CN108484982A - A kind of flyash reinforcing rubber material and preparation method - Google Patents
A kind of flyash reinforcing rubber material and preparation method Download PDFInfo
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- CN108484982A CN108484982A CN201810320479.5A CN201810320479A CN108484982A CN 108484982 A CN108484982 A CN 108484982A CN 201810320479 A CN201810320479 A CN 201810320479A CN 108484982 A CN108484982 A CN 108484982A
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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
- 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
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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
- C08K11/00—Use of ingredients of unknown constitution, e.g. undefined reaction products
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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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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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
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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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
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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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
- 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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- 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
A kind of flyash reinforcing rubber material of present invention offer and preparation method thereof, wherein the raw material of flyash reinforcing rubber material includes flyash, compounding coupling agent, surfactant, nano-particle, second alcohol and water；Preparation method includes carrying out refinement decentralized processing to flyash, obtains pre-treating fly ash；Configuration compounding coupling agent；Coupling agent, second alcohol and water mixing progress hydrolysis will be compounded, the first solution is obtained；Water and surfactant are added in pre-treating fly ash, after stirring evenly, nano-particle and the first solution are added thereto, after stirring at a predetermined temperature, obtains flyash reinforcing rubber material.The present invention is by compounding coupling agent, surfactant, the modes modified coal ash such as nano-particle, in flyash surface grafting organic group, it can improve the processing performance of rubber compound with carbon black and with filled rubber with good reinforcing effect, utilize industrial waste recycling, energy conservation and environmental protection.
Description
Technical field
The present invention relates to rubber additive technical field, more particularly to a kind of flyash reinforcing rubber material and preparation side
Method.
Background technology
Flyash refers generally to the solid emission of thermal power plant discharge, and comprehensive utilization is a huge system work
Journey, in decades, China relevant technical personnel pay huge effort thus.Into after 21 century, environment caused by flyash
Problem causes more concerns.Environmentally protective new trend how is complied under modern society, and the flyash of discharge is made full use of
Get up, is a vital task in suitable long-term from now on.The mainstream Land use systems of flyash are cement industry and mix at present
Solidifying geotechnique's journey, but it is limited using scale, and superfluous flyash is stacked everywhere polluted local environment, and the travel fatigue raised makes expediently
Air quality is severe, and serious haze is even more the health for damaging the people.
Carbon black consumption accounts for about the 94% of carbon black whole consumption in rubber industry, and rubber/carbon black composite material is even more quilt
It is widely used in the manufacturing of tire and other rubber products.If using flyash as rubber-reinforcing filler, raw material sources
Extensively, process for producing is simple, small investment, at low cost, can both save carbon black, also solve the problem that problem of environmental pollution, has notable
Economic benefit and social benefit.But flyash belongs to inorganic polar substance, due to surface as most of inorganic filler
There are hydroxyls, and hydrophily is presented, and surface acidity hydroxyl may postpone to vulcanize and limit its use.Therefore, fine coal is improved
Filling capacity and reinforcing effect of the ash in rubber, it is necessary to surface modification treatment be carried out to flyash, to enhance itself and rubber material
Compatibility between material.
There are expensive, preparation process is complicated, adhesive usage amount is big, treatment effeciency for existing flyash supporting material
It is not high, to it is thermo-responsive a series of problems, such as, therefore, develop a kind of flyash supporting material of low cost, simple for process at
For those skilled in the art's technical problem urgently to be resolved hurrily.
Invention content
The technical issues of present invention need to solve is to provide a kind of flyash reinforcing rubber material and preparation method, existing to solve
There is the problem of higher cost of technology, complex process.
To solve the above-mentioned problems, a kind of flyash reinforcing rubber material of present invention offer and preparation method, take
Technical solution is as follows：
On the one hand, the embodiment of the invention discloses a kind of flyash reinforcing rubber materials comprising flyash, compounding coupling
Agent, surfactant, nano-particle, second alcohol and water.
Further, in parts by weight, flyash：Compound coupling agent：Surfactant：Nano-particle：Ethyl alcohol：Water is
100:(1-5)：(0.5-5)：(1-10)：(1-10)：(5-100).
Preferably, flyash：Compound coupling agent：Surfactant：Nano-particle：Ethyl alcohol：Water is 100:2：(0.5-5)：
(0.5-10)：2:1.
Further, the compounding coupling agent includes silane coupling agent, aluminate coupling agent and titanate coupling agent,
In, by weight, silane coupling agent：Aluminate coupling agent：Titanate coupling agent is (4-7):(6-3):(0-1)；Preferably
5:4:1。
Further, the surfactant is linear paraffin benzene sulfonic acid sodium salt.
Further, the nano-particle includes that nano-calcium carbonate, nano silicon dioxide, nano kaoline are one or more
Mixing.
On the other hand, the embodiment of the invention also discloses the preparation methods of material described in any one of the above embodiments comprising：
Refinement decentralized processing is carried out to flyash, obtains pre-treating fly ash；
Configuration compounding coupling agent；
Coupling agent, second alcohol and water mixing progress hydrolysis will be compounded, the first solution is obtained；
Water and surfactant are added in pre-treating fly ash, after stirring evenly, nano-particle and the are added thereto
One solution obtains flyash reinforcing rubber material after stirring at a predetermined temperature.
Further, when obtaining first solution, it is described compounding coupling agent, second alcohol and water additional proportion be 1:1:
(5-10)。
Further, the flyash carry out refinement decentralized processing include：By flyash fine 5- in the ball mill
10min, grain size can be down to average grain diameter 5um by average grain diameter 30um, increase specific surface area, improve surface-active, easily and silicon
Alkane coupling agent is grafted, and then disperses 1-10min under ultrasonication, is occurred to reduce to reunite.
Further, the hydrolysis is to react 5-30min at 60-90 DEG C.
Further, the predetermined temperature is 70-100 DEG C.
The beneficial effects of the invention are as follows：
The present invention is by compounding coupling agent, adding surfactant, the key ways modified coal ash such as addition nano-particle,
In flyash surface grafting organic group, and then with carbon black and with filled rubber, not only there is good reinforcing effect, and can change
The processing performance of kind rubber compound, furthermore with industrial waste recycling, energy conservation and environmental protection meets the research of contemporary green industry
Trend.
Description of the drawings
Fig. 1 is that the hydrophily of flyash illustrates；
Fig. 2 is that the hydrophily of flyash supporting material obtained illustrates；
Fig. 3 is that the lipophile of flyash illustrates；
Fig. 4 is that the lipophile of flyash supporting material obtained illustrates；
Fig. 5 is that the scanning electron microscope of flyash illustrates；
Fig. 6 is that the scanning electron microscope of flyash supporting material obtained illustrates；
Fig. 7 is that the laser particle size of flyash illustrates；
The laser particle size diagram of flyash after Fig. 8 is fine 5min；
Fig. 9 is that the laser particle size of flyash supporting material obtained illustrates.
Specific implementation mode
With reference to the accompanying drawings and examples, the specific implementation mode of the present invention is described in further detail.
Embodiment 1
Refinement decentralized processing is carried out to the flyash of 100 parts by weight, obtains pre-treating fly ash；
Configuration compounding coupling agent：By 1 parts by weight silane coupling agent, 0.8 parts by weight aluminate coupling agent, 0.2 parts by weight titanium
Acid esters coupling agent is uniformly mixed, and obtains compounding coupling agent；
2 parts by weight are compounded, reaction is hydrolyzed at 85 DEG C of coupling agent, 2 parts by weight of ethanol and 5 parts by weight water mixing
30min obtains the first solution；
50 parts by weight water and 1 parts surfactant are added in pre-treating fly ash, after stirring evenly, are added thereto
Enter 5 parts by weight nano-particles and the first solution, it is in thick to keep solution, after stirring 40min at a temperature of 85 DEG C, obtains powder
Coal ash reinforcing rubber material.
Obtained flyash supporting material is shown in compared with flyash shown in Fig. 1-Fig. 6.Wherein, Fig. 1 is the hydrophilic of flyash
Property diagram, Fig. 2 be flyash supporting material obtained hydrophily illustrate, Fig. 3 be flyash lipophile illustrate, Fig. 4 be system
The lipophile diagram of the flyash supporting material obtained, Fig. 5 are that the scanning electron microscope of flyash illustrates, and Fig. 6 is that flyash obtained is mended
The scanning electron microscope diagram of strong material, Fig. 7 are that the laser particle size of flyash illustrates, and Fig. 8 is the laser of flyash after fine 5min
Granularity illustrates, and Fig. 9 is that the laser particle size of flyash supporting material obtained illustrates.
Embodiment 2
Preparing rubber with formula shown in table 1, (wherein, modified coal ash is the flyash reinforcing rubber material that embodiment 1 obtains
Material), obtained rubber parameters are shown in Table 2.
Table 1
Table 2
| Example 2-1 | Example 2-2 | Example 2-3 | Example 2-4 | Example 2-5 | Example 2-6 | |
| Minimum torque ML (dN.m) | 1.63 | 1.38 | 1.24 | 1.06 | 0.71 | 0.29 |
| Torque capacity MH (dN.m) | 23.17 | 19.26 | 17.45 | 16.12 | 14.25 | 12.19 |
| Time of scorch t10 | 0:29 | 0:28 | 0:29 | 0:32 | 0:32 | 0:37 |
| Sulfurizing time tc90 | 5:32 | 4:59 | 5:12 | 5:11 | 5:14 | 5:35 |
| Tensile strength (MPa) | 16.5 | 18.4 | 19.9 | 20.4 | 22.0 | 23.4 |
| 100% stretching strength (MPa) | 1.77 | 1.88 | 2.04 | 2.28 | 2.83 | 3.17 |
| 300% stretching strength (MPa) | 3.28 | 3.82 | 4.58 | 5.34 | 7.26 | 9.39 |
| Elongation at break (%) | 1067 | 932 | 791 | 684 | 554 | 457 |
Embodiment 3
Refinement decentralized processing is carried out to the flyash of 100 parts by weight, obtains pre-treating fly ash；
Configuration compounding coupling agent：0.4 parts by weight silane coupling agent, 0.6 parts by weight aluminate coupling agent are uniformly mixed, obtained
To compounding coupling agent；
1 parts by weight are compounded, reaction is hydrolyzed at 60 DEG C of coupling agent, 1 parts by weight of ethanol and 20 parts by weight water mixing
5min obtains the first solution；
80 parts by weight water and 0.5 parts surfactant are added in pre-treating fly ash, after stirring evenly, thereto
10 parts by weight nano-particles and the first solution is added, it is in thick to keep solution, after stirring 30min at a temperature of 120 DEG C, is obtained
To flyash reinforcing rubber material.
Embodiment 4
Refinement decentralized processing is carried out to the flyash of 100 parts by weight, obtains pre-treating fly ash；
Configuration compounding coupling agent：By 1.81 parts by weight silane coupling agents, 2.73 parts by weight aluminate coupling agents, 0.45 weight
Part titanate coupling agent is uniformly mixed, and obtains compounding coupling agent；
5 parts by weight are compounded, reaction is hydrolyzed at 90 DEG C of coupling agent, 10 parts by weight of ethanol and 10 parts by weight water mixing
20min obtains the first solution；
90 parts by weight water and 5 parts surfactants are added in pre-treating fly ash, after stirring evenly, are added thereto
Enter 8 parts by weight nano-particles and the first solution, it is in thick to keep solution, after stirring 60min at a temperature of 95 DEG C, obtains powder
Coal ash reinforcing rubber material.
Embodiment 5
Refinement decentralized processing is carried out to the flyash of 100 parts by weight, obtains pre-treating fly ash；
Configuration compounding coupling agent：By 2 parts by weight silane coupling agents, 0.86 parts by weight aluminate coupling agent, 0.14 parts by weight
Titanate coupling agent is uniformly mixed, and obtains compounding coupling agent；
3 parts by weight are compounded, reaction is hydrolyzed at 75 DEG C of coupling agent, 6 parts by weight of ethanol and 1 parts by weight water mixing
18min obtains the first solution；
4 parts by weight water and 3 parts surfactants are added in pre-treating fly ash, after stirring evenly, are added thereto
Enter 1 parts by weight nano-particle and the first solution, it is in thick to keep solution, after stirring 45min at a temperature of 70 DEG C, obtains powder
Coal ash reinforcing rubber material.
By above-described embodiment it is found that flyash supporting material produced by the present invention changes rubber when making rubber
Property, the tensile strength of rubber obtained is slightly below carbon black filled system, and elongation at break is then better than carbon black filled system.
Embodiment of above is merely to illustrate the present invention, and not limitation of the present invention, in relation to the common of technical field
Technical staff can also make a variety of changes and modification without departing from the spirit and scope of the present invention, therefore all
Equivalent technical solution also belongs to scope of the invention, and scope of patent protection of the invention should be defined by the claims.
Claims (10)
1. a kind of flyash reinforcing rubber material, which is characterized in that raw material include flyash, compounding coupling agent, surfactant,
Nano-particle, second alcohol and water.
2. material according to claim 1, which is characterized in that in parts by weight, flyash：Compound coupling agent：It lives on surface
Property agent：Nano-particle：Ethyl alcohol：The ratio of water is 100:(1-5)：(0.5-5)：(1-10)：(1-10)：(5-100).
3. material according to claim 2, which is characterized in that the compounding coupling agent includes silane coupling agent, Aluminate
Coupling agent and titanate coupling agent, wherein by weight, silane coupling agent：Aluminate coupling agent：Titanate coupling agent is
(4-7):(3-6):(0-1)。
4. material according to claim 1 or 2 or 3, which is characterized in that the surfactant is linear paraffin benzene sulfonic acid
Sodium.
5. material according to claim 1 or 2 or 3, which is characterized in that the nano-particle includes nano-calcium carbonate, receives
One or more mixing of rice silica, nano kaoline.
6. the preparation method of the material according to claim 1-5 any one, which is characterized in that including：
Refinement decentralized processing is carried out to flyash, obtains pre-treating fly ash；
Configuration compounding coupling agent；
Coupling agent, second alcohol and water mixing progress hydrolysis will be compounded, the first solution is obtained；
Water and surfactant are added in pre-treating fly ash, after stirring evenly, nano-particle and first molten is added thereto
Liquid obtains flyash reinforcing rubber material after stirring at a predetermined temperature.
7. according to the method described in claim 6, it is characterized in that, when obtaining first solution, the compounding coupling agent, second
The additional proportion of alcohol and water is 1:1:(5-10).
8. according to the method described in claim 6, it is characterized in that, the flyash carry out refinement decentralized processing include：By powder
Coal ash fine 5-10min in the ball mill.
9. according to the method described in claim 6, it is characterized in that, the hydrolysis is to react 5-30min at 60-90 DEG C.
10. according to the method described in claim 6, it is characterized in that, the predetermined temperature is 70-120 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810320479.5A CN108484982A (en) | 2018-04-11 | 2018-04-11 | A kind of flyash reinforcing rubber material and preparation method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111909428A (en) * | 2020-07-29 | 2020-11-10 | 贵州仁宜智科技有限公司 | Superfine powder reinforced rubber and preparation method and application thereof |
| CN112552552A (en) * | 2019-09-25 | 2021-03-26 | 山东科兴化工有限责任公司 | Preparation method of high-strength wear-resistant reinforced filler for nano multilayer porous ball rubber-plastic product |
| CN112707746A (en) * | 2021-03-25 | 2021-04-27 | 北京锦绣新技术发展有限公司 | Fly ash CO2Preparation method and application of trapping agent |
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| CN102010535A (en) * | 2010-12-28 | 2011-04-13 | 济南高新区工业废弃物利用研发中心 | Pulverized coal ash rubber reinforcing agent |
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2018
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| CN102010535A (en) * | 2010-12-28 | 2011-04-13 | 济南高新区工业废弃物利用研发中心 | Pulverized coal ash rubber reinforcing agent |
| CN102850825A (en) * | 2012-09-11 | 2013-01-02 | 安徽理工大学 | Method and application for carrying out fly ash floating bead surface modification by using compound coupling agent |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112552552A (en) * | 2019-09-25 | 2021-03-26 | 山东科兴化工有限责任公司 | Preparation method of high-strength wear-resistant reinforced filler for nano multilayer porous ball rubber-plastic product |
| CN111909428A (en) * | 2020-07-29 | 2020-11-10 | 贵州仁宜智科技有限公司 | Superfine powder reinforced rubber and preparation method and application thereof |
| CN112707746A (en) * | 2021-03-25 | 2021-04-27 | 北京锦绣新技术发展有限公司 | Fly ash CO2Preparation method and application of trapping agent |
| CN112707746B (en) * | 2021-03-25 | 2021-07-16 | 北京锦绣新技术发展有限公司 | Fly ash CO2Preparation method and application of trapping agent |
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