CN109867788A - A kind of preparation method of organosilicon-composite titania material - Google Patents
A kind of preparation method of organosilicon-composite titania material Download PDFInfo
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- CN109867788A CN109867788A CN201910201233.0A CN201910201233A CN109867788A CN 109867788 A CN109867788 A CN 109867788A CN 201910201233 A CN201910201233 A CN 201910201233A CN 109867788 A CN109867788 A CN 109867788A
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Abstract
The invention belongs to technical field of composite materials, and in particular to a kind of preparation method of organosilicon-composite titania material, step 1, methyl trichlorosilane is added and is stirred evenly into toluene, then titanium tetrachloride ultrasonic agitation is added and obtains mixed toluene liquid until stirring evenly；Step 2, microwave reaction 2-4h is slowly added dropwise into mixed toluene liquid in distilled water, until forming acidoid hydrolyzate；Step 3, it is passed through ammonia and adjusts pH to neutrality, catalyst is then added and carries out temperature-pressure polycondensation reaction, until forming dimensional network structure, obtains organosilicon-composite titania material.Present invention process is simple, and production cycle end, low cost product, stability is good, and uvioresistant performance is good.
Description
Technical field
The invention belongs to technical field of composite materials, and in particular to a kind of preparation of organosilicon-composite titania material
Method.
Background technique
Organic siliconresin has excellent weatherability, thermal stability and chemistry since it has-Si-O-Si- skeleton
Stability is widely used in organic pressure-sensitive gel, liquid silastic, coating etc. and cosmetic additive agent.Wherein, organosilicon is being used
When resin is as coating and cosmetic additive agent, in addition to various other performances of product to be considered, because the reason of climate change,
Usually also coating and cosmetics to be made to have anti-ultraviolet function, this function usually can by addition ultravioletlight screening agent come
It obtains.
Nano-titanium dioxide has the function of preferably to absorb ultraviolet light, thus is usually used in combination with organic siliconresin, to change
The ultraviolet absorption ability of kind organic siliconresin.But the prior art is usually simply to mix titanium dioxide with silicone resin
To prepare organic silicone compounds.Recently also there is using two-step method the compound for preparing organic siliconresin and titanium dioxide,
Such as " TiO2The preparation of/MQ silicone resin response type hybrid material and its performance study " (Xiang Hongping, Ge Jianfang, Hu Xinsong, Cui are few
It is big, Cheng Shaohui, organosilicon material, 2011,25 (6), 375) and " TiO2/SiO2The preparation of composite particles characterizes and in cosmetics
In application " (Wu Lin, South China Science & Engineering University's Master's thesis, 2011), method is the precursor sol for first preparing titanium dioxide
Afterwards, then with organic siliconresin or inorganic silicon raw material it is mixed with compound to carry out the modified organic siliconresin in surface with titanium dioxide
Object；For another example, the precursor sol of organic siliconresin is first prepared, then is mixed with titanium dioxide and dioxy is wrapped up with organic siliconresin
Change the organic siliconresin compound of titanium.But in the compound of above method preparation, titanium dioxide is all independent Cheng Yixiang, is covered
It covers in surface of silicone resin or is wrapped in organic siliconresin, only there are a small amount of Ti-O- in interface between two-phase
Si key, thus presence can only absorb 300nm ultraviolet light below, and ultraviolet ray transmissivity is still not less than 5%.In addition, above-mentioned
There is also complex process for two-step method, and the production cycle is long, the high deficiency of product cost.
Summary of the invention
For the problems of the prior art, the present invention provides a kind of preparation method of organosilicon-composite titania material,
Simple process, production cycle end, low cost product, stability is good, and uvioresistant performance is good.
To realize the above technical purpose, the technical scheme is that
A kind of preparation method of organosilicon-composite titania material, includes the following steps:
Step 1, methyl trichlorosilane is added and is stirred evenly into toluene, titanium tetrachloride ultrasonic agitation is then added, until stirring
It mixes uniformly, obtains mixed toluene liquid；
Step 2, microwave reaction 2-4h is slowly added dropwise into mixed toluene liquid in distilled water, until forming acidoid hydrolyzate；
Step 3, it is passed through ammonia and adjusts pH to neutrality, catalyst is then added and carries out temperature-pressure polycondensation reaction, until being formed vertical
Volume grid structure obtains organosilicon-composite titania material.
Concentration of the methyl trichlorosilane in toluene in the step 1 is 3-15g/L, the stirring speed stirred evenly
Degree is 1000-2000r/min.
The additional amount of titanium tetrachloride in the step 1 is the 20-40% of methyl trichlorosilane mole, and the ultrasound is stirred
The supersonic frequency mixed is 40-60kHz, and temperature is 10-30 DEG C.
The additional amount of distilled water in the step 2 is the 1-5% of methyl trichlorosilane mole, the dropwise addition being slowly added dropwise
Speed is 0.2-0.9mL/min.
The microwave power of microwave reaction in the step 2 is 300-700W, and temperature is 5-10 DEG C.
The speed that is passed through of ammonia in the step 3 is 0.1-0.5mL/min.
Catalyst in the step 3 uses alumina silicate.
The pressure of the temperature-pressure polycondensation reaction is 0.2-0.4MPa, and heating uses gradient-heated.
The program of the gradient-heated is as follows:
Methyl trichlorosilane is dissolved in toluene by step 1, forms good solute effect, while titanium tetrachloride being added to first
In benzene, titanium tetrachloride is quickly mixed to methyl trichlorosilane under ultrasound condition, forms mixed toluene solution.
Distilled water is slowly added dropwise to mixed toluene liquid step 2, until acidoid structure is formed, at this point, distilled water exists
Promote toluene trichlorosilane to form hydrolysis under aqueous adjusting, is converted into the disintegration of organosilicon primary water, while titanium tetrachloride can be with
Distilled water reaction forms good and stable titanium hydroxyl and hydrolyzes structure, since distilled water is in a small amount of, and is located at toluene solution
In, TiO 2 precursor is in colloidal, is mixed internal to the disintegration of organosilicon primary water.
Step 3, as acid-base modifier, converts neutrality for hydrolyzate by ammonia, then in catalyst and heat heating item
Disintegrate under part to organosilicon primary water and carry out polycondensation reaction, and it is promoted to convert to dimensional network structure, at the same time, dioxy
The colloform texture for changing titanium precursors is gradually converted into nano-titanium dioxide after dehydration, forms stable nano-titanium dioxide
Grain, and be evenly distributed in the dimensional network structure of organic siliconresin.
From the above, it can be seen that the present invention has following advantages:
1. present invention process is simple, production cycle end, low cost product, stability is good, and uvioresistant performance is good.
2. the present invention uses the cosolvency of methyl trichlorosilane and titanium tetrachloride in toluene, silicon titanium cosolvency is improved,
Effectively improve organosilicon effect in conjunction with the doping of titanium dioxide.
3. the water at low temperature that the present invention is effectively controlled titanium tetrachloride and methyl trichlorosilane by the way of hydrolysis is added dropwise
Effect is solved, hydrolysis between the two is promoted to combine, promotes binding characteristic of the titanium dioxide in organosilicon.
Specific embodiment
The present invention will be described in detail in conjunction with the embodiments, but does not do any restriction to claim of the invention.
Embodiment 1
A kind of preparation method of organosilicon-composite titania material, includes the following steps:
Step 1, methyl trichlorosilane is added and is stirred evenly into toluene, titanium tetrachloride ultrasonic agitation is then added, until stirring
It mixes uniformly, obtains mixed toluene liquid；
Step 2, microwave reaction 2h is slowly added dropwise into mixed toluene liquid in distilled water, until forming acidoid hydrolyzate；
Step 3, it is passed through ammonia and adjusts pH to neutrality, catalyst is then added and carries out temperature-pressure polycondensation reaction, until being formed vertical
Volume grid structure obtains organosilicon-composite titania material.
Concentration of the methyl trichlorosilane in toluene in the step 1 is 3g/L, the mixing speed stirred evenly
For 1000r/min.
The additional amount of titanium tetrachloride in the step 1 is the 20% of methyl trichlorosilane mole, the ultrasonic agitation
Supersonic frequency is 40kHz, and temperature is 10 DEG C.
The additional amount of distilled water in the step 2 is the 1% of methyl trichlorosilane mole, the dropwise addition speed being slowly added dropwise
Degree is 0.2mL/min.
The microwave power of microwave reaction in the step 2 is 300W, and temperature is 5 DEG C.
The speed that is passed through of ammonia in the step 3 is 0.1mL/min.
Catalyst in the step 3 uses alumina silicate.
The pressure of the temperature-pressure polycondensation reaction is 0.2MPa, and heating uses gradient-heated.
The program of the gradient-heated is as follows:
| Temperature | Time |
| 110℃ | 1h |
| 140℃ | 2h |
Embodiment 2
A kind of preparation method of organosilicon-composite titania material, includes the following steps:
Step 1, methyl trichlorosilane is added and is stirred evenly into toluene, titanium tetrachloride ultrasonic agitation is then added, until stirring
It mixes uniformly, obtains mixed toluene liquid；
Step 2, microwave reaction 4h is slowly added dropwise into mixed toluene liquid in distilled water, until forming acidoid hydrolyzate；
Step 3, it is passed through ammonia and adjusts pH to neutrality, catalyst is then added and carries out temperature-pressure polycondensation reaction, until being formed vertical
Volume grid structure obtains organosilicon-composite titania material.
Concentration of the methyl trichlorosilane in toluene in the step 1 is 15g/L, the mixing speed stirred evenly
For 2000r/min.
The additional amount of titanium tetrachloride in the step 1 is the 40% of methyl trichlorosilane mole, the ultrasonic agitation
Supersonic frequency is 60kHz, and temperature is 30 DEG C.
The additional amount of distilled water in the step 2 is the 5% of methyl trichlorosilane mole, the dropwise addition speed being slowly added dropwise
Degree is 0.9mL/min.
The microwave power of microwave reaction in the step 2 is 700W, and temperature is 10 DEG C.
The speed that is passed through of ammonia in the step 3 is 0.5mL/min.
Catalyst in the step 3 uses alumina silicate.
The pressure of the temperature-pressure polycondensation reaction is 0.4MPa, and heating uses gradient-heated.
The program of the gradient-heated is as follows:
| Temperature | Time |
| 12℃ | 2h |
| 150℃ | 4h |
Embodiment 3
A kind of preparation method of organosilicon-composite titania material, includes the following steps:
Step 1, methyl trichlorosilane is added and is stirred evenly into toluene, titanium tetrachloride ultrasonic agitation is then added, until stirring
It mixes uniformly, obtains mixed toluene liquid；
Step 2, microwave reaction 3h is slowly added dropwise into mixed toluene liquid in distilled water, until forming acidoid hydrolyzate；
Step 3, it is passed through ammonia and adjusts pH to neutrality, catalyst is then added and carries out temperature-pressure polycondensation reaction, until being formed vertical
Volume grid structure obtains organosilicon-composite titania material.
Concentration of the methyl trichlorosilane in toluene in the step 1 is 7g/L, the mixing speed stirred evenly
For 1500r/min.
The additional amount of titanium tetrachloride in the step 1 is the 30% of methyl trichlorosilane mole, the ultrasonic agitation
Supersonic frequency is 50kHz, and temperature is 20 DEG C.
The additional amount of distilled water in the step 2 is the 3% of methyl trichlorosilane mole, the dropwise addition speed being slowly added dropwise
Degree is 0.6mL/min.
The microwave power of microwave reaction in the step 2 is 500W, and temperature is 8 DEG C.
The speed that is passed through of ammonia in the step 3 is 0.3mL/min.
Catalyst in the step 3 uses alumina silicate.
The pressure of the temperature-pressure polycondensation reaction is 0.3MPa, and heating uses gradient-heated.
The program of the gradient-heated is as follows:
| Temperature | Time |
| 115℃ | 2h |
| 145℃ | 3h |
Embodiment 4
A kind of preparation method of organosilicon-composite titania material, includes the following steps:
Step 1, methyl trichlorosilane is added and is stirred evenly into toluene, titanium tetrachloride ultrasonic agitation is then added, until stirring
It mixes uniformly, obtains mixed toluene liquid；
Step 2, microwave reaction 3h is slowly added dropwise into mixed toluene liquid in distilled water, until forming acidoid hydrolyzate；
Step 3, it is passed through ammonia and adjusts pH to neutrality, catalyst is then added and carries out temperature-pressure polycondensation reaction, until being formed vertical
Volume grid structure obtains organosilicon-composite titania material.
Concentration of the methyl trichlorosilane in toluene in the step 1 is 12g/L, the mixing speed stirred evenly
For 1800r/min.
The additional amount of titanium tetrachloride in the step 1 is the 35% of methyl trichlorosilane mole, the ultrasonic agitation
Supersonic frequency is 55kHz, and temperature is 25 DEG C.
The additional amount of distilled water in the step 2 is the 4% of methyl trichlorosilane mole, the dropwise addition speed being slowly added dropwise
Degree is 0.7mL/min.
The microwave power of microwave reaction in the step 2 is 600W, and temperature is 8 DEG C.
The speed that is passed through of ammonia in the step 3 is 0.4mL/min.
Catalyst in the step 3 uses alumina silicate.
The pressure of the temperature-pressure polycondensation reaction is 0.3MPa, and heating uses gradient-heated.
The program of the gradient-heated is as follows:
| Temperature | Time |
| 115℃ | 2h |
| 145℃ | 2h |
Performance detection
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example | |
| Ultraviolet light transmittance | 0.1% | 0.1% | 0.1% | 0.1% | 5.8 |
| Visible light transmittance rate | 98.2% | 98.1% | 98.6% | 98.6% | 96.2% |
| Illumination sterilizing rate | 99.7% | 99.8% | 99.9% | 99.9% | 23.3% |
In conclusion the invention has the following advantages that
1. present invention process is simple, production cycle end, low cost product, stability is good, and uvioresistant performance is good.
2. the present invention uses the cosolvency of methyl trichlorosilane and titanium tetrachloride in toluene, silicon titanium cosolvency is improved,
Effectively improve organosilicon effect in conjunction with the doping of titanium dioxide.
3. the water at low temperature that the present invention is effectively controlled titanium tetrachloride and methyl trichlorosilane by the way of hydrolysis is added dropwise
Effect is solved, hydrolysis between the two is promoted to combine, promotes binding characteristic of the titanium dioxide in organosilicon.
It is understood that being merely to illustrate the present invention above with respect to specific descriptions of the invention and being not limited to this
Technical solution described in inventive embodiments.Those skilled in the art should understand that still can be carried out to the present invention
Modification or equivalent replacement, to reach identical technical effect；As long as meet use needs, all protection scope of the present invention it
It is interior.
Claims (9)
1. a kind of preparation method of organosilicon-composite titania material, characterized by the following steps:
Step 1, methyl trichlorosilane is added and is stirred evenly into toluene, titanium tetrachloride ultrasonic agitation is then added, until stirring
It mixes uniformly, obtains mixed toluene liquid；
Step 2, microwave reaction 2-4h is slowly added dropwise into mixed toluene liquid in distilled water, until forming acidoid hydrolyzate；
Step 3, it is passed through ammonia and adjusts pH to neutrality, catalyst is then added and carries out temperature-pressure polycondensation reaction, until being formed vertical
Volume grid structure obtains organosilicon-composite titania material.
2. the preparation method of organosilicon-composite titania material according to claim 1, it is characterised in that: the step
Concentration of the methyl trichlorosilane in toluene in rapid 1 is 3-15g/L, and the mixing speed stirred evenly is 1000-
2000r/min。
3. the preparation method of organosilicon-composite titania material according to claim 1, it is characterised in that: the step
The additional amount of titanium tetrachloride in rapid 1 is the 20-40% of methyl trichlorosilane mole, and the supersonic frequency of the ultrasonic agitation is
40-60kHz, temperature are 10-30 DEG C.
4. the preparation method of organosilicon-composite titania material according to claim 1, it is characterised in that: the step
The additional amount of distilled water in rapid 2 is the 1-5% of methyl trichlorosilane mole, and the rate of addition being slowly added dropwise is 0.2-
0.9mL/min。
5. the preparation method of organosilicon-composite titania material according to claim 1, it is characterised in that: the step
The microwave power of microwave reaction in rapid 2 is 300-700W, and temperature is 5-10 DEG C.
6. the preparation method of organosilicon-composite titania material according to claim 1, it is characterised in that: the step
The speed that is passed through of ammonia in rapid 3 is 0.1-0.5mL/min.
7. the preparation method of organosilicon-composite titania material according to claim 1, it is characterised in that: the step
Catalyst in rapid 3 uses alumina silicate.
8. the preparation method of organosilicon-composite titania material according to claim 1, it is characterised in that: described to add
The pressure of temperature pressurization polycondensation reaction is 0.2-0.4MPa, and heating uses gradient-heated.
9. the preparation method of organosilicon-composite titania material according to claim 8, it is characterised in that: the ladder
The program for spending heating is as follows: the heating-up time from 110 DEG C to 120 DEG C is 1 to 2 hours, the heating-up time from 140 DEG C to 150 DEG C
It is 2 to 4 hours.
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