CN109206755A - A kind of spectacle-frame attapulgite-active calcium silicate modified EPT rubber composite material preparation method - Google Patents
A kind of spectacle-frame attapulgite-active calcium silicate modified EPT rubber composite material preparation method Download PDFInfo
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- CN109206755A CN109206755A CN201810782159.1A CN201810782159A CN109206755A CN 109206755 A CN109206755 A CN 109206755A CN 201810782159 A CN201810782159 A CN 201810782159A CN 109206755 A CN109206755 A CN 109206755A
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions 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
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
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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
- C08K2201/011—Nanostructured additives
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Abstract
The invention discloses a kind of spectacle-frame attapulgite-active calcium silicate modified EPT rubber composite material preparation methods, by ethylene propylene diene rubber thin logical plasticizing on a mill, then it plasticates in mixer, add softening agent atoleine mixing, put into fume colloidal silica, activating agent ethylene glycol, n-octytriethoxysilane pressurization mixing, auxiliary agent is added, titanate esters-silane coupling agent modified synergic attapulgite, break up-active calcium silicate the powder of ball milling modification, the carbon nanotube mixing of phenolic resin coating modification, cooling rubber compound, on twin-roll rubber mixing machine, make rubber compound packet roller, vulcanizing agent cumyl peroxide is added, slice after being kneaded uniformly, vulcanize on vulcanizing press.Ethylene propylene diene rubber is filled with white carbon black, after n-octytriethoxysilane coupling agent treatment, the croop property of ethylene propylene diene rubber is greatly improved, and reduces compression set, and the addition of silane improves the Degree of interaction between rubber and filler.
Description
Technical field
The invention belongs to spectacle lens technical fields, and in particular to a kind of spectacle-frame is modified with attapulgite-active calcium silicate
The preparation method of ternary ethlene propyene rubbercompound material.
Background technique
Organosilan especially alkoxy silane coupling agent, can by functional group reactions, eliminate white carbon black particle surface
Hydroxyl, so that the Compatibility improvement between hard charcoal black track producing particle and non-polar rubber, improves the dispersibility of nanoparticle in the polymer,
The attention of researchers at home and abroad is obtained in recent years.When using white carbon black reinforcing agent such as in " green " energy-saving tire, addition contains
The Si69 silane of sulphur forms preferable interface, cross-linked structure between rubber mass and white carbon black, can obtain rolling resistance
Power grasps the optimum balance between performance and abrasion resistance three.In the research of Nano carbon white-butadiene-styrene rubber system, silicon
Alkane coupling agent can reduce the interaction between particle and can enhance and interact between Nano carbon white and rubber, improves vulcanization
The tensile strength of glue；In white carbon black-ethylene propylene diene rubber system, using Si69 silane treatment white carbon black, sizing material can be significantly improved
Properties, coupling agent dosage and method of modifying have a major impact modified effect.
There are the multiple types such as vinyl, epoxy group, amino, tetrasulfide and alkyl, dialogue in the functional group of alkoxy silane
Carbon blacksurface processing and the influence of rubber performance are different.Active function is paid close attention to people in the research of non-polar rubber more
The coupled action of group such as vinyl, tetrasulfide, it is less to the concern of alkylalkoxy silane.Due to chain alkyl and non-pole
Property polymer between have a preferable compatibility, the present invention is using n-octytriethoxysilane to ethylene propylene diene rubber/white carbon black
System is studied, and preferable result is obtained.
Summary of the invention
The purpose of the present invention is being directed to existing problem, provides a kind of spectacle-frame attapulgite-active calcium silicate and change
Property ternary ethlene propyene rubbercompound material preparation method, according to this method make spectacle-frame it is compound with modified EPT rubber
Material has good mechanical property, durable, be unlikely to deform.
The present invention is achieved by the following technical solutions:
A kind of spectacle-frame attapulgite-active calcium silicate modified EPT rubber composite material preparation method, feature
It is, includes the following steps:
(1) modified synergic on attapulgite surface:
Into 40-50 parts of attapulgite powders, dehydrated alcohol is added in 1:5-10, is sufficiently stirred evenly in a kettle, is added 1.6-2 parts and is mixed
Coupling agent is closed, sealing disperses 1-2h with the revolving speed of 2000rpm, and suction filtration, filter cake are washed with dehydrated alcohol, in 103-107 DEG C of vacuum
It is dry in drying box, it is crushed with planetary ball mill, obtains the attapulgite of modified synergic；
(2) active calcium silicate powder breaks up-ball milling modification:
Into 1-1.2 parts of modifying agent, alcohol solution-forming is added in 1:4-5, is put into high speed disintegrator, with 25-30 parts of active silicic acids
Modified 1-2h is broken up in the mixing of calcium powder body, and then mixing and ball milling is modified 1-2h in planetary ball mill, and gained modified powder is existed
It dries in 105-115 DEG C of air dry oven to constant weight；
(3) the phenolic resin coating modification of carbon nanotube:
Into 10-20 parts of phenolic resin, dehydrated alcohol is added in 1:5-10, and 5-10 parts of multi-walled carbon nanotubes are added in stirring and dissolving, after
Continuous stirring 3-4h is placed in 75-85 DEG C of electric drying oven with forced convection after evaporating in Rotary Evaporators and dries 3-4h, use pulverizer
Pulverization process obtains phenolic resin coating modification carbon nanotube, then carries out vacuum drying treatment 3-4h；
(4) mechanical blending method prepares modified EPT rubber composite material:
By the thin logical plasticizing on a mill of 100-150 parts of ethylene propylene diene rubbers, then plasticate in mixer 2-3min, adds
20-30 parts of softening agent atoleine mixing 2-3min put into 25-30 parts of fume colloidal silicas, 5-10 parts of activating agent ethylene glycol, 4-
5 parts of n-octytriethoxysilanes pressurization mixing 4-5min, are added auxiliary agent and resulting material mixing 3- in (1), (2), (3)
5min, it is cooling that rubber compound makes rubber compound packet roller on twin-roll rubber mixing machine, 5-10 parts of vulcanizing agent peroxidating diisopropyls are added
Benzene, slice after being kneaded uniformly, vulcanizes on 150-170 DEG C of vulcanizing press.
Further, (dioctylphyrophosphoric acid acyloxy) titanate esters of isopropyl three coupling in mixing coupling agent in step (1)
Agent accounts for 45%, remaining is γ-methacryloxypropyl trimethoxy silane.
Further, modifying agent is S base silane coupling agent, concentration of alcohol 90-95% in step (2).
Further, in step (4) auxiliary agent by 1-2 parts of anti-aging agents, 2-3 parts of zinc oxide, 2-3 parts of stearic acid, 2-3 parts it is compound
Promotor, 1-2 parts of sulphur compositions.
The present invention has the advantage that compared with prior art
(1) use silane coupling agent and titanate coupling agent modified synergic attapulgite, the attapulgite surface through modified synergic at
Function grafting as the reaction active sites in sulfidation promotes modified attapulgite filled composite rubber there are many organo-functional group
The raising of glue crosslink density, the organo-functional group of attapulgite surface grafting can promote the shape of compounded rubber network cross-linked structure
At with modified synergic attapulgite filler reinforcement ethylene propylene diene rubber, when its tearing elongation, tensile strength and deformation can be improved
Stress at definite elongation, mechanical property is good.
(2) active calcium silicate powder hole extremely prosperity, large specific surface area, surface is rich in silicone hydroxyl, with modifying agent S base silicon
The coupling agent modified mechanical property of alkane is good；With breaing up-powder filling-modified the ethylene propylene diene rubber of active calcium silicate of ball milling modification,
Filled rubber has the apparent effect for promoting vulcanization early period, and the tearing strength, tensile strength and surrender for improving composite material are strong
Degree.
(3) ethylene propylene diene rubber, after n-octytriethoxysilane coupling agent treatment, ternary second are filled with white carbon black
The croop property of third rubber is greatly improved, and reduces compression set, and the addition of silane improves between rubber and filler
Degree of interaction；
Phenolic resin coating modification is carried out to multi-walled carbon nanotube, is conducive to improve the dispersion of carbon nanotube in the base, will change
Property multi-walled carbon nanotube be filled into ethylene propylene diene rubber improve rubber composite material mechanical property.
Specific embodiment
Embodiment 1
A kind of spectacle-frame attapulgite-active calcium silicate modified EPT rubber composite material preparation method, feature
It is, includes the following steps:
(1) modified synergic on attapulgite surface:
Into 40 parts of attapulgite powders, dehydrated alcohol is added in 1:5, sufficiently stirs evenly in a kettle, 1.6 parts of mixing coupling agents are added,
Sealing disperses 1h with the revolving speed of 2000rpm, and suction filtration, filter cake are washed with dehydrated alcohol, are done in 103-107 DEG C of vacuum oven
It is dry, it is crushed with planetary ball mill, obtains the attapulgite of modified synergic；
(2) active calcium silicate powder breaks up-ball milling modification:
Into 1 part of modifying agent, alcohol solution-forming is added in 1:4, is put into high speed disintegrator, mixed with 25 parts of active calcium silicate powders
Modified 1h is broken up in conjunction, and then mixing and ball milling is modified 1h in planetary ball mill, and gained modified powder is done in 105-115 DEG C of air blast
It dries in dry case to constant weight；
(3) the phenolic resin coating modification of carbon nanotube:
Into 10 parts of phenolic resin, dehydrated alcohol is added in 1:5, and 5 parts of multi-walled carbon nanotubes are added in stirring and dissolving, continues to stir 3h,
After being evaporated in Rotary Evaporators, it is placed in 75-85 DEG C of electric drying oven with forced convection and dries 3h, with pulverizer pulverization process, obtain
Phenolic resin coating modification carbon nanotube, then carry out vacuum drying treatment 3h；
(4) mechanical blending method prepares modified EPT rubber composite material:
By the thin logical plasticizing on a mill of 100 parts of ethylene propylene diene rubbers, then plasticate in mixer 2min, add 20 parts it is soft
Agent atoleine mixing 2min puts into 25 parts of fume colloidal silicas, 5 parts of activating agent ethylene glycol, 4 parts of n-octyl triethoxysilicanes
Alkane pressurizes mixing 4min, is added auxiliary agent and (1), (2), resulting material mixing 3min in (3), cooling rubber compound, in twin-roll
On rubber mixing machine, make rubber compound packet roller, 5 parts of vulcanizing agent cumyl peroxides are added, slice after being kneaded uniformly, at 150-160 DEG C
Vulcanize on vulcanizing press.
Further, (dioctylphyrophosphoric acid acyloxy) titanate esters of isopropyl three coupling in mixing coupling agent in step (1)
Agent accounts for 45%, remaining is γ-methacryloxypropyl trimethoxy silane.
Further, modifying agent is S base silane coupling agent, concentration of alcohol 90% in step (2).
Further, in step (4) auxiliary agent by 1 part of anti-aging agent, 2 parts of zinc oxide, 2 parts of stearic acid, 2 parts of compound accelerants, 1
Part sulphur composition.
Embodiment 2
A kind of spectacle-frame attapulgite-active calcium silicate modified EPT rubber composite material preparation method, feature
It is, includes the following steps:
(1) modified synergic on attapulgite surface:
Into 50 parts of attapulgite powders, dehydrated alcohol is added in 1:10, sufficiently stirs evenly in a kettle, 2 parts of mixing coupling agents are added,
Sealing disperses 2h with the revolving speed of 2000rpm, and suction filtration, filter cake are washed with dehydrated alcohol, are done in 103-107 DEG C of vacuum oven
It is dry, it is crushed with planetary ball mill, obtains the attapulgite of modified synergic；
(2) active calcium silicate powder breaks up-ball milling modification:
Into 1.2 parts of modifying agent, alcohol solution-forming is added in 1:5, is put into high speed disintegrator, with 30 parts of active calcium silicate powders
Modified 2h is broken up in mixing, and then mixing and ball milling is modified 2h in planetary ball mill, by gained modified powder in 105-115 DEG C of air blast
It dries in drying box to constant weight；
(3) the phenolic resin coating modification of carbon nanotube:
Into 20 parts of phenolic resin, dehydrated alcohol is added in 1:10, and stirring and dissolving is added 10 parts of multi-walled carbon nanotubes, continues to stir
4h is placed in 75-85 DEG C of electric drying oven with forced convection after evaporating in Rotary Evaporators and dries 4h, with pulverizer pulverization process, obtain
To phenolic resin coating modification carbon nanotube, then carry out vacuum drying treatment 4h；
(4) mechanical blending method prepares modified EPT rubber composite material:
By the thin logical plasticizing on a mill of 150 parts of ethylene propylene diene rubbers, then plasticate in mixer 3min, add 30 parts it is soft
Agent atoleine mixing 3min puts into 30 parts of fume colloidal silicas, 10 parts of activating agent ethylene glycol, 5 parts of n-octyl triethoxies
Silane pressurizes mixing 5min, is added auxiliary agent and (1), (2), resulting material mixing 5min in (3), cooling rubber compound, in double rollings
On cylinder rubber mixing machine, make rubber compound packet roller, 10 parts of vulcanizing agent cumyl peroxides are added, slice after being kneaded uniformly, in 160-170
Vulcanize on DEG C vulcanizing press.
Further, (dioctylphyrophosphoric acid acyloxy) titanate esters of isopropyl three coupling in mixing coupling agent in step (1)
Agent accounts for 45%, remaining is γ-methacryloxypropyl trimethoxy silane.
Further, modifying agent is S base silane coupling agent, concentration of alcohol 95% in step (2).
Further, in step (4) auxiliary agent by 2 parts of anti-aging agents, 3 parts of zinc oxide, 3 parts of stearic acid, 3 parts of compound accelerants, 2
Part sulphur composition.
There is good mechanical property according to the spectacle-frame modified EPT rubber composite material of the method for the present invention production
Can, it is durable, be unlikely to deform.
Claims (4)
1. a kind of spectacle-frame attapulgite-active calcium silicate modified EPT rubber composite material preparation method, special
Sign is, includes the following steps:
(1) modified synergic on attapulgite surface:
Into 40-50 parts of attapulgite powders, dehydrated alcohol is added in 1:5-10, is sufficiently stirred evenly in a kettle, is added 1.6-2 parts and is mixed
Coupling agent is closed, sealing disperses 1-2h with the revolving speed of 2000rpm, and suction filtration, filter cake are washed with dehydrated alcohol, in 103-107 DEG C of vacuum
It is dry in drying box, it is crushed with planetary ball mill, obtains the attapulgite of modified synergic；
(2) active calcium silicate powder breaks up-ball milling modification:
Into 1-1.2 parts of modifying agent, alcohol solution-forming is added in 1:4-5, is put into high speed disintegrator, with 25-30 parts of active silicic acids
Modified 1-2h is broken up in the mixing of calcium powder body, and then mixing and ball milling is modified 1-2h in planetary ball mill, and gained modified powder is existed
It dries in 105-115 DEG C of air dry oven to constant weight；
(3) the phenolic resin coating modification of carbon nanotube:
Into 10-20 parts of phenolic resin, dehydrated alcohol is added in 1:5-10, and 5-10 parts of multi-walled carbon nanotubes are added in stirring and dissolving, after
Continuous stirring 3-4h is placed in 75-85 DEG C of electric drying oven with forced convection after evaporating in Rotary Evaporators and dries 3-4h, use pulverizer
Pulverization process obtains phenolic resin coating modification carbon nanotube, then carries out vacuum drying treatment 3-4h；
(4) mechanical blending method prepares modified EPT rubber composite material:
By the thin logical plasticizing on a mill of 100-150 parts of ethylene propylene diene rubbers, then plasticate in mixer 2-3min, adds
20-30 parts of softening agent atoleine mixing 2-3min put into 25-30 parts of fume colloidal silicas, 5-10 parts of activating agent ethylene glycol, 4-
5 parts of n-octytriethoxysilanes pressurization mixing 4-5min, are added auxiliary agent and resulting material mixing 3- in (1), (2), (3)
5min, it is cooling that rubber compound makes rubber compound packet roller on twin-roll rubber mixing machine, 5-10 parts of vulcanizing agent peroxidating diisopropyls are added
Benzene, slice after being kneaded uniformly, vulcanizes on 150-170 DEG C of vulcanizing press.
2. a kind of spectacle-frame according to claim 1 is compound with attapulgite-active calcium silicate modified EPT rubber
The preparation method of material, which is characterized in that isopropyl three (dioctylphyrophosphoric acid acyloxy) titanium in mixing coupling agent in step (1)
Acid esters coupling agent accounts for 45%, remaining is γ-methacryloxypropyl trimethoxy silane.
3. a kind of spectacle-frame according to claim 1 is compound with attapulgite-active calcium silicate modified EPT rubber
The preparation method of material, which is characterized in that modifying agent is S base silane coupling agent, concentration of alcohol 90-95% in step (2).
4. a kind of spectacle-frame according to claim 1 is compound with attapulgite-active calcium silicate modified EPT rubber
The preparation method of material, which is characterized in that in step (4) auxiliary agent by 1-2 parts of anti-aging agents, 2-3 parts of zinc oxide, 2-3 parts of stearic acid,
2-3 parts of compound accelerants, 1-2 parts of sulphur compositions.
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| CN201810782159.1A CN109206755A (en) | 2018-07-17 | 2018-07-17 | A kind of spectacle-frame attapulgite-active calcium silicate modified EPT rubber composite material preparation method |
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| CN201810782159.1A CN109206755A (en) | 2018-07-17 | 2018-07-17 | A kind of spectacle-frame attapulgite-active calcium silicate modified EPT rubber composite material preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109810301A (en) * | 2019-02-16 | 2019-05-28 | 齐齐哈尔大学 | A kind of multipurpose memory type side mirror material |
| CN114672095A (en) * | 2022-05-11 | 2022-06-28 | 南京中超新材料股份有限公司 | High-flame-retardancy low-smoke halogen-free cable sheath material and preparation method thereof |
-
2018
- 2018-07-17 CN CN201810782159.1A patent/CN109206755A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109810301A (en) * | 2019-02-16 | 2019-05-28 | 齐齐哈尔大学 | A kind of multipurpose memory type side mirror material |
| CN114672095A (en) * | 2022-05-11 | 2022-06-28 | 南京中超新材料股份有限公司 | High-flame-retardancy low-smoke halogen-free cable sheath material and preparation method thereof |
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