CN107500302A - A kind of hydrophobic precipitated silica and preparation method thereof - Google Patents
A kind of hydrophobic precipitated silica and preparation method thereof Download PDFInfo
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- CN107500302A CN107500302A CN201710893609.XA CN201710893609A CN107500302A CN 107500302 A CN107500302 A CN 107500302A CN 201710893609 A CN201710893609 A CN 201710893609A CN 107500302 A CN107500302 A CN 107500302A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- C—CHEMISTRY; METALLURGY
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Abstract
Hydrophilic precipitated silica is subjected to hydrophobic treatment the invention provides one kind, the method that hydrophobic precipitated silica is finally made.Surface modifier is made first with aliphatic compound and quaternary ammonium salt heating stirring, then by held for some time after the heating stirring of hydrophilic precipitated silica, uniformly hydrophobic precipitated silicon dioxide is made in spray held for some time on hydrophilic precipitated silica after finally surface modifier is atomized under the conditions of 150 230 DEG C.Obtained hydrophobic precipitated silicon dioxide, with particle diameter is small, surface area is big, the advantages of good dispersion, the fields such as engineering plastics, silicon rubber, adhesive, dyestuff, defoamer can be widely applied to, the modifying agent is free of solvent, safety and environmental protection, technique is simpler simultaneously, it is not high to equipment requirement, not using acid base catalysator, harmful effect will not be produced to later stage use.
Description
Technical field
The present invention relates to a kind of hydrophobic precipitated silica and preparation method thereof, belong to technical field of fine.
Technical background
The heat that silica is divided into hydrated SiO 2 made from the precipitation method (being precipitated silica) and gas phase legal system obtains
Silica (being aerosil) is split, is referred to as general silica, they belong to amorphous silica.It is existing
It with this two classes general silica is that base stock produces that hydrophobic silica, which is, is a kind of white, nontoxic, amorphous fine
Powder.Initial size is generally 10~40nm, because surface is contained compared with polyhydroxy, particulate that is hygroscopic and turning into aggregation.
Silica has porous, internal surface area big, polymolecularity, light, chemical stability is good, high temperature resistant, non-ignitable
Burn, the excellent properties such as electrical insulating property is good.The filler of the products such as rubber, plastics, synthetic resin and paint is mainly used as, also may be used
As lubricant and insulating materials.The silica in the whole world 70% is used for rubber industry at present, is excellent rubber reinforcing filler,
Cementing property and tear resistance can be improved, its performance is better than ordinary carbon black.However, due to the particularity of silica surface structure,
I.e. specific surface area is larger and exhibiting high surface hydroxyl make it that the surface energy of white carbon is higher, and hydrophily is strong.Above property have impact on
White carbon is uniformly distributed, and reduces the performance of its function, application of the white carbon in organic field is limited, in order to improve white carbon
The activity hydroxy on surface and organic material invade profit and dispersiveness, reduce paint surface energy, it is necessary to be modified by white carbon surface.In vain
With organic compound bonding reaction occurs for the activity hydroxy of carbon black, and white carbon surface is changed into hydrophobicity by hydrophily, improved
Interface bond strength between white carbon and organic molecule, the combination property and accessories of a product value of material are improved, expands product
Application field.
It is to make hydrophilic silicon oxides by certain process using surface modifier that the surface of silica, which is modified,
Surface hydroxyl reacted with surface modifier, reduce surface hydroxyl quantity, product is changed into hydrophobic from hydrophilic, reduce group
It is poly-, increase its dispersiveness in the polymer.The surface modifier commonly used in domestic and international more scholar's research has organosilicon halogenation
Compound, type siloxane organic compound, alcohol compound, silazane class compound, organic polymer species and silane coupler class.
The surface of H.Barthel dimethyl methoxy silane modified manometer silicon dioxides, its modified effect compare trimethyl
Methoxy silane is modified, and research shows that the interaction that the data of gas absorption are disclosed between particulate is in silicon by polymer
Mutual osmosis is formed during alkanisation.Amino silicane coupling agent (APS) modified nano-silica such as Mathieu Etienne
Silicon.APS and nano silicon are dispersed in reflux in toluene to stir 2 hours, then high temperature assimilation 2 hours, adds grafting
The thickness of layer, improve the degree of cross linking of composite.CN92110674.2 describes to be added in precipitated silica filter cake
Polysiloxane inorganic agent is handled, and by drying, coarse crushing, 150~450 DEG C of high-temperature activations, is crushed and is made hydrophobic two
Silica.It is with dry general silica and organic water repellent agent or inorganic hydrophobic that US4054689, which is described a kind of,
The steam of reason agent contacts and reacts obtained hydrophobic silica.That is introduced in FR2613708 adds people to have into general silica
Machine water-repelling agent and the method that high-temperature high-voltage reaction is carried out in autoclave.CN201310123633 is described using macromolecule modified
Agent emulsion is mixed and modified to silica suspension, by drying, hydrophobic silica made from grinding.CN103450504B
Describe a kind of rubber White carbon black dispersant and preparation method thereof：Fatty acid soaps salt and the ester of pentaerythrite stearic acid four are existed
Stirring, melting mixing under 80-110 degree, stearic amide or acid amides stirring are then added under 100-130 degree, is melted, melting
It is granulated after cooling film-making or melting, the dispersant as rubber white carbon.Described in CN1405238A using containing a large amount of
The method that the silica of water applies in silicone oil and prepares hydrophobic precipitated silicon dioxide in 200~400 DEG C of oxidisability annealing, is obtained
Hydrophobic precipitated silicon dioxide specific surface area be 50~110m2/g.CN101817529A is described silica in logical nitrogen
Under protection, mixed in 250~300 DEG C of heat-activateds 4~5 hours, then by the silica after activation with toluene diisocyanate
Close, anhydrous dimethyl benzene is added into said mixture, be stirred scattered, reheating processing under nitrogen protection, in room temperature, so
After filtered, dry, obtain improved silica.CN1132500A is described by making the water glass solution in pH value be with acid
Reacted when 7.5~11, the ion group in the silica hydrogel for removing generation is washed with the inorganic base aqueous solution of water or dilution
Point, the pH value range of hydrogel is during which maintained 7.5~11, the aqueous phase that is included in hydrogel is replaced with alcohol and then to obtaining
Alcogel carries out supercritical drying.CN101514263A describes handles titanium dioxide by coupling agent and stearic acid-acetone soln
Silicon.Utilize poly- organic hydrogen-containing siloxane, coupling agent and polyethers that polymer occurs under acidic catalyst in CN102286220B anti-
Surface modifier should be obtained, hydrophobically modified then is carried out to hydrophilic precipitated silica, dries pulverizing obtains.With these methods
Hydrophobic treatment is carried out to precipitated silica, complex process is higher to equipment requirement, also needs to locate after carrying out when using solvent
Reason, the residual of acid base catalysator can also influence follow-up application performance.
The present invention is had found by many experiments, is incubated the table of preparation under air-tight state with aliphatic compound and quaternary ammonium salt
Face modifying agent, using surface modifier after insulation carries out hydrophobic treatment to the hydrophilic white carbon of the precipitation method under atomizing spray acts on,
Obtained hydrophobic precipitated silicon dioxide, there is the advantages of particle diameter is small, surface area is big, good dispersion, can be widely applied to
The fields such as engineering plastics, silicon rubber, adhesive, dyestuff, defoamer, the modifying agent be free of solvent, safety and environmental protection, while technique compared with
Simply, it is not high to equipment requirement, not using acid base catalysator, harmful effect will not be produced to later stage use.
The content of the invention
The present invention provides a kind of surface for utilizing the insulated and stirred preparation under air-tight state of aliphatic compound and quaternary ammonium salt
Modifying agent；Then hydrophilic precipitated silica is put into reactor to held for some time after stirring and heating up；Finally by surface
Uniformly spray obtains hydrophobic precipitated silicon dioxide after hydrophilic precipitated silica silicon face, isothermal holding after modifying agent atomization.
Technical scheme
Hydrophobic precipitated silica of the present invention and preparation method thereof, by following material composition：
A, surface modifier A：By aliphatic compound, the insulated and stirred under air-tight state is made with quaternary ammonium salt.
A1, aliphatic compound
The aliphatic compound general structure is as follows：
[(CH3)m(CH2)n(CH)p]R1 q+1
R1Selected from-OH ,-COOH；Q is 0,1 or 2；P is 0 or 1；N is 0-13 integer；M is 0,1 or 2；m+n+p
≤14；M+n+p >=2, the aliphatic compound dosage are the 11~63% of the surface modifier gross mass.
A2, quaternary ammonium salt
The quaternary ammonium salt structure formula is as follows：
R2R3R4R5N+X-
R in structural formula2、R3、R4、R5Can be the straight chained alkyl that carbon number is 1~8, selected from methyl, second with identical or different
Base, butyl, hexyl, heptyl, octyl group；X is selected from chlorine atom, bromine atoms.Dosage for the surface modifier gross mass 37~
89%.
B, hydrophilic precipitated silica
The hydrophilic precipitated silica B, specific surface area 50-500m2/g。
Surface modifier A and hydrophilic precipitated silica B mass ratio is 1: 5~1: 9.
The preparation method of hydrophobic precipitated silicon dioxide of the present invention is as follows：
(1) aliphatic compound A1 and quaternary ammonium salt A2 are put into reaction vessel in proportion, sealed, agitating and heating, in 40
~90 DEG C of 0.5~2h of insulation, obtain surface modifier A；
(2) hydrophilic precipitated silica B is put into reactor and stirs and be warming up to 100-140 DEG C of insulation 0.5-2h；
(3) 150-230 DEG C is continuously heating to, is uniformly sprayed after surface modifier A is atomized on silica B surface,
Insulation 4~6h processing obtains the hydrophobic precipitated silicon dioxide N.
Specific implementation method
Embodiment 1
In 250mL flasks, 34.5g octanoic acid and 65.5g ammonium bromide and tetraoctyl ammonium bromide are put into, sealing, is stirred and water-bath adds
Heat is incubated 1h, obtains surface modifier A1 to 90 DEG C.
It in the hydrophilic precipitated silica input reactors of 500g, will stir and be warming up to 120 DEG C of insulation 1h, be continuously heating to
160 DEG C, uniformly on hydrophilic precipitated silica silicon face, insulation 6h processing obtains hydrophobic spray after surface modifier A1 is atomized
Precipitated silica N1.
Embodiment 2
In 250mL flasks, put into 11g ethanol and 89g four octyl group ammonium chlorides, seal, stir and heating water bath extremely
70 DEG C, 1.5h is incubated, obtains surface modifier A2.
It in the hydrophilic precipitated silica input reactors of 580g, will stir and be warming up to 140 DEG C of insulation 0.5h, continue to heat up
To 190 DEG C, uniformly spray on hydrophilic precipitated silica silicon face, dredged by insulation 4h processing after surface modifier A2 is atomized
Water sedimentation silica N2.
Embodiment 3
In 250mL flasks, 49.7g decyl alcohol and 50.3g TBAB are put into, is sealed, stirs and water-bath adds
Heat is incubated 2h, obtains surface modifier A3 to 80 DEG C.
It in the hydrophilic precipitated silica input reactors of 600g, will stir and be warming up to 100 DEG C of insulation 2h, be continuously heating to
230 DEG C, uniformly on hydrophilic precipitated silica silicon face, insulation 4h processing obtains hydrophobic spray after surface modifier A3 is atomized
Precipitated silica N3.
Embodiment 4
In 250mL flasks, 63g ten tetra-carbonics and 37g tetrabutylammonium chloride are put into, is sealed, stirs and water-bath adds
Heat is incubated 1h, obtains surface modifier A4 to 90 DEG C.
It in the hydrophilic precipitated silica input reactors of 650g, will stir and be warming up to 110 DEG C of insulation 1.5h, continue to heat up
To 210 DEG C, uniformly spray on hydrophilic precipitated silica silicon face, dredged by insulation 5h processing after surface modifier A4 is atomized
Water sedimentation silica N4.
Embodiment 5
In 250mL flasks, 36.8g isooctyl acid and 63.2g methyl tricapryl ammonium chloride are put into, is sealed, stirring is simultaneously
Heating water bath is incubated 2h, obtains surface modifier A5 to 60 DEG C.
It in the hydrophilic precipitated silica input reactors of 700g, will stir and be warming up to 110 DEG C of insulation 1.5h, continue to heat up
To 170 DEG C, uniformly spray on hydrophilic precipitated silica silicon face, dredged by insulation 6h processing after surface modifier A5 is atomized
Water sedimentation silica N5.
Embodiment 6
In 250mL flasks, 42.5g laruyl alcohol and 57.5g four octyl group ammonium chlorides are put into, is sealed, stirs simultaneously water-bath
80 DEG C are heated to, 1.5h is incubated, obtains surface modifier A6.
It in the hydrophilic precipitated silica input reactors of 750g, will stir and be warming up to 130 DEG C of insulation 1h, be continuously heating to
180 DEG C, uniformly on hydrophilic precipitated silica silicon face, insulation 5h processing obtains hydrophobic spray after surface modifier A6 is atomized
Precipitated silica N6.
Embodiment 7
In 250mL flasks, 23.2g propionic acid and 76.8g four heptyl ammonium bromides are put into, is sealed, stirs and water-bath adds
Heat is incubated 1h, obtains surface modifier A7 to 40 DEG C.
It in the hydrophilic precipitated silica input reactors of 850g, will stir and be warming up to 120 DEG C of insulation 1h, be continuously heating to
150 DEG C, uniformly on hydrophilic precipitated silica silicon face, insulation 6h processing obtains hydrophobic spray after surface modifier A7 is atomized
Precipitated silica N7.
Embodiment 8
In 250mL flasks, 29.8g caproic acid and 70.2g ammonium bromide and tetraoctyl ammonium bromide are put into, is sealed, stirs and water-bath adds
Heat is incubated 0.5h, obtains surface modifier A8 to 50 DEG C.
It in the hydrophilic precipitated silica input reactors of 900g, will stir and be warming up to 110 DEG C of insulation 1.5h, continue to heat up
To 200 DEG C, uniformly spray on hydrophilic precipitated silica silicon face, dredged by insulation 4h processing after surface modifier A8 is atomized
Water sedimentation silica N8.
Embodiment 9
In 250mL flasks, put into 36g acetic acid and 64g tetraethylammonium bromide, seal, stir and heating water bath extremely
40 DEG C, 2h is incubated, obtains surface modifier A9.
It in the hydrophilic precipitated silica input reactors of 600g, will stir and be warming up to 100 DEG C of insulation 2h, be continuously heating to
200 DEG C, uniformly on hydrophilic precipitated silica silicon face, insulation 5h processing obtains hydrophobic spray after surface modifier A9 is atomized
Precipitated silica N9.
Embodiment 10
In 250mL flasks, 40g isooctanol and 60g four hexyl ammonium chlorides are put into, is sealed, stirs simultaneously heating water bath
To 50 DEG C, 1.8h is incubated, obtains surface modifier A10.
It in the hydrophilic precipitated silica input reactors of 700g, will stir and be warming up to 110 DEG C of insulation 1.5h, continue to heat up
To 150 DEG C, uniformly on hydrophilic precipitated silica silicon face, insulation 6h processing obtains spray after surface modifier A10 is atomized
Hydrophobic precipitated silicon dioxide N10.
Embodiment 11
In 250mL flasks, put into 17g 7 glycol and 83g ammonium bromide and tetraoctyl ammonium bromide, seal, stir and heating water bath extremely
60 DEG C, 1.6h is incubated, obtains surface modifier A11.
It in the hydrophilic precipitated silica input reactors of 800g, will stir and be warming up to 120 DEG C of insulation 1.2h, continue to heat up
To 180 DEG C, uniformly on hydrophilic precipitated silica silicon face, insulation 5h processing obtains spray after surface modifier A11 is atomized
Hydrophobic precipitated silicon dioxide N11.
Embodiment 12
In 250mL flasks, 28.7g ethanedioic acid and 71.3g four heptyl ammonium chlorides are put into, is sealed, stirs simultaneously water-bath
70 DEG C are heated to, 1.5h is incubated, obtains surface modifier A12.
It in the hydrophilic precipitated silica input reactors of 900g, will stir and be warming up to 130 DEG C of insulation 1h, be continuously heating to
230 DEG C, uniformly spray on hydrophilic precipitated silica silicon face, dredged by insulation 4h processing after surface modifier A12 is atomized
Water sedimentation silica N12.
Embodiment 13
In 250mL flasks, 31.3g glycerine and 68.7g methyl tricapryl ammonium chloride are put into, is sealed, stirring is simultaneously
Heating water bath is incubated 1h, obtains surface modifier A13 to 80 DEG C.
It in the hydrophilic precipitated silica input reactors of 750g, will stir and be warming up to 140 DEG C of insulation 0.5h, continue to heat up
To 220 DEG C, uniformly on hydrophilic precipitated silica silicon face, insulation 5h processing obtains spray after surface modifier A13 is atomized
Hydrophobic precipitated silicon dioxide N13.
Embodiment 14
In 250mL flasks, 42g decanedioic acid and 58g tetrabutylammonium chloride are put into, is sealed, stirs simultaneously heating water bath
To 90 DEG C, 0.5h is incubated, obtains surface modifier A14.
It in the hydrophilic precipitated silica input reactors of 820g, will stir and be warming up to 135 DEG C of insulation 1h, be continuously heating to
160 DEG C, uniformly on hydrophilic precipitated silica silicon face, insulation 5.5h processing obtains spray after surface modifier A14 is atomized
Hydrophobic precipitated silicon dioxide N14.
Embodiment 15
In 250mL flasks, 42g propane diols and 58g tetraethylammonium bromide are put into, is sealed, stirs simultaneously heating water bath
To 75 DEG C, 1.3h is incubated, obtains surface modifier A15.
It in the hydrophilic precipitated silica input reactors of 850g, will stir and be warming up to 115 DEG C of insulation 1.5h, continue to heat up
To 175 DEG C, uniformly on hydrophilic precipitated silica silicon face, insulation 4h processing obtains spray after surface modifier A15 is atomized
Hydrophobic precipitated silicon dioxide N15.
Embodiment 16
In 250mL flasks, 58g adipic acid and 42g tetramethyl ammonium chloride are put into, is sealed, stirs simultaneously heating water bath
To 65 DEG C, 1.5h is incubated, obtains surface modifier A16.
It in the hydrophilic precipitated silica input reactors of 680g, will stir and be warming up to 125 DEG C of insulation 1.5h, continue to heat up
To 215 DEG C, uniformly on hydrophilic precipitated silica silicon face, insulation 4.5h is handled spray after surface modifier A16 is atomized
To hydrophobic precipitated silicon dioxide N16.
Performance test：
Sample outside embodiment hydrophobic precipitated silicon dioxide and commercially available hydrophobic precipitated silicon dioxide is subjected to test comparison：
1st, specific surface area is tested：Tested according to People's Republic of China (PRC) chemical industry standard HG/T-3073-1999；
2nd, pH value is tested：Tested according to People's Republic of China (PRC) chemical industry standard HG/T-3067-2008；
3rd, Hegman fineness grind instrument is tested：Hydrophobic precipitated silicon dioxide is added in mineral oil, at a high speed scattered 30min, then
Tested according to National Standard of the People's Republic of China GB/T 1724-1979.The numerical value of measure is smaller, and dispersiveness is better.Table
1 is real
Apply example and the performance test of outer sample contrasts
| Embodiment | PH value | Specific surface area (BET) m2/g | Grindometer value (μm) |
| Embodiment 1 | 7.2 | 210 | 5 |
| Embodiment 2 | 7.1 | 220 | 5 |
| Embodiment 3 | 7.3 | 215 | 5 |
| Embodiment 4 | 7.2 | 235 | 6 |
| Embodiment 5 | 7.2 | 230 | 6 |
| Embodiment 6 | 7.7 | 240 | 6 |
| Embodiment 7 | 7.5 | 230 | 6 |
| Embodiment 8 | 7.6 | 225 | 5 |
| Embodiment 9 | 7.1 | 215 | 5 |
| Embodiment 10 | 7.2 | 210 | 5 |
| Embodiment 11 | 7.3 | 220 | 5 |
| Embodiment 12 | 7.1 | 210 | 6 |
| Embodiment 13 | 7.4 | 225 | 6 |
| Embodiment 14 | 7.5 | 230 | 6 |
| Embodiment 15 | 7.3 | 240 | 5 |
| Embodiment 16 | 7.6 | 235 | 5 |
| Outer sample | 10.3 | 130 | 15 |
By upper table, it is obvious that inventive silica grindometer value is less than 10 μm, hence it is evident that hydrophobic heavy less than commercially available
Shallow lake silica.
4th, antifoaming performance is tested：
Defoaming agent composition is respectively synthesized with silica of the embodiment of the present invention and commercially available hydrophobic precipitated silicon dioxide, carried out
Antifoaming performance is tested.
Method of testing：It is past using the sodium dodecyl benzene sulfonate aqueous solution of 0.5% (mass percent) as frothing media
The above-mentioned frothing media 50mL of addition in 100mL tool plug graduated cylinders, then adds 0.010g test defoaming agent composition, is hanging down
Stood after the upward shake of Nogata 50 times, it is foam time T that record foam, which disappears to there is the liquid level time,50, then 50 records of shake disappear
Steep time T100, untill total shaking flask number reaches 400 times, the time is shorter, then the antifoaming performance of defoamer is better.
The embodiment of table 2 and the antifoaming performance of outer sample contrast
Claims (6)
1. a kind of preparation method of hydrophobic precipitated silica, it is characterised in that comprise the following steps：
(1) aliphatic compound A1 and quaternary ammonium salt A2 are put into reaction vessel in proportion, sealed, agitating and heating, in 40~90
DEG C insulation 0.5~2h, obtain surface modifier A；
(2) hydrophilic precipitated silica B is put into reactor and stirs and be warming up to 100-140 DEG C of insulation 0.5-2h；
(3) 150-230 DEG C is continuously heating to, uniformly spray is on silica B surface after surface modifier A is atomized, insulation 4
~6h processing obtains the hydrophobic precipitated silicon dioxide N.
2. the aliphatic compound A1 general structures described in claim 1 are as follows：
[(CH3)m(CH2)n(CH)p]R1 q+1
R1Selected from-OH ,-COOH；Q is 0,1 or 2；P is 0 or 1；N is 0-13 integer；M is 0,1 or 2；m+n+p≤14；
m+n+p≥2。
3. the quaternary ammonium salt A2 general structures described in claim 1 are as follows：
R2R3R4R5N+X-
R in structural formula2、R3、R4、R5Can be the straight chained alkyl that carbon number is 1~8, selected from methyl, ethyl, fourth with identical or different
Base, hexyl, heptyl, octyl group；X is selected from chlorine atom, bromine atoms.
4. the aliphatic compound A1 dosages described in claim 1 are the 11-63% of surface modifier A gross masses.
5. the quaternary ammonium salt A2 dosages described in claim 1 are the 37-89% of surface modifier A gross masses.
6. the mass ratio of the surface modifier A and hydrophilic precipitated silica B described in claim 1 is 1: 5~1: 9.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111960428A (en) * | 2020-09-04 | 2020-11-20 | 桂林良物造日用品有限公司 | Modification method of nano white carbon black |
| CN115838176A (en) * | 2022-08-18 | 2023-03-24 | 杭州应星新材料有限公司 | Preparation method of hydrophobic silicon dioxide treated by silicone oil and silicon dioxide |
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| CN104788997A (en) * | 2015-03-18 | 2015-07-22 | 四川长虹技佳精工有限公司 | Modified oxide and powder coating, and preparation methods and applications thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111960428A (en) * | 2020-09-04 | 2020-11-20 | 桂林良物造日用品有限公司 | Modification method of nano white carbon black |
| CN115838176A (en) * | 2022-08-18 | 2023-03-24 | 杭州应星新材料有限公司 | Preparation method of hydrophobic silicon dioxide treated by silicone oil and silicon dioxide |
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