CN114133674A - Chlorosulfonated polyethylene rubber and preparation method thereof - Google Patents

Chlorosulfonated polyethylene rubber and preparation method thereof Download PDF

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CN114133674A
CN114133674A CN202111675151.3A CN202111675151A CN114133674A CN 114133674 A CN114133674 A CN 114133674A CN 202111675151 A CN202111675151 A CN 202111675151A CN 114133674 A CN114133674 A CN 114133674A
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rubber
chlorosulfonated polyethylene
parts
agent
dispersant
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CN114133674B (en
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裴友伟
何延钟
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Xiamen Fuste Rubber & Plastic Co ltd
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Xiamen Fuste Rubber & Plastic Co ltd
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K9/06Ingredients treated with organic substances with silicon-containing compounds
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    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
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    • C08K2003/2241Titanium dioxide
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
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Abstract

The application relates to the field of rubber, and particularly discloses chlorosulfonated polyethylene rubber and a preparation method thereof. The rubber comprises the following raw materials in parts by weight: 40-50 parts of chlorosulfonated polyethylene, 0.32-0.4 part of flow agent, 8-8.4 parts of diisononyl phthalate, 35-45 parts of reinforcing filler, 0.4-0.5 part of vulcanizing agent, 0.7-0.74 part of accelerator, 0.3-0.33 part of flow additive and 1.2-1.8 parts of dispersing agent. The chlorosulfonated polyethylene rubber has the advantages of high integral uniformity, strong mechanical property, smooth surface and high attractiveness.

Description

Chlorosulfonated polyethylene rubber and preparation method thereof
Technical Field
The application relates to the field of rubber, in particular to chlorosulfonated polyethylene rubber and a preparation method thereof.
Background
Chlorosulfonated polyethylene (CSM) is prepared from low-density polyethylene or high-density polyethylene through chlorination or chlorosulfonation reaction, and contains chlorine-containing special elastomer material with high saturated chemical structure. The molecular structure of the rubber material contains a chlorosulfonyl active group, so that the rubber material has high activity, excellent chemical medium corrosion resistance, ozone oxidation resistance, oil corrosion resistance and flame retardance, and simultaneously has the advantages of weather resistance, heat resistance, ion radiation resistance, low temperature resistance, abrasion resistance and electrical insulation, belongs to a special rubber variety with high performance and quality, and is widely applied to the fields of wires and cables, waterproof coiled materials, automobile industry and the like.
In order to further improve the processing properties of chlorosulfonated polyethylene rubber, reinforcing fillers are often added during its processing. However, the currently adopted reinforcing filler is usually inorganic powder, and the powder and the rubber matrix have large surface energy difference, so that the compatibility between the powder and the rubber matrix is poor, the powder and the rubber matrix are not easy to disperse in a rubber material and easy to agglomerate, the uniformity of the whole rubber material is poor, the mechanical property of the rubber is reduced, and the prepared rubber has a rough and unsmooth surface.
Disclosure of Invention
In order to solve the above problems, the present application provides a chlorosulfonated polyethylene rubber and a method for preparing the same.
In a first aspect, the chlorosulfonated polyethylene rubber provided by the application adopts the following technical scheme:
the chlorosulfonated polyethylene rubber comprises the following raw materials in parts by weight:
40-50 parts of chlorosulfonated polyethylene;
0.32-0.4 part of a flow agent;
8-8.4 parts of diisononyl phthalate;
35-45 parts of reinforcing filler;
0.4-0.5 part of vulcanizing agent;
0.7-0.74 parts of accelerator;
0.3-0.33 part of flow assistant;
1.2-1.8 parts of a dispersing agent.
By adopting the technical scheme, the flowing agent WB222 is adopted as the flowing agent, and one of the flowing agent ST and the flowing agent AC is adopted as the flowing agent, or the flowing agent ST and the flowing agent AC are mixed and used in any proportion. According to the rubber material mixing process, the flowing agent WB222, the flowing additive ST and the flowing additive AC are added into the rubber material, the flowability of the rubber material during mixing is fully improved, components such as reinforcing filler can be fully dispersed in the rubber material, all components in the rubber material are mixed more uniformly, the overall uniformity of the rubber is improved, the possibility of uneven stress of the rubber due to uneven distribution of the components such as the reinforcing filler is reduced, the mechanical property of the rubber is improved, and the prepared rubber surface is more smooth and flat.
Meanwhile, the application also adopts the matching use of the dispersing agent, the flow agent WB222, the flow additive ST and the flow additive AC, so that the acting force among reinforcing filler particles is reduced, and the compatibility between the reinforcing filler and other components is improved, thereby fully improving the dispersion degree of the reinforcing filler in the rubber material during mixing, enabling all the components in the rubber material to be mixed more uniformly, improving the integral uniformity degree of the rubber, and improving the mechanical property of the rubber.
In addition, the diisononyl phthalate is used as a plasticizer, so that the plasticity and the strength of the rubber are improved, and the mechanical property of the rubber is improved. The vulcanizing agent of the application adopts vulcanizing agent MC-2.
To sum up, the mechanical property of the rubber is fully improved by adding the diisononyl phthalate and the reinforcing filler into the rubber material, and the dispersibility of the components such as the reinforcing filler in the rubber material is fully improved by adopting the matching of the flow agent WB222, the flow agent ST, the flow agent AC and the dispersing agent, so that all the components in the rubber material are mixed more uniformly, the integral uniformity degree of the rubber is improved, the mechanical property of the rubber is improved, and the surface of the prepared rubber is more smooth.
Preferably, the raw materials comprise the following components in parts by weight:
45 parts of chlorosulfonated polyethylene;
0.36 part of a flow agent;
8.2 parts of diisononyl phthalate;
40 parts of reinforcing filler;
0.45 part of a vulcanizing agent;
0.72 part of an accelerator;
0.315 parts of a flow aid;
1.5 parts of a dispersing agent.
By adopting the technical scheme, the application further controls the use amount of each component, so that the overall fluidity of the rubber material is further improved, all the components in the rubber material are more uniformly mixed, the overall uniformity of the rubber is further improved, and the mechanical property of the rubber is enhanced.
Preferably, the dispersant comprises a dispersant H60EF, a dispersant KT-8A, a dispersant L-12 and a dispersant FL-100 in a weight ratio of 1 (0.8-1.2) to (0.04-0.06) to (0.02-0.04).
By adopting the technical scheme, the dispersing agent H60EF, the dispersing agent KT-8A, the dispersing agent L-12 and the dispersing agent FL-100 are mixed, matched and used, the synergistic effect between the dispersing agent and the dispersing agent is fully exerted, the viscosity of rubber is reduced, the overall fluidity and lubricity of the rubber are improved, the components such as the reinforcing filler are fully infiltrated, the interfacial tension between the reinforcing filler and the chlorosulfonated polyethylene is reduced, the reinforcing filler is more easily dispersed into the rubber, meanwhile, the interaction force between particles of the reinforcing filler is also reduced, the possibility of agglomeration of the reinforcing filler is reduced, the mixing uniformity of the components in the rubber is improved, and the mechanical property of the rubber is improved.
Preferably, the reinforcing filler comprises carbon black, PW-80A, titanium dioxide and light calcium carbonate powder in a weight ratio of (0.35-2.85) (9.95-12.45) (3.75-6.25) (20.95-23.45).
By adopting the technical scheme, the carbon black, the PW-80A, the titanium dioxide and the light calcium carbonate powder are mixed as the reinforcing filler and added into the rubber material, so that the technological property of the rubber can be improved, and various properties such as mechanical property, heat resistance, weather resistance, color brightness, chemical stability and the like of the rubber are improved.
Preferably, the carbon black is modified by the following method:
mixing and stirring the carbon black, the water, the ethanol and the coupling agent in a weight ratio of 1 (4-5) to (15-17) to (18-20) for 1.5-2.0h at the temperature of 60-65 ℃ and the rotation speed of 250-300r/min, then filtering, washing, and drying at the temperature of 100-105 ℃ for 4-5h to obtain the modified carbon black.
By adopting the technical scheme, the carbon black is modified by the coupling agent under the process conditions, so that the surface energy difference between the components such as the carbon black and the chlorosulfonated polyethylene is reduced, and the compatibility of the components such as the carbon black and the chlorosulfonated polyethylene is improved, so that the dispersing capacity of the carbon black in the rubber material is enhanced, the possibility of agglomeration of the carbon black in the rubber material is reduced, the uniformity of the rubber is improved, and the mechanical property of the rubber is enhanced.
Preferably, the coupling agent is one or more of a silane coupling agent KH-570, a silane coupling agent Si-69 and a titanate coupling agent 201.
By adopting the technical scheme, any one of the silane coupling agent KH-570, the silane coupling agent Si-69 and the titanate coupling agent 201 is adopted or mixed according to any proportion for use, so that the compatibility between the carbon black and other components is improved, and the dispersibility and uniformity of the carbon black in the sizing material are improved.
Preferably, the accelerator comprises the accelerator TETD and the accelerator TT in a weight ratio of (0.44-0.46) to (0.26-0.28).
By adopting the technical scheme, the accelerator TETD and the accelerator TT are added into the rubber material, so that the vulcanization time of the rubber material can be shortened, the vulcanization temperature is reduced, the dosage of a vulcanizing agent is reduced, and the mechanical property of the rubber is improved.
In a second aspect, the present application provides a method for preparing a chlorosulfonated polyethylene rubber, comprising the steps of:
s1, firstly, banburying chlorosulfonated polyethylene at the temperature of 120-;
s2, controlling the temperature below 70 ℃, mixing and banburying a vulcanizing agent, an accelerator, a flow assistant and master batch until the temperature reaches 80-90 ℃, discharging to obtain a rubber material, and thinly passing the rubber material for 3-4 times to obtain strips, thereby obtaining the rubber.
By adopting the technical scheme, the fluidity of the rubber material is improved by controlling the temperature of the flowing agent during addition and the initial temperature of the vulcanizing agent, the accelerator and other components during mixing, so that the components are mixed uniformly more easily, and the uniformity of the whole rubber is improved. And the rubber material is passed through the rubber material in a thin mode for many times, so that the integral uniformity of the rubber is further improved, and the surface of the prepared rubber is smoother and smoother.
Preferably, in the step S2, the size needs to be put into an open mill during the thin passing process, and the roll gap of the open mill is controlled to be 0.03-0.05 mm.
Through adopting above-mentioned technical scheme, the distance between this application further control roll spacing can further improve the holistic homogeneity of rubber in specific thinness within range for it is more level and smooth to make the rubber surface.
Preferably, in step S2, the roll gap scale of the open mill during the strip discharging is 0 scale.
Through adopting above-mentioned technical scheme, the scale on this application will the mill is adjusted to 0 scale to extrude the strip with sizing material under this scale, obtain the higher rubber of homogeneity.
In summary, the present application includes at least one of the following beneficial technical effects:
1. the rubber has high fluidity, high dispersibility of components such as reinforcing filler and the like, high integral uniformity and high mechanical property;
2. the rubber surface of the rubber is low in roughness, smooth and flat, and high in attractiveness;
3. the preparation method of the rubber is simple in steps, easy to operate and suitable for large-scale industrial production.
Drawings
FIG. 1 is a photograph of a rubber prepared according to comparative example 1 of the present application without a dispersant added;
FIG. 2 is a photograph of a rubber to which a dispersant was added, prepared according to example 3 of the present application.
Detailed Description
The present application will be described in further detail with reference to examples.
<Sources of materials>
Chlorosulfonated polyethylene, available from Shandong Leon New Material science and technology, Inc., model TS 530;
fluidizer WB222, available from Guangzhou, Mass rubber raw materials trade, Inc.;
diisononyl phthalate, available from Shandong Chengyu chemical Co., Ltd;
flow aid ST, available from Guangzhou City Tuiyuan chemical Co., Ltd;
the flow assistant AC is purchased from Hebei Zhuoyangxiang chemical technology Co., Ltd;
vulcanizing agent MC-2, purchased from chemical Limited of Jinan Haiyuan;
dispersant H60EF, available from Shandong Yanggu Huatai chemical Co., Ltd;
dispersant KT-8A, available from Syzygy chemical Co., Ltd, Guangzhou;
dispersant L-12, available from Hippocampus Atman chemical Co., Ltd;
dispersant FL-100, available from Korea, Inc., Shanghai;
carbon black, available from Guangzhou Penssen New Material science and technology, Inc., model N660;
PW-80A, available from diligent Utility Co, Shanghai;
titanium dioxide, purchased from south yang constant flight chemical ltd;
light calcium powder purchased from mineral processing factories of Lingshou county;
silane coupling agent KH-570, available from Zhongjie New materials, Inc., Guangzhou;
silane coupling agent Si-69, available from Guangzhou Ci Lianben rubber raw materials trade company;
titanate coupling agent 201, available from jinan rong guang chemical ltd;
accelerator TETD, available from guangzhou municipality rubber raw materials trade company;
accelerator TT, available from Guangzhou City local rubber raw materials trade company.
<Examples>
Example 1
A preparation method of chlorosulfonated polyethylene rubber comprises the following steps:
s1, firstly, putting 40kg of chlorosulfonated polyethylene into an internal mixer, internally mixing for 170s at the temperature of 120 ℃, then adding 8kg of diisononyl phthalate, 45kg of reinforcing filler (2.85 kg of carbon black, 12.45kg of PW-80A, 6.25kg of titanium dioxide and 23.45kg of light calcium powder) and 1.8kg of dispersing agent H60EF for continuous internal mixing, adding 0.4kg of flowing agent WB222 for continuous internal mixing when the temperature is 90 ℃, and discharging to obtain master batch when the temperature is 120 ℃;
s2, firstly cooling the internal mixer, controlling the temperature of the internal mixer to be below 70 ℃, putting 0.4kg of vulcanizing agent MC-2, 0.74kg of accelerant (0.46 kg of accelerant TETD and 0.28kg of accelerant TT), 0.3kg of flow assistant ST and master batch into the internal mixer, mixing and internally mixing until the temperature reaches 80 ℃, discharging to obtain a sizing material, then adjusting the roll distance between two rolls of the open mill to be below 0.5mm, passing the sizing material between the two rolls for 3 times, then adjusting the roll distance scale of the open mill to be 0 scale, and discharging to obtain the rubber.
Example 2
A preparation method of chlorosulfonated polyethylene rubber comprises the following steps:
s1, firstly putting 50kg of chlorosulfonated polyethylene into an internal mixer, internally mixing for 190s at the temperature of 130 ℃, then adding 8.4kg of diisononyl phthalate, 35kg of reinforcing filler (0.35 kg of carbon black, 9.95kg of PW-80A, 3.75kg of titanium dioxide and 20.95kg of light calcium powder) and 1.2kg of dispersing agent L-12 for continuous internal mixing, adding 0.32kg of flowing agent WB222 for continuous internal mixing when the temperature is 100 ℃, and discharging to obtain masterbatch when the temperature is 130 ℃;
s2, firstly cooling the internal mixer, controlling the temperature of the internal mixer below 70 ℃, putting 0.5kg of vulcanizing agent MC-2, 0.7kg of accelerant (0.44 kg of accelerant TETD and 0.26kg of accelerant TT), 0.33kg of flow aid (0.2 kg of flow aid ST and 0.13kg of flow aid AC) and master batch into the internal mixer, mixing and internally mixing until the temperature reaches 90 ℃, discharging to obtain a sizing material, then adjusting the roll distance between two rolls of the open mill to be less than 0.5mm, thinly passing the sizing material between the two rolls for 4 times, then adjusting the roll distance scale of the open mill to 0 scale, and discharging to obtain the rubber.
Example 3
A preparation method of chlorosulfonated polyethylene rubber comprises the following steps:
s1, firstly putting 45kg of chlorosulfonated polyethylene into an internal mixer, internally mixing for 180s at the temperature of 125 ℃, then adding 8.2kg of diisononyl phthalate, 40kg of reinforcing filler (1.6 kg of carbon black, 11.2kg of PW-80A, 5kg of titanium dioxide and 22.2kg of light calcium powder) and 1.5kg of dispersant KT-8A for continuous internal mixing, adding 0.36kg of flowing agent WB222 for continuous internal mixing when the temperature is 95 ℃, and discharging to obtain master batch when the temperature is 125 ℃;
s2, firstly cooling the internal mixer, controlling the temperature of the internal mixer to be below 70 ℃, putting 0.45kg of vulcanizing agent MC-2, 0.72kg of accelerant (0.45 kg of accelerant TETD and 0.27kg of accelerant TT), 0.315kg of flow assistant AC and master batch into the internal mixer, mixing and internally mixing until the temperature reaches 85 ℃, discharging to obtain a sizing material, then adjusting the roll distance between two rolls of the open mill to be below 0.5mm, passing the sizing material between the two rolls for 4 times, then adjusting the roll distance scale of the open mill to be 0 scale, and discharging to obtain the rubber.
Example 4
The preparation method of the chlorosulfonated polyethylene rubber is different from that of the example 3 in that: 42kg of chlorosulfonated polyethylene, 8.1kg of diisononyl phthalate, 38kg of reinforcing filler (1.52 kg of carbon black, 10.64kg of PW-80A, 4.75kg of titanium dioxide and 21.09kg of light calcium powder), 1.3kg of dispersant KT-8A, 0.34kg of flow agent WB222, 0.42kg of vulcanizing agent MC-2, 0.71kg of accelerator (0.444 kg of accelerator TETD and 0.266kg of accelerator TT) and 0.31kg of flow aid AC.
Example 5
The preparation method of the chlorosulfonated polyethylene rubber is different from that of the example 3 in that: 48kg of chlorosulfonated polyethylene, 8.3kg of diisononyl phthalate, 42kg of reinforcing filler (1.68 kg of carbon black, 11.76kg of PW-80A, 5.25kg of titanium dioxide and 23.31kg of light calcium powder), 1.7kg of dispersant KT-8A, 0.38kg of flow agent WB222, 0.47kg of vulcanizing agent MC-2, 0.73kg of accelerator (0.456 kg of accelerator TETD and 0.274kg of accelerator TT) and 0.32kg of flow aid AC.
Example 6
The preparation method of the chlorosulfonated polyethylene rubber is different from that of the example 3 in that: the dispersing agent comprises a dispersing agent H60EF, a dispersing agent KT-8A, a dispersing agent L-12 and a dispersing agent FL-100 in a weight ratio of 1:0.8:0.04: 0.02; wherein 0.8kg of dispersant H60EF, 0.65kg of dispersant KT-8A, 0.03kg of dispersant L-12 and 0.02kg of dispersant FL-100.
Example 7
The preparation method of the chlorosulfonated polyethylene rubber is different from that of the example 3 in that: the dispersing agent comprises a dispersing agent H60EF, a dispersing agent KT-8A, a dispersing agent L-12 and a dispersing agent FL-100 in a weight ratio of 1:1.2:0.06: 0.04; wherein 0.65kg of dispersant H60EF, 0.78kg of dispersant KT-8A, 0.04kg of dispersant L-12 and 0.03kg of dispersant FL-100.
Example 8
The preparation method of the chlorosulfonated polyethylene rubber is different from that of the example 3 in that: the dispersant comprises dispersant H60EF, dispersant KT-8A, dispersant L-12 and dispersant FL-100 in a weight ratio of 1:0.46:0.03: 0.01; wherein 1kg of dispersant H60EF, 0.46kg of dispersant KT-8A, 0.03kg of dispersant L-12 and 0.01kg of dispersant FL-100.
Example 9
The preparation method of the chlorosulfonated polyethylene rubber is different from that of the example 3 in that: the dispersant comprises dispersant H60EF, dispersant KT-8A, dispersant L-12 and dispersant FL-100 in a weight ratio of 1:1.5:0.25: 0.25; wherein 0.5kg of dispersant H60EF, 0.75kg of dispersant KT-8A, 0.125kg of dispersant L-12 and 0.125kg of dispersant FL-100.
Example 10
The preparation method of the chlorosulfonated polyethylene rubber is different from that of the example 3 in that: the carbon black was modified by the following method:
under the conditions that the temperature is 60 ℃ and the rotating speed is 250r/min, 1.6kg of carbon black, 6.4kg of water, 24kg of ethanol and 28.8kg of silane coupling agent KH-570 are mixed and stirred for 1.5h, then the mixture is filtered, washed and dried for 4h at the temperature of 100 ℃ to obtain the modified carbon black.
Example 11
The preparation method of the chlorosulfonated polyethylene rubber is different from that of the example 3 in that: the carbon black was modified by the following method:
under the conditions that the temperature is 65 ℃ and the rotating speed is 300r/min, 1.6kg of carbon black, 8kg of water, 27.2kg of ethanol and 32kg of silane coupling agent Si-69 are mixed and stirred for 2 hours, then the mixture is filtered, washed and dried for 5 hours at the temperature of 105 ℃ to obtain the modified carbon black.
Example 12
The preparation method of the chlorosulfonated polyethylene rubber is different from that of the example 3 in that: the carbon black was modified by the following method:
under the conditions that the temperature is 62.5 ℃ and the rotating speed is 275r/min, 1.6kg of carbon black, 7.2kg of water, 25.6kg of ethanol and 30.4kg of titanate coupling agent 201 are mixed and stirred for 1.75h, then the mixture is filtered, washed and dried for 4.5h at the temperature of 102.5 ℃ to obtain the modified carbon black.
Example 13
The preparation method of the chlorosulfonated polyethylene rubber is different from that of the example 3 in that: the carbon black was modified by the following method:
under the conditions that the temperature is 63 ℃ and the rotating speed is 280r/min, 1.6kg of carbon black, 7.68kg of water, 26.4kg of ethanol and 31.2kg of coupling agent (8 kg of silane coupling agent KH-570, 10kg of silane coupling agent Si-69 and 13.2kg of titanate coupling agent 201) are mixed and stirred for 1.6h, then the mixture is filtered, washed and dried for 4.7h at the temperature of 104 ℃ to obtain the modified carbon black.
Example 14
The preparation method of the chlorosulfonated polyethylene rubber is different from that of the example 3 in that: in step S2, the roll gap between the rolls of the open mill was adjusted to 0.03 mm.
Example 15
The preparation method of the chlorosulfonated polyethylene rubber is different from that of the example 3 in that: in step S2, the roll gap between the rolls of the open mill was adjusted to 0.05 mm.
<Comparative example>
Comparative example 1
The difference from example 3 is that: in step S1, no dispersant was added to the internal mixer, and the rest was the same.
Comparative example 2
The difference from example 3 is that: 30kg of chlorosulfonated polyethylene, 6kg of diisononyl phthalate, 50kg of reinforcing filler (2 kg of carbon black, 14kg of PW-80A, 6.25kg of titanium dioxide and 27.75kg of light calcium powder), 2kg of dispersant KT-8A, 1kg of flow agent WB222, 0.2kg of vulcanizing agent MC-2, 1.44kg of accelerator (0.9 kg of accelerator TETD and 0.54kg of accelerator TT) and 0.2kg of flow aid AC, and the rest are the same.
Comparative example 3
The difference from example 3 is that: 60kg of chlorosulfonated polyethylene, 10kg of diisononyl phthalate, 30kg of reinforcing filler (1.2 kg of carbon black, 8.4kg of PW-80A, 3.75kg of titanium dioxide and 16.65kg of light calcium powder), 1kg of dispersant KT-8A, 0.2kg of flow agent WB222, 1kg of vulcanizing agent MC-2, 0.576kg of accelerator (0.36 kg of accelerator TETD and 0.216kg of accelerator TT) and 0.5kg of flow aid AC, and the balance being the same.
Comparative example 4
The difference from example 3 is that: in step S1, the temperature at which the fluidizing agent WB-222 is added is 110 ℃ and the rest is the same.
Comparative example 5
The difference from example 3 is that: in step S2, the internal mixer is cooled to 80 ℃ and the rest is the same.
<Performance detection>
1. The tensile strength and elongation at break of the rubbers prepared in examples 1-15 and comparative examples 1-5 were tested with reference to GB/T528-2009 determination of tensile stress strain Properties of vulcanized rubber or thermoplastic rubber, the test results are shown in Table 1;
2. the rubber obtained in examples 1 to 15 and comparative examples 1 to 5 was measured for tear strength by using a square test specimen with reference to GB/T529-.
Table 1 table of performance test results
Item Tensile Strength (MPa) Elongation at Break (%) Tear Strength (kN/m)
Example 1 25.20 734.22 64.50
Example 2 25.08 733.15 63.87
Example 3 27.56 785.96 69.11
Example 4 25.48 741.15 65.27
Example 5 26.35 752.33 66.35
Example 6 29.11 801.27 75.08
Example 7 30.75 805.66 76.97
Example 8 28.88 791.73 73.28
Example 9 28.19 789.15 72.65
Example 10 28.05 788.44 71.48
Example 11 28.73 789.76 73.06
Example 12 28.55 789.23 72.98
Example 13 29.01 795.41 74.37
Example 14 27.87 786.19 70.46
Example 15 27.93 786.88 70.53
Comparative example 1 19.11 578.24 48.22
Comparative example 2 21.35 608.45 55.14
Comparative example 3 22.08 622.34 54.97
Comparative example 4 22.69 635.17 56.49
Comparative example 5 23.01 641.88 57.01
As can be seen from Table 1, the tensile strength of the rubber prepared in examples 1-3 of the present application is 25.08-27.56MPa, the elongation at break is 733.15-785.96%, and the tear strength is 63.87-69.11kN/m, which indicates that the rubber prepared in the present application has a better uniformity degree and stronger mechanical properties such as tensile strength, elongation at break, tear strength and the like.
The tensile strength, elongation at break and tear strength of the rubbers prepared in examples 4-5 are all lower than those of example 3, which shows that the mixing of the components can be more uniform by further controlling the use amount of the components, and the uniformity of the rubber is further improved, so that the mechanical property of the rubber is improved.
The tensile strength, the elongation at break and the tear strength of the rubbers prepared in the examples 6 to 7 are all higher than those of the rubber prepared in the example 3, which shows that the dispersant H60EF, the dispersant KT-8A, the dispersant L-12 and the dispersant FL-100 are jointly used, so that the synergistic effect among the dispersants can be exerted, the components such as reinforcing filler are fully dispersed, the uniformity of the rubber is improved, and the mechanical property of the rubber is improved.
The tensile strength, the elongation at break and the tear strength of the rubbers prepared in the examples 8-9 are all higher than those of the rubber prepared in the example 3, but the tensile strength, the elongation at break and the tear strength of the rubbers prepared in the examples 8-9 are all lower than those of the rubbers prepared in the examples 6-7, which shows that the synergistic effect among the four can be fully played by further controlling the weight ratio of the dispersing agent H60EF, the dispersing agent KT-8A, the dispersing agent L-12 and the dispersing agent FL-100, and the dispersion degree of each component in the rubber material is further improved, so that the uniformity of the rubber is improved, and the mechanical property of the rubber is enhanced.
The tensile strength, the elongation at break and the tear strength of the rubbers prepared in the examples 10 to 13 are all higher than those of the rubber prepared in the example 3, which shows that the carbon black is modified by the application, so that the dispersibility of the carbon black in a rubber material is improved, the uniformity of the rubber is improved, and the mechanical property of the rubber is enhanced.
The tensile strength, elongation at break and tear strength of the rubbers prepared in examples 14-15 are all higher than those of example 3, which shows that the application further controls the roller spacing of the open mill during thin passing, further improves the uniformity of the whole rubber and enables the rubber surface to be smoother and smoother.
The tensile strength, the elongation at break and the tear strength of the rubber prepared in the comparative example 1 are all smaller than those of the rubber prepared in the example 3, and the application can also be seen by combining the figure 1 and the figure 2, the dispersing agent is added into the rubber material, and can be matched with the flow agent and the flow auxiliary agent, so that the dispersibility of each component in the rubber material is improved, the integral uniformity degree of the rubber is improved, the mechanical property of the rubber is improved, and the surface of the prepared rubber is flat and smooth.
The tensile strength, elongation at break and tear strength of the rubbers obtained in comparative examples 2 to 3 were all lower than those of example 3, which shows that if the amounts of the respective components in the rubbers were not within the ranges of the present application, the uniformity of the rubber as a whole would be reduced, thereby reducing the mechanical properties of the rubbers.
The tensile strength, elongation at break and tear strength of the rubbers prepared in comparative examples 4 to 5 are all lower than those of example 3, which shows that if the temperature at which the flow agent is added and the initial temperature at which the vulcanizing agent, the accelerator and other components are mixed are too high, the fluidity of the rubber compound is reduced, so that the uniformity of the whole rubber is reduced, and the mechanical properties of the rubber are further reduced.
The embodiments of the present invention are preferred embodiments of the present application, and the scope of protection of the present application is not limited by the embodiments, so: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.

Claims (10)

1. The chlorosulfonated polyethylene rubber is characterized by comprising the following raw materials in parts by weight:
40-50 parts of chlorosulfonated polyethylene;
0.32-0.4 part of a flow agent;
8-8.4 parts of diisononyl phthalate;
35-45 parts of reinforcing filler;
0.4-0.5 part of vulcanizing agent;
0.7-0.74 parts of accelerator;
0.3-0.33 part of flow assistant;
1.2-1.8 parts of a dispersing agent.
2. The chlorosulfonated polyethylene rubber according to claim 1, wherein the raw materials comprise the following components in parts by weight:
45 parts of chlorosulfonated polyethylene;
0.36 part of a flow agent;
8.2 parts of diisononyl phthalate;
40 parts of reinforcing filler;
0.45 part of a vulcanizing agent;
0.72 part of an accelerator;
0.315 parts of a flow aid;
1.5 parts of a dispersing agent.
3. The chlorosulfonated polyethylene rubber according to claim 1 or 2, wherein the dispersant comprises dispersant H60EF, dispersant KT-8A, dispersant L-12 and dispersant FL-100 in a weight ratio of 1 (0.8-1.2) to (0.04-0.06) to (0.02-0.04).
4. The chlorosulfonated polyethylene rubber according to claim 1 or 2, wherein the reinforcing filler comprises carbon black, PW-80A, titanium dioxide and calcium carbonate powder in a weight ratio of (0.35-2.85) (9.95-12.45) (3.75-6.25) (20.95-23.45).
5. The chlorosulfonated polyethylene rubber according to claim 4, wherein the carbon black is modified by the following method:
mixing and stirring the carbon black, the water, the ethanol and the coupling agent in a weight ratio of 1 (4-5) to (15-17) to (18-20) for 1.5-2.0h at the temperature of 60-65 ℃ and the rotation speed of 250-300r/min, then filtering, washing, and drying at the temperature of 100-105 ℃ for 4-5h to obtain the modified carbon black.
6. The chlorosulfonated polyethylene rubber according to claim 5, wherein the coupling agent is one or more of a silane coupling agent KH-570, a silane coupling agent Si-69 and a titanate coupling agent 201.
7. The chlorosulfonated polyethylene rubber according to claim 1 or 2, wherein the accelerator comprises an accelerator TETD and an accelerator TT in a weight ratio of (0.44-0.46) to (0.26-0.28).
8. A method for preparing chlorosulfonated polyethylene rubber according to any one of claims 1 to 7, which comprises the steps of:
s1, firstly, banburying chlorosulfonated polyethylene at the temperature of 120-;
s2, controlling the temperature below 70 ℃, mixing and banburying a vulcanizing agent, an accelerator, a flow assistant and master batch until the temperature reaches 80-90 ℃, discharging to obtain a rubber material, and thinly passing the rubber material for 3-4 times to obtain strips, thereby obtaining the rubber.
9. The method as claimed in claim 8, wherein the step S2, the thin pass process is to put the rubber compound into the open mill, and the roll gap of the open mill is controlled to 0.03-0.05 mm.
10. The method as claimed in claim 9, wherein in step S2, the roll gap scale of the open mill is 0 scale when discharging.
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Publication number Priority date Publication date Assignee Title
CN1182109A (en) * 1996-11-13 1998-05-20 于继勇 Curing agent modified chlorosulphonated polythene paint and its preparation
US20020084439A1 (en) * 2000-12-28 2002-07-04 Xerox Corporation Extrudable magnet compound with improved flow properties
CN103819827A (en) * 2014-03-11 2014-05-28 浙江久运车辆部件有限公司 Sulfochlorination polyvinyl sizing material for power steering pipe
CN108676265A (en) * 2018-04-12 2018-10-19 天津大学 High heat conduction degaussing cable sheath material and preparation method

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Publication number Priority date Publication date Assignee Title
CN1182109A (en) * 1996-11-13 1998-05-20 于继勇 Curing agent modified chlorosulphonated polythene paint and its preparation
US20020084439A1 (en) * 2000-12-28 2002-07-04 Xerox Corporation Extrudable magnet compound with improved flow properties
CN103819827A (en) * 2014-03-11 2014-05-28 浙江久运车辆部件有限公司 Sulfochlorination polyvinyl sizing material for power steering pipe
CN108676265A (en) * 2018-04-12 2018-10-19 天津大学 High heat conduction degaussing cable sheath material and preparation method

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