CN103937051A - Organic and inorganic composite vulcanized nitrile rubber for sealing element and preparation method of organic and inorganic composite vulcanized nitrile rubber - Google Patents

Organic and inorganic composite vulcanized nitrile rubber for sealing element and preparation method of organic and inorganic composite vulcanized nitrile rubber Download PDF

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Publication number
CN103937051A
CN103937051A CN201410142193.4A CN201410142193A CN103937051A CN 103937051 A CN103937051 A CN 103937051A CN 201410142193 A CN201410142193 A CN 201410142193A CN 103937051 A CN103937051 A CN 103937051A
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nitrile rubber
organic
inorganic
compound
sealing member
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许一婷
高辉
谢泓辉
叶华立
戴李宗
罗伟昂
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Xiamen University
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Xiamen University
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Priority to PCT/CN2014/093077 priority patent/WO2015154492A1/en
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/06—Sulfur
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/10—Esters; Ether-esters
    • C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/17—Amines; Quaternary ammonium compounds
    • C08K5/18—Amines; Quaternary ammonium compounds with aromatically bound amino groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/10—Encapsulated ingredients
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
    • C08L9/02—Copolymers with acrylonitrile

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Sealing Material Composition (AREA)

Abstract

The invention discloses an organic and inorganic composite vulcanized nitrile rubber for a sealing element and a preparation method of the organic and inorganic composite vulcanized nitrile rubber. The organic and inorganic composite vulcanized nitrile rubber comprises the following components in parts by mass: 100 parts of nitrile rubber, 5-40 parts of carboxyl nitrile rubber-coated Si3N4 nanoparticles, 1-3 parts of accelerant, 2-5 parts of active agent, 1-3 parts of sulphur, 5-10 parts of plasticizer and 1-3 parts of antiager. The Si3N4 nanoparticles are coated with carboxyl nitrile rubber, and heat-resistant Si3N4 nanoparticles are introduced into the nitrile rubber, so that the Si3N4 nanoparticles are evenly dispersed in compound rubber, meanwhile, the carboxyl nitrile rubber of coating the nanoparticles is connected with the nanoparticles by chemical bonds, and can be completely compatible with the nitrile rubber, and thus the problems of compatibility, interfaces and the like cannot happen. Thus, the prepared organic and inorganic composite vulcanized nitrile rubber for the sealing element has excellent high temperature resistance and physical and mechanical properties, and the application range of the nitrile rubber is expanded.

Description

A kind of compound sulfurized nitrile rubber of organic-inorganic for sealing member and preparation method thereof
Technical field
The invention belongs to sealing material technical field, be specifically related to a kind of compound sulfurized nitrile rubber of organic-inorganic for sealing member and preparation method thereof.
Background technology
Paracril (NBR) has oil-proofness, wear resistance and the excellent property such as ageing-resistant, is widely used in especially in the preparation of various oil-resistant articles, antistatic article and various sealing members.But the life-time service temperature of the sealing member that NBR makes can only, below 120 ℃, therefore limit its application in car industry.
In order to improve the resistance to elevated temperatures of NBR, method used in the prior art is as follows: 1, add coupling agent to strengthen the resistance to elevated temperatures (referring to CN103012881A) of paracril; 2, interpolation carbon black N660, high abrasion furnace carbon black N330, titanate coupling agent TMC-TTS, the N-2-(aminoethyl taked) the various fillers such as-3-aminopropyl trimethoxysilane, Silane coupling agent KH550, nano-calcium carbonate and coupling agent carry out the thermotolerance (referring to CN102993502A) of modified butadiene acrylonitrile rubber; 3, taked the blend of terpolymer EP rubber/paracril, and added polynite, formed intercalation configuration, polynite add the oil-proofness to paracril, thermotolerance increase (referring to CN103012972A).But the resistance to elevated temperatures of the paracril that above-mentioned several method is prepared is still difficult to meet the demand of car industry.
Summary of the invention
The object of the present invention is to provide the compound sulfurized nitrile rubber of a kind of organic-inorganic for sealing member.
Another object of the present invention is to provide the preparation method of the above-mentioned compound sulfurized nitrile rubber of organic-inorganic for sealing member.
Technical scheme of the present invention is specific as follows:
For the compound sulfurized nitrile rubber of organic-inorganic of sealing member, its raw material comprises the component of following mass parts:
In a preferred embodiment of the invention, in described paracril, acrylonitrile content is 36%-42%.
In a preferred embodiment of the invention, described carboxyl butyronitrile glue coated Si 3n 4the mass content 5%-45% of carboxyl butyronitrile glue in nanoparticle.
In a preferred embodiment of the invention, described softening agent is dioctyl phthalate (DOP) (DOP) or dibutyl phthalate (DBP).
In a preferred embodiment of the invention, described promotor is N, the two thiamides (TMTD) of N-tetramethyl-two sulphur or 2,2'-dithio-bis-benzothiazole (DM).
In a preferred embodiment of the invention, described promoting agent is zinc oxide or stearic acid.
In a preferred embodiment of the invention, described anti-aging agent is N-sec.-propyl-4-aminodiphenylamine (antioxidant 4010NA), N-(1,3-dimethylbutyl) a kind of in-N'-diphenyl-para-phenylene diamine (antioxidant 4020) and N-phenyl-αnaphthylamine (antioxidant A) or mix.
The preparation method of the above-mentioned compound sulfurized nitrile rubber of organic-inorganic for sealing member, comprises the steps:
Step (1) is prepared carboxyl butyronitrile glue coated Si 3n 4nanoparticle: liquid carboxy nitrile rubber is dissolved in after toluene, adds therein nanometer Si 3n 4powder obtains mixed solution, at N 2under gas protection, above-mentioned mixed solution is carried out to reflux, then drying and ball milling, described carboxyl butyronitrile glue coated Si obtained 3n 4nanoparticle.
Step (2) is prepared rubber: after adding mill mixing under the condition of roll spacing 2-3mm paracril, add carboxyl butyronitrile glue coated Si 3n 4nanoparticle continues mixing under the condition of roll spacing 1-2mm, then plays 8-12 triangle bag, carries out thin-pass, obtains rubber.
Step (3) is prepared finished product: in above-mentioned rubber, add promotor, promoting agent, softening agent and anti-aging agent to carry out mixing, after playing 8-10 triangle bag, add sulphur, beat again after 5-6 triangle bag, vulcanize, obtain the described compound sulfurized nitrile rubber of organic-inorganic for sealing member.
In a preferred embodiment of the invention, the temperature of the reflux of described step (1) is 60-100 ℃, and the time is 2-8h.
In a preferred embodiment of the invention, in described step (3), the condition of sulfuration is 150 ℃ * t 90* 10MPa.
Beneficial effect of the present invention is as follows:
Si 3n 4adding of nanoparticle is significantly improved the thermotolerance that meets sizing material, and 1, the present invention utilizes carboxyl butyronitrile glue coated Si 3n 4nanoparticle is introduced resistant to elevated temperatures Si in paracril 3n 4nanoparticle, makes Si 3n 4nanometer is dispersed in compound sizing material, the simultaneously carboxy nitrile rubber of clad nano particle and nanoparticle chemical bonding and can be completely compatible with paracril, there is not consistency, the problems such as interface, make resistance to elevated temperatures and the physical and mechanical properties of the prepared compound sulfurized nitrile rubber of organic-inorganic for sealing member good, the range of application of the paracril of expansion.
2, preparation method of the present invention utilizes existing processing units, and production technique is controlled, with low cost, is applicable to suitability for industrialized production;
Accompanying drawing explanation
Fig. 1: be the TGA curve of the prepared compound sulfurized nitrile rubber of organic-inorganic of embodiment 5.
Embodiment
By embodiment, by reference to the accompanying drawings technical scheme of the present invention is further detailed and is described below.
In following enforcement, softening agent used is dioctyl phthalate (DOP) (DOP) or dibutyl phthalate (DBP); Promotor used is N, the two thiamides (TMTD) of N-tetramethyl-two sulphur or 2,2'-dithio-bis-benzothiazole (DM); Promoting agent used is that zinc oxide and stearic acid are used by 3:1; Anti-aging agent used is N-sec.-propyl-4-aminodiphenylamine (antioxidant 4010NA), N-(1,3-dimethylbutyl)-N'-diphenyl-para-phenylene diamine (antioxidant 4020) and N-phenyl-αnaphthylamine (antioxidant A).
Embodiment 1-3
Step (1) is got a certain amount of liquid carboxy nitrile rubber and is dissolved in wiring solution-forming in toluene and adds a certain amount of nanometer Si again 3n 4powder is put into 500mL there-necked flask, passes into N 2gas protection, after refluxing under certain temperature, (temperature of reflux is 60-100 ℃, and the time is 2-8h) takes out, and after drying treatment, takes out ball milling, obtains carboxyl butyronitrile glue coated Si 3n 4nanoparticle.Wherein:
Embodiment condition Temperature of reaction Reaction times Carboxy nitrile rubber quality/Si 3N 4Powder
1 60℃ 2h 25%
2 60℃ 8h 25%
3 100℃ 5h 25%
Step (2) adds mill mixing (roll spacing 2-3mm) by paracril, adds in proportion carboxyl butyronitrile glue coated Si 3n 4nanoparticle, continues mixing (roll spacing 1-2mm), plays 8-12 triangle bag, carries out thin-pass, obtains rubber.Wherein: paracril 100 mass parts, carboxyl butyronitrile glue coated Si 3n 4nanoparticle 30 mass parts.
Step material Paracril Carboxyl butyronitrile glue coated Si 3N 4Nanoparticle
Step 2 100 mass parts 30 mass parts
Step (3) adds accelerant N by above-mentioned rubber, two thiamide (TMTD) 2 mass parts of N-tetramethyl-two sulphur, promoting agent zinc oxide 3 mass parts, stearic acid 1 mass parts, plasticizer phthalic acid dioctyl ester (DOP) 7.5 mass parts and anti-aging agent N-sec.-propyl-4-aminodiphenylamine (antioxidant 4010NA) 2 mass parts are carried out mixing, play 8-10 triangle bag and add 2 mass parts sulphur, beat again after 5-6 triangle bag, with vulkameter, measure its curing time, finally sulfuration (150 ℃ * t of cure conditions on vulcanizing press 90* 10MPa), obtain the described compound sulfurized nitrile rubber of organic-inorganic for sealing member.
Embodiment 4-6
Step (1) is got a certain amount of liquid carboxy nitrile rubber and is dissolved in wiring solution-forming in toluene and adds a certain amount of nanometer Si again 3n 4powder is put into 500mL there-necked flask, passes into N 2gas protection, after refluxing under certain temperature, (temperature of reflux is 60-100 ℃, and the time is 2-8h) takes out, and after drying treatment, takes out ball milling, obtains carboxyl butyronitrile glue coated Si 3n 4nanoparticle.Wherein:
Embodiment condition Temperature of reaction Reaction times Carboxy nitrile rubber quality/Si 3N 4Powder
4 80℃ 5h 5%
5 80℃ 5h 25%
6 80℃ 5h 45%
Step (2) adds mill mixing (roll spacing 2-3mm) by paracril, adds in proportion carboxyl butyronitrile glue coated Si 3n 4nanoparticle, continues mixing (roll spacing 1-2mm), plays 8-12 triangle bag, carries out thin-pass, obtains rubber.Wherein: paracril 100 mass parts, carboxyl butyronitrile glue coated Si 3n 4nanoparticle 30 mass parts.
Step material Paracril Carboxyl butyronitrile glue coated Si 3N 4Nanoparticle
Step 2 100 mass parts 30 mass parts
Step (3) adds promoting agent zinc oxide 3 mass parts by above-mentioned rubber, stearic acid 1 mass parts, promotor 2,2'-dithio-bis-benzothiazole (DM) 2 mass parts, plasticizer phthalic acid dibutylester (DBP) 7.5 mass parts and anti-aging agent N-(1,3-dimethylbutyl)-N'-diphenyl-para-phenylene diamine (antioxidant 4020) 2 mass parts are carried out mixing, play 8-10 triangle bag and add 2 mass parts sulphur, beat again after 5-6 triangle bag, with vulkameter, measure its curing time, finally sulfuration (150 ℃ * t of cure conditions on vulcanizing press 90* 10MPa), obtain the described compound sulfurized nitrile rubber of organic-inorganic for sealing member.
Wherein the compound sulfurized nitrile rubber of prepared organic-inorganic of embodiment 5 shows good thermostability (as shown in Figure 1), and the comparing result of itself and the physical and mechanical properties of pure NBR vulcanized rubber after air oven aging test is as shown in the table.
(100 ℃ of aging temperatures, aging duration 72h)
Embodiment 7-9
Step (1) is got a certain amount of liquid carboxy nitrile rubber and is dissolved in wiring solution-forming in toluene and adds a certain amount of nanometer Si again 3n 4powder is put into 500mL there-necked flask, passes into N 2gas protection, after refluxing under certain temperature, (temperature of reflux is 60-100 ℃, and the time is 2-8h) takes out, and after drying treatment, takes out ball milling, obtains carboxyl butyronitrile glue coated Si 3n 4nanoparticle.Wherein: carboxy nitrile rubber quality/Si 3n 4powder is 25%, 80 ℃ of temperature, backflow 5h.
Step condition Temperature of reaction Reaction times Carboxy nitrile rubber quality/Si 3N 4Powder
1 80℃ 5h 25%
Step (2) adds mill mixing (roll spacing 2-3mm) by paracril, adds in proportion carboxyl butyronitrile glue coated Si 3n 4nanoparticle, continues mixing (roll spacing 1-2mm), plays 8-12 triangle bag, carries out thin-pass, obtains rubber.Wherein:
Embodiment material Paracril Carboxyl butyronitrile glue coated Si 3N 4Nanoparticle
7 100 mass parts 5 mass parts
8 100 mass parts 30 mass parts
9 100 mass parts 45 mass parts
Step (3) adds promotor 2 by above-mentioned rubber, 2'-dithio-bis-benzothiazole 2 mass parts, promoting agent zinc oxide 3 mass parts, stearic acid 1 mass parts, plasticizer phthalic acid dibutylester 7.5 mass parts and anti-aging agent N-phenyl-αnaphthylamine (antioxidant A) 2 mass parts are carried out mixing, play 8-10 triangle bag and add 2 mass parts sulphur, beat again after 5-6 triangle bag, with vulkameter, measure its curing time, finally sulfuration (150 ℃ * t of cure conditions on vulcanizing press 90* 10MPa), obtain the described compound sulfurized nitrile rubber of organic-inorganic for sealing member.
Embodiment 10-12
Step (1) is got a certain amount of liquid carboxy nitrile rubber and is dissolved in wiring solution-forming in toluene and adds a certain amount of nanometer Si again 3n 4powder is put into 500mL there-necked flask, passes into N 2gas protection, takes out after refluxing some hours under certain temperature, after drying treatment, takes out ball milling, obtains carboxyl butyronitrile glue coated Si 3n 4nanoparticle.Wherein: carboxy nitrile rubber quality/Si 3n 4powder is 25%, 80 ℃ of temperature, backflow 5h.
Step condition Temperature of reaction Reaction times Carboxy nitrile rubber quality/Si 3N 4Powder
1 80℃ 5h 25%
Step (2) adds mill mixing (roll spacing 2-3mm) by paracril, adds in proportion carboxyl butyronitrile glue coated Si 3n 4nanoparticle, continues mixing (roll spacing 1-2mm), plays 8-12 triangle bag, carries out thin-pass, obtains rubber.Wherein: paracril 100 mass parts, carboxyl butyronitrile glue coated Si 3n 4nanoparticle 25 mass parts.
Material Paracril Carboxyl butyronitrile glue coated Si 3N 4Nanoparticle
Step 2 100 mass parts 25 mass parts
Step (3) is by carboxyl butyronitrile glue coated Si 3n 4nanoparticle/paracril organic and inorganic compound symphysis glue adds accelerant N, the two thiamides (TMTD) of N-tetramethyl-two sulphur, promoting agent zinc oxide and stearic acid are undertaken mixing by 3:1 use, plasticizer phthalic acid dioctyl ester (DOP) and anti-aging agent N-sec.-propyl-4-aminodiphenylamine (antioxidant 4010NA), play 8-10 triangle bag and add sulphur, beat again after 5-6 triangle bag, with vulkameter, measure its curing time, finally sulfuration (150 ℃ * t of cure conditions on vulcanizing press 90* 10MPa), obtain composite sulfuration rubber.Wherein:
The above, be only preferred embodiment of the present invention, therefore can not limit according to this scope of the invention process, the equivalence done according to the scope of the claims of the present invention and description changes and modifies, and all should still belong in the scope that the present invention contains.

Claims (10)

1. for the compound sulfurized nitrile rubber of organic-inorganic of sealing member, it is characterized in that: its raw material comprises the component of following mass parts:
2. the compound sulfurized nitrile rubber of a kind of organic-inorganic for sealing member as claimed in claim 1, is characterized in that: in described paracril, acrylonitrile content is 36%-42%.
3. the compound sulfurized nitrile rubber of a kind of organic-inorganic for sealing member as claimed in claim 1, is characterized in that: described carboxyl butyronitrile glue coated Si 3n 4the mass content 5%-45% of carboxyl butyronitrile glue in nanoparticle.
4. the compound sulfurized nitrile rubber of a kind of organic-inorganic for sealing member as claimed in claim 1, is characterized in that: described softening agent is dioctyl phthalate (DOP) or dibutyl phthalate.
5. the compound sulfurized nitrile rubber of a kind of organic-inorganic for sealing member as claimed in claim 1, is characterized in that: described promotor is N, the two thiamides of N-tetramethyl-two sulphur or 2,2'-dithio-bis-benzothiazole.
6. the compound sulfurized nitrile rubber of a kind of organic-inorganic for sealing member as claimed in claim 1, is characterized in that: described promoting agent is zinc oxide or stearic acid.
7. the compound sulfurized nitrile rubber of a kind of organic-inorganic for sealing member as claimed in claim 1, it is characterized in that: described anti-aging agent is N-sec.-propyl-4-aminodiphenylamine, N-(1,3-dimethylbutyl) a kind of in-N'-diphenyl-para-phenylene diamine and N-phenyl-αnaphthylamine or mix.
8. a preparation method for the compound sulfurized nitrile rubber of organic-inorganic for sealing member described in arbitrary claim in claim 1 to 7, is characterized in that: comprise the steps:
(1) prepare carboxyl butyronitrile glue coated Si 3n 4nanoparticle: liquid carboxy nitrile rubber is dissolved in after toluene, adds therein nanometer Si 3n 4powder obtains mixed solution, at N 2under gas protection, above-mentioned mixed solution is carried out to reflux, then drying and ball milling, described carboxyl butyronitrile glue coated Si obtained 3n 4nanoparticle.
(2) prepare rubber: after adding mill mixing under the condition of roll spacing 2-3mm paracril, add carboxyl butyronitrile glue coated Si 3n 4nanoparticle continues mixing under the condition of roll spacing 1-2mm, then plays 8-12 triangle bag, carries out thin-pass, obtains rubber.
(3) prepare finished product: in above-mentioned rubber, add promotor, promoting agent, softening agent and anti-aging agent to carry out mixing, after playing 8-10 triangle bag, add sulphur, beat again after 5-6 triangle bag, vulcanize, obtain the described compound sulfurized nitrile rubber of organic-inorganic for sealing member.
9. the preparation method of a kind of compound sulfurized nitrile rubber of organic-inorganic for sealing member as claimed in claim 8, is characterized in that: in described step (1), the temperature of reflux is 60-100 ℃, and the time is 2-8h.
10. the preparation method of a kind of compound sulfurized nitrile rubber of organic-inorganic for sealing member as claimed in claim 8, is characterized in that: in described step (3), the condition of sulfuration is 150 ℃ * t 90* 10MPa.
CN201410142193.4A 2014-04-10 2014-04-10 Organic and inorganic composite vulcanized nitrile rubber for sealing element and preparation method of organic and inorganic composite vulcanized nitrile rubber Pending CN103937051A (en)

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PCT/CN2014/093077 WO2015154492A1 (en) 2014-04-10 2014-12-05 Organic-inorganic composite vulcanized nitrile rubber for sealing element and preparation method therefor

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