CN112980066A - Low-modulus high-elasticity combined improved chloroprene rubber and preparation method and application thereof - Google Patents
Low-modulus high-elasticity combined improved chloroprene rubber and preparation method and application thereof Download PDFInfo
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- CN112980066A CN112980066A CN202110214485.4A CN202110214485A CN112980066A CN 112980066 A CN112980066 A CN 112980066A CN 202110214485 A CN202110214485 A CN 202110214485A CN 112980066 A CN112980066 A CN 112980066A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L11/00—Compositions of homopolymers or copolymers of chloroprene
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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Abstract
The invention provides a low-modulus high-elasticity modified chloroprene rubber and a preparation method and application thereof, wherein the raw materials comprise: 60-95 parts of chloroprene rubber, 5-40 parts of natural rubber or butadiene rubber, 3-10 parts of magnesium oxide, 5-10 parts of zinc oxide, 0.5-5 parts of stearic acid, 2-8 parts of naphthenic oil, 1-3 parts of an accelerator, 5-90 parts of carbon black, 1-8 parts of cardanol and 0.5-2 parts of sulfur; the cardanol is used as a compatilizer of the chloroprene rubber and the natural rubber or the butadiene rubber, so that the blending effect of the chloroprene rubber/the natural rubber or the butadiene rubber blended rubber is improved, and a better basis is provided for more effectively exerting the synergistic performance of the two rubber materials. The preparation method of the invention can shorten the vulcanization time of the rubber material, improve the production efficiency, and simultaneously improve the flow property of the rubber compound, and although the tensile strength and the tearing strength of the vulcanized rubber material are slightly reduced, the breaking elongation of the material is greatly increased, and the modulus is greatly reduced.
Description
Technical Field
The invention belongs to the field of rubber materials, and particularly relates to a low-modulus high-elasticity modified chloroprene rubber and a preparation method and application thereof.
Background
Chloroprene rubber is a synthetic rubber, and the molecular chain of chloroprene rubber contains polar chlorine atom groups, so that on one hand, double bonds are protected to weaken the activity of the chloroprene rubber, and on the other hand, the chloroprene rubber also has great stability to non-polar substances. Therefore, the light resistance, heat resistance, aging resistance and other performances of the chloroprene rubber are superior to those of natural rubber. Neoprene has a greater tensile strength comparable to natural rubber. The elasticity of the chloroprene rubber is lower than that of natural rubber, and particularly, the elasticity of the chloroprene rubber is reduced rapidly with the temperature below 15 ℃. The chloroprene rubber has good bonding effect with metal, and is widely used for sealing element materials containing metal inserts or linings. However, chloroprene rubber has disadvantages such as poor low temperature resistance, poor elasticity, and high modulus. Therefore, natural rubber or butadiene rubber is used to compensate for the disadvantages of chloroprene rubber, and rubber is used to replace chloroprene rubber. The mixed glue can make up the defects of the chloroprene rubber, but the solubility parameters of the chloroprene rubber and the chloroprene rubber have larger difference and poorer compatibility.
Disclosure of Invention
The invention aims to provide a low-modulus high-elasticity combined improved chloroprene rubber which has high elasticity, low modulus and excellent processability.
The invention also aims to provide a preparation method of the improved chloroprene rubber with low modulus and high elasticity, which can shorten the vulcanization time of rubber materials, improve the production efficiency and improve the flow property of rubber compound.
It is a final object of the present invention to provide a low modulus, high elasticity, use of the improved neoprene for making rubber vibration damping or sealing articles bonded to metal.
The specific technical scheme of the invention is as follows:
the low-modulus high-elasticity combined improved chloroprene rubber comprises the following raw materials in parts by mass:
the total amount of the chloroprene rubber and the natural rubber or the butadiene rubber is 100 parts.
The promoter is NA22 promoter.
The preparation method of the improved chloroprene rubber with low modulus and high elasticity comprises the following steps:
1) respectively carrying out hot baking on the chloroprene rubber, the natural rubber or the butadiene rubber and the carbon black in the formula ratio;
2) plasticating the natural rubber or butadiene rubber treated in the step 1), and then adding cardanol with a formula amount for uniformly mixing;
3) blending the natural rubber or the butadiene rubber treated in the step 2) and the chloroprene rubber treated in the step 1);
4) then sequentially adding stearic acid, magnesium oxide, an accelerant, carbon black, naphthenic oil, zinc oxide and sulfur according to the formula ratio, and mixing to obtain a mixed colloid;
5) and (4) vulcanizing to obtain the product.
The step 1) of baking refers to baking for 1-3 hours at 50-60 ℃;
the step 2) is specifically as follows: plasticating by adopting a double-roll open mill, wherein the temperature of a front roll is 55-60 ℃, the temperature of a rear roll is 50-55 ℃, adding the natural rubber or butadiene rubber treated by the step 1) for plasticating for 5-15min, adding the cardanol for mixing for 2-10min, and uniformly mixing.
The step 3) is specifically as follows: the method comprises the steps of setting the temperature of a front roller of a double-roller open mill to be 35-45 ℃, setting the temperature of a rear roller to be 40-50 ℃, adding chloroprene rubber processed by 1) and natural rubber or butadiene rubber processed by 2) when the temperature of the open mill reaches a preset temperature, uniformly and continuously wrapping the rubber on the front roller by adopting rubber smashing, rolling and triangular wrapping, reserving a proper amount of accumulation rubber above the roller distance, and rolling and turning for 2-3 minutes to form smooth and gapless roller wrapping rubber.
The step 4) is specifically as follows: sequentially and uniformly adding stearic acid, magnesium oxide, an accelerant, carbon black, naphthenic oil, zinc oxide and sulfur according to the formula ratio along the axis direction of the roller, after each raw material is added, after the raw materials are completely eaten, respectively cutting the left and right 3/4 twice, wherein the interval between the two cutting knives is 20 seconds, and then adding the next raw material; the charging sequence is as follows: stearic acid, magnesium oxide, an accelerator, carbon black, naphthenic oil, zinc oxide and sulfur, finally, cutting off and taking down the rubber material, adjusting the roller spacing, adding the rubber material to carry out thin passing, and carrying out triangular wrapping for 5 times to obtain the rubber compound.
Step 5) the vulcanization is specifically as follows: standing the mixed rubber for 20-25h, and vulcanizing on a flat vulcanizing machine at the vulcanization temperature of 150 ℃ and 170 ℃ for 5-30 min.
The low-modulus high-elasticity modified chloroprene rubber is prepared by the method.
The invention provides application of low-modulus high-elasticity improved chloroprene rubber to manufacturing of rubber products, in particular to manufacturing of rubber damping or sealing products bonded with metal.
The invention utilizes cardanol as a compatilizer of chloroprene rubber and natural rubber or butadiene rubber, and the cardanol structure contains polar hydroxyl and unsaturated carbon 15 straight chain. The unsaturated carbon chains are similar in structure to natural rubber or butadiene rubber and can be cross-linked to the rubber network by a vulcanization reaction; both hydroxyl and chlorine are polar groups. Therefore, the cardanol can improve the blending effect of the blended rubber, further inhibit the crystallization of chloroprene rubber and natural rubber or butadiene rubber, improve the elasticity of the blended rubber, reduce the modulus of the blended rubber and improve the processability of the blended rubber. Other compatibilizers, such as macromolecular compatibilizers like chlorinated butyl rubber, although capable of compatibilization, do not improve the processability of the blend. The macromolecular solubilizer is more difficult to be uniformly dispersed in the rubber compound than the cardanol micromolecular compatilizer, so that the macromolecular compatilizer is very limited for reducing the modulus of the rubber compound and improving the elasticity of the rubber compound. Moreover, the method has the advantages of few steps, simple operation, convenience for large-scale production and obvious effect.
The preparation method provided by the invention can shorten the vulcanization time of the rubber material, improve the production efficiency and improve the flowing property of the rubber compound. The tensile strength and tear strength of the vulcanized rubber compound are slightly reduced, but the elongation at break of the material is greatly increased, and the modulus is greatly reduced. The elasticity of the blended rubber is improved and the modulus is reduced. The low-modulus high-elasticity blended improved chloroprene rubber utilizes cardanol as a compatilizer of the chloroprene rubber and natural rubber or butadiene rubber, improves the blending effect of the blended rubber, and provides a better basis for more effectively exerting the synergistic performance of two rubber materials.
Compared with the prior art, the blend rubber provided by the invention has the advantages of good elasticity, low modulus, simple and practical preparation method, easy industrialization and capability of being directly combined with the existing production process of rubber products.
Drawings
FIG. 1 shows the storage modulus (G') as a function of strain for the mixtures.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
Example 1
The modified chloroprene rubber with low modulus and high elasticity comprises the following raw material components in parts by weight: 70 parts of chloroprene rubber, 30 parts of natural rubber, 4 parts of magnesium oxide, 5 parts of zinc oxide, 1 part of stearic acid, 4 parts of naphthenic oil, 1 part of an accelerator (NA22), 30 parts of carbon black and 1 part of sulfur, wherein the cardanol is respectively 0 part, 2 parts, 5 parts and 7 parts, and is sequentially marked as samples No. 0, No. 1, No. 2 and No. 3.
1) Placing chloroprene rubber, natural rubber and carbon black into an oven to be dried for 2 hours, and setting the temperature of the oven to be 55 ℃;
2) setting the temperature of a front roller of a double-roller open mill to be 55 ℃ and the temperature of a rear roller of the double-roller open mill to be 50 ℃, adding the natural rubber treated by the step 1) to plasticate for 10min when the temperature of the open mill reaches a preset temperature, and then adding the cardanol with the formula amount to mix for 5min uniformly; the addition amounts of cardanol were 0 parts, 2 parts, 5 parts and 7 parts, respectively.
3) Setting the temperature of a front roller of a double-roller open mill to be 45 ℃ and the temperature of a rear roller of the double-roller open mill to be 45 ℃, adding the chloroprene rubber processed by 1) and the natural rubber processed by 2) when the temperature of the open mill reaches a preset temperature, uniformly and continuously wrapping the rubber on the front roller by adopting methods of rubber smashing, rolling, triangular wrapping and the like, reserving a proper amount of accumulation rubber above the roller distance, and rolling and turning for 2-3 minutes to form the smooth gapless roller wrapping rubber.
4) Adding various compounding agents uniformly along the axial direction of the roller in sequence, after all the compounding agents are added each time, respectively cutting the left and right 3/4 knives twice, wherein the interval between the two cutting knives is 20 seconds, and then adding the next raw material; the charging sequence is as follows: 1 part of stearic acid, 4 parts of magnesium oxide, 1 part of an accelerator, 30 parts of carbon black, 4 parts of naphthenic oil, 5 parts of zinc oxide and 1 part of sulfur, cutting off and taking down the rubber material, adjusting the roller spacing, adding the rubber material to carry out thinning, and carrying out triangular wrapping for 5 times to obtain the rubber compound.
5) Standing the rubber compound for 24h, and vulcanizing the rubber compound on a flat vulcanizing machine at the vulcanization temperature of 160 ℃ for the vulcanization time of t in the table 190The time of (d);
the dynamic mechanical properties of the compounded rubber sample prepared in step 4) were tested with RPA3000 (high-speed rail). The test conditions for the strain sweep were: temperature: 60 ℃; frequency: 1 Hz; strain: 0 to 100%. The strain dependence of the dynamic mechanical properties of filled rubbers is often referred to as Payne effect. This effect is related to the dispersibility of the filler and the interaction of the filler with the rubber matrix. FIG. 1 is a plot of storage modulus (G') as a function of strain for the compounds. The amount of carbon black was 30phr, and at lower strains, G' of the mix was slightly higher than CR/NR with only 2 parts Cardanol (CNSL). The cardanol reduces the Payne effect of the rubber compound and improves the dispersibility of the carbon black.
The isothermal vulcanization curve prepared in step 5) was tested using a rubber processing analyzer (RPA3000, high-speed rail). And (3) testing tensile property: according to GB/T528-2009 standard, the test size of the dumbbell-shaped test sample is 2X 4X 20mm3. The test speed was 500 mm/min. The data are shown in table 1 below:
table 1 properties of different samples prepared in example 1
Sample (I) | 0# | 1# | 2# | 3# |
t10(min) | 3.15 | 2.23 | 1.9 | 2.08 |
t90(min) | 13.92 | 13.63 | 10.72 | 10.65 |
MH(dN·m) | 5.73 | 4.78 | 4.47 | 4.4 |
ML(dN·m) | 0.8 | 0.81 | 0.84 | 1.06 |
Tensile Strength (MPa) | 14.87 | 11.77 | 11.02 | 10.65 |
100% stress (MPa) | 0.55 | 0.31 | 0.22 | 0.21 |
300% stress (MPa) | 2.58 | 1.61 | 1.19 | 1.17 |
Elongation at Break (%) | 791.1 | 856.6 | 930.3 | 944.3 |
From the data in Table 1, it can be seen that the 1# -3# compounds compare t with 0# compounds90And MHThe reduction of the content of the components shows that the preparation method of the invention can shorten the vulcanization time, reduce the viscosity of the rubber compound and improve the production efficiency. Meanwhile, tensile experimental data and the like show that the tensile strength of the CR/NR blended rubber prepared by the invention is slightly reduced, but the elongation at break is obviously increased, and the 100% and 300% stress at definite elongation are both greatly reduced, so that the elasticity and the modulus of the prepared blended rubber are obviously increased and reduced.
Claims (9)
2. The low modulus, high elasticity, improved neoprene according to claim 1 wherein the accelerator is NA22 accelerator.
3. A method of preparing a low modulus, high elasticity and improved neoprene according to claim 1 or 2, wherein the method comprises the steps of:
1) respectively carrying out hot baking on the chloroprene rubber, the natural rubber or the butadiene rubber and the carbon black in the formula ratio;
2) plasticating the natural rubber or butadiene rubber treated in the step 1), and then adding cardanol with a formula amount for uniformly mixing;
3) blending the natural rubber or the butadiene rubber treated in the step 2) and the chloroprene rubber treated in the step 1);
4) then sequentially adding stearic acid, magnesium oxide, an accelerant, carbon black, naphthenic oil, zinc oxide and sulfur according to the formula ratio, and mixing to obtain a mixed colloid;
5) and (4) vulcanizing to obtain the product.
4. The preparation method according to claim 3, wherein the baking in step 1) is performed at 50-60 ℃ for 1-3 h.
5. The preparation method according to claim 3 or 4, wherein the step 2) is specifically: plasticating by adopting a double-roll open mill, wherein the temperature of a front roll is 55-60 ℃, the temperature of a rear roll is 50-55 ℃, adding the natural rubber or butadiene rubber treated by the step 1) for plasticating for 5-15min, adding the cardanol for mixing for 2-10min, and uniformly mixing.
6. The preparation method according to claim 3 or 4, wherein step 3) is specifically: the method comprises the steps of setting the temperature of a front roller of a double-roller open mill to be 35-45 ℃, setting the temperature of a rear roller to be 40-50 ℃, adding chloroprene rubber processed by 1) and natural rubber or butadiene rubber processed by 2) when the temperature of the open mill reaches a preset temperature, uniformly and continuously wrapping the rubber on the front roller by adopting rubber smashing, rolling and triangular wrapping, reserving a proper amount of accumulation rubber above the roller distance, and rolling and turning for 2-3 minutes to form smooth and gapless roller wrapping rubber.
7. The preparation method according to claim 3 or 4, wherein the step 4) is specifically: sequentially and uniformly adding stearic acid, magnesium oxide, an accelerant, carbon black, naphthenic oil, zinc oxide and sulfur according to the formula ratio along the axis direction of the roller, after each raw material is added, after the raw materials are completely eaten, respectively cutting the left and right 3/4 twice, wherein the interval between the two cutting knives is 20 seconds, and then adding the next raw material; the charging sequence is as follows: stearic acid, magnesium oxide, an accelerator, carbon black, naphthenic oil, zinc oxide and sulfur, finally, cutting off and taking down the rubber material, adjusting the roller spacing, adding the rubber material to carry out thin passing, and carrying out triangular wrapping for 5 times to obtain the rubber compound.
8. The preparation method according to claim 3 or 4, characterized in that the vulcanization of step 5) is in particular: standing the mixed rubber for 20-25h, and vulcanizing on a flat vulcanizing machine at the vulcanization temperature of 150 ℃ and 170 ℃ for 5-30 min.
9. Use of the low modulus, high elasticity and improved neoprene rubber prepared by the method of any one of claims 3 to 8 for the manufacture of rubber vibration damping or sealing articles bonded to metal.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115124771A (en) * | 2022-07-15 | 2022-09-30 | 安徽工程大学 | Moso bamboo powder modified high-strength nitrile butadiene rubber and preparation method thereof |
CN115785546A (en) * | 2022-12-03 | 2023-03-14 | 常州市坚力橡胶有限公司 | Preparation process of low-modulus high-elasticity improved chloroprene rubber |
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CN106279802A (en) * | 2016-08-14 | 2017-01-04 | 禧玛诺(连云港)实业有限公司 | One is resistance to subdues aging-resistant fishing wader elastomeric material and preparation method thereof |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115124771A (en) * | 2022-07-15 | 2022-09-30 | 安徽工程大学 | Moso bamboo powder modified high-strength nitrile butadiene rubber and preparation method thereof |
CN115124771B (en) * | 2022-07-15 | 2023-11-10 | 安徽工程大学 | High-strength nitrile rubber modified by moso bamboo powder and preparation method thereof |
CN115785546A (en) * | 2022-12-03 | 2023-03-14 | 常州市坚力橡胶有限公司 | Preparation process of low-modulus high-elasticity improved chloroprene rubber |
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