CN108424561A - A kind of neoprene/oligomer ester premixing glue and preparation method thereof - Google Patents
A kind of neoprene/oligomer ester premixing glue and preparation method thereof Download PDFInfo
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- CN108424561A CN108424561A CN201810151044.2A CN201810151044A CN108424561A CN 108424561 A CN108424561 A CN 108424561A CN 201810151044 A CN201810151044 A CN 201810151044A CN 108424561 A CN108424561 A CN 108424561A
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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- 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
- C08J2311/00—Characterised by the use of homopolymers or copolymers of chloroprene
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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
- C08J2411/00—Characterised by the use of homopolymers or copolymers of chloroprene
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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
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/06—Sulfur
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/18—Amines; Quaternary ammonium compounds with aromatically bound amino groups
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Abstract
A kind of neoprene/oligomer ester premixing glue of present invention offer and preparation method thereof.Using pre-dispersion, oligomer ester is blended in advance with neoprene, is added quantitative and with accelerating agent and filler, mixing is squeezed out, is granulated, and obtains neoprene/oligomer ester premixing glue.The premixing glue is convenient for preservation, transport and weighs；Compared with being directly added into oligomer ester, premixing glue 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 neoprene neoprene 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
Technical field
The invention belongs to rubber technical field of composite preparation, especially have high-performance neoprene/oligomer ester
Premixing glue and its application field.
Background technology
Oligomer ester is the multi-functional oils compounding agent of a kind of rubber, but is asked there are many during rubber processing
Topic can glue wall for example, the weighing and charging of thick oligomer ester are all relatively difficult in container, and metering is susceptible to error；Refining
The addition at glue initial stage, oligomer ester causes rubber to skid on rubber mixing equipment, is unfavorable for refining glue；Refining glue later stage, oligomer ester can cause
The serious roll banding of sizing material, causes mixing time to extend, and reduces production efficiency.Therefore, how oils oligomer ester to be added in rubber,
Processing problems are avoided, while the maximum function of oligomer ester can be played, are one of the hot issues in current rubber industry.
Invention content
The purpose of the present invention is to provide a kind of neoprene/oligomer ester premixing glue and preparation methods.
A kind of neoprene/oligomer ester premixing glue, it is characterised in that including following components：100 mass parts of neoprene,
Oligomer ester 100-200 mass parts, accelerating agent 2-4 mass parts, anti-aging agent 2-4 mass parts, filler 5-15 mass parts, magnesia 3-
5 mass parts, zinc oxide 0.5-1 mass parts, chromium stearate 2-5 mass parts.
The accelerating agent is the 2 of TMTD and DM:1 mixture.
The filler is the one or two of N330 and precipitated calcium carbonate, and anti-aging agent is the one of anti-aging agent RD or ODA
Kind or two kinds.
A kind of preparation method of neoprene/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, magnesia and zinc oxide 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 neoprene/oligomer ester premixing glue.
Compared with prior art, the present invention its remarkable advantage is：
（1）Oligomer ester is blended in advance with neoprene, using the unsaturated double-bond in oligomer ester, is promoted by the way that quantitative blending is added
Into agent, magnesia and zinc oxide, the partial dynamic vulcanization of premixing glue is realized on a mill, makes part oligomer ester and neoprene
It crosslinks, forms microgel and solve the problems, such as high oil plant premixing glue low viscosity roll banding to improve the viscosity of sizing material, and
And can subsequent high temperature processing in ensure the normal flow processability energy of sizing material, obtained oligomer ester premixing glue convenient for be granulated,
It preserves, transport and weighs, effectively improve the utilization rate of oligomer ester, avoid being stained with roller problem；
（2）When premixing glue is applied to using neoprene 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
The preparation process of Fig. 1 neoprenes/oligomer ester premixing glue.
Specific implementation mode
Present invention is further described in detail below in conjunction with the accompanying drawings.
A kind of neoprene/oligomer ester premixing glue, it is characterised in that including following components：100 mass parts of neoprene,
Oligomer ester 100-200 mass parts, accelerating agent 2-4 mass parts, anti-aging agent 2-4 mass parts, filler 5-15 mass parts, magnesia 3-
5 mass parts, zinc oxide 0.5-1 mass parts, chromium stearate 2-5 mass parts, the accelerating agent are the 2 of TMTD and DM:1 mixing
Object, filler are the one or two of N330 and precipitated calcium carbonate, and anti-aging agent is anti-aging agent RD or the one or two of ODA.
A kind of preparation method of neoprene/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, magnesia and zinc oxide 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 neoprene/oligomer ester premixing glue.
Obtained premixing glue is applied in neoprene base rubber product, wherein neoprene base rubber product is basic
Formula is：
Table 1
| Raw material title | Mass parts | Raw material title | Mass parts |
| Neoprene | 100 | Zinc oxide | 5 |
| Magnesia | 4 | Sulfur | 1.5 |
| Stearic acid | 1 | Antioxidant D | 2 |
| Accelerant N A-22 | 0.5 | Oligomer ester | 15 |
, and tested as follows the neoprene 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 neoprene rubbers are put into open mill, adjustment roll spacing is 10mm, and 2 parts of anti-aging agent RDs and 2 parts of stearic acid are added
Chromium is kneaded 2min, and 5 parts of N330 are added, and is kneaded 2min, and adjustment roller temperature is added 100 parts of oligomer esters to 5 DEG C, is kneaded 5min, is added 2
Part accelerating agent, 3 parts of magnesia and 0.5 part of zinc oxide, are kneaded 5min, and 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 neoprene/oligomer ester
Premixing glue.Preparation process is as shown in Figure 1.According to the dosage of oligomer ester in the neoprene basic components of table 1, in conjunction in premixing glue
The content of oligomer ester calculates the required dosage of premixing glue, neoprene 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 neoprene rubbers 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 precipitated calcium carbonates are added, and is kneaded 5min, and adjustment roller temperature is added 200 parts of oligomer esters to 5 DEG C, is kneaded
4 parts of accelerating agents, 5 parts of magnesia and 1 part of zinc oxide is added in 7min, is kneaded 8min, and 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 neoprene rubber
Glue/oligomer ester premixing glue.According to the dosage of oligomer ester in the neoprene basic components of table 1, in conjunction with oligomer ester in premixing glue
Content calculates the required dosage of premixing glue, is prepared neoprene base vulcanization of rubber glue, rubber compound and vulcanizate it is detailed
Performance such as table 2.
Embodiment 3
100 parts of neoprene rubbers 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
RD and 5 part of chromium stearate, be kneaded 5min, be added 5 parts of N330 and 10 part of precipitated calcium carbonates, 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, 3 parts of magnesia and 1 part of zinc oxide is added, are kneaded 8min, adjust roller temperature
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, puts into extruder,
It squeezes out pelletizing and obtains neoprene/oligomer ester premixing glue.According to the dosage of oligomer ester in the neoprene basic components of table 1, knot
The content of oligomer ester in premixing glue is closed, the required dosage of premixing glue is calculated, neoprene base vulcanization of rubber glue is prepared, is mixed
Refining glue and the detailed performance of vulcanizate such as table 2.
Comparative example 1
According to the neoprene basic components of table 1, be prepared neoprene 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 neoprene basis of table 1
Side, is prepared neoprene 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 neoprene basis of table 1
Side, is prepared neoprene 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 neoprene of table 1
Neoprene 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 altaxes are added.According to the neoprene base of table 1
Neoprene 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 neoprene basic components of table 1,
Neoprene 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 neoprene basic components, are kneaded together, are prepared neoprene 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 neoprene, is added quantitative and with accelerating agent and filler, mixed
It closes, squeeze out, be granulated, obtain neoprene/oligomer ester premixing glue.The premixing glue is convenient for preservation, transport and weighs；Be directly added into
Oligomer ester is compared, and premixing glue 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 neoprene neoprene 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 premixing glues,
Especially suitable for high-performance, multi-functional oligomer ester premixing glue.
Claims (4)
1. a kind of neoprene/oligomer ester premixing glue, it is characterised in that including following components：100 mass parts of neoprene, together
Polyester 100-200 mass parts, accelerating agent 2-4 mass parts, anti-aging agent 2-4 mass parts, filler 5-15 mass parts, magnesia 3-5
Mass parts, zinc oxide 0.5-1 mass parts, chromium stearate 2-5 mass parts.
2. a kind of neoprene/oligomer ester premixing glue according to claim 1, which is characterized in that the accelerating agent is
The 2 of TMTD and DM:1 mixture.
3. a kind of neoprene/oligomer ester premixing glue according to claim 1, which is characterized in that the filler is
The one or two of N330 and precipitated calcium carbonate, anti-aging agent are the one or two of anti-aging agent RD and anti-aging agent ODA.
4. a kind of preparation method of neoprene/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, magnesia and zinc oxide 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 neoprene/oligomer ester premixing glue.
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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 |
| 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 |
| 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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| CN108517059A (en) * | 2018-02-14 | 2018-09-11 | 王经营 | A kind of novel HNBR oligomer esters predispersion and preparation method thereof |
Cited By (6)
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| CN108456344A (en) * | 2018-02-14 | 2018-08-28 | 王经管 | A kind of butadiene rubber/oligomer ester masterbatch and preparation method thereof |
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| 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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