CN106519524A - High cold-resistant acrylate rubber material and preparation method and application thereof - Google Patents
High cold-resistant acrylate rubber material and preparation method and application thereof Download PDFInfo
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- CN106519524A CN106519524A CN201611018088.5A CN201611018088A CN106519524A CN 106519524 A CN106519524 A CN 106519524A CN 201611018088 A CN201611018088 A CN 201611018088A CN 106519524 A CN106519524 A CN 106519524A
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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
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
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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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a high cold-resistant acrylate rubber material and a preparation method and application thereof. The high cold-resistant acrylate adhesive material is prepared from 80 to 88 parts by weight of acrylate rubber, 10 to 16 parts by weight of nitrile rubber, 2 to 4 parts by weight of silicone rubber, 18 to 22 parts by weight of white carbon black, 1.5 to 1.9 parts by weight of stearic acid, 1.1 to 1.5 parts by weight of a plasticizer TOTM, 1.6 to 2.1 parts by weight of octyl silane bonded silica gel, 14 to 17 parts by weight of silicon micro-powder, 1.0 to 1.5 parts by weight of an antiager 445, 1.8 to 2.4 parts by weight of an antiager RDA, 6.5 to 7.3 parts by weight of N, N'-bis(cinnamal-1, 6-hexamethylenediamine), 2.2 to 2.6 parts by weight of an accelerator BG, and 0.7 to 1.0 part by weight of an accelerator ZDC. Through combination of nitrile rubber, silicone rubber and acrylate rubber, the high cold-resistant acrylate rubber material meets requirements on oil, heat, cold and aging resistance of an automotive oil return pipe.
Description
Technical field
The present invention relates to new material technology field, specifically a kind of high cold-resistant acrylate sizing material and preparation method thereof and should
With.
Background technology
The effect of automobile oil return pipe is to make unnecessary oil return to fuel tank, can play the pressure for mediating gasoline, can also subtract
Few oil consumption；In fuel oil oil pump feed to engine, after forming certain pressure except normal supply fuel nozzle oil spout, remaining fuel oil
Fuel tank is sent back to by return line, also has certainly the unnecessary gasoline vapor that canister is collected fuel tank to be returned to also by oil return pipe.
Therefore, when selecting the material of automobile oil return pipe, it is necessary to be provided simultaneously with excellent oil resistivity and heat-resisting quantity, in addition, also need
Possess certain lower temperature resistance, resistance to ag(e)ing.
ACM (hereinafter referred to as ACM) be with acrylate as main monomer Jing copolymerization obtained by elastomer, its master
Chain is saturated carbon chains, and side base is polar ester groups.Due to special construction give its it is many excellent the characteristics of, such as：Heat-resisting, ageing-resistant,
Oil resistant, resistance to ozone, uvioresistant etc., mechanical property and processing characteristics are better than fluorubber and silicon rubber, its heat-resisting, resistance to ag(e)ing and
Oil resistivity is better than nitrile rubber.ACM is widely used in various high temperature, resistance to oil environment, becomes auto industry in recent years and focuses on
A kind of encapsulant that exploitation is promoted, particularly for the high temperature resistant oil sealing of automobile, bent axle, valve rod, cylinder liner, hydraulic oil pipeline
Deng.However, ACM also has the disadvantages that：Lower temperature resistance is poor, mechanical performance is poor, moisture resistivity, chemical-resistant resistance
Property is poor.Its poor lower temperature resistance, certainly will limit which in terms of higher automobile oil return pipe is required to temperature tolerance, oil resistivity
Using.
The content of the invention
It is an object of the invention to provide a kind of cold-resistant acrylate sizing material of height suitable for automobile oil return pipe and its preparation
Method and application.
For achieving the above object, the present invention provides following technical scheme：
A kind of high cold-resistant acrylate sizing material, in parts by weight, is made up of following raw material：ACM 80～88
Part, 10～16 parts of nitrile rubber, 2～4 parts of silicon rubber, 18～22 parts of white carbon, 1.5～1.9 parts of stearic acid, plasticizer TOTM
1.1～1.5 parts, 1.6～2.1 parts of octyl silane group silica gel, 14～17 parts of silicon powder, 445 1.0～1.5 parts of age resistor,
1.8～2.4 parts of anti-aging agent RD A, N, 6.5～7.3 parts of N'- bis- (cinnamylidene -1,6- hexamethylene diamines), accelerant B G2.2～2.6
Part, 0.7～1.0 part of accelerator ZDC.
As further scheme of the invention：In parts by weight, it is made up of following raw material：ACM 84～86
Part, 12～14 parts of nitrile rubber, 2～3 parts of silicon rubber, 19～21 parts of white carbon, 1.7～1.9 parts of stearic acid, plasticizer TOTM
1.2～1.4 parts, 1.8～2.0 parts of octyl silane group silica gel, 15～16 parts of silicon powder, 445 1.2～1.3 parts of age resistor,
2.0～2.2 parts of anti-aging agent RD A, N, 6.7～7.0 parts of N'- bis- (cinnamylidene -1,6- hexamethylene diamines), accelerant B G2.3～2.5
Part, 0.8～0.9 part of accelerator ZDC.
As further scheme of the invention：In parts by weight, it is made up of following raw material：85 parts of ACM,
13 parts of nitrile rubber, 2.5 parts of silicon rubber, 20 parts of white carbon, 1.8 parts of stearic acid, 1.3 parts of plasticizer TOTM, octane base silane key
Close 1.9 parts of silica gel, 15 parts of silicon powder, 445 1.2 parts of age resistor, 2.1 parts of anti-aging agent RD A, N, bis- (cinnamylidene -1,6- of N'-
Hexamethylene diamine) 6.8 parts, 2.4 parts of accelerant B G, 0.85 part of accelerator ZDC.
The preparation method of the cold-resistant acrylate sizing material of described height, comprises the following steps：
(1) white carbon, octyl silane group silica gel, silicon powder are preheated to into 150～158 DEG C, by stearic acid, plasticizer
TOTM, age resistor 445, anti-aging agent RD A are preheated to 155～162 DEG C, standby；
(2) in proportion by ACM, nitrile rubber, silicon rubber mixing, it is 450～500W, micro- in microwave power
Wave frequency rate, obtains first compound to carry out 2～3min of heating using microwave under conditions of 6～8GHz；
(3) then in proportion the raw material of preheating in step (1) is poured in the first compound of step (2), is kneaded,
Obtain elastomeric compound；
(4) N, N'- bis- (cinnamylidene -1,6- hexamethylene diamines), accelerator are added in proportion toward the elastomeric compound of step (3)
BG, accelerator ZDC, temperature be 158～165 DEG C, pressure be 18～20MPa under conditions of carry out 3～5min of sulfuration, it is naturally cold
But, the cold-resistant acrylate sizing material of described height is obtained.
Application of the cold-resistant acrylate sizing material of described height in terms of automobile oil return pipe is prepared.
Compared with prior art, the invention has the beneficial effects as follows：The present invention selects nitrile rubber, silicon rubber and acrylate
Rubber compounding use, using octyl silane group silica gel and the mixed filler of silicon powder, using age resistor 445 with it is anti-
The mixture of old agent RDA as age resistor, on the basis of the heat-resisting of ACM, oil resistant, ageing-resistant performance is not changed,
Its low temperature cold tolerance is improved.Compared with traditional ACM, cold resistance is significantly improved, fragility temperature
Degree may be up to -59 DEG C without fracture and oil resistant, and ageing-resistant performance is still good, compensate for ACM in use not
Foot, and the performance such as the oil resistant of rubber, oil resistant, ageing-resistant substantially do not change, meets automobile oil return pipe oil resistant, heat-resisting, resistance to
The cold, requirement of ageing-resistant performance.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the invention, rather than the embodiment of whole.Based in the present invention
Embodiment, the every other embodiment obtained under the premise of creative work is not made by those of ordinary skill in the art, all
Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of high cold-resistant acrylate sizing material in parts by weight, is made up of following raw material：Third
80 parts of olefin(e) acid ester rubber, 16 parts of nitrile rubber, 2 parts of silicon rubber, 22 parts of white carbon, 1.5 parts of stearic acid, plasticizer TOTM1.5 parts,
1.6 parts of octyl silane group silica gel, 17 parts of silicon powder, 445 1.0 parts of age resistor, 2.4 parts of anti-aging agent RD A, N, N'- bis- are (sub-
Cinnamyl -1,6- hexamethylene diamines) 6.5 parts, 2.6 parts of accelerant B G, 0.7 part of accelerator ZDC.
The preparation method of the cold-resistant acrylate sizing material of described height, comprises the following steps：
(1) white carbon, octyl silane group silica gel, silicon powder are preheated to into 150 DEG C, by stearic acid, plasticizer TOTM,
Age resistor 445, anti-aging agent RD A are preheated to 155 DEG C, standby；
(2) in proportion by ACM, nitrile rubber, silicon rubber mixing, it is 450W, microwave frequency in microwave power
For heating using microwave 3min is carried out under conditions of 6GHz, first compound is obtained；
(3) then in proportion the raw material of preheating in step (1) is poured in the first compound of step (2), is kneaded,
Obtain elastomeric compound；
(4) N, N'- bis- (cinnamylidene -1,6- hexamethylene diamines), accelerator are added in proportion toward the elastomeric compound of step (3)
BG, accelerator ZDC, temperature be 158 DEG C, pressure be 18MPa under conditions of carry out sulfuration 5min, natural cooling is obtained described
The cold-resistant acrylate sizing material of height.
Embodiment 2
In the embodiment of the present invention, a kind of high cold-resistant acrylate sizing material in parts by weight, is made up of following raw material：Third
88 parts of olefin(e) acid ester rubber, 10 parts of nitrile rubber, 4 parts of silicon rubber, 18 parts of white carbon, 1.9 parts of stearic acid, plasticizer TOTM1.1 parts,
2.1 parts of octyl silane group silica gel, 14 parts of silicon powder, 445 1.5 parts of age resistor, 1.8 parts of anti-aging agent RD A, N, N'- bis- are (sub-
Cinnamyl -1,6- hexamethylene diamines) 7.3 parts, 2.2 parts of accelerant B G, 1.0 parts of accelerator ZDC.
The preparation method of the cold-resistant acrylate sizing material of described height, comprises the following steps：
(1) white carbon, octyl silane group silica gel, silicon powder are preheated to into 158 DEG C, by stearic acid, plasticizer TOTM,
Age resistor 445, anti-aging agent RD A are preheated to 155 DEG C, standby；
(2) in proportion by ACM, nitrile rubber, silicon rubber mixing, it is 500W, microwave frequency in microwave power
For heating using microwave 2min is carried out under conditions of 8GHz, first compound is obtained；
(3) then in proportion the raw material of preheating in step (1) is poured in the first compound of step (2), is kneaded,
Obtain elastomeric compound；
(4) N, N'- bis- (cinnamylidene -1,6- hexamethylene diamines), accelerator are added in proportion toward the elastomeric compound of step (3)
BG, accelerator ZDC, temperature be 165 DEG C, pressure be 20MPa under conditions of carry out sulfuration 3min, natural cooling is obtained described
The cold-resistant acrylate sizing material of height.
Embodiment 3
In the embodiment of the present invention, a kind of high cold-resistant acrylate sizing material in parts by weight, is made up of following raw material：Third
84 parts of olefin(e) acid ester rubber, 14 parts of nitrile rubber, 2 parts of silicon rubber, 21 parts of white carbon, 1.7 parts of stearic acid, plasticizer TOTM1.4 parts,
1.8 parts of octyl silane group silica gel, 16 parts of silicon powder, 445 1.2 parts of age resistor, 2.2 parts of anti-aging agent RD A, N, N'- bis- are (sub-
Cinnamyl -1,6- hexamethylene diamines) 6.7 parts, 2.5 parts of accelerant B G, 0.8 part of accelerator ZDC.
The preparation method of the cold-resistant acrylate sizing material of described height, it is same as Example 1.
Embodiment 4
In the embodiment of the present invention, a kind of high cold-resistant acrylate sizing material in parts by weight, is made up of following raw material：Third
86 parts of olefin(e) acid ester rubber, 12 parts of nitrile rubber, 3 parts of silicon rubber, 19 parts of white carbon, 1.9 parts of stearic acid, plasticizer TOTM1.2 parts,
2.0 parts of octyl silane group silica gel, 15 parts of silicon powder, 445 1.3 parts of age resistor, 2.0 parts of anti-aging agent RD A, N, N'- bis- are (sub-
Cinnamyl -1,6- hexamethylene diamines) 7.0 parts, 2.3 parts of accelerant B G, 0.9 part of accelerator ZDC.
The preparation method of the cold-resistant acrylate sizing material of described height, it is same as Example 2.
Embodiment 5
In the embodiment of the present invention, a kind of high cold-resistant acrylate sizing material in parts by weight, is made up of following raw material：Third
85 parts of olefin(e) acid ester rubber, 13 parts of nitrile rubber, 2.5 parts of silicon rubber, 20 parts of white carbon, 1.8 parts of stearic acid, plasticizer TOTM1.3
Part, 1.9 parts of octyl silane group silica gel, 15 parts of silicon powder, 445 1.2 parts of age resistor, 2.1 parts of anti-aging agent RD A, N, N'- bis-
6.8 parts of (cinnamylidene -1,6- hexamethylene diamines), 2.4 parts of accelerant B G, 0.85 part of accelerator ZDC.
The preparation method of the cold-resistant acrylate sizing material of described height, comprises the following steps：
(1) white carbon, octyl silane group silica gel, silicon powder are preheated to into 155 DEG C, by stearic acid, plasticizer TOTM,
Age resistor 445, anti-aging agent RD A are preheated to 158 DEG C, standby；
(2) in proportion by ACM, nitrile rubber, silicon rubber mixing, it is 480W, microwave frequency in microwave power
For heating using microwave 2.5min is carried out under conditions of 7GHz, first compound is obtained；
(3) then in proportion the raw material of preheating in step (1) is poured in the first compound of step (2), is kneaded,
Obtain elastomeric compound；
(4) N, N'- bis- (cinnamylidene -1,6- hexamethylene diamines), accelerator are added in proportion toward the elastomeric compound of step (3)
BG, accelerator ZDC, temperature be 162 DEG C, pressure be 19MPa under conditions of carry out sulfuration 4min, natural cooling is obtained described
The cold-resistant acrylate sizing material of height.
Comparative example 1
On the basis of the formula of embodiment 5, octyl silane group silica gel is replaced with into silicon powder, remaining and embodiment 5
It is identical.
Comparative example 2
On the basis of the formula of embodiment 5, age resistor ZDC is replaced with into age resistor BG, remaining and 5 complete phase of embodiment
Together.
Comparative example 3
On the basis of the formula of embodiment 5, nitrile rubber is replaced with into silicon rubber, remaining is identical with embodiment 5.
Comparative example 4
On the basis of the formula of embodiment 5, silicon rubber is replaced with into nitrile rubber, remaining is identical with embodiment 5.
Test the mechanical performance of sizing material obtained in each example, heat resistance, cold resistance, resistance to machine oil, oil resistant (IRM 903) property and
Ozone resistance.Test result is as shown in table 1～4.
The mechanical performance of sizing material obtained in 1 each example of table
The heat resistance and cold resistance of sizing material obtained in 2 each example of table
The resistance to machine oil of sizing material obtained in 3 each example of table
The oil resistivity and ozone resistance of sizing material obtained in 4 each example of table
From table 1～4：Compared with control group, sizing material obtained in embodiment 1～5 has preferable mechanical performance, heat-resisting
Property, cold resistance, resistance to machine oil, oil resistivity and ozone resistance；Wherein table 1 illustrates the present invention from nitrile rubber, silicon rubber and third
Olefin(e) acid ester rubber compounding use, and using octyl silane group silica gel and the mixed filler of silicon powder so that sizing material
With preferable mechanical performance, table 2, table 3 and table 4 illustrate that the present invention is multiple from nitrile rubber, silicon rubber and ACM
With use, with preferable heat resistance, cold resistance and oil resistivity, additionally, the present invention can be drawn using age resistor 445 by table 4
With the mixture of anti-aging agent RD A as age resistor, with preferable ozone resistance.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of spirit or essential attributes without departing substantially from the present invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit is required rather than described above is limited, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical scheme in each embodiment can also Jing it is appropriately combined, form those skilled in the art
Understandable other embodiment.
Claims (5)
1. a kind of high cold-resistant acrylate sizing material, it is characterised in that in parts by weight, be made up of following raw material：Acrylate
80～88 parts of rubber, 10～16 parts of nitrile rubber, 2～4 parts of silicon rubber, 18～22 parts of white carbon, 1.5～1.9 parts of stearic acid, increasing
1.1～1.5 parts of modeling agent TOTM, 1.6～2.1 parts of octyl silane group silica gel, 14～17 parts of silicon powder, age resistor 445 1.0
～1.5 parts, 1.8～2.4 parts of anti-aging agent RD A, N, 6.5～7.3 parts of N'- bis- (cinnamylidene -1,6- hexamethylene diamines), accelerant B G
2.2～2.6 parts, 0.7～1.0 part of accelerator ZDC.
2. high cold-resistant acrylate sizing material according to claim 1, it is characterised in that in parts by weight, by following original
Material composition：84～86 parts of ACM, 12～14 parts of nitrile rubber, 2～3 parts of silicon rubber, 19～21 parts of white carbon, tristearin
1.7～1.9 parts of acid, 1.2～1.4 parts of plasticizer TOTM, 1.8～2.0 parts of octyl silane group silica gel, silicon powder 15～16
Part, 445 1.2～1.3 parts of age resistor, 2.0～2.2 parts of anti-aging agent RD A, N, bis- (cinnamylidene -1,6- hexamethylene diamines) 6.7 of N'-
～7.0 parts, 2.3～2.5 parts of accelerant B G, 0.8～0.9 part of accelerator ZDC.
3. high cold-resistant acrylate sizing material according to claim 2, it is characterised in that in parts by weight, by following original
Material composition：85 parts of ACM, 13 parts of nitrile rubber, 2.5 parts of silicon rubber, 20 parts of white carbon, 1.8 parts of stearic acid, plasticising
1.3 parts of agent TOTM, 1.9 parts of octyl silane group silica gel, 15 parts of silicon powder, 445 1.2 parts of age resistor, anti-aging agent RD A 2.1
Part, N, 6.8 parts of N'- bis- (cinnamylidene -1,6- hexamethylene diamines), 2.4 parts of accelerant B G, 0.85 part of accelerator ZDC.
4. the preparation method of the cold-resistant acrylate sizing material of height according to claims 1 to 3 is arbitrary, it is characterised in that include
Following steps：
(1) white carbon, octyl silane group silica gel, silicon powder are preheated to into 150～158 DEG C, by stearic acid, plasticizer
TOTM, age resistor 445, anti-aging agent RD A are preheated to 155～162 DEG C, standby；
(2) in proportion by ACM, nitrile rubber, silicon rubber mixing, it is 450～500W, Microwave Frequency in microwave power
Rate obtains first compound to carry out 2～3min of heating using microwave under conditions of 6～8GHz；
(3) then in proportion the raw material of preheating in step (1) is poured in the first compound of step (2), is kneaded, obtained
Elastomeric compound；
(4) add N in proportion toward the elastomeric compound of step (3), N'- bis- (cinnamylidene -1,6- hexamethylene diamines), accelerant B G, promote
Enter agent ZDC, temperature be 158～165 DEG C, pressure be 18～20MPa under conditions of carry out 3～5min of sulfuration, natural cooling, system
Obtain the cold-resistant acrylate sizing material of described height.
5. the application according to the cold-resistant acrylate sizing material of the arbitrary described height of claims 1 to 3 in terms of automobile oil return pipe is prepared.
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| CN201611018088.5A CN106519524A (en) | 2016-11-18 | 2016-11-18 | High cold-resistant acrylate rubber material and preparation method and application thereof |
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| CN201611018088.5A CN106519524A (en) | 2016-11-18 | 2016-11-18 | High cold-resistant acrylate rubber material and preparation method and application thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102977532A (en) * | 2012-11-27 | 2013-03-20 | 天津鹏翎胶管股份有限公司 | Acrylate rubber composition |
| CN105400015A (en) * | 2015-12-08 | 2016-03-16 | 黄涌芮 | High temperature resistance rubber and preparation method thereof |
-
2016
- 2016-11-18 CN CN201611018088.5A patent/CN106519524A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102977532A (en) * | 2012-11-27 | 2013-03-20 | 天津鹏翎胶管股份有限公司 | Acrylate rubber composition |
| CN105400015A (en) * | 2015-12-08 | 2016-03-16 | 黄涌芮 | High temperature resistance rubber and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 翁国文 等: "《橡胶技术问答》", 31 July 2010, 化学工业出版社 * |
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Application publication date: 20170322 |