CN110964230B - Fine kaolin processing method - Google Patents
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- CN110964230B CN110964230B CN201911319578.2A CN201911319578A CN110964230B CN 110964230 B CN110964230 B CN 110964230B CN 201911319578 A CN201911319578 A CN 201911319578A CN 110964230 B CN110964230 B CN 110964230B
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- coupling agent
- filter cake
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 title claims abstract description 117
- 239000005995 Aluminium silicate Substances 0.000 title claims abstract description 115
- 235000012211 aluminium silicate Nutrition 0.000 title claims abstract description 115
- 238000003672 processing method Methods 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 45
- 238000003756 stirring Methods 0.000 claims abstract description 41
- 239000007822 coupling agent Substances 0.000 claims abstract description 40
- 239000002131 composite material Substances 0.000 claims abstract description 29
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 29
- 239000012065 filter cake Substances 0.000 claims abstract description 24
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 229910052714 tellurium Inorganic materials 0.000 claims description 18
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims description 18
- -1 hydroxyl compound Chemical class 0.000 claims description 11
- 239000004927 clay Substances 0.000 claims description 10
- HHFAWKCIHAUFRX-UHFFFAOYSA-N ethoxide Chemical compound CC[O-] HHFAWKCIHAUFRX-UHFFFAOYSA-N 0.000 claims description 8
- 229920001971 elastomer Polymers 0.000 abstract description 55
- 239000005060 rubber Substances 0.000 abstract description 55
- 230000000694 effects Effects 0.000 abstract description 29
- 238000001354 calcination Methods 0.000 abstract description 18
- 230000003014 reinforcing effect Effects 0.000 abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 12
- 239000000377 silicon dioxide Substances 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052863 mullite Inorganic materials 0.000 abstract description 5
- 238000005054 agglomeration Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 9
- 230000032683 aging Effects 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000006229 carbon black Substances 0.000 description 3
- DEQZTKGFXNUBJL-UHFFFAOYSA-N n-(1,3-benzothiazol-2-ylsulfanyl)cyclohexanamine Chemical compound C1CCCCC1NSC1=NC2=CC=CC=C2S1 DEQZTKGFXNUBJL-UHFFFAOYSA-N 0.000 description 3
- 239000004636 vulcanized rubber Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 244000043261 Hevea brasiliensis Species 0.000 description 2
- 239000004594 Masterbatch (MB) Substances 0.000 description 2
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920003052 natural elastomer Polymers 0.000 description 2
- 229920001194 natural rubber Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229920002725 thermoplastic elastomer Polymers 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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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
-
- 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
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
-
- 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
- C08K3/346—Clay
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention relates to the technical field of kaolin, and provides a fine kaolin processing method aiming at the problem of poor effect of reinforcing rubber, wherein the technical scheme is as follows: the method comprises the following steps: s1, cleaning kaolin; s2, filtering, and keeping a filter cake; s3, drying the filter cake; s4, crushing the filter cake to prepare coarse powder; s5.400-600 ℃ for 20-30 min; s6, grinding into fine powder; and S7, adding a quaternary hydroxyl composite coupling agent and uniformly stirring to obtain fine kaolin. The kaolin is subjected to a partial mullite reaction by low-temperature calcination at the temperature of 400-600 ℃ for 20-30min, so that a silica tetrahedron is exposed, and the quaternary hydroxyl composite coupling agent and the silica tetrahedron are coupled and combined stably when the quaternary hydroxyl composite coupling agent is added and stirred uniformly, so that the kaolin is modified, and has good lipophilicity, high dispersity and difficult agglomeration of the kaolin in rubber, and the effect of reinforcing the rubber by the kaolin is good.
Description
Technical Field
The invention relates to the technical field of kaolin, in particular to a fine kaolin processing method.
Background
Kaolin is a non-metallic mineral, a clay and claystone based on clay minerals of the kaolinite group.
Kaolin has a wide range of applications, primarily in papermaking, ceramics and refractory materials, and secondarily in coatings, rubber fillers, enamel glaze and white cement raw materials.
When the kaolin is used in the rubber, the mechanical property of the rubber is favorably improved, but because the kaolin belongs to an inorganic material and the rubber belongs to an organic material, the compatibility of the kaolin and the rubber is poor, the dispersity of the kaolin in the rubber is low, the effect of reinforcing the rubber is poor, and therefore, the rubber has an improvement space.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a fine kaolin processing method which has the advantage of better rubber reinforcing effect.
In order to achieve the purpose, the invention provides the following technical scheme:
a fine kaolin processing method is characterized by comprising the following steps: the method comprises the following steps:
s1, cleaning kaolin;
s2, filtering, and keeping a filter cake;
s3, drying the filter cake;
s4, crushing the filter cake to prepare coarse powder;
s5.400-600 ℃ for 20-30 min;
s6, grinding into fine powder;
and S7, adding a quaternary hydroxyl composite coupling agent and uniformly stirring to obtain fine kaolin.
By adopting the technical scheme, the kaolin is subjected to a partial mullite reaction by low-temperature calcination at the temperature of 400-600 ℃ for 20-30min, so that a silica tetrahedron is exposed, and the quaternary hydroxyl composite coupling agent and the silica tetrahedron are coupled and combined stably when being added and uniformly stirred, so that the kaolin is modified and has good lipophilicity, the kaolin has high dispersion degree in rubber and is not easy to agglomerate, and the effect of reinforcing the rubber by the kaolin is good;
the filter cake is crushed to be made into coarse powder through the step S4 and then the coarse powder is calcined, so that the loss caused by flying of fine powder during calcination is reduced, and the pollution to the environment during transportation is effectively reduced.
The invention is further configured to: the coarse powder mesh number in the step S4 is 180-220 meshes.
By adopting the technical scheme, the coarse powder is not easy to fly by controlling the mesh number of the coarse powder to be 180-220 meshes, the environment is not easy to be polluted in the process of transporting the coarse powder to the calcining device for calcining, the coarse powder is not easy to fly in the calcining process, and the loss is reduced.
The invention is further configured to: the fine powder mesh number in the step S6 is 950-1050 meshes.
By adopting the technical scheme, the specific surface area of the fine powder is larger by controlling the mesh number of the fine powder to be 950-1050 meshes, the fine powder is easier to combine with the quaternary hydroxyl composite coupling agent, the dispersity of the fine powder filled into rubber is higher, and the effect of reinforcing the rubber is better.
The invention is further configured to: in the step S7, the added mass of the quaternary hydroxyl composite coupling agent is 0.1-0.2% of the mass of the kaolin.
By adopting the technical scheme, the method avoids wetting kaolin due to excessive consumption of the quaternary hydroxyl composite coupling agent and effectively controls the cost by controlling the addition of the quaternary hydroxyl composite coupling agent, and also avoids the condition of poor modification effect due to too little consumption of the quaternary hydroxyl composite coupling agent.
The invention is further configured to: and in the step S7, stirring for 2-3min at the rotating speed of the stirring device of 600r/min during stirring.
By adopting the technical scheme, the stirring effect is better through high-speed stirring, so that the quaternary hydroxyl compound coupling agent is uniformly distributed in the kaolin, the effect of the quaternary hydroxyl compound coupling agent on the modified kaolin is better, and the quality is uniform.
The invention is further configured to: in the step 3, the filter cake is placed under the condition of 120-130 ℃ for drying for 10-12 min.
Through adopting above-mentioned technical scheme, guarantee the effect that the filter cake was dried, guarantee that the filter cake is dry so that the breakage, reduce the filter cake and contain moisture and lead to softer and be difficult to the condition broken.
The invention is further configured to: in the step S7, after the quaternary hydroxyl compound coupling agent is added, tellurium ethoxide is added, and then the fine kaolin is obtained by uniformly stirring.
By adopting the technical scheme, the tellurium ethoxide is added into the kaolin, so that the tensile strength of the rubber is effectively improved after the kaolin is added into the rubber, and the effect of reinforcing the rubber by the kaolin is better.
The invention is further configured to: in the step S7, the mass of the tellurium ethoxide added is 0.03-0.05% of the mass of the kaolin.
By adopting the technical scheme, the tellurium ethoxide is matched with the kaolin in a specific proportion, so that the effect of reinforcing the rubber is better, and the effect of improving the tensile strength of the rubber is better.
In conclusion, the invention has the following beneficial effects:
1. the kaolin is subjected to a partial mullite reaction by low-temperature calcination at the temperature of 400-600 ℃ for 20-30min, so that a silica tetrahedron is exposed, and the quaternary hydroxyl composite coupling agent and the silica tetrahedron are coupled and combined stably when being added and uniformly stirred, so that the kaolin is modified, and has good lipophilicity, so that the kaolin has high dispersity in rubber and is not easy to agglomerate, and the effect of reinforcing the rubber by the kaolin is good;
2. by controlling the addition amount of the quaternary hydroxyl composite coupling agent, the kaolin is prevented from being wetted due to excessive consumption of the quaternary hydroxyl composite coupling agent, the cost is effectively controlled, and the condition that the modification effect is poor due to too little consumption of the quaternary hydroxyl composite coupling agent is avoided;
3. by adding ethanol tellurium into kaolin, the tensile strength of the rubber is effectively improved after the kaolin is added into the rubber, and the effect of reinforcing the rubber by the kaolin is better.
Drawings
FIG. 1 is a schematic flow diagram of a fine kaolin clay processing method of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
In the following examples, comparative examples and experimental examples:
washing kaolin with water sold by Longhua mineral products Limited in Zhangzhou city;
the quaternary hydroxyl compound coupling agent is sold by the Jintailin plastic industry Co., Ltd under the brand name JTL-T3 SE;
the ethanol tellurium is sold by Jinjinle industry Co Ltd in Shanghai;
the natural rubber adopts Vietnam 3L standard rubber sold by Shenzhen Xin Hengzhen rubber Limited company;
the carbon black is N330 carbon black sold by Xuzhou Henglong pigment Co., Ltd;
the sulfur adopts sulfur powder sold by Henan Hongyao chemical product limited company;
the accelerator CZ is a rubber accelerator CZ sold by Hebeichuan general chemical engineering Co.Ltd;
the accelerant D is an environment-friendly rubber and plastic accelerant D-80 sold by Xiamen Hongjin trade company Limited.
Example 1
A method of processing fine kaolin, referring to fig. 1, comprising the steps of:
s1, cleaning kaolin, mixing the kaolin and water according to the weight ratio of 1: 1, stirring at the rotating speed of 60r/min for 10min to form kaolin slurry;
s2, injecting the kaolin slurry into a filter press for filter pressing, discharging water, and keeping a filter cake;
s3, placing the filter cake in a drying furnace, and drying at 120 ℃ for 12 min;
s4, putting the dried filter cake into a grinding device (in the embodiment, the grinding device adopts a 4R Raymond mill), and grinding into coarse powder with the mesh number of 180 meshes;
s5, transporting the coarse powder to a tunnel furnace for low-temperature calcination, wherein the calcination temperature is 400 ℃, and the calcination time is 30 min;
s6, conveying the calcined coarse powder to a ring roller mill for grinding to obtain fine powder with the mesh number of 950 meshes;
and S7, adding the fine powder into a stirring kettle, adding the quaternary hydroxyl composite coupling agent into the stirring kettle, stirring at the rotating speed of 600r/min for 2min to obtain fine kaolin, wherein the mass of the quaternary hydroxyl composite coupling agent added into the stirring kettle is 0.1% of the mass of the kaolin in the stirring kettle.
Example 2
The difference from example 1 is that:
in step S3, the filter cake is placed in a drying oven and dried for 11min at 125 ℃;
in step S4, grinding the dried filter cake into coarse powder with 200 meshes;
in step S5, calcining the coarse powder at 500 ℃ for 25 min;
in step S6, grinding the calcined coarse powder to obtain fine powder with a mesh size of 1000 meshes;
in step S7, adding the fine powder into a stirring kettle, adding the quaternary hydroxyl composite coupling agent into the stirring kettle, stirring at a rotation speed of 600r/min for 2.5min to obtain fine kaolin, wherein the mass of the quaternary hydroxyl composite coupling agent added into the stirring kettle is 0.15% of the mass of the kaolin in the stirring kettle.
Example 3
The difference from example 1 is that:
in step S3, the filter cake is placed in a drying oven and dried for 10min at 130 ℃;
in step S4, grinding the dried filter cake into coarse powder with 220 meshes;
in step S5, calcining the coarse powder for 20min at 600 ℃;
in step S6, grinding the calcined coarse powder to obtain fine powder with 1050 meshes;
and step S7, adding the fine powder into a stirring kettle, adding the quaternary hydroxyl composite coupling agent into the stirring kettle, stirring at the rotating speed of 600r/min for 3min to obtain fine kaolin, wherein the mass of the quaternary hydroxyl composite coupling agent added into the stirring kettle is 0.2% of the mass of the kaolin in the stirring kettle.
Example 4
The difference from example 1 is that:
in step S3, the filter cake is placed in a drying oven and dried for 10min at 125 ℃;
in step S4, grinding the dried filter cake into coarse powder with 200 meshes;
in step S5, calcining the coarse powder at 550 ℃ for 20 min;
in step S6, grinding the calcined coarse powder to obtain fine powder with a mesh size of 1000 meshes;
and step S7, adding the fine powder into a stirring kettle, adding the quaternary hydroxyl composite coupling agent into the stirring kettle, stirring at the rotating speed of 600r/min for 2min to obtain fine kaolin, wherein the mass of the quaternary hydroxyl composite coupling agent added into the stirring kettle is 0.1% of the mass of the kaolin in the stirring kettle.
Example 5
The difference from example 4 is that:
in the step S7, after the quaternary hydroxyl compound coupling agent is added, ethanol tellurium is added, and the mass of the ethanol tellurium added into the stirring kettle is 0.03 percent of the mass of the kaolin in the stirring kettle.
Example 6
The difference from example 4 is that:
in the step S7, after the quaternary hydroxyl compound coupling agent is added, ethanol tellurium is added, and the mass of the ethanol tellurium added into the stirring kettle is 0.04% of the mass of the kaolin in the stirring kettle.
Example 7
The difference from example 4 is that:
in the step S7, after the quaternary hydroxyl compound coupling agent is added, ethanol tellurium is added, and the mass of the ethanol tellurium added into the stirring kettle is 0.05% of the mass of the kaolin in the stirring kettle.
Example 8
The difference from example 4 is that:
in the step S7, ethanol tellurium is added after the quaternary hydroxyl compound coupling agent is added, and the mass of ethanol tellurium added into the stirring kettle is 0.045% of the mass of kaolin in the stirring kettle.
Comparative example 1
The difference from example 4 is that:
in step S5, calcining the coarse powder at 800 ℃ for 20 min;
comparative example 2
The difference from example 4 is that:
in step S5, calcining the coarse powder at 200 ℃ for 20 min;
comparative example 3
The difference from example 4 is that:
in step S7, no quaternary hydroxyl compound coupling agent is added.
Comparative example 4
The difference from example 4 is that:
step S5 is cancelled;
in step S6, the coarse powder is ground to obtain fine powder of 1000 mesh.
Experimental example 1
A preparation method of the rubber comprises the following steps:
s01, adding 100kg of natural rubber into an open mill, performing thin pass for 6 times, and fully plasticating with the roller spacing of 0.5 mm; then putting the mixture into an internal mixer at the temperature of 110 ℃ and laminating for 4min again to obtain plasticated rubber;
s02, controlling the temperature to be 100 ℃ after the plasticated rubber is laminated, and laminating for 2 min; adding 60kg of carbon black and 15kg of kaolin, controlling the temperature to be 140 ℃, pressing for 3min, discharging rubber, conveying to an open mill, tabletting and radiating to obtain master batch;
s03, putting the master batch on an open mill, and pounding for 2min with a roller spacing of 3 mm; 2.5kg of sulfur, 1.2kg of accelerator CZ and 0.6kg of accelerator D0 are added, and the roller spacing is 3 mm; the thin-pass is carried out for three times, and the roller spacing is 1 mm; packaging six rear lower pieces by a triangular bag, wherein the roller spacing is 5 mm; roll temperature: the front roller is less than or equal to 60 ℃, and the rear roller is less than or equal to 60 ℃; vulcanization conditions are as follows: pressure 6kg/cm2The temperature was 150 ℃ and the vulcanization time was 30 minutes.
In this experimental example, the fine kaolin prepared in example 1 was used as the kaolin.
Experimental example 2
The difference from experimental example 1 is that:
the fine kaolin prepared in example 2 was used as the kaolin.
Experimental example 3
The difference from experimental example 1 is that:
the fine kaolin prepared in example 3 was used for the kaolin.
Experimental example 4
The difference from experimental example 1 is that:
the fine kaolin prepared in example 4 was used for the kaolin.
Experimental example 5
The difference from experimental example 1 is that:
the fine kaolin prepared in example 5 was used for the kaolin.
Experimental example 6
The difference from experimental example 1 is that:
the fine kaolin prepared in example 6 was used for the kaolin.
Experimental example 7
The difference from experimental example 1 is that:
the fine kaolin prepared in example 7 was used.
Experimental example 8
The difference from experimental example 1 is that:
the fine kaolin prepared in example 8 was used.
Experimental example 9
The difference from experimental example 1 is that:
the fine kaolin prepared in comparative example 1 was used as the kaolin.
Experimental example 10
The difference from experimental example 1 is that:
the fine kaolin prepared in comparative example 2 was used as the kaolin.
Experimental example 11
The difference from experimental example 1 is that:
the fine kaolin prepared in comparative example 3 was used as the kaolin.
Experimental example 12
The difference from experimental example 1 is that:
the fine kaolin prepared in comparative example 4 was used.
Experimental example 13
The difference from experimental example 1 is that:
the kaolin used was the ordinary kaolin used in example 1 without washing.
Experiment 1
The tensile strength, tear strength and elongation at break of the rubber samples prepared in the experimental examples were measured according to GB/T528-2009 determination of tensile stress strain properties of vulcanized rubber or thermoplastic rubber.
Experiment 2
According to GB/T531.1-2008 "method for Press hardness test of vulcanized rubber or thermoplastic rubber", part 1: the hardness (shore a) of the rubber sample prepared in each experimental example was measured by shore durometer (shore hardness).
Experiment 3
And (3) heating the rubber samples prepared in the experimental examples at 70 ℃ for 72 hours according to GB/T13939-2014 tubular instrument method for vulcanized rubber thermal-oxygen aging experimental method, and detecting the tensile strength change percentage, the tear strength change percentage, the elongation at break change percentage and the hardness change percentage of the samples.
The specific detection data are shown in tables 1 and 2
TABLE 1 Pre-aging test data
| Tensile strength | Tear strength | Elongation at break | Hardness (Shao's A) | |
| Experimental example 1 | 28.12MPa | 56.38MPa | 883％ | 59 |
| Experimental example 2 | 28.21MPa | 56.43MPa | 885％ | 59 |
| Experimental example 3 | 28.18MPa | 56.39MPa | 884％ | 59 |
| Experimental example 4 | 28.22MPa | 56.41MPa | 886％ | 59 |
| Experimental example 5 | 32.45MPa | 60.45MPa | 952％ | 59 |
| Experimental example 6 | 32.51MPa | 60.47MPa | 954％ | 59 |
| Experimental example 7 | 32.48MPa | 60.43MPa | 958％ | 59 |
| Experimental example 8 | 32.49MPa | 60.45MPa | 956％ | 59 |
| Experimental example 9 | 22.38MPa | 50.33MPa | 841％ | 61 |
| Experimental example 10 | 25.67MPa | 53.98MPa | 868％ | 59 |
| Experimental example 11 | 18.89MPa | 46.77MPa | 783％ | 58 |
| Experimental example 12 | 20.35MPa | 48.89MPa | 817％ | 58 |
| Experimental example 13 | 18.40MPa | 45.12MPa | 763％ | 56 |
TABLE 2 percent Change after aging
According to comparison of data of experimental examples 5-8 and experimental example 4 in table 1, the tensile strength, tear strength and elongation at break of the rubber sample are effectively improved by adding tellurium ethoxide into kaolin, and the hardness is not obviously affected, so that the effect of reinforcing the rubber by the kaolin is better.
According to the comparison of the data of the experimental example 9 and the experimental example 4 in the table 1, the kaolin is calcined at high temperature, the mullite reaction is not easy to occur, and the silicon-oxygen tetrahedron can not be exposed outside, so that the effect of combining with the quaternary hydroxyl composite coupling agent is poor, the dispersion of the kaolin in the rubber is poor, the tensile strength, the tearing strength and the elongation at break of the rubber sample are all reduced, the effect of reinforcing the rubber is reduced, and the hardness of the rubber sample is improved a little.
According to the comparison of the data of the experimental example 10 and the experimental example 4 in the table 1, when the kaolin calcination temperature is too low, the mullite reaction is less generated, and only a small amount of silicon-oxygen tetrahedron is exposed outside, so that the effect of combining with the quaternary hydroxyl composite coupling agent is general, the dispersity in the rubber is general, and the effect of reinforcing the rubber is better than that of high-temperature calcination but is poorer than that of proper calcination temperature.
According to the comparison of the data of the experimental example 11 and the data of the example 4 in the table 1, the quaternary hydroxyl composite coupling agent is not added in the kaolin, so that the kaolin has poor compatibility with rubber and poor reinforcing effect, and only plays a role of a filler.
According to the comparison of the data of the experimental example 12 and the experimental example 4 in the table 1, the kaolin has poor combination effect with the quaternary hydroxyl composite coupling agent without being calcined, so that the effect of reinforcing the rubber by the kaolin is poor.
Comparing the data of example 13 and example 4 in Table 1, the untreated kaolin clay is less effective in reinforcing rubber.
According to the comparison of the data of the experimental examples 5-8 and the experimental example 4 in the table 2, the effect of improving the thermal oxygen aging resistance of the rubber sample is improved by adding tellurium ethoxide into the kaolin.
According to the comparison of the data of the experimental example 9 and the experimental example 4 in the table 2, the effect of the kaolin calcined at high temperature for improving the thermal oxygen aging resistance of the rubber sample is reduced.
According to the comparison of the data of the experimental example 10 and the experimental example 4 in the table 2, when the kaolin calcination temperature is too low, the effect of improving the thermal oxygen aging resistance of the rubber sample is reduced.
According to comparison of data of the experimental example 11 and the example 4 in the table 2, the quaternary hydroxyl compound coupling agent is not added to the kaolin, so that the compatibility of the kaolin and the rubber is poor, and the effect of improving the thermal oxygen aging resistance of the rubber sample is poor.
According to the comparison of the data of the experimental example 12 and the experimental example 4 in the table 2, the kaolin has poor combination effect with the quaternary hydroxyl composite coupling agent without being calcined, and the effect of improving the thermal oxygen aging resistance of the rubber sample is poor.
Comparing the data in Table 2 between example 13 and example 4, it can be seen that the untreated kaolin clay has a poor effect of improving the thermal oxygen aging resistance of the rubber sample.
The embodiments of the present invention are preferred embodiments of the present invention, and the scope of the present invention is not limited by these embodiments, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.
Claims (7)
1. A fine kaolin processing method is characterized by comprising the following steps: the method comprises the following steps:
s1, cleaning kaolin;
s2, filtering, and keeping a filter cake;
s3, drying the filter cake;
s4, crushing the filter cake to prepare coarse powder;
s5.400-600 ℃ for 20-30 min;
s6, grinding into fine powder;
s7, adding a quaternary hydroxyl composite coupling agent and uniformly stirring to obtain fine kaolin;
in the step S7, the added mass of the quaternary hydroxyl composite coupling agent is 0.1-0.2% of the mass of the kaolin.
2. The fine kaolin clay processing method of claim 1, wherein: the coarse powder mesh number in the step S4 is 180-220 meshes.
3. The fine kaolin clay processing method of claim 1, wherein: the fine powder mesh number in the step S6 is 950-1050 meshes.
4. The fine kaolin clay processing method of claim 1, wherein: and in the step S7, stirring for 2-3min at the rotating speed of the stirring device of 600r/min during stirring.
5. The fine kaolin clay processing method of claim 1, wherein: in the step 3, the filter cake is placed under the condition of 120-130 ℃ for drying for 10-12 min.
6. The fine kaolin clay processing method as set forth in any one of claims 1-5, wherein: in the step S7, after the quaternary hydroxyl compound coupling agent is added, tellurium ethoxide is added, and then the fine kaolin is obtained by uniformly stirring.
7. The fine kaolin clay processing method of claim 6, wherein: in the step S7, the mass of the tellurium ethoxide added is 0.03-0.05% of the mass of the kaolin.
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Denomination of invention: Fine kaolin processing methods Effective date of registration: 20231117 Granted publication date: 20210713 Pledgee: Fujian Longhai Rural Commercial Bank Co.,Ltd. Pledgor: Zhangzhou Longhua mineral Co.,Ltd. Registration number: Y2023350000237 |
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