CN108424564A - A kind of high-performance HXNBR oligomer ester masterbatch and preparation method thereof - Google Patents
A kind of high-performance HXNBR oligomer ester masterbatch and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C08J2415/00—Characterised by the use of rubber derivatives
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- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
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- 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
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- C08K5/00—Use of organic ingredients
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- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3412—Heterocyclic compounds having nitrogen in the ring having one nitrogen atom in the ring
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Abstract
A kind of high-performance HXNBR oligomer ester masterbatch of present invention offer and preparation method thereof.Using pre-dispersion, oligomer ester is blended in advance with HXNBR, is added quantitative and with accelerating agent and filler, mixing is squeezed out, is granulated, and obtains HXNBR 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 HXNBR rubber products 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 HXNBR oligomer ester masterbatchings
Glue and its application field.
Background technology
Rubber is the important foundation material in industrial production.In the raw material of rubber product, oligomer ester is a kind of more work(
It can oils compounding agent.On the one hand, during rubber processing, the oligomer ester of oils can play the role of softening oil, be conducive to
On the other hand the machine-shaping of rubber contains unsaturated double-bond in oligomer ester, can be participated in the sulfidation of later stage rubber
Vulcanization reaction, to realize the humidification to 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.
Invention content
The purpose of the present invention is to provide a kind of high-performance HXNBR oligomer esters masterbatch and preparation methods.
A kind of high-performance HXNBR oligomer ester masterbatch, it is characterised in that including following components：100 mass parts of HXNBR, together
Polyester 100-200 mass parts, accelerating agent 2-4 mass parts, anti-aging agent 2-4 mass parts, filler 5-15 mass parts, methacrylic acid
Zinc 8-15 mass parts, cumyl peroxide 0.5-1 mass parts, chromium stearate 2-5 mass parts.
The accelerating agent is the 2 of TMTD and NS:1 mixture.
The filler is the one or two of N330 and N774, anti-aging agent be anti-aging agent RD or 4010NA one kind or
Two kinds.
A kind of preparation method of high-performance HXNBR 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, zinc methacrylate and mistake is added
Diisopropylbenzene (DIPB) is aoxidized, 5-8min is kneaded, roll spacing is adjusted to 1mm by adjustment roller temperature to 80 DEG C, the thin logical 10-20min of sizing material, is adjusted
To 5 DEG C, bottom sheet is cut whole roller temperature, puts into extruder, is squeezed out pelletizing and is obtained high-performance HXNBR oligomer ester masterbatch.
Compared with prior art, the present invention its remarkable advantage is：
（1）Oligomer ester is blended in advance with HXNBR, using the unsaturated double-bond in oligomer ester, is promoted by the way that quantitative blending is added
Agent and cumyl peroxide realize the partial dynamic vulcanization of masterbatch on a mill, and part oligomer ester is made to occur with HXNBR
Crosslinking forms microgel and solves the problems, such as high oil plant masterbatch low viscosity roll banding, and energy to improve the viscosity of sizing material
It is enough to ensure the normal flow processability energy of sizing material in subsequent high temperature processing, obtained oligomer ester masterbatch convenient for being granulated, preserving,
Transport and weighing, effectively improve the utilization rate of oligomer ester, avoid being stained with roller problem；
（2）When masterbatch is applied to using HXNBR as in the rubber product of matrix, the microgel in masterbatch and unreacted oligomerisation
Ester continues to participate in the vulcanization reaction of rubber matrix, on the one hand, microgel reacts with rubber matrix, formation and rubber-based
There is the microgel reinforcing agent of chemical bonding in body, further reinforcement, on the other hand, unreacted oligomer ester are realized to rubber matrix
The vulcanization reaction for participating in rubber matrix, forms cross-linked network structure in rubber matrix, is formed with rubber matrix itself vulcanization
Cross-linked network forms interpenetrating, further improves the performance of rubber product.
Description of the drawings
Fig. 1 is the preparation process of high-performance HXNBR oligomer ester masterbatch.
Specific implementation mode
Present invention is further described in detail below in conjunction with the accompanying drawings.
A kind of high-performance HXNBR oligomer ester masterbatch, it is characterised in that including following components：100 mass parts of HXNBR, together
Polyester 100-200 mass parts, accelerating agent 2-4 mass parts, anti-aging agent 2-4 mass parts, filler 5-15 mass parts, methacrylic acid
Zinc 8-15 mass parts, cumyl peroxide 0.5-1 mass parts, chromium stearate 2-5 mass parts, the accelerating agent be TMTD and
The 2 of NS:1 mixture, filler are the one or two of N330 and N774, and anti-aging agent is anti-aging agent RD or one kind of 4010NA
Or two kinds.
A kind of preparation method of high-performance HXNBR 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, zinc methacrylate and mistake is added
Diisopropylbenzene (DIPB) is aoxidized, 5-8min is kneaded, roll spacing is adjusted to 1mm by adjustment roller temperature to 80 DEG C, the thin logical 10-20min of sizing material, is adjusted
To 5 DEG C, bottom sheet is cut whole roller temperature, puts into extruder, is squeezed out pelletizing and is obtained high-performance HXNBR oligomer ester masterbatch.
Obtained masterbatch is applied in HXNBR base rubber products, wherein the basic recipe of HXNBR bases rubber product
For：
Table 1
| Raw material title | Mass parts | Raw material title | Mass parts |
| HXNBR | 100 | Vulcanization accelerator TMTD | 1.5 |
| Zinc methacrylate | 5 | Sulfur | 1.5 |
| Stearic acid | 1 | Carbon black | 50 |
| Anti-aging agent RD | 1 | Oligomer ester | 15 |
, and tested as follows the HXNBR bases in production of articles are 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 HXNBR rubber are put into open mill, adjustment roll spacing is 10mm, and 2 parts of anti-aging agent RDs and 2 parts of chromium stearates are added,
It is kneaded 2min, 5 parts of N330 are added, is kneaded 2min, adjustment roller temperature is added 100 parts of oligomer esters to 5 DEG C, is kneaded 5min, is added 2 parts
Accelerating agent, 8 parts of zinc methacrylates and 0.5 part of cumyl peroxide are kneaded 5min, and adjustment roller temperature is to 80 DEG C, by roll spacing tune
Whole is 1mm, and 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 high property
It can HXNBR oligomer ester masterbatch.Preparation process is as shown in Figure 1.According to the dosage of oligomer ester in the HXNBR basic components of table 1, knot
The content of oligomer ester in masterbatch is closed, the required dosage of masterbatch is calculated, HXNBR base vulcanization of rubber glue is prepared, is kneaded
The detailed performance of glue and vulcanizate such as table 2.
Embodiment 2
100 parts of HXNBR rubber are put into open mill, adjustment roll spacing is 10mm, and 4 parts of antioxidant 4010NAs and 5 parts of tristearin are added
Sour chromium is kneaded 5min, and 15 parts of N774 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, 15 parts of zinc methacrylates and 1 part of cumyl peroxide, is kneaded 8min, adjustment roller temperature is to 80 DEG C, by roller
Away from 1mm is adjusted to, the thin logical 10min of sizing material, to 5 DEG C, bottom sheet is cut adjustment roller temperature, puts into extruder, is squeezed out pelletizing and is obtained
High-performance HXNBR oligomer ester masterbatch.According to the dosage of oligomer ester in the HXNBR basic components of table 1, in conjunction with oligomerisation in masterbatch
The content of ester calculates the required dosage of masterbatch, is prepared HXNBR base vulcanization of rubber glue, rubber compound and vulcanizate it is detailed
Thin performance such as table 2.
Embodiment 3
100 parts of HXNBR rubber are put into open mill, adjustment roll spacing is 10mm, and 2 parts of antioxidant 4010NAs, 2 parts of anti-aging agents are added
RD and 5 part of chromium stearate is kneaded 5min, and 5 parts of N330 and 10 part of N774 are added, and is kneaded 5min, and adjustment roller temperature is added 200 to 5 DEG C
Part oligomer ester, is kneaded 7min, and 4 parts of accelerating agents, 15 parts of zinc methacrylates and 1 part of cumyl peroxide is added, and is kneaded 8min,
Roller temperature is adjusted to 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, is put into
Extruder squeezes out pelletizing and obtains high-performance HXNBR oligomer ester masterbatch.According to the use of oligomer ester in the HXNBR basic components of table 1
Amount calculates the required dosage of masterbatch, HXNBR base vulcanization of rubber glue is prepared in conjunction with the content of oligomer ester in masterbatch,
The detailed performance of rubber compound and vulcanizate such as table 2.
Comparative example 1
According to the HXNBR basic components of table 1, HXNBR base vulcanization of rubber glue, the detailed performance of rubber compound and vulcanizate is prepared
Such as table 2.
Comparative example 2
By the method that specified each component content repeats implementation 2, but accelerating agent is not used.According to the HXNBR basic components of table 1,
HXNBR base vulcanization of rubber glue, the detailed performance such as table 2 of rubber compound and vulcanizate is prepared.
Comparative example 3
By the method that specified each component content repeats implementation 2, it is added without chromium stearate.According to the HXNBR basic components of table 1,
HXNBR base vulcanization of rubber glue, the detailed performance such as table 2 of rubber compound and vulcanizate is prepared.
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 HXNBR bases of table 1
HXNBR base vulcanization of rubber glue, the detailed performance such as table 2 of rubber compound and vulcanizate is prepared in plinth formula.
Comparative example 5
By the method that specified each component content repeats implementation 2, but 4 parts of accelerator NSs are added.According to the bases the HXNBR of table 1
Formula, is prepared HXNBR base vulcanization of rubber glue, the detailed performance such as table 2 of rubber compound and vulcanizate.
Comparative example 6
By the method that specified each component content repeats implementation 2, but without thin logical.According to the HXNBR basic components of table 1, system
It is standby to obtain HXNBR base vulcanization of rubber glue, the detailed performance such as table 2 of rubber compound and vulcanizate.
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 HXNBR basic components, are kneaded together, and HXNBR base vulcanization of rubber glue, the detailed performance of rubber compound and vulcanizate is prepared
Such as table 2.
Table 2
Using pre-dispersion, oligomer ester is blended in advance with HXNBR, is added quantitative and with accelerating agent and filler, mixing is squeezed
Go out, be granulated, obtains HXNBR oligomer ester masterbatch.The masterbatch is convenient for preservation, transport and weighs；Be directly added into oligomer ester phase
Than oligomer ester masterbatch can effectively avoid the problem that roll banding, mixing time in post-production are grown, and can improve oligomer ester
Utilization rate, so that the performance of HXNBR rubber products is further improved, it is the tensile strength power of vulcanizate, tearing strength, wear-resisting
Consumption and heat-resistant stability all increase significantly.It the method can be widely used in all kinds of rubber oils compounding agent masterbatch, it is special
It Shi Yongyu not high-performance, multi-functional oligomer ester masterbatch.
Claims (4)
1. a kind of high-performance HXNBR oligomer ester masterbatch, it is characterised in that including following components：100 mass parts of HXNBR, oligomerisation
Ester 100-200 mass parts, accelerating agent 2-4 mass parts, anti-aging agent 2-4 mass parts, filler 5-15 mass parts, zinc methacrylate
8-15 mass parts, cumyl peroxide 0.5-1 mass parts, chromium stearate 2-5 mass parts.
2. a kind of high-performance HXNBR oligomer ester masterbatch according to claim 1, which is characterized in that the accelerating agent
It is the 2 of TMTD and NS:1 mixture.
3. a kind of high-performance HXNBR oligomer ester masterbatch according to claim 1, which is characterized in that the filler
For the one or two of N330 and N774, anti-aging agent is anti-aging agent RD or the one or two of 4010NA.
4. a kind of preparation method of high-performance HXNBR 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, zinc methacrylate and mistake is added
Diisopropylbenzene (DIPB) is aoxidized, 5-8min is kneaded, roll spacing is adjusted to 1mm by adjustment roller temperature to 80 DEG C, the thin logical 10-20min of sizing material, is adjusted
To 5 DEG C, bottom sheet is cut whole roller temperature, puts into extruder, is squeezed out pelletizing and is obtained high-performance HXNBR oligomer ester masterbatch.
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Cited By (6)
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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 |
| 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 |
| CN108456344A (en) * | 2018-02-14 | 2018-08-28 | 王经管 | A kind of butadiene rubber/oligomer ester masterbatch 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: 20180821 |