CN111253637B - Preparation method of wear-resistant rice hulling rubber roll - Google Patents

Preparation method of wear-resistant rice hulling rubber roll Download PDF

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CN111253637B
CN111253637B CN202010153823.3A CN202010153823A CN111253637B CN 111253637 B CN111253637 B CN 111253637B CN 202010153823 A CN202010153823 A CN 202010153823A CN 111253637 B CN111253637 B CN 111253637B
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rubber
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tea polyphenol
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wear
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CN111253637A (en
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梅锐
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Anlu Quansheng Grain Machinery Co ltd
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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
    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C08K3/042—Graphene or derivatives, e.g. graphene oxides
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/15—Heterocyclic compounds having oxygen in the ring
    • C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
    • C08K5/1545—Six-membered rings
    • 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
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/08—Oxygen-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2296—Oxides; Hydroxides of metals of zinc

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  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The invention provides a preparation method of an abrasion-resistant rice hulling rubber roll, which comprises the following steps: adding the modified calcium sulfate whiskers into the nitrile rubber, then continuously adding an acetic acid solution, and stirring while adding the acetic acid solution until the nitrile rubber is cured to obtain solid rubber; repeatedly washing the solid rubber by using water until the washed solution is neutral, and then drying the solid rubber; placing the accelerator DM, the dried solid rubber, the graphene, the tea polyphenol derivative, the zinc oxide, the stearic acid and the sulfur on an open type rubber mixing mill for mixing to obtain a rubber material; coating the rubber material on the outer side of the roller core by adopting an extrusion winding rubber coating method to form a rubber coating layer on the outer side of the roller core; and (3) conveying the roller core containing the rubber coating layer into a vulcanizing tank for vulcanizing to obtain the wear-resistant rice hulling rubber roller.

Description

Preparation method of wear-resistant rice hulling rubber roll
Technical Field
The invention relates to the technical field of rubber rollers, in particular to a preparation method of a wear-resistant rice hulling rubber roller.
Background
The rice huller rubber roll is a key part on the rice huller, and has the advantages of high rotating speed, large relative friction force and high heat generation. Therefore, the rice hulling rubber roll is required to have higher wear resistance, heat resistance, tensile resistance, tear resistance and moderate hardness and elasticity. Rice huller rubber roll reinforcer is mostly precipitation method white carbon black, because there are a large amount of active silanol groups and hydroxyl on white carbon black surface, make it have stronger hydrophilicity and auto-agglutination nature, consequently white carbon black is compatible relatively poorly with the rubber substrate, mainly lean on the lower hydrogen bond of bond energy and van der Waals' force to combine between the filler rubber simultaneously, and the high chemical bond of non-bond energy combines, thereby lead to under the effect of shearing force field, white carbon black granule is constantly peeled off and is formed the particle in the rice huller rubber roll, cause rice pollution, environmental pollution, and rice huller rubber roll life cycle is short.
Disclosure of Invention
In view of the above, the invention provides a preparation method of an abrasion-resistant rice hulling rubber roll, and the rice hulling rubber roll prepared by the method has high abrasion resistance, heat resistance, tensile resistance, tear resistance and moderate hardness and elasticity.
The invention provides a preparation method of an abrasion-resistant rice hulling rubber roll, which comprises the following steps:
s1, weighing 100 parts of nitrile rubber, 15-25 parts of modified calcium sulfate whisker, 10-18 parts of graphene, 5-10 parts of tea polyphenol derivative, 3-5 parts of accelerator DM, 6-8 parts of zinc oxide, 3-5 parts of stearic acid and 3-5 parts of sulfur for later use;
s2, adding the modified calcium sulfate whiskers into the nitrile rubber, then continuously adding an acetic acid solution, and stirring while adding the acetic acid solution until the nitrile rubber is solidified to obtain solid rubber;
s3, repeatedly washing the solid rubber by using water until the washed solution is neutral, and then drying the solid rubber;
s4, placing the accelerator DM, the dried solid rubber, the graphene, the tea polyphenol derivative, the zinc oxide, the stearic acid and the sulfur on an open type rubber mixing mill for mixing to obtain a rubber material;
s5, coating the rubber material on the outer side of the roller core by adopting an extrusion winding rubber coating method, and forming a rubber coating layer on the outer side of the roller core;
and S6, conveying the roller core containing the rubber coating layer into a vulcanizing tank for vulcanizing to obtain the wear-resistant rice hulling rubber roller.
Further, in step S1, 100 parts of nitrile rubber, 20 parts of modified calcium sulfate whisker, 15 parts of graphene, 8 parts of tea polyphenol derivative, 4 parts of accelerator DM, 7 parts of zinc oxide, 4 parts of stearic acid, and 4 parts of sulfur are weighed for later use.
Further, the tea polyphenol derivative is tea polyphenol-Zn2+A complex of said tea polyphenol-Zn2+The preparation process of the complex comprises the following steps: adding a proper amount of distilled water into tea polyphenol, and fully dissolving the tea polyphenol after ultrasonic oscillation for 10 minutes to obtain a tea polyphenol solution; adding 0.6mol/L zinc chloride water solution into tea polyphenol solution, mixing thoroughly, adding 0.8mol/L sodium bicarbonate water solution to adjust pH value, reacting at room temperature for 2.5h after pH value reaches 7, standing for 30h after reaction, centrifuging, washing, and drying to obtain tea polyphenol-Zn2+And (3) a complex.
Further, the preparation method of the modified calcium sulfate whisker comprises the following steps: weighing water, absolute ethyl alcohol and a silane coupling agent, hydrolyzing for 2min at 55-70 ℃ to obtain a hydrolysate, uniformly spraying the hydrolysate on the surface of the calcium sulfate whisker, drying the calcium sulfate whisker at 30-50 ℃, and stirring for 6-15 min at 100-120 ℃ to obtain the modified calcium sulfate whisker; wherein the volume ratio of water to absolute ethyl alcohol to the silane coupling agent is 1: 16: 1, the dosage of the silane coupling agent is 2.5 percent of the mass of the calcium sulfate whisker.
Further, in step S2, the mass ratio of acetic acid to water in the acetic acid solution is 1: 3.
Further, in step S4, the temperature of the open mill is set to 110 to 135 ℃, and the kneading time is 3 to 5 minutes.
Further, in step S5, the winding encapsulation method specifically includes: adding the rubber material into a screw extruder for extrusion molding to obtain a rubber sheet, and then coating the rubber sheet on the outer side of the roller core by using a rubber coating machine to form a rubber coating layer on the outer side of the roller core.
Further, in step S6, the pressure in the vulcanizing tank is set to 0.4MPa to 0.6 MPa.
The technical scheme provided by the invention has the beneficial effects that: the preparation method provided by the invention adds tea polyphenol-Zn in the mixing process2+Complexes, tea polyphenols-Zn2+Zn in the complex2+Rubber vulcanization can be promoted; according to the preparation method provided by the invention, the white carbon black is replaced by the modified calcium sulfate whisker, so that rice pollution is avoided, the modified calcium sulfate whisker and the nitrile rubber are mixed in a liquid phase environment, and the calcium sulfate whisker is uniformly dispersed in a rubber matrix in an original particle size, so that the reinforcing effect of the calcium sulfate whisker is fully exerted, the prepared rubber material has few defects and more interface phases, and therefore, the prepared rubber material has better mechanical properties; according to the preparation method provided by the invention, the graphene is added in the mixing process, has flexibility and thinner thickness, is easy to disperse in the mixing process, improves the mixing uniformity, and can improve the tear resistance and wear resistance of the rubber material by adding the graphene.
Drawings
Fig. 1 is a schematic flow chart of a preparation method of the wear-resistant rice hulling rubber roll of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
Referring to fig. 1, an embodiment of the present invention provides a method for preparing an abrasion-resistant rice hulling rubber roll, including the following steps:
step S1, weighing 100 parts of nitrile rubber, 15-25 parts of modified calcium sulfate whisker, 10-18 parts of graphene, 5-10 parts of tea polyphenol derivative, 3-5 parts of accelerator DM, 6-8 parts of zinc oxide, 3-5 parts of stearic acid and 3-5 parts of sulfur for later use;
step S2, adding the modified calcium sulfate whiskers into the nitrile rubber, then continuously adding an acetic acid solution, and stirring while adding the acetic acid solution until the nitrile rubber is cured to obtain solid rubber; the mass ratio of acetic acid to water in the acetic acid solution is 1: 3;
step S3, repeatedly washing the solid rubber by water until the washed solution is neutral, and then drying the solid rubber;
step S4, placing the accelerator DM, the dried solid rubber, the graphene, the tea polyphenol derivative, the zinc oxide, the stearic acid and the sulfur on an open type rubber mixing mill for mixing to obtain a rubber material; the temperature of the open rubber mixing mill is set to be 110-135 ℃, and the mixing time is 3-5 minutes;
step S5, adding the rubber material into a screw extruder for extrusion molding to obtain a rubber sheet, and then coating the rubber sheet on the outer side of the roller core by using a rubber coating machine to form a rubber coating layer on the outer side of the roller core;
step S6, sending the roller core containing the rubber coating layer into a vulcanizing tank for vulcanization treatment to obtain the wear-resistant rice hulling rubber roller; the pressure intensity in the vulcanizing tank is set to be 0.4MPa to 0.6 MPa.
Wherein the tea polyphenol derivative is tea polyphenol-Zn2+Complexes, tea polyphenols-Zn2+The preparation process of the complex comprises the following steps: adding a proper amount of distilled water into tea polyphenol, and fully dissolving the tea polyphenol after ultrasonic oscillation for 10 minutes to obtain a tea polyphenol solution; adding tea polyphenols solution with concentration of0.6mol/L zinc chloride water solution is fully mixed, then 0.8mol/L sodium bicarbonate water solution is added to adjust the pH value, the reaction is carried out for 2.5h at room temperature after the pH value reaches 7, the mixture is kept stand for 30h after the reaction is finished, and then the mixture is centrifuged, washed and dried to obtain the tea polyphenol-Zn2+And (3) a complex.
The preparation method of the modified calcium sulfate whisker comprises the following steps: weighing water, absolute ethyl alcohol and a silane coupling agent, hydrolyzing for 2min at 55-70 ℃ to obtain a hydrolysate, uniformly spraying the hydrolysate on the surface of the calcium sulfate whisker, drying the calcium sulfate whisker at 30-50 ℃, and stirring for 6-15 min at 100-120 ℃ to obtain the modified calcium sulfate whisker; the volume ratio of water to absolute ethyl alcohol to the silane coupling agent is 1: 16: 1, the dosage of the silane coupling agent is 2.5 percent of the mass of the calcium sulfate whisker.
The preparation method of the wear-resistant rice hulling rubber roll provided by the invention is described in detail with reference to the following embodiments.
Example 1:
weighing 20kg of modified calcium sulfate whiskers, adding the modified calcium sulfate whiskers into 100kg of nitrile rubber, then continuously adding an acetic acid solution, and stirring while adding the acetic acid solution until the nitrile rubber is cured to obtain solid rubber; repeatedly washing the solid rubber by using water until the washed solution is neutral, and then drying the solid rubber; weighing 4kg of accelerator DM, dried solid rubber, 15kg of graphene, 8kg of tea polyphenol derivative, 7kg of zinc oxide, 4kg of stearic acid and 4kg of sulfur, placing on an open rubber mixing mill, and mixing for 3 minutes to obtain a rubber material, wherein the temperature of the open rubber mixing mill is set to be 120 ℃; adding the rubber material into a screw extruder for extrusion molding to obtain a rubber sheet, and then coating the rubber sheet on the outer side of the roller core by using a rubber coating machine to form a rubber coating layer on the outer side of the roller core; and (3) conveying the roller core containing the rubber coating layer into a vulcanizing tank for vulcanization treatment to obtain the wear-resistant rice hulling rubber roller, wherein the pressure in the vulcanizing tank is set to be 0.4 MPa.
In example 1, one portion per 1 kg.
Comparative example 1:
comparative example 1 differs from example 1 only in that: comparative example 1 no graphene was added during the mixing process; the rest is basically the same as the embodiment 1.
Comparative example 2:
comparative example 2 differs from example 1 only in that: comparative example 2 no tea polyphenol derivative was added during the mixing process; the rest is basically the same as the embodiment 1.
Comparative example 3:
comparative example 3 differs from example 1 only in that: in comparative example 3, 20kg of white carbon black is used to replace 20kg of modified calcium sulfate whiskers; the rest is basically the same as the embodiment 1.
Example 2:
weighing 18.5kg of modified calcium sulfate whiskers, adding the modified calcium sulfate whiskers into 100kg of nitrile rubber, then continuously adding an acetic acid solution, and stirring while adding the acetic acid solution until the nitrile rubber is cured to obtain solid rubber; repeatedly washing the solid rubber by using water until the washed solution is neutral, and then drying the solid rubber; weighing 3.5kg of accelerator DM, dried solid rubber, 12kg of graphene, 6kg of tea polyphenol derivative, 6.5kg of zinc oxide, 3.5kg of stearic acid and 4.5kg of sulfur, placing the materials on an open type rubber mixing mill, and mixing for 5 minutes to obtain a rubber material, wherein the temperature of the open type rubber mixing mill is set to be 125 ℃; adding the rubber material into a screw extruder for extrusion molding to obtain a rubber sheet, and then coating the rubber sheet on the outer side of the roller core by using a rubber coating machine to form a rubber coating layer on the outer side of the roller core; and (3) conveying the roller core containing the rubber coating layer into a vulcanizing tank for vulcanization treatment to obtain the wear-resistant rice hulling rubber roller, wherein the pressure in the vulcanizing tank is set to be 0.5 MPa.
In example 2, one portion per 1 kg.
Example 3:
weighing 23kg of modified calcium sulfate whisker, adding the modified calcium sulfate whisker into 100kg of nitrile rubber, then continuously adding an acetic acid solution, and stirring while adding the acetic acid solution until the nitrile rubber is cured to obtain solid rubber; repeatedly washing the solid rubber by using water until the washed solution is neutral, and then drying the solid rubber; weighing 4.5kg of accelerator DM, dried solid rubber, 16kg of graphene, 9.5kg of tea polyphenol derivative, 7.5kg of zinc oxide, 4.5kg of stearic acid and 4.5kg of sulfur, placing the materials on an open type rubber mixing mill, and mixing for 5 minutes to obtain a rubber material, wherein the temperature of the open type rubber mixing mill is set to be 120 ℃; adding the rubber material into a screw extruder for extrusion molding to obtain a rubber sheet, and then coating the rubber sheet on the outer side of the roller core by using a rubber coating machine to form a rubber coating layer on the outer side of the roller core; and (3) conveying the roller core containing the rubber coating layer into a vulcanizing tank for vulcanization treatment to obtain the wear-resistant rice hulling rubber roller, wherein the pressure in the vulcanizing tank is set to be 0.6 MPa.
In example 3, one portion per 1 kg.
The performance test was carried out on the appropriate amount of the rubber compound prepared in example 1-example 3 and comparative example 1-comparative example 3:
stress strain: according to GB 528-; abrasion performance: according to GB/T1689-2014; shore A hardness: according to GB/T2411-2008; tear performance: according to GB/T529-2008; the results are shown in Table 1.
Table 1: results of Performance testing
Figure GDA0003290828320000071
As can be seen from Table 1, the rubber compound prepared by the preparation method of the invention has excellent mechanical properties and wear resistance.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (7)

1. The preparation method of the wear-resistant rice hulling rubber roll is characterized by comprising the following steps:
s1, weighing 100 parts of nitrile rubber, 15-25 parts of modified calcium sulfate whisker, 10-18 parts of graphene, 5-10 parts of tea polyphenol derivative, 3-5 parts of accelerator DM, 6-8 parts of zinc oxide, 3-5 parts of stearic acid and 3-5 parts of sulfur for later use; the tea polyphenol derivative is tea polyphenol-Zn2+A complex;
s2, adding the modified calcium sulfate whiskers into the nitrile rubber, then continuously adding an acetic acid solution, and stirring while adding the acetic acid solution until the nitrile rubber is solidified to obtain solid rubber;
s3, repeatedly washing the solid rubber by using water until the washed solution is neutral, and then drying the solid rubber;
s4, placing the accelerator DM, the dried solid rubber, the graphene, the tea polyphenol derivative, the zinc oxide, the stearic acid and the sulfur on an open type rubber mixing mill for mixing to obtain a rubber material;
s5, coating the rubber material on the outer side of the roller core by adopting an extrusion winding rubber coating method, and forming a rubber coating layer on the outer side of the roller core;
and S6, conveying the roller core containing the rubber coating layer into a vulcanizing tank for vulcanizing to obtain the wear-resistant rice hulling rubber roller.
2. The preparation method of the wear-resistant rice huller rubber roll according to claim 1, wherein in step S1, 100 parts of nitrile rubber, 20 parts of modified calcium sulfate whisker, 15 parts of graphene, 8 parts of tea polyphenol derivative, 4 parts of accelerator DM, 7 parts of zinc oxide, 4 parts of stearic acid and 4 parts of sulfur are weighed for later use.
3. The preparation method of the wear-resistant rice huller rubber roll as claimed in claim 1, wherein the tea polyphenol-Zn2+The preparation process of the complex comprises the following steps: adding distilled water into tea polyphenol, and performing ultrasonic oscillation to fully dissolve the tea polyphenol to obtain a tea polyphenol solution; adding zinc chloride solution into tea polyphenol solution, mixing thoroughly, adding sodium bicarbonate solution to adjust pH value to 7, reacting at room temperature for 2.5 hr, standing for 30 hr after reaction, centrifuging, washing, and drying to obtain tea polyphenol-Zn2+And (3) a complex.
4. The preparation method of the wear-resistant rice huller rubber roll according to claim 1, wherein the preparation method of the modified calcium sulfate whisker comprises the following steps: weighing water, absolute ethyl alcohol and a silane coupling agent, hydrolyzing for 2min at 55-70 ℃ to obtain a hydrolysate, uniformly spraying the hydrolysate on the surface of the calcium sulfate whisker, drying the calcium sulfate whisker at 30-50 ℃, and stirring for 6-15 min at 100-120 ℃ to obtain the modified calcium sulfate whisker.
5. The preparation method of the wear-resistant rice huller rubber roll as claimed in claim 1, wherein in step S2, the mass ratio of acetic acid to water in the acetic acid solution is 1: 3.
6. The preparation method of the wear-resistant rice hulling rubber roll according to claim 1, wherein in step S4, the temperature of the open rubber mixer is set to be 110-135 ℃, and the mixing time is 3-5 minutes.
7. The preparation method of the wear-resistant rice hulling rubber roll as claimed in claim 1, wherein in step S6, the pressure in the vulcanizing tank is set to 0.4 MPa-0.6 MPa.
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