuclear radiation according to claim 4, is characterized in that, curing temperature described in step 3 is 160 DEG C, and curing time is 20min.
6. the method for preparing the nuclear island sealing seamless rubber item of resistance to nuclear radiation according to claim 4, is characterized in that, curing temperature described in step 4 is 160 DEG C, and curing time is 20min.
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| CN103612352B (en) * | 2013-11-15 | 2016-03-30 | 陕西特种橡胶制品有限公司 | A kind of method utilizing thermograde to control nuclear power plant's rubber physical dimension |
| CN104194680A (en) * | 2014-09-18 | 2014-12-10 | 太仓荣南密封件科技有限公司 | Sealing strip heat vulcanization connector glue solution as well as preparation method and application thereof |
| CN107118449A (en) * | 2017-06-27 | 2017-09-01 | 苏州菱慧电子科技有限公司 | A kind of elastomeric material of resistance to nuclear radiation |
| CN107722471B (en) * | 2017-10-23 | 2020-07-31 | 陕西特种橡胶制品有限公司 | Radiation-resistant rubber for nuclear power steam generator closure plate air bag and preparation method thereof |
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Address after: No. 1, South Section of Chaoyang 6th Road, Weicheng District, Xianyang City, Shaanxi Province, 712042 Patentee after: SHAANXI SPECIAL RUBBER PRODUCTS Co.,Ltd. Patentee after: SHANGHAI NUCLEAR ENGINEERING RESEARCH & DESIGN INSTITUTE Co.,Ltd. Address before: No. 1, South Section of Chaoyang 6th Road, Weicheng District, Xianyang City, Shaanxi Province, 712042 Patentee before: SHAANXI SPECIAL RUBBER PRODUCTS Co.,Ltd. Patentee before: SHANGHAI NUCLEAR ENGINEERING RESEARCH & DESIGN INSTITUTE Address after: No. 1, South Section of Chaoyang 6th Road, Weicheng District, Xianyang City, Shaanxi Province, 712042 Patentee after: SHAANXI SPECIAL RUBBER PRODUCTS Co.,Ltd. Patentee after: Shanghai Nuclear Engineering Research and Design Institute Co.,Ltd. Address before: No. 1, South Section of Chaoyang 6th Road, Weicheng District, Xianyang City, Shaanxi Province, 712042 Patentee before: SHAANXI SPECIAL RUBBER PRODUCTS Co.,Ltd. Patentee before: SHANGHAI NUCLEAR ENGINEERING RESEARCH & DESIGN INSTITUTE Co.,Ltd. |