CN106634055A - Method for emulsifying and modifying silicon dioxide at high speed - Google Patents
Method for emulsifying and modifying silicon dioxide at high speed Download PDFInfo
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- CN106634055A CN106634055A CN201611069345.8A CN201611069345A CN106634055A CN 106634055 A CN106634055 A CN 106634055A CN 201611069345 A CN201611069345 A CN 201611069345A CN 106634055 A CN106634055 A CN 106634055A
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- silica
- silicon dioxide
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/309—Combinations of treatments provided for in groups C09C1/3009 - C09C1/3081
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a method for emulsifying and modifying silicon dioxide at a high speed. The method comprises the following steps: preparing an alcohol-water solution with a mass ratio of ethanol to deionized water of (8 to 2) to (19 to 1), adding a surfactant, after ultrasonically dispersing the solution for 30 min, transferring the solution into a high-speed emulsification machine, adding silicon dioxide, and performing surface modification treatment; washing the emulsified slurry in a centrifuging way, drying, and crushing to obtain modified silicon dioxide, wherein the mass of the added surfactant is 5 to 50 percent of the mass of the silicon dioxide, the high-speed emulsification time is 1 to 5 h, and the rotation speed is 1000 to 5000 r/min. On the technical basis of the traditional silicon dioxide modification, the dispersion and surface modification process of the silicon dioxide can be further realized by virtue of the high-speed emulsification technology, and silicon dioxide powder with good dispersity and good lyophobic performance can be obtained.
Description
Technical field
The present invention relates to a kind of method of the precipitated silica that is modified come surface using high speed emulsification.
Technical background
Precipitated silica main component is hydrated SiO 2, and its composition can be expressed as SiO2nH2O.As one kind
Nano material, its initial particle is typically in 10～40nm, because silica surface can contain great amount of hydroxy group, itself is easily
Mutually absorption forms the particle of bigger particle diameter.At present silica is widely used in reinforcing rubber field, occupies titanium dioxide
More than the 70% of silicon total quantity consumed.Silica is applied in rubber, tearing strength, the anti-wear performance of rubber can be effectively improved
And wet-sliding resistant performance, effectively reduce rolling resistance, rubber heat.With the development of green tire from now on and popularization, titanium dioxide
The importance of silicon is highlighted further.
But silica, due to the presence of surface hydroxyl, silica presents extremely strong hydrophilicity, causes dioxy
Mutual agglomeration is serious between SiClx powder.It is same that this reunion behavior of silica itself has also had a strong impact on silica
The combination of rubber matrix so that silica is difficult to be spread out well in rubber matrix, and then reduces silica
Reinforcing effect in rubber.Silica surface is modified by the way that surface is modified, silicon-dioxide powdery can be improved
Hydrophobic performance, increases the dispersiveness of silica, significant to the practical application of silica.Silane idol is used at present
It is a kind of more universal modified method that connection agent is modified to silica.Modified by surface, silane coupler can effectively take
For the hydroxyl of silica surface, change the chemical environment of silica surface, by silicon-dioxide powdery by original hydrophily
It is changed into hydrophobicity.At present, general surface modifying method mainly has wet-process modified and dry method modification.Wherein wet-process modified application is more
Plus extensively, and it is general it is wet-process modified be directly in the solution to mix silicon-dioxide powdery with surface modifier, by changing
The empirical factors such as temperature, time are carrying out surface modification treatment.
The content of the invention
In view of the above problems, a kind of new silica surface modified method of present invention design, can obtain dispersiveness
The good silicon-dioxide powdery of hydrophobic performance.Concrete technical scheme is as follows：
A kind of method that high speed emulsifies modified precipitated silica, it is characterised in that comprise the following steps：
1) prepare 30～60ml alcohol solutions, be added thereto to the silane coupler of silica quality 5%～50%, and ultrasound
Process a period of time.
2) solution is poured into high-speed emulsifying machine, and adds the silica of certain mass, make silica and alcohol solution
Mass ratio is：2～10%, carry out high speed emulsification treatment.It is 1～5h to arrange high speed emulsification times, and at a high speed emulsification rotating speed is 1000
～5000r/min.After at a high speed emulsification terminates, by pulp centrifuged washing, drying, crushing obtains the silica being modified.
Ethanol and deionized water solution ratio are 8 in the alcohol solution:2～19:1.
Advantages of the present invention and effective effect are as follows：Precipitated silica as a kind of rubber-reinforcing filler, its own
Dispersiveness reinforcing effect is had a major impact.The modified polarity that can effectively reduce silica in the surface of silica, is reduced
Silica surface hydroxyl value.Reunite between silica so as to reduce, strengthen the reinforcing effect of silica.It is traditional at present
Modifying process seldom has decentralized processing to silicon-dioxide powdery, and emulsifies modifying process at a high speed and contain to silicon-dioxide powdery
High speed emulsion dispersion process, this dispersion process can effectively reduce the particle diameter of silica, silica particle diameter in the solution
Reduction can effectively improve the modified effect of silica.
Description of the drawings
Fig. 1 is the contact angle schematic diagram of the silica sample of embodiment 1；
Fig. 2 is the infrared spectrum of the silica sample of embodiment 1；
Fig. 3 is the thermal multigraph of the silica sample of embodiment 1；
Fig. 4 is the contact angle schematic diagram of the silica sample of embodiment 2；
Fig. 5 is the infrared spectrum of the silica sample of embodiment 2；
Fig. 6 is the thermal multigraph of the silica sample of embodiment 2；
Fig. 7 is the contact angle schematic diagram of the silica sample of embodiment 3；
Fig. 8 is the infrared spectrum of the silica sample of embodiment 3；
Fig. 9 is the thermal multigraph of the silica sample of embodiment 3；
Figure 10 is the contact angle schematic diagram of the silica sample of embodiment 4；
Figure 11 is the infrared spectrum of the silica sample of embodiment 4；
Figure 12 is the thermal multigraph of the silica sample of embodiment 4.
It is embodied as example
The present invention is specifically described below by embodiment, it is necessary to it is pointed out here that, following examples are served only for right
The present invention is described further, it is impossible to be interpreted as limiting the scope of the invention, professional and technical personnel in the field according to
Some nonessential modifications and adaptations that the content of invention is made, still fall within protection scope of the present invention.
Embodiment 1
(ethanol and deionized water ratio are 19 to take 100mL alcohol solutions:1) 0.5g silane couplers, are added thereto to.By solution
After ultrasonic a period of time, in pouring high-speed emulsifying machine into, and 10g silica is added.Emulsify at a high speed under the rotating speed of 4000r/min
2h.After at a high speed emulsification terminates, the silica that pulp centrifuged washing, drying, crushing are obtained being modified.The contact angle of sample shows
It is intended to as shown in figure 1, infrared spectrum is as shown in Fig. 2 thermogravimetric result is as shown in Figure 3.The contact angle that modified sample can be seen is
111.5 °, its infrared spectrum is in 2916cm-1、2849cm-1Place occurs in that the vibration peak of methyl and methylene, after being heated to 800 DEG C
Quality Down 11%.
Embodiment 2
(ethanol and deionized water ratio are 9 to take 100mL alcohol solutions:1) 1.4g silane couplers, are added thereto to.By solution
After ultrasonic a period of time, in pouring high-speed emulsifying machine into, and 7g silica is added.Emulsify at a high speed under the rotating speed of 5000r/min
5h.After at a high speed emulsification terminates, by the pulp centrifuged silica for obtaining and being modified.The contact angle schematic diagram of sample as shown in figure 4,
Infrared spectrum is as shown in figure 5, thermogravimetric result is as shown in Figure 6.The contact angle that modified sample can be seen is 102 °, its infrared spectrum
In 2910cm-1、2850cm-1The vibration peak of methyl and methylene is occurred in that, Quality Down 9% after being heated to 800 DEG C.
Embodiment 3
(ethanol and deionized water ratio are 8 to take 100mL alcohol solutions：1) 1.2g coupling agents, are added thereto to.By solution ultrasound
After a period of time, in pouring high-speed emulsifying machine into, and 4g silica is added.Emulsify 4h at a high speed under the rotating speed of 1000r/min.It is high
After speed emulsification terminates, the silica that pulp centrifuged washing, drying, crushing are obtained being modified.The contact angle schematic diagram of sample
As shown in fig. 7, infrared spectrum is as shown in figure 8, thermogravimetric result is as shown in Figure 9.The contact angle that modified sample can be seen is 93 °,
Its infrared spectrum is in 2918cm-1、2845cm-1The vibration peak of methyl and methylene is occurred in that, Quality Down after being heated to 800 DEG C
11%.
Embodiment 4
(ethanol and deionized water ratio are 19 to take 100mL alcohol solutions:1) 1g coupling agents, are added thereto to.By solution ultrasound one
After the section time, in pouring high-speed emulsifying machine into, and 2g silica is added.Emulsify 1h at a high speed under the rotating speed of 3000r/min.At a high speed
After emulsification terminates, the silica that pulp centrifuged washing, drying, crushing are obtained being modified.The contact angle schematic diagram of sample is such as
Shown in Figure 10, as shown in figure 11, thermogravimetric result is as shown in figure 12 for infrared spectrum.The contact angle that modified sample can be seen is
106 °, its infrared spectrum is in 2916cm-1、2840cm-1The vibration peak of methyl and methylene is occurred in that, quality after being heated to 800 DEG C
Decline 17%.
The present invention realizes titanium dioxide by high speed emulsifying technology in the technical foundation that traditional silicon dioxide is modified come a step
The dispersion and surface modification process of silicon, can obtain all good SiO 2 powder of dispersiveness and hydrophobic performance.
Claims (3)
1. a kind of method that high speed emulsifies improved silica, it is characterised in that comprise the following steps：
It is 8 in ethanol and deionized water quality ratio:2～19:In 1 alcohol solution, surfactant is added, above-mentioned solution is surpassed
After sound 30min, in being transferred to high-speed emulsifying machine, and silica is added, carry out surface modification treatment；By slurry after the completion of emulsification
Centrifuge washing, drying, crushing obtains modified silica；
The surfactant qualities of the addition are the 5%～50% of silica quality；
The time of the high speed emulsification is 1～5h, and rotating speed is 1000～5000r/min.
2. silica surface modified method according to claim 1, it is characterised in that adopt surface modification, institute
It is 2～10% with the mass ratio of alcohol solution and silica.
3. silica surface modified method according to claim 1, it is characterised in that the surface modifier is silane
Coupling agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611069345.8A CN106634055A (en) | 2016-11-29 | 2016-11-29 | Method for emulsifying and modifying silicon dioxide at high speed |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611069345.8A CN106634055A (en) | 2016-11-29 | 2016-11-29 | Method for emulsifying and modifying silicon dioxide at high speed |
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| CN106634055A true CN106634055A (en) | 2017-05-10 |
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| CN201611069345.8A Pending CN106634055A (en) | 2016-11-29 | 2016-11-29 | Method for emulsifying and modifying silicon dioxide at high speed |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111019400A (en) * | 2019-12-25 | 2020-04-17 | 烟台大学 | Silicon dioxide surface modification method based on homogeneous reaction system |
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| CN102408757A (en) * | 2011-09-15 | 2012-04-11 | 中国科学院金属研究所 | Solvent-based nano silicon oxide concentrated pulp and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111019400A (en) * | 2019-12-25 | 2020-04-17 | 烟台大学 | Silicon dioxide surface modification method based on homogeneous reaction system |
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