CN105271251A - White carbon black as well as preparation method and application thereof - Google Patents
White carbon black as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention provides white carbon black as well as a preparation method and an application thereof. Alkyl polyglycoside is added as a dispersing agent in a white carbon black preparing process with a precipitation method, and the white carbon black is prepared. The preparation method is simple, the product has good stability, alkyl polyglycoside is added as the dispersing agent, so that the white carbon black has high dispersion, the BET specific surface area is 90-127 m<2>/g, the DBP (dibutyl phthalate) oil absorption value is 2.16-2.45 mL/g, the structural property of the product is high, the Mooney viscosity of a rubber product prepared from the white carbon black is reduced to 63.4-69.2, the plasticity of the white carbon black rubber product is improved, and further, the tensile stress-strain performance, vulcanization and the like of the rubber product are improved by the aid of addition of alkyl polyglycoside, so that the high-dispersion white carbon black with excellent combination property can be obtained with the preparation method, can be used as a reinforcing agent for automobile tire rubber and has good technological and economic performance.
Description
Technical field
The invention belongs to white carbon black preparing technical field, relate to a kind of white carbon black and its preparation method and application.
Background technology
The chemical name of white carbon black is hydrated amorphous silicas, surface containing silicone hydroxyl, easily water suction and become the particulate of gathering.Excellent properties such as there is porousness, specific surface area is large, polymolecularity, light weight, chemical stability are good, high temperature resistant, do not burn, electrical insulating property is good.
The current white carbon black of global 70% is used for rubber industry, and be excellent rubber reinforcing filler, can improve cementing property and wear resistance, its performance is better than ordinary carbon black.Along with the enhancing of environmental protection and awareness of saving energy, tire production producer applies white carbon black gradually to replace carbon black.White carbon black tread rubber reduces about 20% than the friction resistance of carbon black tread rubber, plays the effect of energy-saving and emission-reduction, is conducive to energy-conserving and environment-protective, have important practical significance and industrial value for rubber for tire industrial expansion.
Compared with thermal silica, there is the problems such as surface silanol group content is high, specific surface area distribution is wide in the white carbon black that ordinary precipitation process is produced, cause the dispersiveness of white carbon black in rubber size not high and easily reunite, make the degradation such as rubber tearing toughness, wear resistance, have impact on Using Life of Tyre and security.Therefore need to improve traditional processing condition to prepare the precipitated silica of polymolecularity.
CN102951649A discloses a kind of preparation method of modification precipitated silica, adds the liquid sodium silicate of 10% ~ 50% first in the reactor; In reactor, add the water glass of residue 50% ~ 90% more simultaneously and be the aqueous sulfuric acid of 10% ~ 30% with the concentration of whole water glass equimolar amount, and add properties-correcting agent sodium lauryl sulphate or stearic acid or Zinic stearas, be warming up to 50 DEG C ~ 95 DEG C, under agitation react 1 ~ 2h; Then regulate pH value to 7 ~ 9 with ammoniacal liquor, add sinking agent 12 hydrazine aluminum sulfate potassium simultaneously, continue reaction 0.5 ~ 2h; Finally resultant of reaction is carried out washing, suction filtration, and carry out drying, obtain modification precipitated silica.Utilize this inventive method only to improve the dispersiveness of white carbon black, the concrete structure angle value not introducing white carbon black also unexposed the method for the improvement of other performances of white carbon black.
CN102092721A discloses the method for sulfuric acid precipitation legal system for white carbon black, take water glass as raw material, utilize sulfuric acid for precipitation agent, prepare the nano-scale white carbon black of high-quality by tensio-active agent and the dispersion aids regulation and control hydrolysis rate of silicate and the polymerization degree of silicic acid molecule.Select alkylbenzene sulfonate or polymerization alcohols as tensio-active agent in the invention, organic molecule ketone or organic molecule alcohols are as dispersion aids, and it act as the regulation and control hydrolysis rate of silicate and the polymerization degree of silicic acid molecule, thus control the quality of white carbon black, but the oil-absorption(number) of the white carbon black prepared thus is only 1.90cm
3/ g, structure level is still lower.
Therefore, in this area, expect to prepare a kind of white carbon black with excellent comprehensive performance with polymolecularity and higher structure level.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of white carbon black and its preparation method and application.
For reaching this goal of the invention, the present invention by the following technical solutions:
On the one hand, the invention provides a kind of preparation method of white carbon black, described method is included in utilize in the process of preparing white carbon black by precipitation method and adds alkyl glycoside as dispersion agent.
In preparation process, add this nonionogenic tenside of alkyl glycoside, define coated to the Silicon dioxide, hydrate surface of precipitation, stop the reunion between silicon dioxide granule, ensure that product has high dispersiveness and high structure level.Thus the white carbon black prepared can be made when being applied to rubber item, effectively prevent the generation of gel, and then improve the consistency of white carbon black and rubber molecule.
In addition, due to adding of alkyl glycoside, make other performances of white carbon black, such as tensile stress-strain performance, mooney viscosity and vulcanization characteristics etc. obtain improvement to a certain extent, make white carbon black have excellent over-all properties.
Alkyl glycoside, APG for short, synthesized by fatty alcohol and glucose, it is the more comprehensive new non-ionic surfactants of a kind of performance, have the characteristic of conventional nonionic and anion surfactant concurrently, have high surface, good ecological security and intermiscibility, be internationally recognized first-selection " green " functional surfactant, its general molecular formula is as follows:
Wherein R is C
8-18, n=1 ~ 8.
In the preparation method of white carbon black of the present invention, the add-on of described alkyl glycoside is 0.16 ~ 4% of white carbon black theoretical yield, such as 0.16%, 0.18%, 0.2%, 0.5%, 0.8%, 1%, 1.3%, 1.5%, 1.8%, 2%, 2.3%, 2.5%, 2.8%, 3%, 3.3%, 3.5%, 3.8% or 4%, be preferably 2 ~ 4%, more preferably 2%.
In the preparation method of white carbon black of the present invention, the mean polymerisation degree of described alkyl glycoside is 1.2 ~ 1.8, such as 1.2,1.3,1.4,1.5,1.6,1.7 or 1.8.
The preparation method of white carbon black of the present invention comprises the following steps: water glass solution and alkyl glycoside are added reactor, is warming up to 85 ~ 95 DEG C, drips sulphuric acid soln, carry out precipitin reaction, after reaction terminates, adjust ph to 5 ~ 6, carry out ageing reaction, obtain described white carbon black.
In the preparation method of white carbon black of the present invention, the modulus of described water glass is 3.2 ~ 3.5, such as 3.2,3.3,3.4 or 3.5.
Preferably, SiO in described water glass solution
2volumetric molar concentration be 0.67 ~ 2.01mol/L, such as 0.67mol/L, 0.70mol/L, 0.75mol/L, 0.78mol/L, 0.8mol/L, 0.85mol/L, 0.9mol/L, 0.95mol/L, 1.0mol/L, 1.2mol/L, 1.4mol/L, 1.6mol/L, 1.8mol/L, 1.9mol/L, 2.0mol/L or 2.01mol/L, be preferably 1.34mol/L.
In the preparation method of white carbon black of the present invention, the volumetric molar concentration of described sulphuric acid soln is 1.5 ~ 3.5mol/L, such as 1.5mol/L, 1.55mol/L, 1.6mol/L, 1.7mol/L, 1.8mol/L, 1.9mol/L, 2.0mol/L, 2.2mol/L, 2.4mol/L, 2.5mol/L, 2.6mol/L, 2.8mol/L, 3.0mol/L, 3.1mol/L, 3.2mol/L, 3.3mol/L, 3.4mol/L or 3.5mol/L, preferred 2.5mol/L.
Preferably, the volume ratio of described sulphuric acid soln consumption and water glass solution is 1:3 ~ 9, such as 1:3,1:4,1:5,1:6,1:7,1:8 or 1:9, is preferably 1:6.02.
In the preparation method of white carbon black of the present invention, the temperature of described precipitin reaction is 85 ~ 95 DEG C, such as 85 DEG C, 86 DEG C, 87 DEG C, 88 DEG C, 89 DEG C, 90 DEG C, 91 DEG C, 92 DEG C, 93 DEG C, 94 DEG C or 95 DEG C, be preferably 85 ~ 90 DEG C, more preferably 90 DEG C.
Preferably, the time of described precipitin reaction is 70 ~ 130min, such as 70min, 75min, 78min, 80min, 83min, 85min, 88min, 90min, 92min, 95min, 98min, 100min, 105min, 108min, 110min, 115min, 118min, 120min, 122min, 125min, 128min or 130min, be preferably 100 ~ 130min, more preferably 100min.
Preferably, the temperature of ageing reaction is 85 ~ 95 DEG C, such as 85 DEG C, 86 DEG C, 87 DEG C, 88 DEG C, 89 DEG C, 90 DEG C, 91 DEG C, 92 DEG C, 93 DEG C, 94 DEG C or 95 DEG C, is preferably 85 ~ 90 DEG C, more preferably 90 DEG C.
Preferably, the time of ageing reaction is 20 ~ 50min, such as 20min, 23min, 25min, 28min, 30min, 33min, 35min, 38min, 40min, 42min, 45min, 48min or 50min, is preferably 30min.
In the preparation method of white carbon black of the present invention, after ageing reaction terminates, carry out washing, be separated, drying obtains described white carbon black.
Preferably, described separation adopts and filters or centrifugal realization.
Preferably, described drying temperature is 95 ~ 115 DEG C, such as 95 DEG C, 98 DEG C, 100 DEG C, 103 DEG C, 105 DEG C, 108 DEG C, 110 DEG C, 113 DEG C or 115 DEG C.
As the preferred technical solution of the present invention, the preparation method of described white carbon black comprises the following steps: the alkyl glycoside being 0.16 ~ 4% of white carbon black theoretical yield by water glass solution and consumption adds reactor, be warming up to 85 ~ 95 DEG C, dropping and the volume ratio of water glass solution are 1.5 ~ 3.5mol/L sulphuric acid soln of 1:3 ~ 9, precipitin reaction is carried out at 85 ~ 95 DEG C, after reaction 70 ~ 130min, adjust ph to 5 ~ 6, at 85 ~ 95 DEG C, carry out ageing 20 ~ 50min, and after washing, separation, drying obtain described white carbon black.
As further optimal technical scheme, the preparation method of white carbon black of the present invention comprises the following steps:
The alkyl glycoside being 2% of white carbon black theoretical yield by water glass solution and consumption adds reactor, be warming up to 90 DEG C, dropping and the volume ratio of water glass solution are the 2.5mol/L sulphuric acid soln of 1:6.02, precipitin reaction is carried out at 90 DEG C, after reaction 100min, adjust ph to 5 ~ 6, carry out ageing 30min at 90 DEG C, and after washing, separation, drying obtain described white carbon black.
Term used in the present invention " water glass " can be replaced " water glass ".
The present invention only needs single step reaction just can obtain white carbon black product, avoids the problems such as technique is loaded down with trivial details in traditional two-step reaction, and the white carbon black product prepared has the high and reinforcing high advantage of good dispersity, structure level.
On the other hand, the invention provides the white carbon black prepared by preparation method described in first aspect.
On the other hand, the invention provides the white carbon black prepared by preparation method described in first aspect and prepare the application in rubber reinforcing filler.
High-dispersion white carbon black prepared by the present invention is the ideal product as high-performance tire goods strengthening agent.Have data to prove, the tire that with the addition of high-dispersion white carbon black can reduce rolling resistance more than 30%, and then oil consumption also obtains the decline of 4.5 ~ 6%, decreases exhaust emissions, and energy-conserving and environment-protective are described as " green tire ".
Relative to prior art, the present invention has following beneficial effect:
The present invention is simple to the preparation method of white carbon black, and processing ease, product stability is good, by adding alkyl glycoside as dispersion agent, makes white carbon black have polymolecularity, and BET specific surface area is 90 ~ 127m
2/ g, DBP oil-absorption(number) is 2.16 ~ 2.45mL/g, the structural height of product, and adding of alkyl glycoside makes the mooney viscosity of the rubber item be made up of white carbon black be reduced to 63.4-69.2, improve the plasticity-of rubber item, the aspect tools such as the tensile stress-strain performance of rubber and vulcanization characteristics all make moderate progress, therefore a kind of high-dispersion white carbon black with excellent comprehensive performance can be obtained by preparation method of the present invention, can be used as doughnut rubber strengthening agent, there is good Technical Economy.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of white carbon black prepared by embodiment 1;
Fig. 2 is the transmission electron microscope photo of white carbon black prepared by comparative example 1;
Fig. 3 is the transmission electron microscope photo of white carbon black prepared by comparative example 2.
Embodiment
Technical scheme of the present invention is further illustrated below by embodiment.Those skilled in the art should understand, described embodiment is only help to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment 1
Pipette that 380mL modulus is 3.3, SiO
2volumetric molar concentration is the water glass solution of 1.34mol/L, add 0.62g alkyl glycoside (mean polymerisation degree 1.2 ~ 1.8, for 2% of white carbon black theoretical yield), join in 1L stirred autoclave, stir (rotating speed 250rpm) and be warming up to 90 DEG C, dripping 63.1mL concentration is the sulphuric acid soln of 2.5mol/L, carry out precipitin reaction 100min, adjust ph to 5.5, keep temperature 90 DEG C, after ageing 30min, filter, be washed with distilled water to μ s/cm in specific conductivity≤100 in water, be 6wt% at 105 DEG C of oven dryings to product water ratio, obtain precipitated silica powder product.
Utilize transmission electron microscope (JEM-2100, Jeol Ltd.) appearance structure of product is characterized, result as shown in Figure 1, as seen from the figure, the white carbon black that the present embodiment obtains is very well dispersed, wherein silica particles defines chain, ring texture, and the gap between particle is larger, structural height.Other performances of product and rubber applications test result are in table 1.
Embodiment 2
Pipette that 380mL modulus is 3.3, SiO
2volumetric molar concentration is 1.34mol/L water glass solution, and (mean polymerisation degree 1.2 ~ 1.8 is SiO to add 1.24g alkyl glycoside
24% of theoretical yield), join in 1L stirred autoclave, stir (rotating speed 250rpm) and be warming up to 90 DEG C, dripping concentration is 2.5mol/L sulphuric acid soln, carries out precipitin reaction 100min.Adjust ph to 5.5, keeps temperature 90 DEG C, after ageing 20min, filters, is washed with distilled water to μ s/cm in specific conductivity≤100 in water, be 5.8wt%, obtain precipitated silica powder product at 105 DEG C of oven dryings to product water ratio.Product property and rubber applications test result are in table 1.
Embodiment 3
Pipette that 380mL modulus is 3.3, SiO
2volumetric molar concentration is 1.34mol/L water glass solution, add 1.24g alkyl glycoside (mean polymerisation degree 1.2 ~ 1.8, for 4% of white carbon black theoretical yield), join in 1L stirred autoclave, stir (rotating speed 250rpm) and be warming up to 90 DEG C, dripping concentration is the sulphuric acid soln of 2.5mol/L, carry out precipitin reaction 100min, adjust ph to 5.5, keeps temperature 90 DEG C, after ageing 30min, filter, be washed with distilled water to μ s/cm in specific conductivity≤100 in water, be 5.8wt% at 105 DEG C of oven dryings to product water ratio, obtain precipitated silica powder product.Product property and rubber applications test result are in table 1.
Embodiment 4
Pipette that 380mL modulus is 3.3, SiO
2volumetric molar concentration is the water glass solution of 1.34mol/L, and (mean polymerisation degree 1.2 ~ 1.8 is SiO to add 0.31g alkyl glycoside
21% of theoretical yield), join in 1L stirred autoclave, stir (rotating speed 250rpm) and be warming up to 90 DEG C, dripping concentration is 2.5mol/L sulphuric acid soln, carry out precipitin reaction 100min, adjust ph to 5.5, keeps temperature 90 DEG C, after ageing 30min, filter, be washed with distilled water to μ s/cm in specific conductivity≤100 in water, be 6.5wt% at 105 DEG C of oven dryings to product water ratio, obtain precipitated silica powder product.Product property and rubber applications test result are in table 1.
Embodiment 5
Pipette that 380mL modulus is 3.3, SiO
2volumetric molar concentration is the water glass solution of 1.34mol/L, and (mean polymerisation degree 1.2 ~ 1.8 is SiO to add 0.05g alkyl glycoside
20.16% of theoretical yield), join in 1L stirred autoclave, stir (rotating speed 250rpm) and be warming up to 85 DEG C, dripping concentration is 2.5mol/L sulphuric acid soln, carry out precipitin reaction 70min, adjust ph to 5.5, keeps temperature 85 DEG C, after ageing 30min, filter, be washed with distilled water to μ s/cm in specific conductivity≤100 in water, be 6.4wt% at 105 DEG C of oven dryings to product water ratio, obtain precipitated silica powder product.Product property and rubber applications test result are in table 1.
Comparative example 1
This comparative example difference from Example 1 is only, alkyl glycoside is not added in preparation process, the charging capacity of rest materials and reaction conditions are all identical with embodiment 1, the transmission electron microscope phenogram of the white carbon black product prepared as shown in Figure 2, as seen from the figure, this product agglomeration is serious, dispersed low.Other performances of product and rubber applications test result are in table 1.
Comparative example 2
This comparative example difference from Example 1 is only, the amount of the alkyl glycoside of adding in preparation process is 1.86g, namely the addition of alkyl glycoside is 6% of white carbon black theoretical yield, the charging capacity of rest materials and reaction conditions are all identical with embodiment 1, the transmission electron microscope phenogram of the white carbon black product prepared as shown in Figure 3, as seen from the figure, this product has agglomeration, and other performances of product and rubber applications test result are in table 1.
Comparative example 3
This comparative example difference from Example 1 is only, the amount of the alkyl glycoside of adding in preparation process is 0.03g, namely the addition of alkyl glycoside is 0.1% of white carbon black theoretical yield, the charging capacity of rest materials and reaction conditions are all identical with embodiment 1, it is serious, dispersed low that the white carbon black product prepared characterizes same this product agglomeration of display through transmission electron microscope.Other performances of product and rubber applications test result are in table 1.
Examination criteria or the method for performance perameter involved by table 1 are as follows:
The specific surface area of white carbon black is measured according to GB/T3073-1999 " the mensuration N2 adsorption method of precipitated hydrated silica specific surface ".
The oil-absorption(number) of white carbon black is measured according to GB/T3072-2008 " mensuration of precipitated hydrated silica dibutyl phthalate (DBP) oil-absorption(number) ".
Rubber processing is carried out according to HG/T2404-2008 " qualification of precipitated hydrated silica in butadiene-styrene rubber ".Stress-strain behavior presses GB/T528-2009 " mensuration of vulcanized rubber or thermoplastic elastomer tensile stress-strain performance " test, mooney viscosity is by GB/T1232 " unvulcanized rubber disk is sheared viscometer and carried out measuring first part: the mensuration of mooney viscosity " test, and vulcanization characteristics presses GB/T9869-1997 " mensuration (oscillating disc curemeter method) of rubber size vulcanization characteristics " test.
Table 1
The transmission electron microscope characterization result of the white carbon black prepared from embodiment and comparative example, when be incorporated as in preparation process white carbon black theoretical yield 2% alkyl glycoside time the dispersiveness of white carbon black (embodiment 1) that obtains significantly better than the dispersiveness of white carbon black when not adding alkyl glycoside (comparative example 1), and when the amount of the alkyl glycoside added too much or very few time (comparative example 2 and 3), the dispersiveness of the white carbon black prepared is poor, agglomeration is more serious, structure level is not high, assembles the Large stone showed increased of formation in size distribution.
As can be seen from table 1 result, the moderate (90 ~ 127m of white carbon black specific surface area that the present invention makes to prepare by adding alkyl glycoside in preparation process
2/ g), DBP oil-absorption(number) is 2.16 ~ 2.45mL/g, the structure properties of product obviously promotes, when being applied to the rubber items such as tire, the mooney viscosity of the rubber unvulcanizate made by white carbon black prepared by the present invention is 63.4-69.2, and when prepare in white carbon black process do not add alkyl glycoside or add too much or how many alkyl glycoside time, mooney viscosity is at 79.2-80.4, therefore reduce mooney viscosity after proving to add alkyl glycoside, the plasticity-of rubber item is strengthened.And the present invention is by adding alkyl glycoside preparing in white carbon black process, and the curing time (Tc10, Tc90) of the rubber item making white carbon black make all decreases, and vulcanization characteristics obviously improves, and the mechanical property of cross-linked rubber also improves greatly.
Applicant states, the present invention illustrates processing method of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned processing step, does not namely mean that the present invention must rely on above-mentioned processing step and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of raw material selected by the present invention, all drops within protection scope of the present invention and open scope.
Claims (10)
1. a preparation method for white carbon black, is characterized in that, described method is included in utilize in the process of preparing white carbon black by precipitation method and adds alkyl glycoside as dispersion agent.
2. preparation method according to claim 1, is characterized in that, the add-on of described alkyl glycoside is 0.16 ~ 4% of white carbon black theoretical yield, is preferably 2 ~ 4%, more preferably 2%.
3. preparation method according to claim 1 and 2, is characterized in that, the mean polymerisation degree of described alkyl glycoside is 1.2 ~ 1.8.
4. preparation method according to any one of claim 1-3, it is characterized in that, said method comprising the steps of: water glass solution and alkyl glycoside are added reactor, be warming up to 85 ~ 95 DEG C, drip sulphuric acid soln, carry out precipitin reaction, after reaction terminates, adjust ph to 5 ~ 6, carry out ageing reaction, obtain described white carbon black.
5. the preparation method according to any one of claim 1-4, is characterized in that, the modulus of described water glass is 3.2 ~ 3.5;
Preferably, SiO in described water glass solution
2volumetric molar concentration be 0.67 ~ 2.01mol/L, be preferably 1.34mol/L.
6. the preparation method according to any one of claim 1-5, is characterized in that, the volumetric molar concentration of described sulphuric acid soln is 1.5 ~ 3.5mol/L, is preferably 2.5mol/L;
Preferably, the volume ratio of described sulphuric acid soln consumption and water glass solution is 1:3 ~ 9, is preferably 1:6.02.
7. the preparation method according to any one of claim 1-6, is characterized in that, the temperature of described precipitin reaction is 85 ~ 95 DEG C, is preferably 85 ~ 90 DEG C, more preferably 90 DEG C;
Preferably, the time of described precipitin reaction is 70 ~ 130min, is preferably 100 ~ 130min, more preferably 100min;
Preferably, the temperature of ageing reaction is 85 ~ 95 DEG C, is preferably 85 ~ 90 DEG C, more preferably 90 DEG C;
Preferably, the time of ageing reaction is 20 ~ 50min, is preferably 30min.
Preferably, after ageing reaction terminates, carry out washing, be separated, drying obtains described white carbon black;
Preferably, described separation adopts and filters or centrifugal realization;
Preferably, described drying temperature is 95 ~ 115 DEG C.
8. the preparation method according to any one of claim 1-7, is characterized in that, said method comprising the steps of: be 3.2 ~ 3.5 by modulus, SiO
2the alkyl glycoside of volumetric molar concentration to be the water glass solution of 0.67 ~ 2.01mol/L and consumption be 0.16 ~ 6% of white carbon black theoretical yield add reactor, be warming up to 85 ~ 95 DEG C, dropping and the volume ratio of water glass solution are 1.5 ~ 3.5mol/L sulphuric acid soln of 1:3 ~ 9, precipitin reaction is carried out at 85 ~ 95 DEG C, after reaction 70 ~ 130min, adjust ph to 5 ~ 6, carry out ageing 20 ~ 50min at 85 ~ 95 DEG C, and after washing, separation, drying obtain described white carbon black.
9. the white carbon black that the preparation method according to any one of claim 1-8 prepares.
10. the application in rubber reinforcing filler prepared by white carbon black according to claim 9.
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| CN106966400A (en) * | 2017-04-24 | 2017-07-21 | 确成硅化学股份有限公司 | A kind of preparation method of big pore volume high-dispersion white carbon black |
| CN108069430A (en) * | 2017-12-28 | 2018-05-25 | 无锡恒诚硅业有限公司 | A kind of preparation method of high dispersive precipitated silica and precipitated silica therefrom |
| CN111807395A (en) * | 2018-05-28 | 2020-10-23 | 福建远翔新材料股份有限公司 | Preparation method of low-oil-absorption nano silicon dioxide for high-elasticity silicone rubber |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106966400A (en) * | 2017-04-24 | 2017-07-21 | 确成硅化学股份有限公司 | A kind of preparation method of big pore volume high-dispersion white carbon black |
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| CN111807395A (en) * | 2018-05-28 | 2020-10-23 | 福建远翔新材料股份有限公司 | Preparation method of low-oil-absorption nano silicon dioxide for high-elasticity silicone rubber |
| CN111807395B (en) * | 2018-05-28 | 2022-07-19 | 福建远翔新材料股份有限公司 | Preparation method of low-oil-absorption nano silicon dioxide for high-elasticity silicone rubber |
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