CN108440847A - A kind of EP rubbers base oligomer ester premixing glue and preparation method thereof - Google Patents

A kind of EP rubbers base oligomer ester premixing glue and preparation method thereof Download PDF

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Publication number
CN108440847A
CN108440847A CN201810151053.1A CN201810151053A CN108440847A CN 108440847 A CN108440847 A CN 108440847A CN 201810151053 A CN201810151053 A CN 201810151053A CN 108440847 A CN108440847 A CN 108440847A
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oligomer ester
rubbers
mass parts
premixing glue
glue
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王经管
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/16Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers

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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)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)

Abstract

A kind of EP rubbers base oligomer ester premixing glue of present invention offer and preparation method thereof.Using pre-dispersion, oligomer ester is blended in advance with EP rubbers, is added quantitative and with accelerating agent and filler, mixing is squeezed out, is granulated, and obtains premixing glue.The premixing glue is convenient for preservation, transport and weighs;Compared with being directly added into oligomer ester, the problem that can effectively avoid the roll banding in post-production, mixing time from growing improves the utilization rate of oligomer ester, the performance of EP rubbers product is made to be further improved.It the method can be widely used in all kinds of rubber oils compounding agent premixing glues, especially suitable for high-performance, multi-functional oligomer ester premixing glue.

Description

A kind of EP rubbers base oligomer ester premixing glue and preparation method thereof
Technical field
The invention belongs to rubber technical field of composite preparation, especially have EP rubbers base oligomer ester premixing glue And its application field.
Background technology
Oligomer ester is a kind of Multifunctional rubber oils compounding agent, and during rubber processing, the oligomer ester of oils is not only It can play the role of softening oil, be conducive to the machine-shaping of rubber, moreover it is possible in the sulfidation of later stage rubber, participate in 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, and wall can be glued in container, and metering is susceptible to error;Refining glue initial stage, The addition of oligomer ester causes rubber to skid on rubber mixing equipment, is unfavorable for refining glue;Refining glue later stage, oligomer ester can cause sizing material serious Roll banding causes mixing time to extend, and reduces production efficiency.Therefore, how oils oligomer ester to be preferably added in rubber, is kept away Exempt from processing problems, 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 EP rubbers base oligomer ester premixing glue and preparation methods.
A kind of EP rubbers base oligomer ester premixing glue, it is characterised in that including following components:100 mass parts of EP rubbers, 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 DZ:1 mixture.
The filler is the one or two of N220 and precipitated calcium carbonate, and anti-aging agent is antioxidant 264 or 4010NA One or two.
A kind of preparation method of EP rubbers base oligomer ester premixing glue, 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 EP rubbers base oligomer ester premixing glue.
Compared with prior art, the present invention its remarkable advantage is:
(1)Oligomer ester is blended in advance with EP rubbers, 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 premixing glue is realized on a mill, makes part oligomer ester and the third rubber of second Glue crosslinks, and forms microgel and solves the problems, such as high oil plant premixing glue 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 premixing glue 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 premixing glue is applied to using EP rubbers as in the rubber product of matrix, the microgel in premixing glue 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 EP rubbers base oligomer ester premixing glue.
Specific implementation mode
Present invention is further described in detail below in conjunction with the accompanying drawings.
A kind of EP rubbers base oligomer ester premixing glue, it is characterised in that including following components:100 mass parts of EP rubbers, 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 DZ:1 mixture, filler For the one or two of N220 and precipitated calcium carbonate, anti-aging agent is antioxidant 264 or the one or two of 4010NA.
A kind of preparation method of EP rubbers base oligomer ester premixing glue, 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 EP rubbers base oligomer ester premixing glue.
Obtained premixing glue is applied in EP rubbers base rubber product, wherein EP rubbers base rubber product is basic Formula is:
Table 1
Raw material title Mass parts Raw material title Mass parts
EP rubbers 100 Anti-aging agent RD 1
Oligomer ester 15 Sulfur 0.25
Sodium stearate 1.75 Potassium stearate 0.75
, and tested as follows the EP rubbers 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 EP rubbers rubber are put into open mill, adjustment roll spacing is 10mm, and 2 parts of antioxidant 264s and 2 parts of tristearin are added Sour chromium is kneaded 2min, and 5 parts of N220 are added, and is kneaded 2min, and adjustment roller temperature is added 100 parts of oligomer esters to 5 DEG C, is kneaded 5min, adds Enter 2 parts of accelerating agents and 0.5 part of cumyl peroxide, be kneaded 5min, roll spacing is adjusted to 1mm, glue by adjustment roller temperature to 80 DEG C Expect thin logical 20min, to 5 DEG C, bottom sheet is cut adjustment roller temperature, puts into extruder, is squeezed out pelletizing and is obtained EP rubbers base oligomer ester Premixing glue.Preparation process is as shown in Figure 1.According to the dosage of oligomer ester in the EP rubbers basic components of table 1, in conjunction in premixing glue The content of oligomer ester calculates the required dosage of premixing glue, EP rubbers base vulcanization of rubber glue, rubber compound and vulcanization is prepared The detailed performance of glue such as table 2.
Embodiment 2
100 parts of EP rubbers rubber are put into open mill, adjustment roll spacing is 10mm, and 4 parts of antioxidant 4010NAs are added and 5 parts hard Resin acid chromium is kneaded 5min, and 15 parts of precipitated calcium carbonates are added, and is kneaded 5min, and adjustment roller temperature is added 200 parts of oligomer esters to 5 DEG C, mixes 7min is refined, 4 parts of accelerating agents and 1 part of cumyl peroxide is added, is kneaded 8min, roll spacing is adjusted to by adjustment roller temperature to 80 DEG C 1mm, 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 EP rubbers Base oligomer ester premixing glue.According to the dosage of oligomer ester in the EP rubbers basic components of table 1, contain in conjunction with oligomer ester in premixing glue Amount calculates the required dosage of premixing glue, is prepared EP rubbers base vulcanization of rubber glue, rubber compound and vulcanizate it is details It can be such as table 2.
Embodiment 3
100 parts of EP rubbers rubber are put into open mills, adjustment roll spacing is 10mm, be added 2 parts of antioxidant 4010NAs, 2 parts prevent Old agent 264 and 5 parts of chromium stearates are kneaded 5min, and 5 parts of N220 and 10 part of precipitated calcium carbonates are added, and are kneaded 5min, adjustment roller temperature is extremely 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, adjust roller Temperature is adjusted to 1mm to 80 DEG C, by roll spacing, and the thin logical 10min of sizing material, to 5 DEG C, bottom sheet is cut adjustment roller temperature, puts into extrusion Machine squeezes out pelletizing and obtains EP rubbers base oligomer ester premixing glue.According to the use of oligomer ester in the EP rubbers basic components of table 1 Amount calculates the required dosage of premixing glue, the EP rubbers base vulcanization of rubber is prepared in conjunction with the content of oligomer ester in premixing glue The detailed performance of glue, rubber compound and vulcanizate such as table 2.
Comparative example 1
According to the EP rubbers basic components of table 1, be prepared EP rubbers 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 EP rubbers basis of table 1 Side, is prepared EP rubbers 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 EP rubbers basis of table 1 Side, is prepared EP rubbers 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 EP rubbers of table 1 EP rubbers 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 accelerator DZs are added.According to the EP rubbers base of table 1 EP rubbers 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 EP rubbers basic components of table 1, EP rubbers 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 premixing glue, in conjunction with table 1 EP rubbers basic components, are kneaded together, are prepared EP rubbers 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 EP rubbers, is added quantitative and with accelerating agent and filler, mixed It closes, squeeze out, be granulated, obtain EP rubbers base oligomer ester premixing glue.The premixing glue is convenient for preservation, transport and weighs;With directly plus Enter oligomer ester to compare, premixing glue can effectively avoid the problem that roll banding, mixing time in post-production are grown, and can improve neat The utilization rate of polyester makes the performance of EP rubbers product be further improved, the tensile strength power of vulcanizate, tearing strength, Abrasion performance and heat-resistant stability all increase significantly.It the method can be widely used in all kinds of rubber oils compounding agent premixing glues In, especially suitable for high-performance, multi-functional oligomer ester premixing glue.

Claims (4)

1. a kind of EP rubbers base oligomer ester premixing glue, it is characterised in that including following components:100 mass parts of EP rubbers, 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 EP rubbers base oligomer ester premixing glue according to claim 1, which is characterized in that the accelerating agent is The 2 of TMTD and DZ:1 mixture.
3. a kind of EP rubbers base oligomer ester premixing glue according to claim 1, which is characterized in that the filler is The one or two of N220 and precipitated calcium carbonate, anti-aging agent are antioxidant 264 or the one or two of 4010NA.
4. a kind of preparation method of EP rubbers base oligomer ester premixing glue, 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 EP rubbers base oligomer ester premixing glue.
CN201810151053.1A 2018-02-14 2018-02-14 A kind of EP rubbers base oligomer ester premixing glue and preparation method thereof Withdrawn CN108440847A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103319792A (en) * 2013-06-07 2013-09-25 深圳市科聚新材料有限公司 Ethylene propylene diene monomer (EPDM) composite material and preparation method thereof
CN105400082A (en) * 2015-11-13 2016-03-16 江苏宝利来斯橡胶有限公司 Improved highly-filled ethylene propylene diene monomer master batch
CN107603112A (en) * 2017-09-22 2018-01-19 江阴海达橡塑股份有限公司 A kind of high-performance high ferro outer hood elastomeric material and its compression molding preparation method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103319792A (en) * 2013-06-07 2013-09-25 深圳市科聚新材料有限公司 Ethylene propylene diene monomer (EPDM) composite material and preparation method thereof
CN105400082A (en) * 2015-11-13 2016-03-16 江苏宝利来斯橡胶有限公司 Improved highly-filled ethylene propylene diene monomer master batch
CN107603112A (en) * 2017-09-22 2018-01-19 江阴海达橡塑股份有限公司 A kind of high-performance high ferro outer hood elastomeric material and its compression molding preparation method

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