CN110387145A - A kind of preparation method of the high abrasion white carbon black for butadiene-styrene rubber reinforcement - Google Patents
A kind of preparation method of the high abrasion white carbon black for butadiene-styrene rubber reinforcement Download PDFInfo
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- CN110387145A CN110387145A CN201910649966.0A CN201910649966A CN110387145A CN 110387145 A CN110387145 A CN 110387145A CN 201910649966 A CN201910649966 A CN 201910649966A CN 110387145 A CN110387145 A CN 110387145A
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- carbon black
- white carbon
- butadiene
- styrene rubber
- high abrasion
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
Abstract
The present invention relates to a kind of preparation method of high abrasion white carbon black for butadiene-styrene rubber reinforcement, this method is modified using silica wetcake as raw material using coupling agent phenyltrimethoxysila,e, prepares the high abrasion white carbon black for butadiene-styrene rubber reinforcement.White carbon black modification temperature is 70-90 DEG C, modification time 30-150min in this method, and modified pH value is 2.5-4.5, and coupling agent phenyl trimethoxy dosage is the 2.94%-6.85% of wet cake weight.Present invention reduces the surface hydroxyl numbers of white carbon black, improve the hydrophobic performance of traditional white carbon black, solve the problems, such as the excessive caused and butadiene-styrene rubber poor compatibility of white carbon black surface hydroxyl, substantially increase the wearability of butadiene-styrene rubber.The processing performance and mechanical property of rubber are also improved simultaneously.The method simple process, product stability is good, is easy to industrialization, has good Technical Economy.
Description
Technical field
The present invention relates to white carbon black preparation technical field, specially a kind of high abrasion white carbon black for butadiene-styrene rubber reinforcement
Preparation method.
Background technique
White carbon black is hydrated SiO 2, a kind of unformed white powder nano material, molecular formula SiO2·
nH2O.Silica is widely used, can be used as grinding agent for toothpaste, can be as corrosion inhibiter for storing drug in medicine
It is used for catalyst carrier in reaction, is alternatively arranged as reinforcing agent for rubber for tire, the white carbon black close to 75% is used in rubber.
Michelin proposed the concept of " green tire " in 1992 first, and the white carbon black beginning is used in the rubber compounding of tire later.It is white
Carbon black be added rubber tyre after, the rolling resistance of tire 20%-30% can be reduced, and be able to maintain tire anti-slippery and
Wearability, greatly reduces the cost of tire, while saving the oil consumption of vehicle driving, for environmental protection, it is energy saving have weight
Want meaning.Since there are a large amount of hydroxyls on white carbon black surface, after butadiene-styrene rubber is added, white carbon black can not in butadiene-styrene rubber
Macromolecular structure combines well, and the hydroxyl and rubber macromolecule binding force of white carbon black are weak, and poor compatibility causes white carbon black can not
It is dispersed in rubber well, to reduce the performance of rubber.Furthermore the hydroxyl of white carbon black is excessive, can adsorb in mixing process
Promotor causes vulcanization time elongated, reduces production capacity.Therefore, it is necessary to select modifying agent to be modified white carbon black, improves it and dredge
Aqueous energy and its wear-resisting property.
Summary of the invention
The object of the present invention is to provide the preparation method for a kind of high abrasion white carbon black for butadiene-styrene rubber reinforcement, with
Solve above-mentioned technical problem.Compared with traditional white carbon black, surface hydroxyl number is reduced the white carbon black being prepared by this method,
Hydrophobicity is improved, and after Reinforcing Styrene-butadiene Rubber, wear-resisting property is greatly improved, while vulcanizate processing performance and power
Learning performance is improved.According to technical solution provided by the invention, the high abrasion white carbon black for butadiene-styrene rubber reinforcement
Preparation method contains following steps:
Silica wetcake and deionized water are added in a kettle, with oil bath pan agitating and heating, is warming up to modified temperature
After degree, it is adjusted to the modification pH value of setting with dilute sulfuric acid, adds certain proportion coupling agent phenyltrimethoxysila,e, is changed
Property reaction last washing, filter, be dry, obtain the high abrasion white carbon black for butadiene-styrene rubber reinforcement.
As limitation of the present invention, modification temperature is 70-90 DEG C, modification time 30-150min, and modified pH value is
2.5-4.5, coupling agent phenyl trimethoxy dosage are the 2.94%-6.85% of wet cake weight.
As to further limitation of the invention, in method of the present invention, modification temperature is 80 DEG C, and modification time is
90min, modified PH are 3.5, and coupling agent phenyl trimethoxy dosage is the 6.85% of wet cake weight.
Detailed description of the invention:
Fig. 1 is 1 gained TG map of the embodiment of the present invention 5 and comparative example, and wherein curve 1 is that (comparison is implemented before modified
Example 1) product TG map, curve 2 is modified (embodiment 5) product TG map, it can be seen that as the rising of temperature, 1,2 is bent
Line mass starts to lose, but big in the mass loss of 30-500 DEG C of inner curve 1, and about 12.9%, and 2 mass loss of curve is slow,
This is because modified sample surfaces hydroxyl value is few, in 30-500 DEG C the combination water of white carbon black itself and free water start
It is evaporated, and surface hydroxyl starts to be condensed dehydration.Continuing to increase temperature, the organic structure being grafted on white carbon black starts to decompose,
Quality starts biggish loss occur, so 2 mass loss of curve at this time is big.TG figure illustrates coupling agent phenyltrimethoxysila,e
It has been grafted to white carbon black surface.
Fig. 2 is 1 gained FT-IR map of the embodiment of the present invention 5 and comparative example, and wherein curve 1 is that (comparison is real before modified
Apply example 1) product F T-IR map, curve 2 is modified (embodiment 5) product F T-IR map, as can be seen from the figure 964cm-1
Place is the bending vibration absorption peak of Si-OH key;474cm-1Place is the bending vibration absorption peak of Si-O-Si key;798cm-1Place is
The antisymmetric stretching vibration absorption peak of Si-O-Si key;1107cm-1The absorption peak at place is that the symmetrical stretching vibration of Si-O-Si key is inhaled
Receive peak;1600cm-1Place is H-O-H flexural vibrations peak;3400cm-1Place is the stretching vibration peak of-OH.It is red after comparison before modified
External spectrum the figure, it is found that-OH vibration absorption peak of modified silica obviously weakens, and illustrates the surface of modified white carbon black
Hydroxyl is obviously reduced, and illustrates that phenyltrimethoxysila,e has been grafted to white carbon black surface.
Fig. 3 is 1 gained TEM map of the embodiment of the present invention 5 and comparative example, and wherein A figure is (comparative example before modified
1) product TEM map, B figure is modified (embodiment 5) product TEM map, it can be seen that the primary particle of white carbon black is
Spherical shape, and primary particle is connected with each other, and constitutes reticular structure.In addition, white carbon black aggregation extent is high before modified, modified two
Silica aggregation extent is small, illustrates that the dispersibility of modified silica is more preferable.The partial size of white carbon black is 19-23nm before modified,
Modified white carbon black partial size is 21-24nm, and modified initial particle becomes larger.
Advantages of the present invention:
White carbon black prepared by the present invention, obtained beneficial effect is: compared with traditional white carbon black i.e. precipitation method preparation, this hair
The white carbon black of bright preparation has hydrophobicity, can have good compatibility with the molecule in butadiene-styrene rubber, can promote butadiene-styrene rubber
Wear-resisting property, processing performance and mechanical property.When white carbon black activation grade reaches 100%, the hydrophobicity of white carbon black is best, oleophylic
Change degree is maximum, and when being used for butadiene-styrene rubber reinforcement, the more traditional white carbon black of volume worn reduces 21.1%, and wear-resisting property obtains
It improves, while reducing the mooney viscosity and vulcanization time of butadiene-styrene rubber, tensile strength improves 6.18%, pulls apart growth rate and mentions
High by 9.04%, white carbon black prepared by the present invention is used for butadiene-styrene rubber reinforcement, and the hydrophobic performance and wear-resisting property of rubber are obviously excellent
In traditional white carbon black.
Specific embodiment
The present invention will be described further in conjunction with the embodiments, these embodiments are only to illustrate to be used, without that should be solved
It is interpreted as the limitation that the present invention is implemented.
Test method
1) activation grade measures:
It accurately weighs 1.0g modified white carbon black to be placed in a beaker, adds 50ml distilled water, stirred with certain revolving speed
30min is then transported in 250mL separatory funnel, is stood for 24 hours, will be sunk to white carbon black filtering, drying, the weighing of bottom, root
Activation grade is calculated according to formula:
2) lipophilic degree measures:
It accurately weighs 1.0g white carbon black to be placed in a beaker, adds 50ml distilled water, dehydrated alcohol is added dropwise until white carbon black
It is all infiltrated, records the consumption V (mL) of dehydrated alcohol at this time, lipophilic degree is calculated according to formula:
3) surface hydroxyl number measures:
It accurately weighs 2.0g white carbon black to be placed in 200ml beaker, is subsequently added into dehydrated alcohol 25ml, mass fraction 20%
NaCl solution 75ml.It is stirred with magnetic stirring apparatus with certain speed, NaOH (HCl) titer that 0.1mol/L is added dropwise adjusts examination
To 4, the NaOH for then starting to be added dropwise 0.1mol/L makes test solution PH reach 9.0 and 20s to keep PH constant the pH value of liquid.According to formula
Calculate the hydroxyl number (N) on white carbon black every square nanometers white carbon black surface:
4) thermogravimetric TG, infrared spectroscopy FTIR, transmission electron microscope TEM, specific surface area BET measurement carry out in accordance with the following methods.
Thermogravimetric TG is measured using the resistance to company's T G 209F3 type thermogravimetric analyzer of speeding of Germany.
Infrared spectroscopy FTIR carries out FTIR measurement using Japan's Shimadzu Corporation IRAffinity-1 type infrared spectrometer.
Transmission electron microscope TEM is measured using Jeol Ltd. JEM-2100 type transmission electron microscope.
Specific surface area BET is according to GB/T3073-2008 " the measurement N2 adsorption method of precipitated hydrated silica specific surface "
Measure the specific surface area of silica.
5) Mooney of sizing material, abrasion, curability and mechanics performance determining.
Refining glue experiment is carried out by HG/T2404-2008 " identification of the precipitated hydrated silica in butadiene-styrene rubber ".
By GB/T1232 " half finished rubber shears viscosimeter with disk and is measured first part: the measurement of Mooney viscosity "
Test the Mooney viscosity of rubber.
By GB/T9867-2008 " measurement (the rotating roller cartridge type abrasion machine of vulcanized rubber or thermoplastic elastomer wear-resisting property
Method " test rubber wear-resisting property.
By the sulphur of GB/T9869-2014 " measurement (oscillating disc curemeter method) of rubber size vulcanization characteristics " test rubber
Changeization characteristic.
Stress-is carried out by GB/T528-2009 " measurement of vulcanized rubber or thermoplastic elastomer tensile stress-strain performance " to answer
Become the test of characteristic.
Embodiment 1
400g silica wetcake is added in 2L reaction kettle, 200g deionized water is added, is heated to oil bath pan
80 DEG C, with dilute sulfuric acid adjusting solution pH value to 3.5, coupling agent phenyltrimethoxysila,e 11.74g is added and is modified reaction,
Modification time is 1.5h.It finally washes, filter, is dry, obtaining the high abrasion white carbon black for butadiene-styrene rubber reinforcement.
Embodiment 2
400g silica wetcake is added in 2L reaction kettle, 200g deionized water is added, is heated to oil bath pan
80 DEG C, with dilute sulfuric acid adjusting solution pH value to 3.5, coupling agent phenyltrimethoxysila,e 19.57g is added and is modified reaction,
Modification time is 1.5h.It finally washes, filter, is dry, obtaining the high abrasion white carbon black for butadiene-styrene rubber reinforcement.
Embodiment 3
400g silica wetcake is added in 2L reaction kettle, 200g deionized water is added, is heated to oil bath pan
80 DEG C, with dilute sulfuric acid adjusting solution pH value to 3.5, coupling agent phenyltrimethoxysila,e 15.66g is added and is modified reaction,
Modification time is 1.5h.It finally washes, filter, is dry, obtaining the high abrasion white carbon black for butadiene-styrene rubber reinforcement.
Embodiment 4
400g silica wetcake is added in 2L reaction kettle, 200g deionized water is added, is heated to oil bath pan
80 DEG C, with dilute sulfuric acid adjusting solution pH value to 4.0, coupling agent phenyltrimethoxysila,e 15.66g is added and is modified reaction,
Modification time is 2h.It finally washes, filter, is dry, obtaining the high abrasion white carbon black for butadiene-styrene rubber reinforcement.
Embodiment 5
400g silica wetcake is added in 2L reaction kettle, 200g deionized water is added, is heated to oil bath pan
80 DEG C, with dilute sulfuric acid adjusting solution pH value to 3.5, coupling agent phenyltrimethoxysila,e 27.40g is added and is modified reaction,
Modification time is 1.5h.It finally washes, filter, is dry, obtaining the high abrasion white carbon black for butadiene-styrene rubber reinforcement.
Embodiment 6
400g silica wetcake is added in 2L reaction kettle, 200g deionized water is added, is heated to oil bath pan
80 DEG C, with dilute sulfuric acid adjusting solution pH value to 3.5, coupling agent phenyltrimethoxysila,e 23.48g is added and is modified reaction,
Modification time is 1.5h.It finally washes, filter, is dry, obtaining the high abrasion white carbon black for butadiene-styrene rubber reinforcement.
Embodiment 7
400g silica wetcake is added in 2L reaction kettle, 200g deionized water is added, is heated to oil bath pan
70 DEG C, with dilute sulfuric acid adjusting solution pH value to 2.5, coupling agent phenyltrimethoxysila,e 11.74g is added and is modified reaction,
Modification time is 2h.It finally washes, filter, is dry, obtaining the high abrasion white carbon black for butadiene-styrene rubber reinforcement.
Embodiment 8
400g silica wetcake is added in 2L reaction kettle, 200g deionized water is added, is heated to oil bath pan
90 DEG C, with dilute sulfuric acid adjusting solution pH value to 4.5, coupling agent phenyltrimethoxysila,e 19.57g is added and is modified reaction,
Modification time is 1.5h.It finally washes, filter, is dry, obtaining the high abrasion white carbon black for butadiene-styrene rubber reinforcement.
Embodiment 9
400g silica wetcake is added in 2L reaction kettle, 200g deionized water is added, is heated to oil bath pan
80 DEG C, with dilute sulfuric acid adjusting solution pH value to 3.5, coupling agent phenyltrimethoxysila,e 15.66g is added and is modified reaction,
Modification time is 0.5h.It finally washes, filter, is dry, obtaining the high abrasion white carbon black for butadiene-styrene rubber reinforcement.
Embodiment 10
400g silica wetcake is added in 2L reaction kettle, 200g deionized water is added, is heated to oil bath pan
80 DEG C, with dilute sulfuric acid adjusting solution pH value to 3.5, coupling agent phenyltrimethoxysila,e 15.66g is added and is modified reaction,
Modification time is 2.5h.It finally washes, filter, is dry, obtaining the high abrasion white carbon black for butadiene-styrene rubber reinforcement.
Comparative example 1
Silica wetcake is directly dried, the white carbon black for butadiene-styrene rubber reinforcement is obtained.
Product prepared in the above embodiments is tested for the property, concrete outcome is shown in Table 1, table 2.
The performance indicator of 1 product of the present invention modified white carbon black of table
The rubber mechanical performance index of 2 product of the present invention modified white carbon black of table
It is seen from the above data that product of the present invention changes compared with comparative example 1 by phenyltrimethoxysila,e
The white carbon black of property, the lipophilic degree and activation grade of white carbon black obviously get a promotion, and white carbon black surface hydroxyl number substantially reduces, hard charcoal
Black hydrophobicity is enhanced.Vulcanization time, the mooney viscosity of butadiene-styrene rubber reduce, and processing performance is improved, is applied to
When butadiene-styrene rubber reinforcement, tensile strength improves 6.18%, pulls apart growth rate and improves 9.04%, the mechanical property of vulcanizate obtains
To promotion, meanwhile, volume worn reduces 21.1%, it is seen that wear-resisting property is greatly improved.
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete
The change and modification of multiplicity can be carried out without departing from the scope of the technological thought of the present invention' entirely.This invention it is technical
Range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.
Claims (3)
1. a kind of preparation method of the high abrasion white carbon black for butadiene-styrene rubber reinforcement, which is characterized in that the method includes with
Lower step: being added silica wetcake and deionized water in a kettle, with oil bath pan agitating and heating, is warming up to modified temperature
After degree, it is adjusted to the modification pH value of setting with dilute sulfuric acid, adds certain proportion coupling agent phenyltrimethoxysila,e and is changed
Property reaction, finally wash, filter, is dry, obtain the high abrasion white carbon black for butadiene-styrene rubber reinforcement.
2. a kind of preparation method of high abrasion white carbon black for butadiene-styrene rubber reinforcement according to claim 1, feature
It is, the modification temperature is 70-90 DEG C;Modified PH is 2.5-4.5;Modification time is 30-150min;Coupling agent phenyl front three
Oxysilane dosage is the 2.94%-6.85% of wet cake weight.
3. a kind of according to claim 1, preparation method of the high abrasion white carbon black for butadiene-styrene rubber reinforcement described in 2, special
Sign is that the modification temperature is 80 DEG C, and modified PH is 3.5, modification time 90min, coupling agent phenyltrimethoxysila,e
Dosage is the 6.85% of wet cake weight.
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CN111019400A (en) * | 2019-12-25 | 2020-04-17 | 烟台大学 | Silicon dioxide surface modification method based on homogeneous reaction system |
CN111892741A (en) * | 2020-07-06 | 2020-11-06 | 广州市绿原环保材料有限公司 | Hydrophobic modifier, hydrophobic modified sponge, and preparation method and application thereof |
CN113651332A (en) * | 2021-08-11 | 2021-11-16 | 常州大学 | Preparation method of high-performance white carbon black based on styrene butadiene rubber reinforcement |
CN115651424A (en) * | 2022-10-24 | 2023-01-31 | 山东阳谷华泰化工股份有限公司 | Preparation method of modified white carbon black and obtained product |
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Cited By (6)
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CN111019400A (en) * | 2019-12-25 | 2020-04-17 | 烟台大学 | Silicon dioxide surface modification method based on homogeneous reaction system |
CN111892741A (en) * | 2020-07-06 | 2020-11-06 | 广州市绿原环保材料有限公司 | Hydrophobic modifier, hydrophobic modified sponge, and preparation method and application thereof |
CN113651332A (en) * | 2021-08-11 | 2021-11-16 | 常州大学 | Preparation method of high-performance white carbon black based on styrene butadiene rubber reinforcement |
CN113651332B (en) * | 2021-08-11 | 2023-10-27 | 常州大学 | Preparation method of high-performance white carbon black based on styrene-butadiene rubber reinforcement |
CN115651424A (en) * | 2022-10-24 | 2023-01-31 | 山东阳谷华泰化工股份有限公司 | Preparation method of modified white carbon black and obtained product |
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