CN114133674B - Chlorosulfonated polyethylene rubber and preparation method thereof - Google Patents

Chlorosulfonated polyethylene rubber and preparation method thereof Download PDF

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CN114133674B
CN114133674B CN202111675151.3A CN202111675151A CN114133674B CN 114133674 B CN114133674 B CN 114133674B CN 202111675151 A CN202111675151 A CN 202111675151A CN 114133674 B CN114133674 B CN 114133674B
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chlorosulfonated polyethylene
rubber
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dispersing agent
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CN114133674A (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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    • 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 raw materials used for the rubber comprise the following components in parts by weight: 40-50 parts of chlorosulfonated polyethylene, 0.32-0.4 part of flowing 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 flowing auxiliary agent and 1.2-1.8 parts of dispersing agent. The chlorosulfonated polyethylene rubber has the advantages of high overall uniformity, high mechanical property, smooth and 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 by chlorination or chlorosulfonation, and contains chlorine-containing special elastomer material with high saturated chemical structure. The molecular structure of the modified polyurethane resin contains chlorosulfonyl active groups, so that the modified polyurethane resin has high activity, excellent chemical medium corrosion resistance, ozone oxidation resistance, oil corrosion resistance and flame retardance, and also has 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 processability of chlorosulfonated polyethylene rubber, reinforcing fillers are generally added during the processing thereof. However, the reinforcing filler adopted at present is usually inorganic powder, and because of the large surface energy difference between the powder and the rubber matrix, the compatibility between the powder and the rubber matrix is poor, the reinforcing filler is not easy to disperse in the rubber material and is easy to agglomerate, so that the uniformity of the whole rubber material is poor, the mechanical property of the rubber is reduced, and the surface of the prepared rubber is rough and not smooth.
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 present application provides a chlorosulfonated polyethylene rubber, which 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 flowing 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 promoter;
0.3-0.33 part of flow aid;
1.2-1.8 parts of dispersing agent.
By adopting the technical scheme, the flowing agent WB222 is adopted as the flowing agent, and one of the flowing aid ST and the flowing aid AC is adopted as the flowing aid, or the flowing aids ST and the flowing aid AC are mixed and used in any proportion. According to the method, the flowing agent WB222, the flowing aid ST and the flowing aid AC are added into the rubber material, so that the fluidity of the rubber material during mixing is fully improved, components such as the reinforcing filler and the like can be fully dispersed in the rubber material, all the components in the rubber material are uniformly mixed, 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 and the like is reduced, the mechanical property of the rubber is improved, and the surface of the prepared rubber is smoother.
Meanwhile, the dispersing agent is matched with the flowing agent WB222, the flowing aid ST and the flowing aid AC, acting force among reinforcing filler particles is reduced, compatibility between the reinforcing filler and other components is improved, and therefore the dispersion degree of the reinforcing filler in a sizing material during mixing is fully improved, all components in the sizing material are mixed more uniformly, the overall uniformity degree of rubber is improved, and the mechanical property of the rubber is improved.
In addition, the diisononyl phthalate is used as a plasticizer, so that the plasticity and strength of the rubber are improved, and the mechanical properties of the rubber are improved. The vulcanizing agent MC-2 is adopted as the vulcanizing agent.
In summary, the mechanical properties of rubber are fully improved by adding the diisononyl phthalate and the reinforcing filler into the rubber material, and the dispersibility of components such as the reinforcing filler in the rubber material is fully improved by adopting the flowing agent WB222, the flowing aid ST, the flowing aid AC and the dispersing agent for use in a matching way, so that all the components in the rubber material are uniformly mixed, the overall uniformity of the rubber is improved, the mechanical properties of the rubber are improved, and the surface of the prepared rubber is smoother.
Preferably, the raw materials comprise the following components in parts by weight:
45 parts of chlorosulfonated polyethylene;
0.36 parts of a flow agent;
8.2 parts of diisononyl phthalate;
40 parts of reinforcing filler;
0.45 parts of vulcanizing agent;
0.72 parts of promoter;
0.315 parts of a flow aid;
1.5 parts of dispersing agent.
Through adopting above-mentioned technical scheme, this application has further controlled the use amount of each component for the holistic mobility of sizing material obtains further improvement, and all components in the sizing material mix more evenly, thereby has further improved the holistic degree of uniformity of rubber, has strengthened the mechanical properties of rubber.
Preferably, the dispersing agent comprises dispersing agent H60EF, dispersing agent KT-8A, dispersing agent L-12 and dispersing agent FL-100 in a weight ratio of 1 (0.8-1.2): (0.04-0.06): (0.02-0.04).
Through adopting above-mentioned technical scheme, this application is through adopting dispersant H60EF, dispersant KT-8A, dispersant L-12 and dispersant FL-100 to mix the collocation to use, full play each other's synergism, the viscosity of sizing material has been reduced, the holistic mobility and the lubricity of sizing material have been improved, make components such as reinforcement filler obtain abundant infiltration, interfacial tension between components such as reinforcement filler and chlorosulfonated polyethylene has been reduced, make reinforcement filler more disperse into the sizing material, the while has also reduced the interaction force between reinforcement filler self particle, the possibility that the agglomeration takes place for reinforcement filler has been reduced, thereby the homogeneity degree that each component in the sizing material mixed has been improved, the mechanical properties of rubber has been improved.
Preferably, the reinforcing filler comprises carbon black, PW-80A, titanium pigment and light calcium 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, PW-80A, titanium pigment and light calcium powder are mixed to be used as reinforcing filler to be added into rubber materials, so that the technical performance of the rubber can be improved, and the mechanical property, heat resistance, weather resistance, color vividness, chemical stability and other properties of the rubber are improved.
Preferably, the carbon black is modified by the following method:
mixing and stirring carbon black, water, ethanol and a coupling agent for 1.5-2.0h with the weight ratio of 1 (4-5) (15-17) (18-20) at the temperature of 60-65 ℃ and the rotating speed of 250-300r/min, 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 coupling agent is adopted to carry out modification treatment on the carbon black under the process conditions, so that the surface energy difference between the carbon black and components such as chlorosulfonated polyethylene is reduced, the compatibility of the carbon black and the components such as chlorosulfonated polyethylene is improved, the dispersion capacity of the carbon black in the sizing material is enhanced, the possibility of agglomeration of the carbon black in the sizing material is reduced, the uniformity of rubber is further 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, 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 an accelerator TETD and an accelerator TT in a weight ratio of (0.44-0.46): (0.26-0.28).
Through adopting above-mentioned technical scheme, this application adds promoter TETD and promoter TT in the sizing material, can shorten the vulcanization time of sizing material, reduces the vulcanization temperature, reduces the quantity of vulcanizing agent, improves the mechanical properties of rubber simultaneously.
In a second aspect, the present application provides a method for preparing chlorosulfonated polyethylene rubber, comprising the steps of:
s1, firstly, banburying chlorosulfonated polyethylene at the temperature of 120-130 ℃ for 170-190 seconds, then adding diisononyl phthalate, reinforcing filler and dispersing agent for continuous banburying, when the temperature is 90-100 ℃, then adding a flowing agent for continuous banburying, and when the temperature is 120-130 ℃, discharging to obtain master batch;
s2, controlling the temperature below 70 ℃, mixing and banburying a vulcanizing agent, an accelerator, a flow aid and a masterbatch until the temperature reaches 80-90 ℃, discharging to obtain a sizing material, and then conducting 3-4 times of thin-pass on the sizing material, and discharging to obtain the rubber.
Through adopting above-mentioned technical scheme, this application is through the temperature when controlling flowing agent and add to and initial temperature when the component such as vulcanizing agent, accelerator mixes, has improved the mobility of sizing material for each component is mixed more easily evenly, has improved the holistic homogeneity of rubber. And the rubber material is thinned and passed for a plurality of times, so that the uniformity of the whole rubber is further improved, and the surface of the prepared rubber is smoother.
Preferably, in the step S2, the thin pass is to put the rubber material into an open mill, and the roll gap of the open mill is controlled to be 0.03-0.05mm.
Through adopting above-mentioned technical scheme, this application further controls the distance between the roll gap in specific thinness within range, can further improve the holistic homogeneity of rubber for make the rubber surface more level and smooth.
Preferably, in the step S2, the roll gap scale of the open mill is a 0 scale when the strip is discharged.
Through adopting above-mentioned technical scheme, this application is adjusted 0 scale with the scale on the mill 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 fluidity and the dispersibility of components such as reinforcing filler and the like of the rubber are higher, the uniformity degree of the whole rubber is higher, and the mechanical property is stronger;
2. the rubber surface of the application has lower roughness, flatness and smoothness and higher aesthetic degree;
3. the preparation method of the rubber has simple steps and easy operation, and is suitable for large-scale industrial production.
Drawings
FIG. 1 is a photograph of rubber without dispersant prepared according to comparative example 1 of the present application;
FIG. 2 is a photograph of the dispersant-added rubber prepared according to example 3 of the present application.
Detailed Description
The present application is described in further detail below with reference to examples.
<Material source>
Chlorosulfonated polyethylene, available from Shandong Liang New Material technologies Co., ltd., model TS530;
flowage agent WB222, available from guangzhou municipal large rubber raw material trade company;
diisononyl phthalate, available from Shandong Chen chemical Co., ltd;
flow aid ST, available from guangzhou city, sco source chemical company, inc;
flow aid AC, purchased from hebei condition flying chemical technology limited;
vulcanizing agent MC-2, purchased from Mian Hai Yuan chemical Co., ltd;
dispersing agent H60EF, available from shandong yang valley huaitai chemical company limited;
dispersant KT-8A, available from Setaria chemical Co., ltd;
dispersant L-12, available from Shanghai Telman chemical Co., ltd;
dispersant FL-100, available from Shanghai head-Stand, inc.;
carbon black, available from pentasen new materials technology, inc., guangzhou, model N660;
PW-80A from Shanghai general industries, inc.;
titanium dioxide, purchased from Nanyang Heng Xiang chemical industry Co., ltd;
light calcium powder purchased from mineral processing plants in the Ministry of life;
silane coupling agent KH-570, available from Guangzhou, gmbH;
silane coupling agent Si-69, purchased from Guangzhou City rubber raw material trade company;
titanate coupling agent 201, available from Jinan Rong chemical Co., ltd;
accelerator TETD, purchased from the cantonese market force rubber raw material trade company;
accelerator TT, available from Guangzhou City rubber raw material trade company.
<Examples>
Example 1
A method for preparing chlorosulfonated polyethylene rubber, comprising the following steps:
s1, firstly, putting 40kg of chlorosulfonated polyethylene into an internal mixer, carrying out internal 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, continuing internal mixing, when the temperature is 90 ℃, adding 0.4kg of flowing agent WB222, continuing internal mixing, and when the temperature is 120 ℃, discharging to obtain masterbatch;
s2, firstly cooling an internal mixer, controlling the temperature of the internal mixer below 70 ℃, putting 0.4kg of vulcanizing agent MC-2, 0.74kg of accelerator (0.46 kg of accelerator TETD, 0.28kg of accelerator TT), 0.3kg of flow aid ST and the masterbatch into the internal mixer, mixing and banburying until the temperature reaches 80 ℃, discharging to obtain a rubber material, then adjusting the roll gap between two rolls of the open mill to be below 0.5mm, passing the rubber material through the two rolls for 3 times, then adjusting the roll gap scale of the open mill to 0 scale, and discharging to obtain the rubber.
Example 2
A method for preparing chlorosulfonated polyethylene rubber, comprising the following steps:
s1, firstly, putting 50kg of chlorosulfonated polyethylene into an internal mixer, carrying out internal mixing for 190 seconds 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 dispersant L-12 for continuous internal mixing, when the temperature is 100 ℃, adding 0.32kg of flowing agent WB222 for continuous internal mixing, and when the temperature is 130 ℃, discharging to obtain masterbatch;
s2, firstly cooling an internal mixer, controlling the temperature of the internal mixer below 70 ℃, putting 0.5kg of vulcanizing agent MC-2, 0.7kg of accelerator (0.44 kg of accelerator TETD, 0.26kg of accelerator TT), 0.33kg of flow aid (0.2 kg of flow aid ST, 0.13kg of flow aid AC) and masterbatch into the internal mixer, mixing and banburying until the temperature reaches 90 ℃, discharging to obtain a rubber material, then adjusting the roll gap between two rollers of the internal mixer to be less than 0.5mm, passing the rubber material between the two rollers for 4 times, adjusting the roll gap scale of the internal mixer to 0 scale, and discharging to obtain the rubber.
Example 3
A method for preparing chlorosulfonated polyethylene rubber, comprising the following steps:
s1, firstly putting 45kg of chlorosulfonated polyethylene into an internal mixer, carrying out internal mixing for 180 seconds 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 pigment and 22.2kg of light calcium powder) and 1.5kg of dispersing agent KT-8A, continuing internal mixing, when the temperature is 95 ℃, adding 0.36kg of flowing agent WB222, continuing internal mixing, and when the temperature is 125 ℃, discharging to obtain master batch;
s2, firstly cooling an internal mixer, controlling the temperature of the internal mixer below 70 ℃, putting 0.45kg of vulcanizing agent MC-2, 0.72kg of accelerator (0.45 kg of accelerator TETD, 0.27kg of accelerator TT), 0.315kg of flow aid AC and master batch into the internal mixer, mixing and banburying until the temperature reaches 85 ℃, discharging to obtain a rubber material, then adjusting the roll gap between two rolls of the open mill to be below 0.5mm, passing the rubber material through the two rolls for 4 times, then adjusting the roll gap scale of the open mill to 0 scale, and discharging to obtain the rubber.
Example 4
A method for producing chlorosulfonated polyethylene rubber, which is different from 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 pigment and 21.09kg of light calcium powder), 1.3kg of dispersing agent 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, 0.266kg of accelerator TT) and 0.31kg of flow aid AC.
Example 5
A method for producing chlorosulfonated polyethylene rubber, which is different from 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 pigment and 23.31kg of light calcium powder), 1.7kg of dispersing agent 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, 0.274kg of accelerator TT) and 0.32kg of flow aid AC.
Example 6
A method for producing chlorosulfonated polyethylene rubber, which is different from 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 the dispersant H60EF is 0.8kg, the dispersant KT-8A is 0.65kg, the dispersant L-12 is 0.03kg, and the dispersant FL-100 is 0.02kg.
Example 7
A method for producing chlorosulfonated polyethylene rubber, which is different from 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 the dispersant H60EF is 0.65kg, the dispersant KT-8A is 0.78kg, the dispersant L-12 is 0.04kg, and the dispersant FL-100 is 0.03kg.
Example 8
A method for producing chlorosulfonated polyethylene rubber, which is different from 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 1:0.46:0.03:0.01; wherein the dispersant H60EF is 1kg, the dispersant KT-8A is 0.46kg, the dispersant L-12 is 0.03kg, and the dispersant FL-100 is 0.01kg.
Example 9
A method for producing chlorosulfonated polyethylene rubber, which is different from 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 1:1.5:0.25:0.25; wherein the dispersant H60EF is 0.5kg, the dispersant KT-8A is 0.75kg, the dispersant L-12 is 0.125kg, and the dispersant FL-100 is 0.125kg.
Example 10
A method for producing chlorosulfonated polyethylene rubber, which is different from example 3 in that: the carbon black is modified by the following method:
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 1.5 hours at the temperature of 60 ℃ and the rotating speed of 250r/min, and then filtered, washed and dried for 4 hours at the temperature of 100 ℃ to obtain the modified carbon black.
Example 11
A method for producing chlorosulfonated polyethylene rubber, which is different from example 3 in that: the carbon black is modified by the following method:
under the conditions of 65 ℃ and 300r/min of rotating speed, 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, filtered, washed and dried for 5 hours at 105 ℃ to obtain the modified carbon black.
Example 12
A method for producing chlorosulfonated polyethylene rubber, which is different from example 3 in that: the carbon black is modified by the following method:
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 1.75 hours at the temperature of 62.5 ℃ and the rotating speed of 275r/min, and then filtered, washed and dried for 4.5 hours at the temperature of 102.5 ℃ to obtain the modified carbon black.
Example 13
A method for producing chlorosulfonated polyethylene rubber, which is different from example 3 in that: the carbon black is modified by the following method:
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 1.6 hours at the temperature of 63 ℃ and the rotating speed of 280r/min, and then filtered, washed and dried for 4.7 hours at the temperature of 104 ℃ to obtain the modified carbon black.
Example 14
A method for producing chlorosulfonated polyethylene rubber, which is different from example 3 in that: in the step S2, the roll gap between the two rolls of the open mill is adjusted to be 0.03mm.
Example 15
A method for producing chlorosulfonated polyethylene rubber, which is different from example 3 in that: in the step S2, the roll gap between the two rolls of the open mill is adjusted to be 0.05mm.
<Comparative example>
Comparative example 1
The difference from example 3 is that: in the step S1, no dispersing agent is added into the internal mixer, and the rest are 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 pigment and 27.75kg of light calcium powder), 2kg of dispersing agent KT-8A, 1kg of flow agent WB222, 0.2kg of vulcanizing agent MC-2, 1.44kg of accelerator (0.9 kg of accelerator TETD, 0.54kg of accelerator TT), 0.2kg of flow aid AC and the balance being 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 pigment and 16.65kg of light calcium powder), 1kg of dispersing agent KT-8A, 0.2kg of flow agent WB222, 1kg of vulcanizing agent MC-2, 0.576kg of accelerator (0.36 kg of accelerator TETD, 0.216kg of accelerator TT), 0.5kg of flow aid AC and the balance of the above are the same.
Comparative example 4
The difference from example 3 is that: in step S1, the temperature at which the fluidizing agent WB-222 was added was 110℃and the rest was the same.
Comparative example 5
The difference from example 3 is that: in step S2, after the internal mixer is cooled, the temperature of the internal mixer is 80 ℃, and the rest are the same.
<Performance detection>
1. The tensile strength and elongation at break of the rubbers prepared in examples 1 to 15 and comparative examples 1 to 5 were tested with reference to GB/T528-2009 "determination of tensile stress Strain Properties of vulcanized rubber or thermoplastic rubber", and the test results are shown in Table 1;
2. the tear strength of the rubbers produced in examples 1 to 15 and comparative examples 1 to 5 was measured by using a square-shaped test piece with reference to GB/T529-2008 "measurement of tear strength of vulcanized rubber or thermoplastic rubber", and the test results are shown in Table 1.
Table 1 results of performance test table
Project 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%, the tear strength is 63.87-69.11kN/m, which indicates that the rubber prepared in the present application has better uniformity, and the tensile strength, elongation at break, tear strength and other mechanical properties are stronger.
The tensile strength, elongation at break and tear strength of the rubber prepared in examples 4-5 are all smaller than those of example 3, which shows that the application can further control the use amount of each component to ensure that each component is mixed more uniformly, and further improve the uniformity of the rubber, thereby improving the mechanical property of the rubber.
The tensile strength, elongation at break and tear strength of the rubber prepared in examples 6-7 are all greater than those of example 3, which shows that the application adopts the dispersant H60EF, the dispersant KT-8A, the dispersant L-12 and the dispersant FL-100 together, so that the synergistic effect of the dispersants can be exerted, the components such as reinforcing filler and the like can be fully dispersed, the uniformity of the rubber is improved, and the mechanical property of the rubber is improved.
The tensile strength, elongation at break and tear strength of the rubber prepared in examples 8-9 are all greater than those of the rubber prepared in example 3, but the tensile strength, elongation at break and tear strength of the rubber prepared in examples 8-9 are all smaller than those of the rubber prepared in examples 6-7, which shows that the weight ratio of the dispersing agent H60EF, the dispersing agent KT-8A, the dispersing agent L-12 and the dispersing agent FL-100 is further controlled, the synergistic effect among the four can be fully exerted, the dispersion degree of each component in the rubber material is further 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 rubber prepared in examples 10-13 are all greater than those of the rubber prepared in example 3, which shows that the modification treatment is carried out on the carbon black, so that the dispersibility of the carbon black in the 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 rubber prepared in examples 14-15 are all greater than those of the rubber prepared in example 3, which shows that the roll gap of the open mill is further controlled during thin pass, the overall uniformity of the rubber is further improved, and the surface of the rubber is smoother.
The tensile strength, elongation at break and tear strength of the rubber prepared in comparative example 1 are all smaller than those of example 3, and as can be seen by combining with fig. 1 and 2, the dispersing agent is added into the rubber material, so that the dispersing agent can be matched with the flowing agent and the flowing auxiliary agent, the dispersibility of each component in the rubber material is improved, the overall uniformity 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 prepared in comparative examples 2 to 3 are all smaller than those in example 3, indicating that if the amounts of the components used in the rubbers are out of the ranges of the present application, the uniformity of the rubber as a whole is lowered, thereby lowering the mechanical properties of the rubber.
The tensile strength, elongation at break and tear strength of the rubber prepared in comparative examples 4-5 are all less than those of example 3, indicating that if the temperature of the flow agent is too high and the initial temperature of the vulcanizing agent, accelerator and other components are too high, the flowability of the rubber is reduced, thereby reducing the overall uniformity of the rubber and further reducing the mechanical properties of the rubber.
The embodiments of the present invention are all preferred embodiments of the present application, and are not intended to limit the scope of the present application in this way, therefore: all equivalent changes in structure, shape and principle of this application should be covered in the protection scope of this application.

Claims (9)

1. The chlorosulfonated polyethylene rubber is characterized by comprising the following raw materials in parts by weight:
40-50 parts of chlorosulfonated polyethylene;
2220.32-0.4 part of flowing agent WB;
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 promoter;
0.3-0.33 parts of flow aid ST and/or flow aid AC;
1.2-1.8 parts of dispersing agent;
the dispersing agent comprises dispersing agent H60EF, dispersing agent KT-8A, dispersing agent L-12 and dispersing agent FL-100 in a weight ratio of 1 (0.8-1.2) (0.04-0.06) (0.02-0.04).
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;
2220.36 parts of a flow agent WB;
8.2 parts of diisononyl phthalate;
40 parts of reinforcing filler;
0.45 parts of vulcanizing agent;
0.72 parts of promoter;
flow aid ST and/or flow aid AC0.315 parts;
1.5 parts of dispersing agent.
3. A chlorosulfonated polyethylene rubber according to claim 1 or 2, wherein the reinforcing filler comprises carbon black, PW-80A, titanium pigment and light calcium powder in a weight ratio of (0.35-2.85): (9.95-12.45): (3.75-6.25): (20.95-23.45).
4. A chlorosulfonated polyethylene rubber according to claim 3, wherein the carbon black is modified by the following method:
mixing and stirring carbon black, water, ethanol and a coupling agent for 1.5-2.0h with the weight ratio of 1 (4-5) (15-17) (18-20) at the temperature of 60-65 ℃ and the rotating speed of 250-300r/min, filtering, washing, and drying at the temperature of 100-105 ℃ for 4-5h to obtain the modified carbon black.
5. The chlorosulfonated polyethylene rubber according to claim 4, wherein the coupling agent is one or more of silane coupling agent KH-570, silane coupling agent Si-69 and titanate coupling agent 201.
6. A chlorosulfonated polyethylene rubber according to claim 1 or 2, wherein the accelerator comprises accelerator TETD and accelerator TT in a weight ratio of (0.44-0.46): (0.26-0.28).
7. A process for producing chlorosulfonated polyethylene rubber as claimed in any one of claims 1 to 6, comprising the steps of:
s1, firstly, banburying chlorosulfonated polyethylene at the temperature of 120-130 ℃ for 170-190 seconds, then adding diisononyl phthalate, reinforcing filler and dispersing agent for continuous banburying, when the temperature is 90-100 ℃, then adding a flowing agent for continuous banburying, and when the temperature is 120-130 ℃, discharging to obtain master batch;
s2, controlling the temperature below 70 ℃, mixing and banburying a vulcanizing agent, an accelerator, a flow aid and a masterbatch until the temperature reaches 80-90 ℃, discharging to obtain a sizing material, and then conducting 3-4 times of thin-pass on the sizing material, and discharging to obtain the rubber.
8. The method for preparing chlorosulfonated polyethylene rubber according to claim 7, wherein in the step S2, the thin pass is performed by placing the rubber material into an open mill and controlling the roll gap of the open mill to be 0.03-0.05mm.
9. The method for preparing chlorosulfonated polyethylene rubber according to claim 8, wherein in the step S2, the roll gap scale of the open mill is 0 scale when the strip is discharged.
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