CN108456344A - A kind of butadiene rubber/oligomer ester masterbatch and preparation method thereof - Google Patents
A kind of butadiene rubber/oligomer ester masterbatch and preparation method thereof Download PDFInfo
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- CN108456344A CN108456344A CN201810151045.7A CN201810151045A CN108456344A CN 108456344 A CN108456344 A CN 108456344A CN 201810151045 A CN201810151045 A CN 201810151045A CN 108456344 A CN108456344 A CN 108456344A
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- butadiene rubber
- oligomer ester
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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
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
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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
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
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Abstract
A kind of butadiene rubber/oligomer ester masterbatch of present invention offer and preparation method thereof.Using pre-dispersion, oligomer ester is blended in advance with butadiene rubber, is added quantitative and with accelerating agent and filler, mixing is squeezed out, is granulated, and obtains butadiene rubber/oligomer ester masterbatch.The masterbatch is convenient for preservation, transport and weighs；Compared with being directly added into oligomer ester, masterbatch can effectively avoid the problem that roll banding, mixing time in post-production are grown, and improve the utilization rate of oligomer ester, the performance of butadiene rubber product is made to be further improved.It the method can be widely used in all kinds of rubber oils compounding agent masterbatch, especially suitable for high-performance, multi-functional oligomer ester masterbatch.
Description
Technical field
The invention belongs to rubber technical field of composite preparation, especially have high-performance butadiene rubber/oligomer ester
Masterbatch and its application field.
Background technology
Oligomer ester is a kind of oils compounding agent in rubber product.But there are problems during the addition process in oligomer ester,
For example, the weighing and charging of thick oligomer ester are all relatively difficult, wall can be glued in container, metering is susceptible to error；Refining glue
The addition at initial stage, oligomer ester causes rubber to skid on rubber mixing equipment, is unfavorable for refining glue；Refining glue later stage, oligomer ester can lead to glue
Expect serious roll banding, mixing time is caused to extend, reduces production efficiency.Therefore, how oils oligomer ester is preferably added to rubber
In glue, processing problems are avoided, while the maximum function of oligomer ester can be played, is one of the hot issue in current rubber industry.
If the oligomer ester of high concentration is blended by the technology of premix with rubber, it is prepared into the masterbatch of high-content, if can
To solve the problems, such as this.Answer is negative, this is because oils compounding agent can seriously reduce the viscosity of rubber, therefore it is neat when preparing
When polyester masterbatch, the high concentration oils oligomer ester of addition can cause the viscosity of masterbatch very low, bring more intractable
Mixing problem.Therefore, at present for the report of the premix technology of oils compounding agent big similar to this dosage of oligomer ester, more than function
Road is considerably less.
Invention content
The purpose of the present invention is to provide a kind of butadiene rubber/oligomer ester masterbatch and preparation methods.
A kind of butadiene rubber/oligomer ester masterbatch, it is characterised in that including following components：100 mass parts of butadiene rubber,
Oligomer ester 100-200 mass parts, accelerating agent 2-4 mass parts, anti-aging agent 2-4 mass parts, filler 5-15 mass parts, peroxidating two
Isopropylbenzene 0.5-1 mass parts, chromium stearate 2-5 mass parts.
The accelerating agent is the 2 of TMTD and CZ:1 mixture.
The filler is vapor phase method SiO2With the one or two of N550, anti-aging agent is the one of antioxidant A W or ODA
Kind or two kinds.
A kind of preparation method of butadiene rubber/oligomer ester masterbatch, it is characterised in that comprise the steps of：
Rubber is put into open mill, adjustment roll spacing is 10mm, and anti-aging agent and chromium stearate is added, and is kneaded 2-5min, and addition is filled out
Material is kneaded 2-4min, and adjustment roller temperature is added oligomer ester to 5 DEG C, is kneaded 5-7min, and accelerating agent and cumyl peroxide is added,
It is kneaded 5-8min, roll spacing is adjusted to 1mm by adjustment roller temperature to 80 DEG C, the thin logical 10-20min of sizing material, adjusts roller temperature to 5 DEG C, under
Piece is cut, and puts into extruder, is squeezed out pelletizing and is obtained butadiene rubber/oligomer ester masterbatch.
Compared with prior art, the present invention its remarkable advantage is：
（1）Oligomer ester is blended in advance with butadiene rubber, using the unsaturated double-bond in oligomer ester, is promoted by the way that quantitative blending is added
Into agent and cumyl peroxide, the partial dynamic vulcanization of masterbatch is realized on a mill, makes part oligomer ester and suitable fourth rubber
Glue crosslinks, and forms microgel and solves the problems, such as high oil plant masterbatch low viscosity roll banding to improve the viscosity of sizing material,
And it can ensure the normal flow processability energy of sizing material in subsequent high temperature processing, obtained oligomer ester masterbatch is convenient for making
Grain is preserved, transports and is weighed, and is effectively improved the utilization rate of oligomer ester, is avoided being stained with roller problem；
（2）When masterbatch is applied to using butadiene rubber as in the rubber product of matrix, the microgel in masterbatch with it is unreacted
Oligomer ester continues to participate in the vulcanization reaction of rubber matrix, on the one hand, microgel reacts with rubber matrix, formation and rubber
There is the microgel reinforcing agent of chemical bonding in matrix body, further reinforcement is realized to rubber matrix, on the other hand, unreacted neat
Polyester participates in the vulcanization reaction of rubber matrix, and cross-linked network structure is formed in rubber matrix, vulcanizes shape with rubber matrix itself
At cross-linked network formed interpenetrating, further improve the performance of rubber product.
Description of the drawings
Fig. 1 is the preparation process of butadiene rubber/oligomer ester masterbatch.
Specific implementation mode
Present invention is further described in detail below in conjunction with the accompanying drawings.
A kind of butadiene rubber/oligomer ester masterbatch, it is characterised in that including following components：100 mass parts of butadiene rubber,
Oligomer ester 100-200 mass parts, accelerating agent 2-4 mass parts, anti-aging agent 2-4 mass parts, filler 5-15 mass parts, peroxidating two
Isopropylbenzene 0.5-1 mass parts, chromium stearate 2-5 mass parts, the accelerating agent are the 2 of TMTD and CZ:1 mixture, filler
For vapor phase method SiO2With the one or two of N550, anti-aging agent is the one or two of antioxidant A W or ODA.
A kind of preparation method of butadiene rubber/oligomer ester masterbatch, it is characterised in that comprise the steps of：
Rubber is put into open mill, adjustment roll spacing is 10mm, and anti-aging agent and chromium stearate is added, and is kneaded 2-5min, and addition is filled out
Material is kneaded 2-4min, and adjustment roller temperature is added oligomer ester to 5 DEG C, is kneaded 5-7min, and accelerating agent and cumyl peroxide is added,
It is kneaded 5-8min, roll spacing is adjusted to 1mm by adjustment roller temperature to 80 DEG C, the thin logical 10-20min of sizing material, adjusts roller temperature to 5 DEG C, under
Piece is cut, and puts into extruder, is squeezed out pelletizing and is obtained butadiene rubber/oligomer ester masterbatch.
Obtained masterbatch is applied in butadiene rubber base rubber product, wherein butadiene rubber base rubber product is basic
Formula is：
Table 1
| Raw material title | Mass parts | Raw material title | Mass parts |
| Butadiene rubber | 100 | Vulcanization accelerator TMTD | 1.5 |
| Zinc oxide | 3 | Sulfur | 1.5 |
| Stearic acid | 2 | HAF | 60 |
| Accelerator NS | 0.9 | Oligomer ester | 15 |
, and tested as follows the butadiene rubber base in production of articles is rubber mixed.
（1）Mixing time
After all compounding agents are added to rubber mixing machine, every 5min by sizing material slice, film is hung, from the upper, middle and lower of film
One piece of glue is respectively taken, its time of scorch and sulfurizing time are tested, when the time of scorch of three pieces of glue and the deviation of sulfurizing time exist
Within 5%, you can think that rubber compounding is uniform, record from be fed to rubber compounding with the required time, when being denoted as mixing
Between.Mixing time is shorter, and sizing material skids, roll banding degree is smaller, and production efficiency is higher.
（2）Mooney viscosity
According to GB/T 1232.1-2000, the MV2-2000 intelligent computer types produced using Wuxi Li Garden Chemical Equipment Co., Ltd.
Mooney viscosity instrument tests rubber compound sample, measures Mooney viscosity.
Obtained rubber compound is vulcanized into 30min at 160 DEG C, obtains corresponding vulcanization of rubber glue, and carry out to vulcanizate
Following test event.
（3）Hardness test
According to GB/T531-1999, the LX-A rubber hardness testers produced from nine measurer Co., Ltds using Shanghai are to vulcanizate
The hardness of sample is tested.
（4）Tensile property
Thought carefully in Shenzhen according to GB/T528-2009 standards and is tested on CMT4254 electronic universal puller systems, tensile speed
500mm/min records the tensile strength of vulcanizate sample, and the sample with bigger tensile strength is better.
（5）Tear resistance
Tear resistance test is thought carefully according to GB/T529-2008 standards in Shenzhen is surveyed on CMT4254 electronic universal puller systems
Examination, speed 500mm/min record the tearing strength of vulcanizate sample, and the sample with bigger tearing strength is better.
（6）Wear hardness
Wear hardness tests wear-resisting property according to GB 1689-2014, in Akron abrasion machine, calculates the abrasion of vulcanizate sample
Volume, the sample with smaller wear volume are better.
（7）Heat stability testing
Vulcanizate sample is surveyed using the microcomputer differential thermal analyzer of the DTG-60/60H types of Japanese SHIMADZU companies production
Examination.Test temperature is 40 ~ 600 DEG C, and heating rate is 10 DEG C/min, and air atmosphere, gas flow rate is 20 mL/min, and record loses
The weightless temperature T that weight is 5%5, have the thermal stability of the vulcanizate sample of bigger weightless temperature better.
Below by embodiment and comparative example, the invention will be further described.
Embodiment 1
100 parts of butadiene rubber rubber are put into open mill, adjustment roll spacing is 10mm, and 2 parts of antioxidant A W and 2 parts of stearic acid are added
Chromium is kneaded 2min, and 5 parts of vapor phase method SiO are added2, it is kneaded 2min, adjustment roller temperature is added 100 parts of oligomer esters to 5 DEG C, is kneaded
2 parts of accelerating agents and 0.5 part of cumyl peroxide is added in 5min, is kneaded 5min, and roll spacing is adjusted to by adjustment roller temperature to 80 DEG C
1mm, the thin logical 20min of sizing material, to 5 DEG C, bottom sheet is cut adjustment roller temperature, puts into extruder, is squeezed out pelletizing and is obtained along fourth rubber
Glue/oligomer ester masterbatch.Preparation process is as shown in Figure 1.According to the dosage of oligomer ester in the butadiene rubber basic components of table 1, knot
The content of oligomer ester in masterbatch is closed, the required dosage of masterbatch is calculated, butadiene rubber base vulcanization of rubber glue is prepared, is mixed
Refining glue and the detailed performance of vulcanizate such as table 2.
Embodiment 2
100 parts of butadiene rubber rubber are put into open mill, adjustment roll spacing is 10mm, and 4 parts of anti-aging agent ODA and 5 parts of tristearin are added
Sour chromium is kneaded 5min, and 15 parts of N550 are added, and is kneaded 5min, and adjustment roller temperature is added 200 parts of oligomer esters to 5 DEG C, is kneaded 7min, adds
Enter 4 parts of accelerating agents and 1 part of cumyl peroxide, be kneaded 8min, roll spacing is adjusted to 1mm, sizing material by adjustment roller temperature to 80 DEG C
Thin logical 10min, to 5 DEG C, bottom sheet is cut adjustment roller temperature, puts into extruder, is squeezed out pelletizing and is obtained butadiene rubber/oligomer ester mother
Refining glue.It is calculated female in conjunction with the content of oligomer ester in masterbatch according to the dosage of oligomer ester in the butadiene rubber basic components of table 1
Butadiene rubber base vulcanization of rubber glue, the detailed performance such as table 2 of rubber compound and vulcanizate is prepared in the required dosage of refining glue.
Embodiment 3
100 parts of butadiene rubber rubber are put into open mill, adjustment roll spacing is 10mm, and 2 parts of anti-aging agent ODA, 2 parts of anti-aging agents are added
AW and 5 part of chromium stearate is kneaded 5min, and 5 parts of vapor phase method SiO are added2With 10 parts of N550, be kneaded 5min, adjustment roller temperature to 5 DEG C,
200 parts of oligomer esters are added, are kneaded 7min, 4 parts of accelerating agents and 1 part of cumyl peroxide is added, are kneaded 8min, adjustment roller temperature is extremely
80 DEG C, roll spacing is adjusted to 1mm, the thin logical 10min of sizing material, to 5 DEG C, bottom sheet is cut adjustment roller temperature, puts into extruder, is squeezed
Go out pelletizing and obtains butadiene rubber/oligomer ester masterbatch.According to the dosage of oligomer ester in the butadiene rubber basic components of table 1, in conjunction with
The content of oligomer ester in masterbatch calculates the required dosage of masterbatch, butadiene rubber base vulcanization of rubber glue is prepared, and is kneaded
The detailed performance of glue and vulcanizate such as table 2.
Comparative example 1
According to the butadiene rubber basic components of table 1, be prepared butadiene rubber base vulcanization of rubber glue, rubber compound and vulcanizate it is detailed
Thin performance such as table 2.
Comparative example 2
By the method that specified each component content repeats implementation 2, but accelerating agent is not used.Matched according to the butadiene rubber basis of table 1
Side, is prepared butadiene rubber base vulcanization of rubber glue, the detailed performance such as table 2 of rubber compound and vulcanizate.
Comparative example 3
By the method that specified each component content repeats implementation 2, it is added without chromium stearate.Matched according to the butadiene rubber basis of table 1
Side, is prepared butadiene rubber base vulcanization of rubber glue, the detailed performance such as table 2 of rubber compound and vulcanizate.
Comparative example 4
By the method that specified each component content repeats implementation 2, but 4 parts of Vulcanization accelerator TMTDs are added.According to the butadiene rubber of table 1
Butadiene rubber base vulcanization of rubber glue, the detailed performance such as table 2 of rubber compound and vulcanizate is prepared in basic components.
Comparative example 5
By the method that specified each component content repeats implementation 2, but 4 parts of accelerant CZs are added.According to the butadiene rubber base of table 1
Butadiene rubber base vulcanization of rubber glue, the detailed performance such as table 2 of rubber compound and vulcanizate is prepared in plinth formula.
Comparative example 6
By the method that specified each component content repeats implementation 2, but without thin logical.According to the butadiene rubber basic components of table 1,
Butadiene rubber base vulcanization of rubber glue, the detailed performance such as table 2 of rubber compound and vulcanizate is prepared.
Comparative example 7
By the method that specified each component content repeats implementation 2, but directly proportionally by the raw material of masterbatch, in conjunction with table
1 butadiene rubber basic components, are kneaded together, are prepared butadiene rubber base vulcanization of rubber glue, rubber compound and vulcanizate it is detailed
Thin performance such as table 2.
Table 2
Using pre-dispersion, oligomer ester is blended in advance with butadiene rubber, is added quantitative and with accelerating agent and filler, mixed
It closes, squeeze out, be granulated, obtain butadiene rubber/oligomer ester masterbatch.The masterbatch is convenient for preservation, transport and weighs；Be directly added into
Oligomer ester is compared, and masterbatch can effectively avoid the problem that roll banding, mixing time in post-production are grown, and can improve oligomerisation
The utilization rate of ester makes the performance of butadiene rubber product be further improved, the tensile strength power of vulcanizate, tearing strength, resistance to
Abrasivity and heat-resistant stability all increase significantly.It the method can be widely used in all kinds of rubber oils compounding agent masterbatch,
Especially suitable for high-performance, multi-functional oligomer ester masterbatch.
Claims (4)
1. a kind of butadiene rubber/oligomer ester masterbatch, it is characterised in that including following components：100 mass parts of butadiene rubber, together
Polyester 100-200 mass parts, accelerating agent 2-4 mass parts, anti-aging agent 2-4 mass parts, filler 5-15 mass parts, peroxidating two are different
Propyl benzene 0.5-1 mass parts, chromium stearate 2-5 mass parts.
2. a kind of butadiene rubber/oligomer ester masterbatch according to claim 1, which is characterized in that the accelerating agent is
The 2 of TMTD and CZ:1 mixture.
3. a kind of butadiene rubber/oligomer ester masterbatch according to claim 1, which is characterized in that the filler is
Vapor phase method SiO2With the one or two of N550, anti-aging agent is the one or two of antioxidant A W and anti-aging agent ODA.
4. a kind of preparation method of butadiene rubber/oligomer ester masterbatch, it is characterised in that comprise the steps of：
Rubber is put into open mill, adjustment roll spacing is 10mm, and anti-aging agent and chromium stearate is added, and is kneaded 2-5min, and addition is filled out
Material is kneaded 2-4min, and adjustment roller temperature is added oligomer ester to 5 DEG C, is kneaded 5-7min, and accelerating agent and cumyl peroxide is added,
It is kneaded 5-8min, roll spacing is adjusted to 1mm by adjustment roller temperature to 80 DEG C, the thin logical 10-20min of sizing material, adjusts roller temperature to 5 DEG C, under
Piece is cut, and puts into extruder, is squeezed out pelletizing and is obtained butadiene rubber/oligomer ester masterbatch.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108424555A (en) * | 2018-02-14 | 2018-08-21 | 王经营 | A kind of NBR/ oligomer esters masterbatch and preparation method thereof |
| CN108424561A (en) * | 2018-02-14 | 2018-08-21 | 王经管 | A kind of neoprene/oligomer ester premixing glue and preparation method thereof |
| CN108424564A (en) * | 2018-02-14 | 2018-08-21 | 王经营 | A kind of high-performance HXNBR oligomer ester masterbatch and preparation method thereof |
| CN108440801A (en) * | 2018-02-14 | 2018-08-24 | 王经营 | A kind of high-performance NR/ oligomer ester premixing glues and preparation method thereof |
| CN108503913A (en) * | 2018-02-14 | 2018-09-07 | 王经营 | A kind of multi-functional SBR/ oligomer esters masterbatch and preparation method thereof |
| CN108517059A (en) * | 2018-02-14 | 2018-09-11 | 王经营 | A kind of novel HNBR oligomer esters predispersion and preparation method thereof |
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Application publication date: 20180828 |