CN101775157A - Preparation method of nano white carbon black for high dispersing rubber ingredient - Google Patents
Preparation method of nano white carbon black for high dispersing rubber ingredient Download PDFInfo
- Publication number
- CN101775157A CN101775157A CN201010017176A CN201010017176A CN101775157A CN 101775157 A CN101775157 A CN 101775157A CN 201010017176 A CN201010017176 A CN 201010017176A CN 201010017176 A CN201010017176 A CN 201010017176A CN 101775157 A CN101775157 A CN 101775157A
- Authority
- CN
- China
- Prior art keywords
- carbon black
- white carbon
- coupling agent
- silane coupling
- white
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention relates to a preparation method of nano white carbon black for a high dispersing rubber ingredient, which is characterized by comprising the following steps of: firstly, dispersing white carbon black in deionized water and sufficiently dispersing to form a reaction system; then dropping a silane coupling agent aqueous solution into the reaction system; and reacting the reaction system to which the silane coupling agent aqueous solution is added at the temperature of 75-85 DEG C for 1 hour and 20 minutes to 1 hour and 40 minutes to obtain the nano white carbon black. The DBP oil absorption value of the prepared nano white carbon black is 3.2-35cm<3>/g. In the invention, a modifier is dissolved by using a solvent with low cost and zero pollution; the nano white carbon black is modified by using the modifier so as to greatly increase the DBP oil absorption value of the nano white carbon black and obviously improve the dispersity of the white carbon black. Compared with the traditional methods, the preparation method can especially effectively increase the DBP oil absorption value of the nano white carbon black, improves the dispersity of the white carbon black in rubber, and reduces the production cost.
Description
Technical field
The present invention relates to the preparation method of a kind of rubber ingredients of high dispersive, belong to the Application in Chemical Engineering technical field with Nano carbon white.
Background technology
Direct Zhi Bei Nano carbon white, be a kind of white, nontoxic, unbodied fines shape silicon compound, have porousness, dispersibility, light weight, chemical property stable, high temperature resistant, do not burn, excellent properties such as electrical insulating property is good, can play thickening and strengthening action to rubber.
But the activated silica alcohol radical on the poly-silica of Nano carbon white inside, surface and to the absorption of water makes it be wetting ability.And because there is hydroxyl in the Nano carbon white surface, surface energy is bigger, and aggregate always tends to cohesion.These factors make Nano carbon white be difficult to a large amount of dispersions in rubber, and have limited the application of white carbon black in rubber.Thereby the dispersiveness that how to improve Nano carbon white is the matter of utmost importance of its widespread use in rubber.
The modification of Nano carbon white at present mainly is that ethanol solution with the KH-silane coupling agent is as properties-correcting agent, through after the modification, though the DBP oil-absorption(number) of Nano carbon white increases, dispersing property improves, but improve still not remarkable, and make solvent with dehydrated alcohol, production cost is very high, and environment is had certain pollution.Therefore, how significantly to improve the dispersiveness of Nano carbon white, reduce production costs, become the bottleneck of Nano carbon white widespread use in rubber.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, the preparation method of a kind of rubber ingredients of high dispersive with Nano carbon white is provided, Nano carbon white after this method modification, its DBP oil-absorption(number) can significantly improve, in rubber, can better disperse, greatly the intensity of Reinforced Rubber is simultaneously free from environmental pollution again.
According to technical scheme provided by the invention, the rubber ingredients of the described high dispersive preparation method of Nano carbon white may further comprise the steps:
(1), white carbon black is scattered in the deionization, fully disperse to form reaction system, the mass ratio of white carbon black and deionized water is 1: 8～12;
(2), in reaction system, drip the silane coupling agent aqueous solution, rate of addition is 2～4ml/min, the volumetric molar concentration of the silane coupling agent aqueous solution is 0.3～0.5mol/l, the add-on of the silane coupling agent aqueous solution is 24～28ml/10g white carbon black;
(3), the reaction system of the adding silane coupling agent aqueous solution is reacted down at 75～85 ℃ and was obtained Nano carbon white in 1 hour 20 minutes to 1 hour 40 minutes.
The DBP oil-absorption(number) of the Nano carbon white that makes is 3.2～35cm
3/ g.
Described DBP value is meant that under the test conditions of regulation, the 1g white carbon black absorbs the volume (cm of dibutyl phthalate (DBP, di-n-butyl phthalate)
3) number.Be used for characterizing the aggregation extent of white carbon black.The DBP value can be calculated the void volume between the white carbon black aggregate, so be measuring of white carbon black gathering and degree of agglomeration.When white carbon black was used as rubber filler, its aggregation of particles degree influenced the use properties of white carbon black cross-linked rubber.
Described silane coupling agent is silane coupling agent KH-570, silane coupling agent KH-560 or silane resin acceptor kh-550.
The chemical name of described silane coupling agent KH-570: γ-methacryloxypropyl trimethoxy silane, can be available from the upright chemical industry company limited etc. that sends in Nanjing.Be equivalent to U.S. union carbide corporation A-174, the Z-6030 of Dow corning company, the KBM-503 of Japan XINYUE, the German Hua Ke GF-31 of company.Be a kind of colourless transparent liquid, 255 ℃ of boiling points, density P25 ℃ of 1.045g/cm
3, refractive index n25D1.429,88 ℃ of flash-points are dissolved in organic solvents such as toluene, ether, halohydrocarbon, hydrolysis under acidity or alkaline condition.
The chemical name of silane coupling agent KH-560: γ-(2.3-glycidoxy) propyl trimethoxy silicane can be available from blue sky, Hubei Chemicals company limited.
The chemical name of silane resin acceptor kh-550 (SG-Si1100): γ-An Bingjisanyiyangjiguiwan, English name-Aminopropyltriethoxysilane, CAS numbering: 919-30-2.
The present invention comes soluble modified dose with low-cost, free of contamination solvent, and Nano carbon white is carried out modification, greatly improves the DBP oil-absorption(number) of Nano carbon white, significantly improves the dispersiveness of Nano carbon white; Compare with existing method, can improve the DBP oil-absorption(number) of Nano carbon white especially effectively, improve its dispersiveness in rubber, and reduce production costs.
Embodiment
The present invention will be further elaborated in the following embodiments, but this should not become the restriction to invention scope.White carbon black of the present invention, silane coupling agent are commercially available.
Embodiment 1
The commercially available Nano carbon white of 30 grams is scattered in the 300ml deionized water and forms reaction system, the silane coupling agent KH-570 aqueous solution that with the 80ml volumetric molar concentration is 0.3mol/l dropwise joins in the reaction system with the speed of 3ml/min, reaction system was reacted in 80 ℃ water-bath 1 hour 30 minutes, and its DBP oil-absorption(number) can reach 3.40cm
3/ g.
Embodiment 2
The commercially available Nano carbon white of 20 grams is scattered in the 160ml deionized water, the aqueous solution that with the 50ml volumetric molar concentration is the silane coupling agent KH-560 of 0.4mol/l dropwise joins in the reaction system with the speed of 2ml/min, reaction system was reacted in 75 ℃ water-bath 1 hour 40 minutes, and its DBP oil-absorption(number) can reach 3.20cm3/g.
Embodiment 3
The commercially available Nano carbon white of 40 grams is scattered in the 480ml deionized water, the silane resin acceptor kh-550 aqueous solution that with the 98ml volumetric molar concentration is 0.5mol/l dropwise joins in the reaction system with the speed of 4ml/min, reaction system was reacted in 85 ℃ water-bath 1 hour 20 minutes, and its DBP oil-absorption(number) can reach 3.50cm
3/ g.
Claims (3)
1. the rubber ingredients of a high dispersive is characterized in that with the preparation method of Nano carbon white, said method comprising the steps of:
(1), white carbon black is scattered in the deionization, fully disperse to form reaction system, the mass ratio of white carbon black and deionized water is 1: 8～12;
(2), in reaction system, drip the silane coupling agent aqueous solution, rate of addition is 2～4ml/min, the volumetric molar concentration of the silane coupling agent aqueous solution is 0.3～0.5mol/1, the add-on of the silane coupling agent aqueous solution is 24～28ml/10g white carbon black;
(3), the reaction system of the adding silane coupling agent aqueous solution is reacted down at 75～85 ℃ and was obtained Nano carbon white in 1 hour 20 minutes～1 hour 40 minutes.
2. preparation method as claimed in claim 1 is characterized in that: the DBP oil-absorption(number) of the Nano carbon white that makes is 3.2～35cm
3/ g.
3. preparation method as claimed in claim 1 is characterized in that: described silane coupling agent is silane resin acceptor kh-550, silane coupling agent KH-560 or silane coupling agent KH-570.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010017176A CN101775157A (en) | 2010-01-04 | 2010-01-04 | Preparation method of nano white carbon black for high dispersing rubber ingredient |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010017176A CN101775157A (en) | 2010-01-04 | 2010-01-04 | Preparation method of nano white carbon black for high dispersing rubber ingredient |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101775157A true CN101775157A (en) | 2010-07-14 |
Family
ID=42511754
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010017176A Pending CN101775157A (en) | 2010-01-04 | 2010-01-04 | Preparation method of nano white carbon black for high dispersing rubber ingredient |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101775157A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948638A (en) * | 2010-10-12 | 2011-01-19 | 江南大学 | Method for modifying nano white carbon black for highly dispersed rubber ingredients |
| CN101974256A (en) * | 2010-10-12 | 2011-02-16 | 江南大学 | Method for preparing highly-dispersed modified nano-white carbon black for rubber compound ingredients |
| CN103466638A (en) * | 2013-09-02 | 2013-12-25 | 无锡恒诚硅业有限公司 | Method for increasing DBP (di-n-butyl phthalate) absorption of white carbon black prepared by sulfate precipitation method |
| CN105086419A (en) * | 2015-08-11 | 2015-11-25 | 东华大学 | Fluorine-contained polyimide modified engineering plastic alloy capable of being electroplated and preparation method thereof |
| CN106833027A (en) * | 2017-01-12 | 2017-06-13 | 温州市炬邦新材料有限公司 | A kind of improved silica production technology |
-
2010
- 2010-01-04 CN CN201010017176A patent/CN101775157A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948638A (en) * | 2010-10-12 | 2011-01-19 | 江南大学 | Method for modifying nano white carbon black for highly dispersed rubber ingredients |
| CN101974256A (en) * | 2010-10-12 | 2011-02-16 | 江南大学 | Method for preparing highly-dispersed modified nano-white carbon black for rubber compound ingredients |
| CN103466638A (en) * | 2013-09-02 | 2013-12-25 | 无锡恒诚硅业有限公司 | Method for increasing DBP (di-n-butyl phthalate) absorption of white carbon black prepared by sulfate precipitation method |
| CN105086419A (en) * | 2015-08-11 | 2015-11-25 | 东华大学 | Fluorine-contained polyimide modified engineering plastic alloy capable of being electroplated and preparation method thereof |
| CN105086419B (en) * | 2015-08-11 | 2017-08-01 | 东华大学 | A kind of electrodepositable fluorinated polyimide modified engineered plastic alloy and preparation method thereof |
| CN106833027A (en) * | 2017-01-12 | 2017-06-13 | 温州市炬邦新材料有限公司 | A kind of improved silica production technology |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101948638A (en) | Method for modifying nano white carbon black for highly dispersed rubber ingredients | |
| CN103131189B (en) | Inorganic or organic hybridization nanocomposite for packaging light emitting diode (LED) and preparation method thereof | |
| CN101679639B (en) | Polyalkylsilsesquioxane particulates and a preparation method thereof | |
| CN101775157A (en) | Preparation method of nano white carbon black for high dispersing rubber ingredient | |
| CN102030906B (en) | Preparation of organic-inorganic hybrid resin for high temperature resistant heavy anti-corrosion paint | |
| CN104231264B (en) | A kind of preparation method and application of graphene oxide/silicon dioxide/polyaniline composite material | |
| CN101812289B (en) | Nanometer polysilicon particles and preparation method and application thereof | |
| CN101259964B (en) | Constant pressure and dry preparation method for high-performance silicon dioxide aerogel by using rice husk ash as raw material | |
| CN102391529A (en) | Preparation method of silicone resin type organic/inorganic hybrid material for packaging | |
| JP6262261B2 (en) | Composite coating liquid doped with Si-Mg-Al sol and core-shell microspheres and its production application | |
| CN103333358A (en) | Reusable low-cost silica aerogel oil-absorbing sponge and preparation method thereof | |
| CN102942895A (en) | Heat-conduction electronic potting adhesive and preparation method thereof | |
| CN101070380B (en) | Long-chain polyether type silane coupler of glycidol-ether-radical end-capping | |
| CN109957328A (en) | A kind of windshield film coating agent and preparation method thereof | |
| CN100567393C (en) | A kind of surface modified spherical SiO 2The preparation method of particulate epoxy resin composite material | |
| CN104910649A (en) | Quartz powder surface active composite modification method | |
| CN109401442A (en) | A kind of silver-plated electrically conductive ink of UV curing nano and preparation method thereof | |
| CN102001671A (en) | Method for preparing white carbon black by using silicon tetrachloride | |
| CN103848427B (en) | A kind of high dispersive precipitated silica and preparation method thereof | |
| CN103059617B (en) | Preparation method for nanometer anti-reflection self-cleaning coating solution | |
| CN101362836B (en) | Method for preparing microencapsulated ammonium polyphosphate | |
| CN1810902A (en) | Alkyd paint for ship cabin and its production process | |
| CN103360798A (en) | Method for preparing hydrophobic white carbon black | |
| CN101891205B (en) | Method for preparing nano silica subjected to surface modification by urushiol | |
| CN105086556A (en) | Preparation method of nanometer particles used for anti-corrosion coating |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Open date: 20100714 |