CN112143259A - Treatment process for improving reinforcing effect of white carbon black - Google Patents

Treatment process for improving reinforcing effect of white carbon black Download PDF

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Publication number
CN112143259A
CN112143259A CN202011108448.7A CN202011108448A CN112143259A CN 112143259 A CN112143259 A CN 112143259A CN 202011108448 A CN202011108448 A CN 202011108448A CN 112143259 A CN112143259 A CN 112143259A
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carbon black
white carbon
reinforcing effect
treatment
improving
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刘艺
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Anhui Jinhua Zinc Oxide Co ltd
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Anhui Jinhua Zinc Oxide Co ltd
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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
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/309—Combinations of treatments provided for in groups C09C1/3009 - C09C1/3081
    • 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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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
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    • 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
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    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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    • 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
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    • 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
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3045—Treatment with inorganic compounds
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3063—Treatment with low-molecular organic compounds
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3072—Treatment with macro-molecular organic compounds
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    • 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
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3081—Treatment with organo-silicon compounds
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    • 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
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/10—Treatment with macromolecular organic compounds
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12—Treatment with organosilicon compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area

Abstract

The invention discloses a treatment process for improving the reinforcing effect of white carbon black; relates to the technical field of white carbon black, comprising the following steps: the method comprises the following steps: (1) treating the corn straws; (2) preparing water glass filtrate; (3) preparing primary white carbon black; (4) performing composite treatment; the white carbon black prepared by the method has higher specific surface area and excellent rubber reinforcing effect, and can remarkably improve the vulcanization characteristic of rubber and improve the mechanical property of the rubber.

Description

Treatment process for improving reinforcing effect of white carbon black
Technical Field
The invention belongs to the technical field of white carbon black, and particularly relates to a treatment process for improving the reinforcing effect of white carbon black.
Background
White carbon black is a general term for white powdery X-ray amorphous silicic acid and silicate products, mainly referring to precipitated silica, fumed silica and ultrafine silica gel, and also including powdery synthetic aluminum silicate, calcium silicate, and the like. White carbon black is a porous substance, and the composition of the white carbon black can be represented by SiO2 & nH2O, wherein nH2O exists in the form of surface hydroxyl. It is soluble in caustic alkali and hydrofluoric acid, and insoluble in water, solvent and acid (except hydrofluoric acid). High-temperature resistance, non-combustion, tastelessness, odorless and good electrical insulation.
The white carbon black is largely classified into precipitated white carbon black and fumed white carbon black according to the production method. The fumed silica is white amorphous flocculent semitransparent solid colloidal nano particles (the particle size is less than 100 nm) in a normal state, is nontoxic and has a huge specific surface area. The fumed silica is completely nano silicon dioxide, the product purity can reach 99%, the particle size can reach 10-20 nm, but the preparation process is complex and the price is high; the precipitated silica is classified into conventional precipitated silica and special precipitated silica, the former is prepared from sulfuric acid, hydrochloric acid, and CO2The silicon dioxide produced by taking water glass as a basic raw material refers to the silicon dioxide produced by adopting a special method such as a supergravity technology, a sol-gel method, a chemical crystal method, a secondary crystallization method or a reversed-phase micelle microemulsion method. The precipitated white carbon black is mainly used as a reinforcing agent of natural rubber and synthetic rubber, a toothpaste friction agent and the like.
However, the white carbon black prepared in the prior art is directly added into rubber as a reinforcing agent, the compatibility between the white carbon black and rubber molecules is general, and aggregation is easily caused after the addition amount is increased, so that the mechanical property of the rubber is reduced to a certain extent.
Disclosure of Invention
The invention aims to provide a treatment process for improving the reinforcing effect of white carbon black, so as to solve the defects in the prior art.
The technical scheme adopted by the invention is as follows:
a treatment process for improving the reinforcing effect of white carbon black comprises the following steps:
(1) treating the corn straws:
crushing and sieving the corn straws to obtain corn straw powder;
adding the corn straw powder into a pyrolysis furnace, carrying out pyrolysis treatment for 30-35min at 700-750 ℃ to obtain pyrolysis corn straw powder, then carrying out acid pickling treatment on the pyrolysis corn straw powder, and carrying out suction filtration to obtain acid-pickled pyrolysis powder;
(2) preparing water glass filtrate:
adding the acid-washing pyrolysis powder into a hot sodium hydroxide solution, and stirring for 30min to obtain a mixed dispersion liquid;
adding the mixed dispersion liquid into a vacuum reaction kettle, adjusting the temperature to 110-114 ℃, preserving heat, stirring for 2.5-3 hours, taking out, standing for 2 hours, and then carrying out suction filtration to obtain water glass filtrate;
(3) preparing primary white carbon black:
adding water glass filtrate into a reaction kettle, then adding absolute ethyl alcohol and a silane coupling agent, stirring at the rotating speed of 500r/min for 40-50min, then dropwise adding an ammonium chloride solution, after dropwise adding is finished, carrying out ultrasonic treatment at the frequency of 40kHz and the power of 350W for 10min, continuing stirring for 2 hours, standing for 1 hour, filtering white precipitate, cleaning, drying to constant weight, crushing and sieving to obtain primary white carbon black;
(4) performing composite treatment:
heating a torque rheometer to 110-115 ℃, then sequentially adding primary white carbon black and trans-polyisoprene, carrying out heat preservation treatment for 2 hours, then adding maleic anhydride and an initiator, continuing heat preservation treatment for 40 minutes, then discharging, cooling to room temperature, crushing, and sieving to obtain the finished product composite white carbon black material.
The granularity of the corn straw powder is 200 meshes;
the atmosphere in the pyrolysis furnace is air atmosphere.
The acid pickling treatment comprises the following steps: adding the pyrolytic corn straw powder into a hydrochloric acid solution with the mass 2 times that of the pyrolytic corn straw powder, stirring at the rotating speed of 1000r/min for 55min, standing for 1 h, performing suction filtration, and washing with water to be neutral to obtain acid-washed pyrolytic powder;
the concentration of the hydrochloric acid solution is 1.5 mol/L.
The hot sodium hydroxide solution is a sodium hydroxide solution with the mass fraction of 10% and the temperature of 70-75 ℃;
the mixing ratio of the hot sodium hydroxide solution to the acid pickling pyrolysis powder is as follows: 500 mL: 85-90 g.
The vacuum degree in the vacuum reaction kettle is 50-80 Pa.
The mixing mass ratio of the water glass filtrate, the absolute ethyl alcohol and the silane coupling agent is as follows: 50-60: 80-85:1-2.
The silane coupling agent is vinyl tri (beta-methoxy ethoxy) silane.
The mixing mass ratio of the ammonium chloride solution to the water glass filtrate is 1: 2;
the mass fraction of the ammonium chloride solution is 5%.
The rotating speed of the rotor of the torque rheometer is 80 r/min;
the primary white carbon black, the trans-polyisoprene, the maleic anhydride and the initiator are mixed according to the following weight parts: 15-20:6-8:3-5:0.2-0.4.
The initiator is dicumyl peroxide.
During the reaction process of preparing the primary white carbon black, thick spherical isolated white carbon black particles are gradually formed, the aggregation degree of primary particle aggregates is generally called the structure degree of the white carbon black, the aggregation degree of the primary particle aggregates is cooperated with ultrasonic treatment at a certain frequency along with the reaction, so that the number and the size of the primary particles are gradually increased, when the viscosity of a system reaches a gel point and the concentration of silicate reaches a key value, the primary particles start to form the aggregates through Si-O-Si bonds, and the Si-O-Si bonds are very stable.
After further increase by the number and size of aggregates followed by subsequent reaction, until aggregates are brought together by reversible hydrogen bonding, forming agglomerates. Through certain ultrasonic treatment, the number of silicon hydroxyl groups among primary particles can be increased, and the structure degree of the aggregate is increased. The high aggregate structure degree can resist compression in the subsequent drying process, so that larger void degree is generated between aggregates, and the reinforcing effect of the aggregate in the rubber field can be further improved.
The surface of the white carbon black prepared by the method contains silicon oxygen groups and silicon hydroxyl groups, and the number of the silicon hydroxyl groups on the surface, the types of adsorbed moisture and the pH value determine the surface chemical properties of the white carbon black. The surface of the white carbon black prepared by the method comprises 3 hydroxyl groups: lone site silicon hydroxyl, with 1 hydroxyl on 1 silicon atom; ortho-silicon hydroxyl, 2 hydroxyl groups on 2 adjacent silicon atoms; geminal silicon hydroxyl groups, 2 hydroxyl groups on the same silicon atom. The adjacent silicon hydroxyl groups, such as geminal silicon hydroxyl groups, have strong water absorption capacity. The ratio of gem-position silicon hydroxyl contained on the surface of the white carbon black prepared by the method is less than 20 percent, and the white carbon black shows stronger reinforcing and dispersing properties.
Has the advantages that: the white carbon black prepared by the method has higher specific surface area and excellent rubber reinforcing effect, can obviously improve the vulcanization characteristic of rubber and improve the mechanical property of the rubber, the specific surface area of the primary white carbon black prepared by the method is greatly increased, the surface area of the white carbon black is an important factor determining the reinforcing capability of the white carbon black, the white carbon black prepared by the method can obviously improve the vulcanization characteristic when being applied to natural rubber, the crosslinking degree of rubber materials is higher, the dispersibility of the white carbon black prepared by the process is better, the adsorption capability of the white carbon black on rubber molecular chains is greatly enhanced, so that the crosslinking degree of the rubber can be improved, the adsorption of the white carbon black on an accelerator is enhanced due to the strong polar silicon hydroxyl on the surface of the traditional white carbon black, the t90 of the rubber material is prolonged, the vulcanization efficiency is lower, and the surface polarity of the white carbon black prepared by the process is reduced, the dispersibility in a rubber matrix is improved, the adsorption to an accelerant is weakened, and the vulcanization efficiency of the rubber material is improved.
Detailed Description
A treatment process for improving the reinforcing effect of white carbon black comprises the following steps:
(1) treating the corn straws:
crushing and sieving the corn straws to obtain corn straw powder;
adding the corn straw powder into a pyrolysis furnace, carrying out pyrolysis treatment for 30-35min at 700-750 ℃ to obtain pyrolysis corn straw powder, then carrying out acid pickling treatment on the pyrolysis corn straw powder, and carrying out suction filtration to obtain acid-pickled pyrolysis powder;
(2) preparing water glass filtrate:
adding the acid-washing pyrolysis powder into a hot sodium hydroxide solution, and stirring for 30min to obtain a mixed dispersion liquid;
adding the mixed dispersion liquid into a vacuum reaction kettle, adjusting the temperature to 110-114 ℃, preserving heat, stirring for 2.5-3 hours, taking out, standing for 2 hours, and then carrying out suction filtration to obtain water glass filtrate;
(3) preparing primary white carbon black:
adding water glass filtrate into a reaction kettle, then adding absolute ethyl alcohol and a silane coupling agent, stirring at the rotating speed of 500r/min for 40-50min, then dropwise adding an ammonium chloride solution, after dropwise adding is finished, carrying out ultrasonic treatment at the frequency of 40kHz and the power of 350W for 10min, continuing stirring for 2 hours, standing for 1 hour, filtering white precipitate, cleaning, drying to constant weight, crushing and sieving to obtain primary white carbon black;
(4) performing composite treatment:
heating a torque rheometer to 110-115 ℃, then sequentially adding primary white carbon black and trans-polyisoprene, carrying out heat preservation treatment for 2 hours, then adding maleic anhydride and an initiator, continuing heat preservation treatment for 40 minutes, then discharging, cooling to room temperature, crushing, and sieving to obtain the finished product composite white carbon black material.
The granularity of the corn straw powder is 200 meshes;
the atmosphere in the pyrolysis furnace is air atmosphere.
The acid pickling treatment comprises the following steps: adding the pyrolytic corn straw powder into a hydrochloric acid solution with the mass 2 times that of the pyrolytic corn straw powder, stirring at the rotating speed of 1000r/min for 55min, standing for 1 h, performing suction filtration, and washing with water to be neutral to obtain acid-washed pyrolytic powder;
the concentration of the hydrochloric acid solution is 1.5 mol/L.
The hot sodium hydroxide solution is a sodium hydroxide solution with the mass fraction of 10% and the temperature of 70-75 ℃;
the mixing ratio of the hot sodium hydroxide solution to the acid pickling pyrolysis powder is as follows: 500 mL: 85-90 g.
The vacuum degree in the vacuum reaction kettle is 50-80 Pa.
The mixing mass ratio of the water glass filtrate, the absolute ethyl alcohol and the silane coupling agent is as follows: 50-60: 80-85:1-2.
The silane coupling agent is vinyl tri (beta-methoxy ethoxy) silane.
The mixing mass ratio of the ammonium chloride solution to the water glass filtrate is 1: 2;
the mass fraction of the ammonium chloride solution is 5%.
The rotating speed of the rotor of the torque rheometer is 80 r/min;
the primary white carbon black, the trans-polyisoprene, the maleic anhydride and the initiator are mixed according to the following weight parts: 15-20:6-8:3-5:0.2-0.4.
The initiator is dicumyl peroxide.
The following will clearly and completely describe the technical solutions of the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A treatment process for improving the reinforcing effect of white carbon black comprises the following steps:
(1) treating the corn straws:
crushing and sieving the corn straws to obtain corn straw powder;
adding the corn straw powder into a pyrolysis furnace, carrying out pyrolysis treatment for 30min at 700 ℃ to obtain pyrolyzed corn straw powder, then carrying out acid pickling treatment on the pyrolyzed corn straw powder, and carrying out suction filtration to obtain acid-pickled pyrolyzed powder; the granularity of the corn straw powder is 200 meshes; the atmosphere in the pyrolysis furnace is air atmosphere. The acid pickling treatment comprises the following steps: adding the pyrolytic corn straw powder into a hydrochloric acid solution with the mass 2 times that of the pyrolytic corn straw powder, stirring at the rotating speed of 1000r/min for 55min, standing for 1 h, performing suction filtration, and washing with water to be neutral to obtain acid-washed pyrolytic powder; the concentration of the hydrochloric acid solution is 1.5 mol/L.
(2) Preparing water glass filtrate:
adding the acid-washing pyrolysis powder into a hot sodium hydroxide solution, and stirring for 30min to obtain a mixed dispersion liquid;
adding the mixed dispersion liquid into a vacuum reaction kettle, adjusting the temperature to 110 ℃, preserving heat, stirring for 2.5 hours, taking out, standing for 2 hours, and then carrying out suction filtration to obtain water glass filtrate; the hot sodium hydroxide solution is a sodium hydroxide solution with the mass fraction of 10% and the temperature of 70 ℃; the mixing ratio of the hot sodium hydroxide solution to the acid pickling pyrolysis powder is as follows: 500 mL: 85 g. The vacuum degree in the vacuum reaction kettle is 50 Pa.
(3) Preparing primary white carbon black:
adding water glass filtrate into a reaction kettle, then adding absolute ethyl alcohol and a silane coupling agent, stirring at the rotating speed of 500r/min for 40min, then dropwise adding an ammonium chloride solution, carrying out ultrasonic treatment at the frequency of 40kHz and the power of 350W for 10min after dropwise adding is finished, continuing stirring for 2 hours, standing for 1 hour, filtering white precipitate, cleaning, drying to constant weight, crushing and sieving to obtain primary white carbon black; the mixing mass ratio of the water glass filtrate, the absolute ethyl alcohol and the silane coupling agent is as follows: 50: 80:1. The silane coupling agent is vinyl tri (beta-methoxy ethoxy) silane. The mixing mass ratio of the ammonium chloride solution to the water glass filtrate is 1: 2; the mass fraction of the ammonium chloride solution is 5%.
(4) Performing composite treatment:
heating a torque rheometer to 110 ℃, then sequentially adding primary white carbon black and trans-polyisoprene, carrying out heat preservation treatment for 2 hours, then adding maleic anhydride and an initiator, continuing heat preservation treatment for 40 minutes, then discharging, cooling to room temperature, crushing, and sieving to obtain the finished product composite white carbon black material. The rotating speed of the rotor of the torque rheometer is 80 r/min; the primary white carbon black, the trans-polyisoprene, the maleic anhydride and the initiator are mixed according to the following weight parts: 15:6:3:0.2. The initiator is dicumyl peroxide.
Example 2
A treatment process for improving the reinforcing effect of white carbon black comprises the following steps:
(1) treating the corn straws:
crushing and sieving the corn straws to obtain corn straw powder;
adding the corn straw powder into a pyrolysis furnace, carrying out pyrolysis treatment for 35min at 750 ℃ to obtain pyrolyzed corn straw powder, then carrying out acid pickling treatment on the pyrolyzed corn straw powder, and carrying out suction filtration to obtain acid-pickled pyrolyzed powder; the granularity of the corn straw powder is 200 meshes; the atmosphere in the pyrolysis furnace is air atmosphere. The acid pickling treatment comprises the following steps: adding the pyrolytic corn straw powder into a hydrochloric acid solution with the mass 2 times that of the pyrolytic corn straw powder, stirring at the rotating speed of 1000r/min for 55min, standing for 1 h, performing suction filtration, and washing with water to be neutral to obtain acid-washed pyrolytic powder; the concentration of the hydrochloric acid solution is 1.5 mol/L.
(2) Preparing water glass filtrate:
adding the acid-washing pyrolysis powder into a hot sodium hydroxide solution, and stirring for 30min to obtain a mixed dispersion liquid;
adding the mixed dispersion liquid into a vacuum reaction kettle, adjusting the temperature to 114 ℃, preserving heat, stirring for 3 hours, taking out, standing for 2 hours, and then carrying out suction filtration to obtain water glass filtrate; the hot sodium hydroxide solution is a sodium hydroxide solution with the mass fraction of 10% and the temperature of 75 ℃; the mixing ratio of the hot sodium hydroxide solution to the acid pickling pyrolysis powder is as follows: 500 mL: 90 g. The vacuum degree in the vacuum reaction kettle is 80 Pa.
(3) Preparing primary white carbon black:
adding water glass filtrate into a reaction kettle, then adding absolute ethyl alcohol and a silane coupling agent, stirring at the rotating speed of 500r/min for 50min, then dropwise adding an ammonium chloride solution, carrying out ultrasonic treatment at the frequency of 40kHz and the power of 350W for 10min after dropwise adding is finished, continuing stirring for 2 hours, standing for 1 hour, filtering white precipitate, cleaning, drying to constant weight, crushing and sieving to obtain primary white carbon black; the mixing mass ratio of the water glass filtrate, the absolute ethyl alcohol and the silane coupling agent is as follows: 60: 85:2. The silane coupling agent is vinyl tri (beta-methoxy ethoxy) silane. The mixing mass ratio of the ammonium chloride solution to the water glass filtrate is 1: 2; the mass fraction of the ammonium chloride solution is 5%.
(4) Performing composite treatment:
heating a torque rheometer to 115 ℃, then sequentially adding primary white carbon black and trans-polyisoprene, carrying out heat preservation treatment for 2 hours, then adding maleic anhydride and an initiator, continuing heat preservation treatment for 40 minutes, then discharging, cooling to room temperature, crushing, and sieving to obtain the finished product composite white carbon black material. The rotating speed of the rotor of the torque rheometer is 80 r/min; the primary white carbon black, the trans-polyisoprene, the maleic anhydride and the initiator are mixed according to the following weight parts: 20:8:5:0.4. The initiator is dicumyl peroxide.
Example 3
A treatment process for improving the reinforcing effect of white carbon black comprises the following steps:
(1) treating the corn straws:
crushing and sieving the corn straws to obtain corn straw powder;
adding the corn straw powder into a pyrolysis furnace, carrying out pyrolysis treatment for 31min at 720 ℃ to obtain pyrolyzed corn straw powder, then carrying out acid pickling treatment on the pyrolyzed corn straw powder, and carrying out suction filtration to obtain acid-pickled pyrolysis powder; the granularity of the corn straw powder is 200 meshes; the atmosphere in the pyrolysis furnace is air atmosphere. The acid pickling treatment comprises the following steps: adding the pyrolytic corn straw powder into a hydrochloric acid solution with the mass 2 times that of the pyrolytic corn straw powder, stirring at the rotating speed of 1000r/min for 55min, standing for 1 h, performing suction filtration, and washing with water to be neutral to obtain acid-washed pyrolytic powder; the concentration of the hydrochloric acid solution is 1.5 mol/L.
(2) Preparing water glass filtrate:
adding the acid-washing pyrolysis powder into a hot sodium hydroxide solution, and stirring for 30min to obtain a mixed dispersion liquid;
adding the mixed dispersion liquid into a vacuum reaction kettle, adjusting the temperature to 113 ℃, keeping the temperature, stirring for 2.8 hours, taking out, standing for 2 hours, and then carrying out suction filtration to obtain water glass filtrate; the hot sodium hydroxide solution is a sodium hydroxide solution with the mass fraction of 10% and the temperature of 72 ℃; the mixing ratio of the hot sodium hydroxide solution to the acid pickling pyrolysis powder is as follows: 500 mL: 88 g. The vacuum degree in the vacuum reaction kettle is 60 Pa.
(3) Preparing primary white carbon black:
adding water glass filtrate into a reaction kettle, then adding absolute ethyl alcohol and a silane coupling agent, stirring for 45min at the rotating speed of 500r/min, then dropwise adding an ammonium chloride solution, after dropwise adding is finished, carrying out ultrasonic treatment for 10min at the frequency of 40kHz and the power of 350W, continuously stirring for 2 h, standing for 1 h, filtering white precipitate, cleaning, drying to constant weight, crushing and sieving to obtain primary white carbon black; the mixing mass ratio of the water glass filtrate, the absolute ethyl alcohol and the silane coupling agent is as follows: 55: 82:1.3. The silane coupling agent is vinyl tri (beta-methoxy ethoxy) silane. The mixing mass ratio of the ammonium chloride solution to the water glass filtrate is 1: 2; the mass fraction of the ammonium chloride solution is 5%.
(4) Performing composite treatment:
heating a torque rheometer to 114 ℃, then sequentially adding primary white carbon black and trans-polyisoprene, carrying out heat preservation treatment for 2 hours, then adding maleic anhydride and an initiator, continuing heat preservation treatment for 40 minutes, then discharging, cooling to room temperature, crushing, and sieving to obtain the finished product composite white carbon black material. The rotating speed of the rotor of the torque rheometer is 80 r/min; the primary white carbon black, the trans-polyisoprene, the maleic anhydride and the initiator are mixed according to the following weight parts: 16:7:3.5:0.25. The initiator is dicumyl peroxide.
Example 4
A treatment process for improving the reinforcing effect of white carbon black comprises the following steps:
(1) treating the corn straws:
crushing and sieving the corn straws to obtain corn straw powder;
adding the corn straw powder into a pyrolysis furnace, carrying out pyrolysis treatment for 35min at 720 ℃ to obtain pyrolyzed corn straw powder, then carrying out acid pickling treatment on the pyrolyzed corn straw powder, and carrying out suction filtration to obtain acid-pickled pyrolysis powder; the granularity of the corn straw powder is 200 meshes; the atmosphere in the pyrolysis furnace is air atmosphere. The acid pickling treatment comprises the following steps: adding the pyrolytic corn straw powder into a hydrochloric acid solution with the mass 2 times that of the pyrolytic corn straw powder, stirring at the rotating speed of 1000r/min for 55min, standing for 1 h, performing suction filtration, and washing with water to be neutral to obtain acid-washed pyrolytic powder; the concentration of the hydrochloric acid solution is 1.5 mol/L.
(2) Preparing water glass filtrate:
adding the acid-washing pyrolysis powder into a hot sodium hydroxide solution, and stirring for 30min to obtain a mixed dispersion liquid;
adding the mixed dispersion liquid into a vacuum reaction kettle, adjusting the temperature to 110 ℃, preserving heat, stirring for 2.5 hours, taking out, standing for 2 hours, and then carrying out suction filtration to obtain water glass filtrate; the hot sodium hydroxide solution is a sodium hydroxide solution with the mass fraction of 10% and the temperature of 75 ℃; the mixing ratio of the hot sodium hydroxide solution to the acid pickling pyrolysis powder is as follows: 500 mL: 86 g. The vacuum degree in the vacuum reaction kettle is 65 Pa.
(3) Preparing primary white carbon black:
adding water glass filtrate into a reaction kettle, then adding absolute ethyl alcohol and a silane coupling agent, stirring at the rotating speed of 500r/min for 50min, then dropwise adding an ammonium chloride solution, carrying out ultrasonic treatment at the frequency of 40kHz and the power of 350W for 10min after dropwise adding is finished, continuing stirring for 2 hours, standing for 1 hour, filtering white precipitate, cleaning, drying to constant weight, crushing and sieving to obtain primary white carbon black; the mixing mass ratio of the water glass filtrate, the absolute ethyl alcohol and the silane coupling agent is as follows: 54: 83:1.5. The silane coupling agent is vinyl tri (beta-methoxy ethoxy) silane. The mixing mass ratio of the ammonium chloride solution to the water glass filtrate is 1: 2; the mass fraction of the ammonium chloride solution is 5%.
(4) Performing composite treatment:
heating a torque rheometer to 112 ℃, then sequentially adding primary white carbon black and trans-polyisoprene, carrying out heat preservation treatment for 2 hours, then adding maleic anhydride and an initiator, continuing heat preservation treatment for 40 minutes, then discharging, cooling to room temperature, crushing, and sieving to obtain the finished product composite white carbon black material. The rotating speed of the rotor of the torque rheometer is 80 r/min; the primary white carbon black, the trans-polyisoprene, the maleic anhydride and the initiator are mixed according to the following weight parts: 18:6.5:4:0.3. The initiator is dicumyl peroxide.
Detecting the specific surface area of the primary white carbon black in the examples and the comparative examples by adopting a BET method;
TABLE 1
Figure DEST_PATH_IMAGE001
Comparative example 1: application No. 201410700622.5, preparation method of white carbon black;
as can be seen from Table 1, the specific surface area of the primary white carbon black prepared by the method of the present invention is greatly increased, and the surface area of the white carbon black is an important factor for determining the reinforcing ability of the white carbon black.
Detection of reinforcement effect:
sample (parts by weight): 80 parts of natural rubber, 30 parts of white carbon black in examples and comparative examples, 4 parts of zinc oxide, 2 parts of stearic acid, 1.5 parts of rubber oil, 40201.2 parts of anti-aging agent, 1.35 parts of sulfur and 0.3 part of accelerator D;
3-stage banburying is carried out in an internal mixer, the initial temperature of the first-stage banburying, the second-stage banburying and the third-stage banburying are respectively set to be 90 ℃, 115 ℃ and 120 ℃, the rotor rotating speed is 90 r/min, the white carbon black and the rubber oil in the examples and the comparative examples are added in the banburying process, and the banburying is carried out for 6 min, and then the rubber is discharged. The dense rubber is milled on a double-roll mill, and zinc oxide, stearic acid, accelerator D, anti-aging agent 4020 and sulfur are added in sequence after roll wrapping. Uniformly mixing the rubber materials, then thinly passing for 7 times, and adjusting the roller spacing for sheet feeding to obtain a sample;
test for vulcanization Properties
Testing the vulcanization characteristic of the material by a rotor-free vulcanization instrument, wherein the temperature is 143 ℃;
TABLE 2
Figure 611965DEST_PATH_IMAGE002
Comparative example 1: application No. 201410700622.5, preparation method of white carbon black; (ii) a
It can be seen from table 2 that, when the white carbon black prepared by the method of the present invention is applied to natural rubber, the vulcanization characteristic can be significantly improved, the crosslinking degree of the rubber material is higher, the dispersibility of the white carbon black prepared by the process of the present invention is better, and the adsorption capability of the white carbon black to rubber molecular chains is greatly enhanced, such that the crosslinking degree of the rubber can be promoted to be improved, whereas the adsorption of the white carbon black to accelerators is enhanced due to the strong polar silicon hydroxyl group on the surface of the traditional white carbon black, such that t90 of the rubber material is prolonged, and the vulcanization efficiency is lower, whereas the surface polarity of the white carbon black prepared by the process of the present invention is reduced, the dispersibility in the rubber matrix is improved, the adsorption.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention, and the present invention is not limited to the illustrated embodiments, and all the modifications and equivalents of the embodiments may be made without departing from the spirit of the present invention.

Claims (10)

1. A treatment process for improving the reinforcing effect of white carbon black is characterized by comprising the following steps:
(1) treating the corn straws:
crushing and sieving the corn straws to obtain corn straw powder;
adding the corn straw powder into a pyrolysis furnace, carrying out pyrolysis treatment for 30-35min at 700-750 ℃ to obtain pyrolysis corn straw powder, then carrying out acid pickling treatment on the pyrolysis corn straw powder, and carrying out suction filtration to obtain acid-pickled pyrolysis powder;
(2) preparing water glass filtrate:
adding the acid-washing pyrolysis powder into a hot sodium hydroxide solution, and stirring for 30min to obtain a mixed dispersion liquid;
adding the mixed dispersion liquid into a vacuum reaction kettle, adjusting the temperature to 110-114 ℃, preserving heat, stirring for 2.5-3 hours, taking out, standing for 2 hours, and then carrying out suction filtration to obtain water glass filtrate;
(3) preparing primary white carbon black:
adding water glass filtrate into a reaction kettle, then adding absolute ethyl alcohol and a silane coupling agent, stirring at the rotating speed of 500r/min for 40-50min, then dropwise adding an ammonium chloride solution, after dropwise adding is finished, carrying out ultrasonic treatment at the frequency of 40kHz and the power of 350W for 10min, continuing stirring for 2 hours, standing for 1 hour, filtering white precipitate, cleaning, drying to constant weight, crushing and sieving to obtain primary white carbon black;
(4) performing composite treatment:
heating a torque rheometer to 110-115 ℃, then sequentially adding primary white carbon black and trans-polyisoprene, carrying out heat preservation treatment for 2 hours, then adding maleic anhydride and an initiator, continuing heat preservation treatment for 40 minutes, then discharging, cooling to room temperature, crushing, and sieving to obtain the finished product composite white carbon black material.
2. The treatment process for improving the reinforcing effect of white carbon black according to claim 1, characterized in that: the granularity of the corn straw powder is 200 meshes;
the atmosphere in the pyrolysis furnace is air atmosphere.
3. The treatment process for improving the reinforcing effect of white carbon black according to claim 1, characterized in that: the acid pickling treatment comprises the following steps: adding the pyrolytic corn straw powder into a hydrochloric acid solution with the mass 2 times that of the pyrolytic corn straw powder, stirring at the rotating speed of 1000r/min for 55min, standing for 1 h, performing suction filtration, and washing with water to be neutral to obtain acid-washed pyrolytic powder;
the concentration of the hydrochloric acid solution is 1.5 mol/L.
4. The treatment process for improving the reinforcing effect of white carbon black according to claim 1, characterized in that: the hot sodium hydroxide solution is a sodium hydroxide solution with the mass fraction of 10% and the temperature of 70-75 ℃;
the mixing ratio of the hot sodium hydroxide solution to the acid pickling pyrolysis powder is as follows: 500 mL: 85-90 g.
5. The treatment process for improving the reinforcing effect of white carbon black according to claim 1, characterized in that: the vacuum degree in the vacuum reaction kettle is 50-80 Pa.
6. The treatment process for improving the reinforcing effect of white carbon black according to claim 1, characterized in that: the mixing mass ratio of the water glass filtrate, the absolute ethyl alcohol and the silane coupling agent is as follows: 50-60: 80-85:1-2.
7. The treatment process for improving the reinforcing effect of white carbon black according to claim 6, characterized in that: the silane coupling agent is vinyl tri (beta-methoxy ethoxy) silane.
8. The treatment process for improving the reinforcing effect of white carbon black according to claim 6, characterized in that: the mixing mass ratio of the ammonium chloride solution to the water glass filtrate is 1: 2;
the mass fraction of the ammonium chloride solution is 5%.
9. The treatment process for improving the reinforcing effect of white carbon black according to claim 1, characterized in that: the rotating speed of the rotor of the torque rheometer is 80 r/min;
the primary white carbon black, the trans-polyisoprene, the maleic anhydride and the initiator are mixed according to the following weight parts: 15-20:6-8:3-5:0.2-0.4.
10. The treatment process for improving the reinforcing effect of white carbon black according to claim 1 or 9, which is characterized in that: the initiator is dicumyl peroxide.
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