CN107936330A - A kind of preparation method of salt tolerant modified butadiene acrylonitrile rubber polyurethane resin vulcanizate sealing material - Google Patents
A kind of preparation method of salt tolerant modified butadiene acrylonitrile rubber polyurethane resin vulcanizate sealing material Download PDFInfo
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- CN107936330A CN107936330A CN201711324681.7A CN201711324681A CN107936330A CN 107936330 A CN107936330 A CN 107936330A CN 201711324681 A CN201711324681 A CN 201711324681A CN 107936330 A CN107936330 A CN 107936330A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L15/00—Compositions of rubber derivatives
- C08L15/005—Hydrogenated nitrile rubber
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08C—TREATMENT OR CHEMICAL MODIFICATION OF RUBBERS
- C08C19/00—Chemical modification of rubber
- C08C19/02—Hydrogenation
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Sealing Material Composition (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of preparation method of salt tolerant modified butadiene acrylonitrile rubber polyurethane resin vulcanizate sealing material, water and the molecular sieve of activation is added to carry out ball milling in lignin and calcium carbonate, with the NBR latex of hydrazine hydrate method hydrogenation modification, coupling agent is added to be modified with reactions such as initiators, wet process fusion blending adds compounded mix when being plasticated, add the auxiliary agents such as polyacrylic resin, solid softener to be kneaded, add the fully mixing sulfidization molding such as polyurethane macromolecular reacting resin powder and both obtain sealing material.After the modified NBR latex of the present invention, mixing vulcanization is carried out with polyurethane, compatibility is good, and the sealing material of preparation shows preferable salt tolerance and water imbibition, and tensile strength is high.
Description
Technical field
The invention belongs to field of functional materials, and in particular to a kind of salt tolerant modified butadiene acrylonitrile rubber-polyurethane resin vulcanizate
The preparation method of sealing material.
Background technology
Nitrile rubber has excellent oil resistant, heat-resisting and physical mechanical property, has become and prepares oil resistant rubber product
Standard elastomer.In recent years, the oil-resistant gasket seal made of nitrile rubber is more and more widely used.With polyurethane
The elastomeric material of preparation for composite has water imbibition, and hydrone, which enters in polyurethane resin network, makes polyurethane that there is swelling to make
With, and then the locomitivity of strand is improved, be conducive to the entrance and diffusion of hydrone, so as to improve water sucting rubber
Mechanical property, solves the problem of water-absorbing resin precipitation after immersion, improves the service life of material.
The content of the invention
The present invention provides a kind of preparation method of salt tolerant modified butadiene acrylonitrile rubber-polyurethane resin vulcanizate sealing material, this
After the modified NBR latex of invention, mixing vulcanization is carried out with polyurethane, compatibility is good, and the sealing material of preparation is shown preferably
Salt tolerance and water imbibition, tensile strength are high.
The present invention is achieved by the following technical solutions：
A kind of preparation method of salt tolerant modified butadiene acrylonitrile rubber-polyurethane resin vulcanizate sealing material, it is characterised in that including with
Lower step：
（1）The preparation of compounded mix
By 5-10 parts by weight lignin and 5-10 weight parts of calcium carbonate by putting into agate jar, add suitable quantity of water and be used as and divide
Powder, 1-5 parts by weight molecular sieves are put into high temperature furnace and carry out high-temperature heating activation, and compound fill out is milled to after being added to ball grinder
Material average grain diameter no longer changes, and isolates agate bead, obtained compounded mix is stand-by；
（2）Modified NBR latex
By 40-50 parts by weight NBR latex after 2-3 parts by weight hydrazine hydrates are added dropwise to while stirring, 10-20 parts by weight water is added,
Stirring 30-40 minute is up to after mixing, then is added dropwise to 2-10 part by weight of boric acid and hydrogen peroxide 1:1 mixture, is adjusted anti-
Temperature is answered to 45-55 DEG C, after being added dropwise, 0.5-5 parts by weight coupling agent A-151 is added, adds in torque rheometer,
After being mixed 10-15 minutes at 110-130 DEG C, add 1-2 parts by weight benzyltriphenylphosphonium chloride, reaction 1-2 it is small when after add
It is stand-by when 0.1-0.5 part by weight of catalyst and 2-10 parts by weight of bisphenol A, the reaction was continued 4-5 are small；
（3）It is kneaded modified butadiene acrylonitrile rubber and polyurethane resin
By step（2）The modified butadiene acrylonitrile rubber of gained carries out taking wet method to melt after plasticating thin logical 10-15 minutes on rubber mixing machine is driven
Melt blending technology and add step（1）Gained compounded mix, be kneaded 1-1.5 it is small when after, then sequentially add 5-15 parts by weight poly- third
Olefin(e) acid sodium resin, 1-3 parts by weight solids softening agent, 1-3 parts by weight accelerating agent, 1-3 parts by weight antioxidant, 10-15 parts by weight charcoals
It is black, it is quick to beat 3-5 triangle bag, addition 20-35 parts by weight of polyurethane macromolecular reactions toner, 1-2 parts by weight vulcanizing agent,
2-5 parts by weight assistant crosslinking agents are fully kneaded, and beat 5-10 all over triangle bags, adjust roll spacing, and extruding obtains rubber compound, it is thin it is logical under
Piece, it is stand-by；
（4）Sulfidization molding
By step（3）After gains are when room temperature placement 18-24 is small, rubber compound is molded using compression molding instrument and is vulcanized, shaping,
Trimming, storage both obtain salt tolerant modified butadiene acrylonitrile rubber-polyurethane resin vulcanizate sealing material.
The high temperature furnace is Muffle furnace.
The plasticating temperature is at 120-150 DEG C, rotating speed 20-35r/min.
The wet process fusion blending technology is uniformly to pour into mix with modified NBR latex after compounded mix is soaked to melt
Melt blending.
The melting temperature is 170-180 DEG C, and mixing time is 40-60 minutes.
The curing temperature is 100-160 DEG C, is vulcanized 8-10 minutes.
It is an advantage of the invention that：
Lignin and calcium carbonate are added water and the molecular sieve of activation to carry out ball milling by the present invention, with the butyronitrile of hydrazine hydrate method hydrogenation modification
Latex, adds coupling agent and is modified with reactions such as initiators, and wet process fusion blending addition compounded mix, adds when being plasticated
The auxiliary agents such as polyacrylic resin, solid softener are kneaded, and are added polyurethane macromolecular reacting resin powder etc. and are fully kneaded
Sulfidization molding both obtains sealing material.The addition of lignin and calcium carbonate ball milling can promote the scattered of calcium carbonate, reduce and reunite, ball
After mill enters molecular sieve pore passage inside, realize preferable load, weaken the intermolecular effect of nitrile rubber, hydrogenated with hydrazine hydrate method
Modified NBR latex is respectively provided with higher physical property at ambient and elevated temperatures, after nucleophilic is carried out on nitrile rubber strand
The phenolic hydroxyl group of substitution reaction, prepares branched polyphenol hydroxyl nitrile rubber, introduces phenyl ring, phenolic hydroxyl group and silicon oxygen bond, tensile strength and carries
Height, and compatibility is good, is kneaded chemical graft with polyurethane, forms graft crosslinking network structure, polyurethane resin and butyronitrile
Rubber compatibility is good, shows preferable salt tolerance and water imbibition.After the modified NBR latex of the present invention, mixed with polyurethane
Refining vulcanization, compatibility is good, and the sealing material of preparation shows preferable salt tolerance and water imbibition, and tensile strength is high.
Embodiment
A kind of preparation method of salt tolerant modified butadiene acrylonitrile rubber-polyurethane resin vulcanizate sealing material, it is characterised in that bag
Include following steps：
（1）The preparation of compounded mix
By 7 parts by weight lignin and 8 weight parts of calcium carbonate by putting into agate jar, suitable quantity of water is added as dispersant,
2 parts by weight molecular sieves are put into high temperature furnace and carry out high-temperature heating activation, is added to after ball grinder and is milled to compounded mix and is averaged
Particle diameter no longer changes, and isolates agate bead, obtained compounded mix, stand-by；
（2）Modified NBR latex
By 45 parts by weight NBR latexes after 2 parts by weight hydrazine hydrates are added dropwise to while stirring, 15 parts by weight water are added, stir 35 points
Clock is until after mixing, then is added dropwise to 5 part by weight of boric acid and hydrogen peroxide 1:1 mixture, adjusts reaction temperature to 40 DEG C, drop
After adding, 1 parts by weight coupling agent A-151 is added, is added in torque rheometer, after being mixed 15 minutes at 120 DEG C, adds 2
Parts by weight benzyltriphenylphosphonium chloride, when reaction 1.5 is small after add 0.2 part by weight of catalyst and 5 parts by weight of bisphenol A, continue anti-
Answer 4 it is small when, it is stand-by；
（3）It is kneaded modified butadiene acrylonitrile rubber and polyurethane resin
By step（2）The modified butadiene acrylonitrile rubber of gained carry out plasticating on rubber mixing machine is driven it is thin it is 15 minutes logical after take wet process fusion to be total to
Mixed technique adds step（1）Gained compounded mix, be kneaded 1 it is small when after, then sequentially add 5 parts by weight of polypropylene acid sodium resins, 2
Parts by weight solids softening agent, 2 parts by weight accelerating agents, 2 parts by weight antioxidants, 15 parts by weight of carbon black per, quickly make a call to 3 triangle bags, add
Enter 35 parts by weight of polyurethane macromolecular reaction toners, 1 parts by weight vulcanizing agent, 2 parts by weight assistant crosslinking agents to be fully kneaded,
8 times triangle bags are made a call to, adjust roll spacing, extruding obtains rubber compound, and thin logical bottom sheet is stand-by；
（4）Sulfidization molding
By step（3）After gains are when room temperature placement 24 is small, rubber compound is molded using compression molding instrument and is vulcanized, is molded, repaiies
Cut, be put in storage both salt tolerant modified butadiene acrylonitrile rubber-polyurethane resin vulcanizate sealing material.
The high temperature furnace is Muffle furnace.
The plasticating temperature is at 130 DEG C, rotating speed 20-35r/min.
The wet process fusion blending technology is uniformly to pour into mix with modified NBR latex after compounded mix is soaked to melt
Melt blending.
The melting temperature is 180 DEG C, and mixing time is 40 minutes.
The curing temperature is 140 DEG C, is vulcanized 8 minutes.
Claims (6)
- A kind of 1. preparation method of salt tolerant modified butadiene acrylonitrile rubber-polyurethane resin vulcanizate sealing material, it is characterised in that including Following steps：（1）The preparation of compounded mixBy 5-10 parts by weight lignin and 5-10 weight parts of calcium carbonate by putting into agate jar, add suitable quantity of water and be used as and divide Powder, 1-5 parts by weight molecular sieves are put into high temperature furnace and carry out high-temperature heating activation, and compound fill out is milled to after being added to ball grinder Material average grain diameter no longer changes, and isolates agate bead, obtained compounded mix is stand-by；（2）Modified NBR latexBy 40-50 parts by weight NBR latex after 2-3 parts by weight hydrazine hydrates are added dropwise to while stirring, 10-20 parts by weight water is added, Stirring 30-40 minute is up to after mixing, then is added dropwise to 2-10 part by weight of boric acid and hydrogen peroxide 1:1 mixture, is adjusted anti- Temperature is answered to 45-55 DEG C, after being added dropwise, 0.5-5 parts by weight coupling agent A-151 is added, adds in torque rheometer, After being mixed 10-15 minutes at 110-130 DEG C, add 1-2 parts by weight benzyltriphenylphosphonium chloride, reaction 1-2 it is small when after add It is stand-by when 0.1-0.5 part by weight of catalyst and 2-10 parts by weight of bisphenol A, the reaction was continued 4-5 are small；（3）It is kneaded modified butadiene acrylonitrile rubber and polyurethane resinBy step（2）The modified butadiene acrylonitrile rubber of gained carries out taking wet method to melt after plasticating thin logical 10-15 minutes on rubber mixing machine is driven Melt blending technology and add step（1）Gained compounded mix, be kneaded 1-1.5 it is small when after, then sequentially add 5-15 parts by weight poly- third Olefin(e) acid sodium resin, 1-3 parts by weight solids softening agent, 1-3 parts by weight accelerating agent, 1-3 parts by weight antioxidant, 10-15 parts by weight charcoals It is black, it is quick to beat 3-5 triangle bag, addition 20-35 parts by weight of polyurethane macromolecular reactions toner, 1-2 parts by weight vulcanizing agent, 2-5 parts by weight assistant crosslinking agents are fully kneaded, and beat 5-10 all over triangle bags, adjust roll spacing, and extruding obtains rubber compound, it is thin it is logical under Piece, it is stand-by；（4）Sulfidization moldingBy step（3）After gains are when room temperature placement 18-24 is small, rubber compound is molded using compression molding instrument and is vulcanized, shaping, Trimming, storage both obtain salt tolerant modified butadiene acrylonitrile rubber-polyurethane resin vulcanizate sealing material.
- 2. according to a kind of preparation method of salt tolerant modified butadiene acrylonitrile rubber of claim 1-polyurethane resin vulcanizate sealing material, its It is characterized in that, the high temperature furnace is Muffle furnace.
- 3. according to a kind of preparation method of salt tolerant modified butadiene acrylonitrile rubber of claim 1-polyurethane resin vulcanizate sealing material, its It is characterized in that, the plasticating temperature is at 120-150 DEG C, rotating speed 20-35r/min.
- 4. according to a kind of preparation method of salt tolerant modified butadiene acrylonitrile rubber of claim 1-polyurethane resin vulcanizate sealing material, its It is characterized in that, the wet process fusion blending technology is uniformly to pour into mix with modified NBR latex after compounded mix is soaked to melt Melt blending.
- 5. according to a kind of preparation method of salt tolerant modified butadiene acrylonitrile rubber of claim 1-polyurethane resin vulcanizate sealing material, its It is characterized in that, the melting temperature is 170-180 DEG C, and mixing time is 40-60 minutes.
- 6. according to a kind of preparation method of salt tolerant modified butadiene acrylonitrile rubber of claim 1-polyurethane resin vulcanizate sealing material, its It is characterized in that, the curing temperature is 100-160 DEG C, is vulcanized 8-10 minutes.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711324681.7A CN107936330A (en) | 2017-12-13 | 2017-12-13 | A kind of preparation method of salt tolerant modified butadiene acrylonitrile rubber polyurethane resin vulcanizate sealing material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711324681.7A CN107936330A (en) | 2017-12-13 | 2017-12-13 | A kind of preparation method of salt tolerant modified butadiene acrylonitrile rubber polyurethane resin vulcanizate sealing material |
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| CN107936330A true CN107936330A (en) | 2018-04-20 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102532634A (en) * | 2010-12-09 | 2012-07-04 | 江山圆正化工科技有限公司 | Preparation method of high-temperature-resisting oil-swelling sealing material |
| CN102617901A (en) * | 2012-03-22 | 2012-08-01 | 北京化工大学 | Application of hydrogenated nitrile latex |
| CN104877199A (en) * | 2015-06-29 | 2015-09-02 | 湖南师范大学 | Method for preparing rubber masterbatch by calcium carbonate dispersed by lignin |
| CN105968594A (en) * | 2016-06-23 | 2016-09-28 | 安徽荣达阀门有限公司 | Weather-resistant water-swelling waterproof rubber sealing material and preparation method thereof |
-
2017
- 2017-12-13 CN CN201711324681.7A patent/CN107936330A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102532634A (en) * | 2010-12-09 | 2012-07-04 | 江山圆正化工科技有限公司 | Preparation method of high-temperature-resisting oil-swelling sealing material |
| CN102617901A (en) * | 2012-03-22 | 2012-08-01 | 北京化工大学 | Application of hydrogenated nitrile latex |
| CN104877199A (en) * | 2015-06-29 | 2015-09-02 | 湖南师范大学 | Method for preparing rubber masterbatch by calcium carbonate dispersed by lignin |
| CN105968594A (en) * | 2016-06-23 | 2016-09-28 | 安徽荣达阀门有限公司 | Weather-resistant water-swelling waterproof rubber sealing material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 胡晓云 等: "耐盐型遇水膨胀橡胶的制备与性能", 《弹性体》 * |
| 胡晓云: "耐盐型遇水膨胀橡胶的制备与性能", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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