CN109666195A - A kind of preparation method of rubber composite material - Google Patents
A kind of preparation method of rubber composite material Download PDFInfo
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- CN109666195A CN109666195A CN201811581467.4A CN201811581467A CN109666195A CN 109666195 A CN109666195 A CN 109666195A CN 201811581467 A CN201811581467 A CN 201811581467A CN 109666195 A CN109666195 A CN 109666195A
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- tripoli
- carbon black
- white carbon
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- composite material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
-
- 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
-
- 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
- C08J2307/00—Characterised by the use of natural rubber
- C08J2307/02—Latex
-
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
-
- 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
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- 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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- 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
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Thermal Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
A kind of preparation method of rubber composite material, belongs to field of material preparation, it is characterised in that: weighs tripoli slurry, is made into suspension, stirring carries out pre-dispersed；Coupling agent is added dropwise at room temperature, tripoli is added；Stirring is sufficiently mixed coupling agent and tripoli suspension uniformly, and the tripoli suspension of activation modification is made；In kind prepare modified white carbon black；Modified silica suspension or modified white carbon black dispersion pH value are adjusted, Heveatex is then weighed and is added in dispersion, be dispersed with stirring with electric mixer；It is coagulated altogether with calcium chloride solution, obtains tripoli or white carbon black filling natural rubber masterbatch through crepe, granulation；White carbon black/natural rubber masterbatch and tripoli/natural rubber masterbatch are kneaded according to the ratio.After tripoli is added, more evenly, rolling resistance reduces white carbon black/tripoli filling sizing material filler network；The hardness of vulcanizate slightly reduces, and stress at definite elongation, tensile strength, tearing strength and elongation rate of tensile failure increase, and physical property improves.
Description
Technical field
The invention belongs to field of material preparation more particularly to a kind of preparation methods of rubber composite material.
Background technique
Increasingly reinforcement with global resources crisis and people to environmental protection consciousness, green tire are automotive wheels from now on
Tire industrial expansion direction, pushes white carbon black to be increasingly being applied in tire tread glue.Compared with carbon black, white carbon black energy
Vulcanizate rolling resistance is reduced, reduces hysteresis loss, but there is also some problems.Since there are a large amount of silicon hydroxyls on white carbon black surface
Base, polarity is stronger, and with most of hydrocarbon rubbers poor compatibilities, higher surface can make agglomeration between hard charcoal black track producing particle serious,
It is caused more to be difficult to disperse in rubber.
Tripoli is a kind of novel metalloid mineral, and the Neubuerger in Germany finds and develops use first, then in India
Rajasthan and Tamil Nadu discovery.In recent years, the Si clusters large-scale in Fujian China discovery, are formed in more than 100,000,000
The more than one hundred million tons of volcanic eruption proved reserves before year, chemical composition is similar with Germany's tripoli of Neubuerger, but crystal type and potassium from
Sub- content is different.German Neubuerger tripoli is mainly made of spherical cryogenic quartz and sheet kaolinite, and Fujian China
Tripoli is mainly made of fine flakey low quartz and layered illite.
Summary of the invention
The present invention is intended to provide a kind of preparation method of rubber composite material.
The preparation method of rubber composite material of the present invention, includes the following steps:
(1) tripoli slurry is weighed, the suspension that mass fraction is 0.1 is made into, places it on electric mixer and stir, is carried out pre-
Dispersion；Under electric mixer high-speed stirred, the ethyl alcohol that coupling agent Si69 is slowly added dropwise into tripoli suspension at room temperature is molten
Liquid, additional amount are the 3%-5% of tripoli quality；High-speed stirred is sufficiently mixed coupling agent Si69 and tripoli suspension uniformly, is made
The tripoli suspension of activation modification；
(2) modified white carbon black is in kind prepared, and grinds 30-35min in colloid mill；
(3) modified silica suspension is adjusted with potassium hydroxide or modified white carbon black dispersion pH value is 9 or so, then weigh day
Right latex is added in dispersion, is dispersed with stirring 2h with electric mixer；
(4) it is coagulated with calcium chloride solution, through crepe, is granulated altogether, dry 48 h at 55-65 DEG C obtain tripoli or white carbon black filling
Natural rubber masterbatch；
(5) white carbon black/natural rubber masterbatch and tripoli/natural rubber masterbatch are kneaded according to the ratio.
The preparation method of rubber composite material of the present invention, the calendering process is successively are as follows: masterbatch-stearic acid, oxygen
Change zinc and anti-aging agent-promotor and Sulfur-it is thin it is 6 times logical after amplify roll spacing, bottom sheet；Rubber compound carries out sulphur on vulcanizing press
Change.
The preparation method of rubber composite material of the present invention, the curing temperature are 150 DEG C.
The preparation method of rubber composite material of the present invention, the mass fraction of the ethanol solution are 0.1.
The preparation method of rubber composite material of the present invention, the high-speed stirred time are 30min.
The preparation method of rubber composite material of the present invention, the frequency of the electric mixer are 300 rpms.
The preparation method of rubber composite material of the present invention, the mass fraction of the calcium chloride solution are 0.2.
The preparation method of rubber composite material of the present invention, by modified white carbon black and tripoli suspension respectively with natural gum
Cream is blended, and white carbon black/natural rubber masterbatch and tripoli/natural rubber masterbatch is made, and two kinds of masterbatch are pressed different proportion
It is blended, white carbon black/tripoli/native rubber composite material is made.Tripoli is conducive to improve white carbon black in natural rubber matrix
Dispersion promotes rubber vulcanization.After a certain amount of tripoli is added, white carbon black/tripoli filling sizing material filler network more evenly, rolls resistance
Power reduces；The hardness of vulcanizate slightly reduces, and stress at definite elongation, tensile strength, tearing strength and elongation rate of tensile failure increase, physical
It can improve.
Specific embodiment
Below by embodiment to the preparation method of rubber composite material of the present invention, it is described in detail.
Example one
The preparation method of rubber composite material of the present invention, includes the following steps:
(1) tripoli slurry is weighed, the suspension that mass fraction is 0.1 is made into, places it on electric mixer and stir, is carried out pre-
Dispersion；Under electric mixer high-speed stirred, the ethyl alcohol that coupling agent Si69 is slowly added dropwise into tripoli suspension at room temperature is molten
Liquid, additional amount are the 3% of tripoli quality；High-speed stirred is sufficiently mixed coupling agent Si69 and tripoli suspension uniformly, and activation is made
Modified tripoli suspension；
(2) modified white carbon black is in kind prepared, and grinds 30min in colloid mill；
(3) modified silica suspension is adjusted with potassium hydroxide or modified white carbon black dispersion pH value is 9 or so, then weigh day
Right latex is added in dispersion, is dispersed with stirring 2h with electric mixer；
(4) it is coagulated with calcium chloride solution, through crepe, is granulated altogether, dry 48 h, obtain tripoli or white carbon black filled natural at 55 DEG C
Rubber masterbatch；
(5) white carbon black/natural rubber masterbatch and tripoli/natural rubber masterbatch are kneaded according to the ratio.
The preparation method of rubber composite material of the present invention, the calendering process is successively are as follows: masterbatch-stearic acid, oxygen
Change zinc and anti-aging agent-promotor and Sulfur-it is thin it is 6 times logical after amplify roll spacing, bottom sheet；Rubber compound carries out sulphur on vulcanizing press
Change.
The preparation method of rubber composite material of the present invention, the curing temperature are 150 DEG C.
The preparation method of rubber composite material of the present invention, the mass fraction of the ethanol solution are 0.1.
The preparation method of rubber composite material of the present invention, the high-speed stirred time are 30min.
The preparation method of rubber composite material of the present invention, the frequency of the electric mixer are 300 rpms.
The preparation method of rubber composite material of the present invention, the mass fraction of the calcium chloride solution are 0.2.
As tripoli dosage increases, the F of rubber compoundLValue reduces, and the mobility of sizing material is obviously improved, this is because hard charcoal
Black specific surface area is big compared with tripoli, and tendency of reuniting is big, and peptizaiton is played in the addition of a certain amount of fine flakey tripoli, makes glue
Expect to be improved in the flowing of initial vulcanization step；The F of white carbon black filling rubber compoundmaxValue is significantly greater than tripoli and fills rubber compound, this is
Since the specific surface area of tripoli is significantly less than white carbon black, surface-active crosslinking points are few, thus be added tripoli after sizing material crosslinking it is close
Degree reduces, and rigidity reduces；FmaxThe size of one value and the crosslink density of sizing material are related, Fmax - FLIt is worth bigger, the crosslinking of sizing material
Degree is bigger, and the crosslink density of tripoli filling sizing material is significantly less than white carbon black filling sizing material, this is because the specific surface of white carbon black
Product is big compared with tripoli, and system crosslinking points are more；White carbon black/tripoli filling sizing material crosslink density is respectively less than white carbon black and tripoli is filled out
Sizing material is filled, this may be because more evenly, free rubber molecular chain is reduced filler distribution when white carbon black is blended with tripoli； Vc
Reflect rubber vulcanization rate speed, VcBigger, rate of cure is bigger.As tripoli dosage increases, the V of rubber compoundcBecome in increasing
Gesture, this is opposite with the result that conventional dry prepares rubber compound.In dry process, tripoli has obvious postpone effect to rubber vulcanization
It answers, this is mainly due to rate of cures to be influenced by system acid-base property, filler surface hydroxyl etc..
As tripoli dosage increases, combine glue content in trend is decreased obviously in rubber compound, this shows that a certain amount of silicon is added
After soil, reduced with the rubber molecular chain that filler grain is combined closely, filler network degree reduces, entire one rubber network of filler
It more tends to uniformly；When tripoli dosage is 40 parts, system cannot form close rubber binder course, and rubber all dissolves.
RPA can test certain frequency, in temperature and range of strain rubber various dynamic properties, be that analysis rubber compound adds
Work performance, the filler grain effective means of dispersibility and interface cohesion situation in sizing material.Payne effect is the dynamic of filled rubber
The phenomenon that morphotype amount sharply declines as strain increases, it is mainly dispersed and interface cohesion situation in rubber compound by filler
It influences, reflects one filler Degree of interaction of filler.
As strain increases, the G of white carbon black filling rubber compound is obviously reduced, and shows apparent Payne effect；It is added
After tripoli, the AG of rubber compound is significantly less than white carbon black filling rubber compound, and Payne effect is obviously reduced, this with tripoli unique
Layer structure is related, and tripoli interacts between reducing hard charcoal black track producing particle, makes filler network more evenly and is not easy to be destroyed；By
In limitation of the cross-bond to sub-chain motion, the G of vulcanizate is significantly increased, and Payne effect change rule is consistent with t elder brother's refining glue.
Loss factor values can be used to characterize the hysteretic properties and rolling resistance of rubber material.Loss factor values are smaller, and rolling resistance is smaller,
Therefore the effective way for reducing tire drag is to reduce loss factor values.
As strain increases, the loss factor values of vulcanizate are significantly lower than rubber compound, this illustrates filler-rubber of vulcanizate
It interacts and significantly increases between rubber-rubber；Under same strain, the loss factor values changing rule and rubber compound of vulcanizate
On the contrary, this can be construed to, glue content is combined to influence the loss factor values size of vulcanizate, white carbon black before vulcanization, in rubber compound
Large specific surface area, the rubber content combined closely with filler is high, and the loss modulus of rubber compound is small, thus have lower loss because
Subvalue, after vulcanization, rubber-filler and rubber-rubber Interaction enhanced are simultaneously redistributed, and the vulcanizate filler net of tripoli is added
More evenly, loss factor values are smaller for network, advantageously reduce rolling resistance.
Embodiment two
On the basis of example 1, the preparation method of rubber composite material of the present invention, includes the following steps:
(1) tripoli slurry is weighed, the suspension that mass fraction is 0.1 is made into, places it on electric mixer and stir, is carried out pre-
Dispersion；Under electric mixer high-speed stirred, the ethyl alcohol that coupling agent Si69 is slowly added dropwise into tripoli suspension at room temperature is molten
Liquid, additional amount are the 4% of tripoli quality；High-speed stirred is sufficiently mixed coupling agent Si69 and tripoli suspension uniformly, and activation is made
Modified tripoli suspension；
(2) modified white carbon black is in kind prepared, and grinds 33min in colloid mill；
(3) modified silica suspension is adjusted with potassium hydroxide or modified white carbon black dispersion pH value is 9 or so, then weigh day
Right latex is added in dispersion, is dispersed with stirring 2h with electric mixer；
(4) it is coagulated with calcium chloride solution, through crepe, is granulated altogether, dry 48 h, obtain tripoli or white carbon black filled natural at 60 DEG C
Rubber masterbatch；
(5) white carbon black/natural rubber masterbatch and tripoli/natural rubber masterbatch are kneaded according to the ratio.
Embodiment three
The preparation method of rubber composite material of the present invention, includes the following steps:
(1) tripoli slurry is weighed, the suspension that mass fraction is 0.1 is made into, places it on electric mixer and stir, is carried out pre-
Dispersion；Under electric mixer high-speed stirred, the ethyl alcohol that coupling agent Si69 is slowly added dropwise into tripoli suspension at room temperature is molten
Liquid, additional amount are the 5% of tripoli quality；High-speed stirred is sufficiently mixed coupling agent Si69 and tripoli suspension uniformly, and activation is made
Modified tripoli suspension；
(2) modified white carbon black is in kind prepared, and grinds 35min in colloid mill；
(3) modified silica suspension is adjusted with potassium hydroxide or modified white carbon black dispersion pH value is 9 or so, then weigh day
Right latex is added in dispersion, is dispersed with stirring 2h with electric mixer；
(4) it is coagulated with calcium chloride solution, through crepe, is granulated altogether, dry 48 h, obtain tripoli or white carbon black filled natural at 65 DEG C
Rubber masterbatch；
(5) white carbon black/natural rubber masterbatch and tripoli/natural rubber masterbatch are kneaded according to the ratio.
Claims (7)
1. a kind of preparation method of rubber composite material, it is characterised in that include the following steps:
(1) tripoli slurry is weighed, the suspension that mass fraction is 0.1 is made into, places it on electric mixer and stir, is carried out pre-
Dispersion；Under electric mixer high-speed stirred, the ethyl alcohol that coupling agent Si69 is slowly added dropwise into tripoli suspension at room temperature is molten
Liquid, additional amount are the 3%-5% of tripoli quality；High-speed stirred is sufficiently mixed coupling agent Si69 and tripoli suspension uniformly, is made
The tripoli suspension of activation modification；
(2) modified white carbon black is in kind prepared, and grinds 30-35min in colloid mill；
(3) modified silica suspension is adjusted with potassium hydroxide or modified white carbon black dispersion pH value is 9 or so, then weigh day
Right latex is added in dispersion, is dispersed with stirring 2h with electric mixer；
(4) it is coagulated with calcium chloride solution, through crepe, is granulated altogether, dry 48 h at 55-65 DEG C obtain tripoli or white carbon black filling
Natural rubber masterbatch；
(5) white carbon black/natural rubber masterbatch and tripoli/natural rubber masterbatch are kneaded according to the ratio.
2. the preparation method of rubber composite material according to claim 1, it is characterised in that: the calendering process is successively are as follows:
Amplify roll spacing, bottom sheet after masterbatch-stearic acid, zinc oxide and anti-aging agent-promotor and Sulfur-thin logical 6 times；Rubber compound is in plate
Vulcanized on vulcanizer.
3. the preparation method of rubber composite material according to claim 2, it is characterised in that: the curing temperature is 150 DEG C.
4. the preparation method of rubber composite material according to claim 3, it is characterised in that: the quality of the ethanol solution point
Number is 0.1.
5. the preparation method of rubber composite material according to claim 4, it is characterised in that: the high-speed stirred time is
30min。
6. the preparation method of rubber composite material according to claim 5, it is characterised in that: the frequency of the electric mixer
It is 300 rpms.
7. the preparation method of rubber composite material according to claim 6, it is characterised in that: the quality of the calcium chloride solution
Score is 0.2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811581467.4A CN109666195A (en) | 2018-12-24 | 2018-12-24 | A kind of preparation method of rubber composite material |
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| CN201811581467.4A CN109666195A (en) | 2018-12-24 | 2018-12-24 | A kind of preparation method of rubber composite material |
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| CN109666195A true CN109666195A (en) | 2019-04-23 |
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| CN201811581467.4A Pending CN109666195A (en) | 2018-12-24 | 2018-12-24 | A kind of preparation method of rubber composite material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110734585A (en) * | 2019-10-24 | 2020-01-31 | 江苏清荷材料科技有限公司 | rubber master batch and preparation method thereof, and rubber and preparation method thereof |
| CN115368755A (en) * | 2022-10-07 | 2022-11-22 | 江苏爱特恩高分子材料有限公司 | Preparation method of vermiculite/white carbon black composite material for rubber filling |
-
2018
- 2018-12-24 CN CN201811581467.4A patent/CN109666195A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110734585A (en) * | 2019-10-24 | 2020-01-31 | 江苏清荷材料科技有限公司 | rubber master batch and preparation method thereof, and rubber and preparation method thereof |
| CN115368755A (en) * | 2022-10-07 | 2022-11-22 | 江苏爱特恩高分子材料有限公司 | Preparation method of vermiculite/white carbon black composite material for rubber filling |
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