CN101746764A - Hydrophobic silica and preparation method thereof - Google Patents
Hydrophobic silica and preparation method thereof Download PDFInfo
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- CN101746764A CN101746764A CN200810203830A CN200810203830A CN101746764A CN 101746764 A CN101746764 A CN 101746764A CN 200810203830 A CN200810203830 A CN 200810203830A CN 200810203830 A CN200810203830 A CN 200810203830A CN 101746764 A CN101746764 A CN 101746764A
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Abstract
The invention provides hydrophobic silica and a preparation method thereof; the method mainly comprises that general hydrophilic silica (the surface area is 100 to 400m2/g), silicone oil, a dispersant, a catalyst and a molecular weight regulator react under appropriate conditions to prepare a solid powdery silica with polysiloxane graft on the surface, and the hydrophobic contact angle thereof reaches 70 to 150 degrees; and the invention not only has good hydrophobic nature, and simultaneously has a deforming function, and is applicable to a textile dyeing and finishing process.
Description
Technical field
The present invention relates to silicon-dioxide, specifically, the present invention relates to a kind of hydrophobic silica and manufacture method thereof.
Background technology
The silicon-dioxide purposes is very extensive, at coating, in printing ink, plastics, rubber and the makeup, all can add silicon-dioxide usually to increase performance, as oil suction, delustring, reinforcement mechanicalness etc., can reduce cost simultaneously.Its surface property must meet the characteristic that is added thing, so that can homodisperse.The general industry grade silicon dioxide is because preparation technology's difference can be divided into two kinds, a kind of is dry type, sintered type, and a kind of is wet type, sedimentation type, both surface-area differences, the hydroxyl that its surface has is (OH) also different, in general, the former is less, and the latter is more, wetting ability all is partial on the two surface, if will be applied in the lipophilicity polymer then silica sphere to be anticipated into hydrophobicity, have effect preferably as coating, rubber etc.
General hydrophobic method that silica sphere is anticipated into commonly used is to utilize the absorption of solid surface to tensio-active agent, changes the polarity of solid surface.As Zinc Stearate is dissolved in the polar solvent, adding silicon-dioxide removes and desolvates, and then the zine ion part is towards silicon-dioxide, and hard ester dialkylaminobenzoic acid part is towards the outside, thus formation particle surface hydrophobicity; Perhaps, silicon-dioxide is added silicoorganic compound, methoxyl group on the Siliciumatom becomes moving oxygen base, can (OH) react with the hydroxyl of silica sphere, organic moiety (vinyl, epoxy group(ing), propenyl etc.) then outward, this not only can make silica sphere be hydrophobicity, has more reactivity, thereby also can increase its physical strength with part interlinkages such as lipophilicity polymers.
But, though transferring hydrophobic method to by wetting ability, above-mentioned silicon-dioxide make silica sphere be hydrophobic property, do not have good their defoaming function.Therefore, the object of the present invention is to provide a kind of silicon-dioxide of surface grafting polysiloxane, surface-area is 100～400m
2/ g, surperficial tool hydrophobicity and have their defoaming function concurrently, preparation technology is simple, can be in normal pressure, operation below 100 ℃, and do not produce byproduct (as hydrogenchloride).
Summary of the invention
First aspect of the present invention provides a kind of manufacture method of hydrophobic silica, may further comprise the steps:
(1) at normal temperatures, wetting ability silica solid powder, silicone oil, molecular weight regulator, dispersion agent and catalyst are mixed, the weight ratio of wherein said wetting ability silica solid powder, silicone oil, molecular weight regulator is 2-3: 1: 0.005-0.02, the weight of described dispersion agent is 2.7 times of above-mentioned three kinds of reactant gross weights, stirred 5-20 minute, the contact angle of wherein said wetting ability silica solid powder is every gram 100-400m less than 70 °, surface-area
2Described molecular weight regulator is a kind of in hexamethyldisiloxane, pentamethyl-methoxy silane, the tetramethyl disiloxane, and described dispersion agent is mineral oil, prestox Fourth Ring siloxanes or dimethylbenzene; Described catalyst is Lewis acid or Lewis base;
(2) be warming up to 60 ℃-80 ℃, continue to mix 30-120 minute, form hydrophobic silica with reaction;
(3) wash and filter described hydrophobic silica with organic solvent extracting; And
(4) remove described organic solvent and remaining reactants.
Preferably, the weight ratio of wetting ability silica solid powder, silicone oil and molecular weight regulator is 2-3 in the described step (1): 1: 0.01.
Preferably, Lewis acid or Lewis base are sodium hydroxide, potassium hydroxide, volatile salt or sulfuric acid in the described step (1), and consumption is 0.1-1wt%.
Preferably, mixing in the described step (1) is to carry out in clarifixator.
Preferably, be warming up to 80 ℃ in the described step (2), mixing time is 30 minutes.
Preferably, organic solvent is a dimethylbenzene in the described step (3).
Preferably, described step (4) drying in 120 ℃ of baking ovens was finished in 6 hours.
In Glass Containers, add
(1) dispersion agent as mineral oil, organic solvent (dimethylbenzene), prestox Fourth Ring siloxanes or silicone oil, can make the surface of silicon-dioxide fully contact with polysiloxane molecule;
(2) wetting ability silica solid powder, its surface-area are 100～400m
2/ g, contact angle is less than 70 °;
(3) silicone oil;
(4) catalyst, as aqueous sodium hydroxide solution, potassium hydroxide aqueous solution, soda acids such as ammonium carbonate solution or sulfuric acid;
(5) molecular weight regulator, its purpose are to make the silicon compound molecular weight that grafts on the silicon dioxide granule suitable, and be commonly used as tetramethyl disiloxane, hexamethyldisiloxane or pentamethyl-methoxy silane.
Homogenized 5 to 20 minutes with the clarifixator mixing, be warming up to 60 ℃～80 ℃ then, continue to stir and to homogenize 30 to 120 minutes, filter and wash the hydrophobic silica pressed powder of reaction gained, in about 120 ℃ baking oven dry about 6 hours with organic solvent (as dimethylbenzene) collection.
Second hydrophobic silica that the aspect provides aforesaid method to make of the present invention, its hydrophobic contact angle is 70-150 °.
Beneficial effect of the present invention is:
The silica surface area of surface grafting polysiloxane of the present invention is 100～400m
2/ g, surperficial tool hydrophobicity and have their defoaming function concurrently, preparation technology is simple, can be in normal pressure, operation below 100 ℃, and do not produce byproduct (as hydrogenchloride), applicable to the textile dyeing and finishing process.
Embodiment
Below for a more detailed description with embodiment to the present invention.These embodiment only are the descriptions to best mode for carrying out the invention, scope of the present invention are not had any restriction.
Embodiment:
Get 80g dimethylbenzene, place the Glass Containers of 200ml, add 10g silicone oil, the 0.1g hexamethyldisiloxane, 2 10wt% sodium hydroxide, 20g wetting ability silica solid powder, the particle diameter of this wetting ability silica solid powder is 30nm, surface-area is 200m
2/ g spoon.Mix to homogenize 10 minutes with clarifixator, reheat to 80 ℃ continues to mix homogenizing 30 minutes, filters, and washes with the dimethylbenzene collection again, obtains polysiloxane and connects skill silica solid powder, places 120 ℃ of baking ovens, dry about 6 hours.
Claims (8)
1. the manufacture method of a hydrophobic silica may further comprise the steps:
(1) at normal temperatures, wetting ability silica solid powder, silicone oil, molecular weight regulator, dispersion agent and catalyst are mixed, the weight ratio of wherein said wetting ability silica solid powder, silicone oil, molecular weight regulator is 2-3: 1: 0.005-0.02, the weight of described dispersion agent is 2.7 times of above-mentioned three kinds of reactant gross weights, stirred 5-20 minute, the contact angle of wherein said wetting ability silica solid powder is every gram 100-400m less than 70 °, surface-area
2Described molecular weight regulator is a kind of in hexamethyldisiloxane, pentamethyl-methoxy silane, the tetramethyl disiloxane, and described dispersion agent is mineral oil, prestox Fourth Ring siloxanes or dimethylbenzene; Described catalyst is Lewis acid or Lewis base;
(2) be warming up to 60 ℃-80 ℃, continue to mix 30-120 minute, form hydrophobic silica with reaction;
(3) wash and filter described hydrophobic silica with organic solvent extracting; And
(4) remove described organic solvent and remaining reactants.
2. manufacture method as claimed in claim 1 is characterized in that, the weight ratio of wetting ability silica solid powder, silicone oil and molecular weight regulator is 2-3 in the described step (1): 1: 0.01.
3. manufacture method as claimed in claim 1 is characterized in that, Lewis acid or Lewis base are sodium hydroxide, potassium hydroxide, volatile salt or sulfuric acid in the described step (1), and consumption is 0.1-1wt%.
4. manufacture method as claimed in claim 1 is characterized in that, mixing in the described step (1) is to carry out in clarifixator.
5. manufacture method as claimed in claim 1 is characterized in that, is warming up to 80 ℃ in the described step (2), and mixing time is 30 minutes.
6. manufacture method as claimed in claim 1 is characterized in that, organic solvent is a dimethylbenzene in the described step (3).
7. manufacture method as claimed in claim 1 is characterized in that, described step (4) drying in 120 ℃ of baking ovens was finished in 6 hours.
8. the described method of claim 1 and the hydrophobic silica that makes, its hydrophobic contact angle is 70-150 °.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810203830A CN101746764A (en) | 2008-12-02 | 2008-12-02 | Hydrophobic silica and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810203830A CN101746764A (en) | 2008-12-02 | 2008-12-02 | Hydrophobic silica and preparation method thereof |
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| CN101746764A true CN101746764A (en) | 2010-06-23 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN200810203830A Pending CN101746764A (en) | 2008-12-02 | 2008-12-02 | Hydrophobic silica and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106854368A (en) * | 2015-12-08 | 2017-06-16 | 信越化学工业株式会社 | Inorganic particle silicone composites, the dispersion comprising compound and solid material and preparation method |
| CN108083286A (en) * | 2018-01-05 | 2018-05-29 | 江苏联瑞新材料股份有限公司 | A kind of preparing spherical SiO 2 micro mist and its preparation method and application |
| CN109592690A (en) * | 2018-12-18 | 2019-04-09 | 山东东岳有机硅材料股份有限公司 | A method of hydrophobic silica is prepared using fumed silica |
-
2008
- 2008-12-02 CN CN200810203830A patent/CN101746764A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106854368A (en) * | 2015-12-08 | 2017-06-16 | 信越化学工业株式会社 | Inorganic particle silicone composites, the dispersion comprising compound and solid material and preparation method |
| CN108083286A (en) * | 2018-01-05 | 2018-05-29 | 江苏联瑞新材料股份有限公司 | A kind of preparing spherical SiO 2 micro mist and its preparation method and application |
| CN109592690A (en) * | 2018-12-18 | 2019-04-09 | 山东东岳有机硅材料股份有限公司 | A method of hydrophobic silica is prepared using fumed silica |
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Open date: 20100623 |