CN106883453B - The preparation method of modified white carbon black with chemical isolation structure - Google Patents
The preparation method of modified white carbon black with chemical isolation structure Download PDFInfo
- Publication number
- CN106883453B CN106883453B CN201710165061.7A CN201710165061A CN106883453B CN 106883453 B CN106883453 B CN 106883453B CN 201710165061 A CN201710165061 A CN 201710165061A CN 106883453 B CN106883453 B CN 106883453B
- Authority
- CN
- China
- Prior art keywords
- carbon black
- white carbon
- modified
- silica
- suspension
- 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.)
- Active
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 239
- 239000006229 carbon black Substances 0.000 title claims abstract description 169
- 238000002955 isolation Methods 0.000 title claims abstract description 30
- 239000000126 substance Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 241000872198 Serjania polyphylla Species 0.000 title claims abstract description 13
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- 239000000725 suspension Substances 0.000 claims description 102
- 239000000377 silicon dioxide Substances 0.000 claims description 24
- 239000002002 slurry Substances 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 20
- 239000010866 blackwater Substances 0.000 claims description 19
- 230000004048 modification Effects 0.000 claims description 18
- 238000012986 modification Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000001694 spray drying Methods 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 13
- 239000011164 primary particle Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000010907 mechanical stirring Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims 6
- 239000012530 fluid Substances 0.000 claims 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 2
- 150000004756 silanes Chemical class 0.000 claims 2
- -1 diamine compound Chemical class 0.000 claims 1
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- 230000002194 synthesizing effect Effects 0.000 claims 1
- 238000004506 ultrasonic cleaning Methods 0.000 claims 1
- 229920000642 polymer Polymers 0.000 abstract description 8
- 239000011159 matrix material Substances 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003610 charcoal Substances 0.000 abstract description 3
- 229910000077 silane Inorganic materials 0.000 abstract description 3
- 239000002105 nanoparticle Substances 0.000 abstract 3
- 239000000945 filler Substances 0.000 abstract 1
- 125000000524 functional group Chemical group 0.000 abstract 1
- 235000019241 carbon black Nutrition 0.000 description 138
- 239000007788 liquid Substances 0.000 description 10
- 230000002572 peristaltic effect Effects 0.000 description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 239000012065 filter cake Substances 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- 230000003247 decreasing effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000000274 adsorptive effect Effects 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 125000000962 organic group Chemical group 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The preparation method of modified white carbon black with chemical isolation structure is related to for the method for chemical isolation being applied to the modified field of white carbon black.White carbon black can be grafted on using silane coupling agent, and the characteristics of the organo-functional group in silane coupling agent can be reacted with particular functional group, prepares the modified white carbon black being isolated between white carbon black nano particle by organic segment.The modified white carbon black can as filler in use, stable evenly dispersed with nanoparticle form in a polymer matrix.The method of modifying is characterized in that, by a variety of methods, (I) or (II) structure is constructed between white carbon black nanoparticle, hard charcoal black track producing particle is isolated using the structure.This method can be both directly realized by with the acceptor modified white carbon black of (I) or (II) structure；The white carbon black modified by silane coupling agent of (III) structure can also be used, then further reacts to realize indirectly with by the compound of (IV) structure silane coupler modified white carbon black or (V) structure.
Description
Technical field:
This application involves inorganic nanometer powder technical field of modification, the method for more particularly relating to white carbon black nano modification.
Background technique:
White carbon black is hydrated SiO 2 (SiO2-nH2Being commonly called as O) is a kind of to be usually used in the inorganic of enhancing by polymer field
Powder body material.Disclosed in the micromorphology of white carbon black is studied by forefathers already, the white carbon black of naturally occurring has a three-decker: the
One layer is primary partical or primary particle, is that the spheroidal particle for forming random three-dimensional chain branch structure is keyed by Si-O；The
Two layers of hydroxyls dehydrate between a large amount of predecessors through surface is linked together to form secondary structure；Third layer is secondary knot
Aggregation is continued by model ylid bloom action power and hydrogen bond between structure and forms big loose agglomerates.The primary particle partial size of white carbon black exists
It is a kind of powder of Nano grade between 10-40nm, therefore, when white carbon black is increased in the form of primary particle for polymer material
Qiang Shi, nanometer enhancement effect is significant, and reinforcing effect is good.However, there are a large amount of hydroxyls for unmodified white carbon black particle surface
Base, this makes hard charcoal black track producing particle be extremely easy to reunite because of the effect of hydrogen bond between each other, this makes white carbon black be used directly in polymerization
, can not be evenly dispersed with nanoscale primary partical in matrix in object enhancing, but deposited in the form of aggregation not of uniform size
It is in matrix, it is special cannot to play nanofiller institute far beyond nano-scale in the base in this way for the size of the aggregate
Some nanometer enhancement effects.To solve this problem, forefathers early have proposed the modified theory and method of white carbon black, wherein use
White carbon black modified by silane coupling agent is accepted and is used extensively by people at present.It could be theoretically argued that silane coupling agent has silicon simultaneously
Hydroxyl and organic group, silicone hydroxyl can be reacted with white carbon black surface hydroxyl, and organic group can make modified white carbon black
It is not easy to autohemagglutination each other, so that white carbon black be promoted to disperse in a polymer matrix in the form of primary particle.However, traditional idol
Connection agent modification does not ensure that modified white carbon black is evenly dispersed in a polymer matrix, and cannot be completely secured white carbon black with
Primary particle form exists.Therefore, to guarantee in the polymer, white carbon black is long-term, is steadily dispersed in the form of primary particle.This
Invention describe it is a kind of can steadily in the form of chemical isolation existing for modified white carbon black preparation method, it is white using the modification
Carbon black enhances polymer, and the white carbon black in polymer may be implemented and be uniformly distributed in the form of single particle for a long time.This preparation method
Simple and easy, raw material is cheap and easy to get, and product applicable surface is extensive and easy to use.
Summary of the invention:
The present invention constructs a kind of chemical isolation structure between white carbon black primary particle, to make modified white carbon black can
With stable nano-dispersed structure reinforced polymer material.Meanwhile it is such with chemical isolation knot invention describes preparing
The specific method of the modified white carbon black of structure.
The present invention is realized by following three kinds of specific embodiments:
Scheme one:
1. the preparation of white carbon black suspension:
Precipitated silica (filter cake, powder, suspension) plus water are taken, by white carbon black quality adjustment to suspension gross mass
3%wt-25%wt.According to the difference of white carbon black original state, stirred in the mechanical stirring equipment that revolving speed is 1000-5000rpm
3-10h etc. is mixed, uniform, stable white carbon black-water slurry is obtained.With in suspension, whether white carbon black average grain diameter reaches
The following are standards by 600nm, judge whether the preparation of white carbon black suspension is completed.
2. white carbon black suspension temperature is adjusted:
Suspension known to above-mentioned white carbon black content is transferred in the ultrasonic cleaner with heating function, it is outstanding to this
Supernatant liquid is stirred, and setting revolving speed is 500-2000rpm, to keep the suspension to have good mobility.Simultaneously to suspension
Liquid heating, stablizes its temperature in a certain temperature value in 50-80 DEG C of section, sets supersonic frequency as 15-
40KHz。
3. white carbon black is modified:
Xiang Yixiang or more keeps constant addition white carbon black solid matter in the white carbon black suspension of temperature and holding flow regime
The isolation modified version silane coupling agent with formula (I) or formula (II) structure feature for measuring 4%wt-18%wt, continues to be kept stirring
And sonic oscillation.Modification time is 1-8 hours, guarantees that white carbon black suspension has good mobility during this period.
4. the drying of modified white carbon black:
The tank body inlet temperature of spray drying device is adjusted to 160-220 DEG C, while controlling equipment export temperature and existing
105-125℃.Above-mentioned modified isolated form white carbon black suspension is sucked in spray drying device tank body using peristaltic pump,
After all white carbon black suspension are completely dried, dry isolated form modified white carbon black powder is collected.
Scheme two:
1. the preparation of white carbon black suspension:
Precipitated silica (filter cake, powder, suspension) plus water are taken, by white carbon black quality adjustment to suspension gross mass
3%wt-25%wt.According to the difference of white carbon black original state, stirred in the mechanical stirring equipment that revolving speed is 1000-5000rpm
3-10h etc. is mixed, uniform, stable white carbon black-water slurry is obtained.With in suspension, whether white carbon black average grain diameter reaches
The following are standards by 600nm, judge whether the preparation of white carbon black suspension is completed.
2. white carbon black suspension temperature is adjusted:
Suspension known to above-mentioned white carbon black content is transferred in the ultrasonic cleaner with heating function, it is outstanding to this
Supernatant liquid is stirred, and setting revolving speed is 500-2000rpm, to keep the suspension to have good mobility.Simultaneously to suspension
Liquid heating, stablizes its temperature in a certain temperature value in 50-80 DEG C of section, sets supersonic frequency as 15-
40KHz。
3. white carbon black is modified:
The above white carbon black suspension is equally divided into two parts.To addition white carbon black solid masses 3%wt-15% in first part
The silane coupling agent with formula (III) structure feature of wt, to addition white carbon black solid masses 3.5%wt-18%wt in second part
The silane coupling agent with formula (IV) structure feature.Control the additional amount ratio with the silane coupling agent of formula (IV) structure feature
The addition mole of silane coupling agent with formula (III) structure has more 15% to 35%.Continue to keep revolving speed to be 500-
The stirring of 2000rpm and sonic oscillation, it is 1-6 hours modified.
4. the building of white carbon black isolation structure:
Both the above is mixed by different silane coupler modified white carbon black suspension respectively, the use of revolving speed is 500-
2000rpm mechanical stirring is uniformly mixed it, heats to the suspension, stablizes its temperature in 70-90 DEG C of section
In a certain temperature value.With the use of ultrasonator, 2-10 hours are reacted
5. the drying of modified white carbon black:
The tank body inlet temperature of spray drying device is adjusted to 160-220 DEG C, while controlling equipment export temperature and existing
105-125℃.Above-mentioned modified isolated form white carbon black suspension is sucked in spray drying device tank body using peristaltic pump,
After all white carbon black suspension are completely dried, dry isolated form modified white carbon black powder is collected.
Scheme three:
1. the preparation of white carbon black suspension:
Precipitated silica (filter cake, powder, suspension) plus water are taken, by white carbon black quality adjustment to suspension gross mass
3%wt-25%wt.According to the difference of white carbon black original state, stirred in the mechanical stirring equipment that revolving speed is 1000-5000rpm
3-10h etc. is mixed, uniform, stable white carbon black-water slurry is obtained.With in suspension, whether white carbon black average grain diameter reaches
The following are standards by 600nm, judge whether the preparation of white carbon black suspension is completed.
2. white carbon black suspension temperature is adjusted:
Suspension known to above-mentioned white carbon black content is transferred in the ultrasonic cleaner with heating function, it is outstanding to this
Supernatant liquid is stirred, and setting revolving speed is 500-2000rpm, to keep the suspension to have good mobility.Simultaneously to suspension
Liquid heating, stablizes its temperature in a certain temperature value in 50-80 DEG C of section, sets supersonic frequency as 15-
40KHz。
3. white carbon black is modified:
White carbon black solid masses 4% is added into the white carbon black suspension for keeping constant temperature and holding flow regime above
The isolation modified version silane coupling agent with formula (III) structure feature of wt-15%wt.Keeping revolving speed is the height of 500-2000rpm
Speed stirring, and it is used cooperatively ultrasonator.The modification time is 1-8 hours, should guarantee white carbon black suspension always during this
With good mobility.
4. the building of white carbon black isolation structure:
By rear white carbon black suspension modified above, continuing to use revolving speed is 500-2000rpm mechanical stirring, and outstanding to this
Supernatant liquid heating, stablizes its temperature in a certain temperature value in 70-90 DEG C of section.Being added has formula (V) structure
The compound of feature, additional amount is the 15-30% of the silane coupling agent additional amount with formula (III) structure, with the use of ultrasound
Oscillator, reacts 4-8 hour, should guarantee during this white carbon black suspension with good mobility always.
H2N-R3-NH2
(Ⅴ)
5. the drying of modified white carbon black:
The tank body inlet temperature of spray drying device is adjusted to 160-220 DEG C, while controlling equipment export temperature and existing
105-125℃.Above-mentioned modified isolated form white carbon black suspension is sucked in spray drying device tank body using peristaltic pump,
After all white carbon black suspension are completely dried, dry isolated form modified white carbon black powder is collected.
Prepared isolation modified white carbon black is characterized by experiment, organic is changed the results show that prepared by the present invention
Property white carbon black structure is more loose, it is lipophilic dramatically increase, partial size is decreased obviously.The organically-modified white carbon black is added to polymer
In matrix, it is uniformly dispersed good, significantly more efficient reinforcing effect can be played.
Detailed description of the invention:
Fig. 1 is by isolated form modified white carbon black made from preparation method described in embodiment 1 and the coupling agent modified hard charcoal of tradition
Black scanning electron microscope (TEM) photo.
Fig. 2 is thermogravimetric (TG) map by isolated form modified white carbon black made from preparation method described in embodiment 2.
Fig. 3 is the contact angle figure by isolated form modified white carbon black made from preparation method described in embodiment 3.
Specific embodiment:
For a further understanding of the present invention, below with reference to embodiment to silane coupling agent of the present invention and preparation method thereof
It is described with using preferred embodiment, but it is to be understood that these descriptions are intended merely to that spy of the invention is described in more detail
It seeks peace advantage, but the claims in the present invention is not limited in any way.
Embodiment 1:
White carbon black VN3 powder is taken to be stirred by mass percentage for 15:85 with water, this white carbon black suspension is further
It is stirred 10 hours under the speed of 3500rpm using high-speed stirred, uniform, stable white carbon black-water slurry is obtained with this, it is white
The partial size of carbon black in water is 538nm after tested.The white carbon black-water slurry 600g is taken, is transferred to super with heating function
In sound wave rinse bath, while the suspension is stirred, setting revolving speed is 800rpm, good to keep the suspension to have
Mobility.Suspension is heated, until 75 DEG C, supersonic frequency is set as 30KHz.Silane coupling agent (A) is added into the suspension
9g is kept stirring, and keeps modification temperature, reacts it 4 hours.The tank body inlet temperature of spray drying device is adjusted to
160-220 DEG C, while equipment export temperature is controlled at 105-125 DEG C.By above-mentioned modified isolated form white carbon black suspension benefit
With in peristaltic pump sucking spray drying device tank body, after all white carbon black suspension are completely dried, dry isolated form is collected
Modified white carbon black powder.The modified white carbon black with chemical isolation structure is taken to be scanned electron microscope (SEM) observation, and
Scheme to compare with the SEM of traditional acceptor modified white carbon black, it is possible to find there is white carbon black entirety after chemical isolation structure more to dredge
Pine, dispersibility are more preferable.See Fig. 1.
Silane coupling agent (A)
Embodiment 2:
It takes white carbon black Z2000 suspension slurry to mix with water, white carbon black solid masses is adjusted to suspension gross mass
12%, and be stirred, this white carbon black suspension is further stirred 8 hours under the speed of 4500rpm, is obtained with this
One, stable white carbon black-water slurry, the dispersity of white carbon black in water is good, and partial size is 513nm after tested.Take this
White carbon black-water slurry 1000g is transferred in the ultrasonic cleaner with heating function, while stirring the suspension
It mixes, setting revolving speed is 600rpm, to keep the suspension to have good mobility.Suspension is heated, until 70 DEG C, setting is super
Acoustic frequency is 25KHz.Silane coupling agent (B) 10g is added into the suspension, is kept stirring, keeps modification temperature, makes its reaction
3 hours.The tank body inlet temperature of spray drying device is adjusted to 160-220 DEG C, while controlling equipment export temperature and existing
105-125℃.Above-mentioned modified isolated form white carbon black suspension is sucked in spray drying device tank body using peristaltic pump,
After all white carbon black suspension are completely dried, dry isolated form modified white carbon black powder is collected.Take the powder through organic solvent
Thermogravimetric analysis is carried out after extracting, and is compared with the thermogravimetric result of unmodified white carbon black, thus determines silane coupling agent (B)
Scion grafting plays the role of that modified white carbon black is isolated, demonstrates white carbon black modification side of the present invention with this in white carbon black surface
Method can effective modified white carbon black.See Fig. 2.
Silane coupling agent (B)
Embodiment 3:
It takes white carbon black K170 suspension slurry to mix with water, white carbon black solid masses is adjusted to suspension gross mass
10%, and be stirred, this white carbon black suspension is further used into high-speed stirred under the speed of 4000rpm and is stirred 9 hours,
Uniform, stable white carbon black-water slurry is obtained with this, the dispersity of white carbon black in water is good, and partial size is after tested
487nm.The white carbon black-water slurry 500g is taken, is transferred in the ultrasonic cleaner with heating function, while to the suspension
Liquid is stirred, and setting revolving speed is 800rpm, to keep the suspension to have good mobility.Suspension is heated, until 70
DEG C, supersonic frequency is set as 30KHz.Silane coupling agent (C) 5g is added into the white carbon black-water slurry, is kept stirring, keeps
Modification temperature reacts it 4 hours.The white carbon black-water slurry 500g is taken again, and it is clear to be transferred to the ultrasonic wave with heating function
In washing trough, while the suspension is stirred, setting revolving speed is 800rpm, to keep the suspension to have good flowing
Property.Suspension is heated, until 70 DEG C, supersonic frequency is set as 30KHz.It is added into the white carbon black-water slurry silane coupled
Agent (D) 4g, is kept stirring, and keeps modification temperature, reacts it 4 hours.Both the above is changed by different silane coupling agents respectively
Property the mixing of white carbon black suspension, suspension is heated, until 80 DEG C, sets supersonic frequency as 20KHz.It is in speed of agitator
In the case where 600rpm, react 5 hours.Above-mentioned modified isolated form white carbon black suspension is sucked into spraying do using peristaltic pump
In dry equipment tank body, after all white carbon black suspension are completely dried, dry isolated form modified white carbon black powder is collected.It should
After powder tabletting, the contact angle of water and the modified white carbon black is tested, and by the water contact angle of the contact angle and unmodified white carbon black
It compares, sees Fig. 3.It can be seen that the hydrophily of modified white carbon black is remarkably decreased, this illustrates that organic coupling agent is present in white carbon black
Surface, it was demonstrated that white carbon black method of modifying of the present invention can effective modified white carbon black.
Silane coupling agent (C)
Silane coupling agent (D)
Embodiment 4:
It takes white carbon black K160 filter cake to mix with water, white carbon black solid masses is adjusted to the 6% of suspension gross mass, and stir
Mixing is mixed, this white carbon black suspension is further used into high-speed stirred under the speed of 3000rpm and is stirred 6 hours, is obtained with this
Uniform, stable white carbon black-water slurry, the dispersity of white carbon black in water is good, and partial size is 459nm after tested.It takes
The white carbon black-water slurry 1000g is transferred in the ultrasonic cleaner with heating function, while being carried out to the suspension
Stirring, setting revolving speed are 600rpm, to keep the suspension to have good mobility.Suspension is heated, until 60 DEG C, setting
Supersonic frequency is 35KHz.Silane coupling agent (C) 4g is added into the white carbon black-water slurry, is kept stirring, keeps modified temperature
Degree reacts it 4 hours.Compound (E) 0.6g is added later, keeps conditions above, futher stirs reaction 4 hours.It will be upper
Modified isolated form white carbon black suspension is stated using in peristaltic pump sucking spray drying device tank body, is suspended in all white carbon blacks
After liquid is completely dried, dry isolated form modified white carbon black powder is collected.To the powder carry out partial size test, and with it is unmodified white
The partial size of carbon black compares, and as a result see the table below one.It can be seen that the white carbon black with chemical isolation structure has minimum partial size, it is white
Because of the building of chemical isolation structure, reunion volume is decreased obviously carbon black.
Compound (E)
Table one
| Unmodified white carbon black | Traditional modified white carbon black | Modified white carbon black is isolated | |
| Partial size | 459nm | 352nm | 268nm |
Embodiment 5:
It takes white carbon black K160 suspension to mix with water, white carbon black solid masses is adjusted to the 10% of suspension gross mass,
And be stirred, this white carbon black suspension is further used into high-speed stirred under the speed of 4000rpm and is stirred 7 hours, with this
Uniform, stable white carbon black-water slurry is obtained, the dispersity of white carbon black in water is good, and partial size is after tested
473nm.The white carbon black-water slurry 500g is taken, is transferred in the ultrasonic cleaner with heating function, while to the suspension
Liquid is stirred, and setting revolving speed is 1000rpm, to keep the suspension to have good mobility.Suspension is heated, until 80
DEG C, supersonic frequency is set as 30KHz.Silane coupling agent (C) 3.5g is added into the white carbon black-water slurry, is kept stirring, protects
Modification temperature is held, reacts it 5 hours.Compound (F) 0.5g is added later, keeps conditions above, it is small to futher stir reaction 5
When.Above-mentioned modified isolated form white carbon black suspension is sucked in spray drying device tank body using peristaltic pump, all white
After carbon black suspension is completely dried, dry isolated form modified white carbon black powder is collected.The powder is taken to carry out the survey of DBP adsorptive value
Examination, as a result see the table below two.Between silica particles with chemical isolation structure, there is apparent organic isolated interstice, therefore,
The white carbon black that oil factor can be modified much larger than tradition.
Table two
| Unmodified white carbon black | Traditional modified white carbon black | Modified white carbon black is isolated | |
| DBP adsorptive value (cm3/g) | 2.01 | 2.91 | 3.82 |
Compound (F).
Claims (7)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710165061.7A CN106883453B (en) | 2017-03-20 | 2017-03-20 | The preparation method of modified white carbon black with chemical isolation structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710165061.7A CN106883453B (en) | 2017-03-20 | 2017-03-20 | The preparation method of modified white carbon black with chemical isolation structure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106883453A CN106883453A (en) | 2017-06-23 |
| CN106883453B true CN106883453B (en) | 2019-05-17 |
Family
ID=59180995
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710165061.7A Active CN106883453B (en) | 2017-03-20 | 2017-03-20 | The preparation method of modified white carbon black with chemical isolation structure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106883453B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109354876A (en) * | 2018-10-09 | 2019-02-19 | 河南骏化发展股份有限公司 | A kind of preparation method of silicon rubber modified white carbon black |
| CN110092946B (en) * | 2019-05-22 | 2022-02-08 | 湖南工学院 | Non-migration type anti-aging agent and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4147712A (en) * | 1977-06-28 | 1979-04-03 | Union Carbide Corporation | Amino substituted mercapto organosilicon compounds |
| CN104220446A (en) * | 2012-03-30 | 2014-12-17 | 株式会社Lg化学 | Siloxane-based compound, and photosensitive composition and photosensitive material including same |
| CN106003942A (en) * | 2016-05-16 | 2016-10-12 | 安徽天恩旅行用品科技有限公司 | Manufacturing method of luggage leather |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3427465B2 (en) * | 1994-02-16 | 2003-07-14 | 信越化学工業株式会社 | Modifier for composite material, method for producing the same, and composite material |
| US8906973B2 (en) * | 2010-11-30 | 2014-12-09 | Aspen Aerogels, Inc. | Modified hybrid silica aerogels |
-
2017
- 2017-03-20 CN CN201710165061.7A patent/CN106883453B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4147712A (en) * | 1977-06-28 | 1979-04-03 | Union Carbide Corporation | Amino substituted mercapto organosilicon compounds |
| CN104220446A (en) * | 2012-03-30 | 2014-12-17 | 株式会社Lg化学 | Siloxane-based compound, and photosensitive composition and photosensitive material including same |
| CN106003942A (en) * | 2016-05-16 | 2016-10-12 | 安徽天恩旅行用品科技有限公司 | Manufacturing method of luggage leather |
Non-Patent Citations (2)
| Title |
|---|
| "Syntheses of polyamine-bridged polysilsesquioxanes hybrid materials combining solegel processing and molecular imprinting applied to selective adsorption for copper";Changmei Sun等;《Materials Chemistry and Physics》;20150107;第153卷;第307-315页 |
| "高性能橡胶纳米复合材料的制备及结构性能研究";叶欣;《中国博士学位论文全文数据库 工程科技I辑》;20101015(第10期);第B020-86页 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106883453A (en) | 2017-06-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Arkhireeva et al. | Synthesis of sub-200 nm silsesquioxane particles using a modified Stöber sol–gel route | |
| WO2021109729A1 (en) | Inorganic powder modification system | |
| CN106883453B (en) | The preparation method of modified white carbon black with chemical isolation structure | |
| CN104387671B (en) | A kind of preparation method of PA6/PP/ CNT High performance nanometer composite material | |
| CN101787171B (en) | Silicon oxide (SiOX)/polymethyl methacrylate (PMMA) nano composite resin and preparation and application thereof | |
| CN110211757A (en) | With amphipathic and magnetic nano particle and preparation method thereof | |
| CN105727884A (en) | Bentonite clay particles and preparation method thereof | |
| CN103755898A (en) | Preparation method of POSS (Polyhedral Oligomeric Silsesquioxane) modified nanoparticles | |
| CN101838479A (en) | Method for preparing dispersible ultra-fine silicon dioxide | |
| CN105670038A (en) | Light-sensitive nanometer silicon dioxide and method for preparing same | |
| CN110194461A (en) | A kind of preparation method of size tunable monodisperse meso-scale preparing spherical SiO 2 | |
| CN107254211B (en) | Preparation method of modified nano-calcium carbonate powder for high-end water-based coatings | |
| CN103333262A (en) | Preparation method of modified starch nanocrystal | |
| CN110282633A (en) | A kind of method of modifying of nano oxidized silicon materials | |
| CN104445240A (en) | Method for in-situ preparation of organized mixed-dimension nanometer material by using attapulgite | |
| CN110128851B (en) | Preparation method of hydrophobic nano calcium carbonate | |
| CN112299467B (en) | Preparation method of monodisperse oil-phase nano barium sulfate dispersoid | |
| CN102174278A (en) | Surface oleophilic modification method of inorganic nanometer powder | |
| CN110407212B (en) | High-dispersity nano carbonate gel as well as preparation method and application thereof | |
| CN107746059A (en) | A kind of preparation method of the hollow silica microsphere of surface silane-containing modification | |
| CN111218024B (en) | Method for continuously preparing core-shell hydrophilic-hydrophobic bipolar composite aerogel powder | |
| CN106883454B (en) | Rubber with white carbon black chemical isolation structure/white carbon black rubber master batch preparation method | |
| CN111748220A (en) | A method for regulating the surface wettability of nano-silica based on chemical modification | |
| CN111825926A (en) | Organic/inorganic hybrid three-component Janus particles and preparation method | |
| CN116621186A (en) | Vermicular nano silicon dioxide and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |