CN111154150A - high-Mooney natural rubber foaming rubber compound and preparation method thereof - Google Patents
high-Mooney natural rubber foaming rubber compound and preparation method thereof Download PDFInfo
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- CN111154150A CN111154150A CN201911391779.3A CN201911391779A CN111154150A CN 111154150 A CN111154150 A CN 111154150A CN 201911391779 A CN201911391779 A CN 201911391779A CN 111154150 A CN111154150 A CN 111154150A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/107—Nitroso compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2307/00—Characterised by the use of natural rubber
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
- C08J2491/06—Waxes
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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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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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
- C08K3/02—Elements
- C08K3/04—Carbon
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Abstract
The invention discloses a high-Mooney natural rubber foaming rubber compound and a preparation method thereof, and relates to the technical field of natural rubber foaming. The invention comprises 100 parts of natural rubber, 10-15 parts of an active agent, 1.5-4.5 parts of an anti-aging agent, 20-40 parts of a softener, 1.5-4 parts of a vulcanizing agent, 3.5-5 parts of an accelerator, 0.5-3 parts of a dispersant, 200-260 parts of a filler, 4-6 parts of a foaming agent and 2-4 parts of a foaming auxiliary agent BK. The invention prepares the master batch by the first-stage mixing of the internal mixer, and then prepares the foaming rubber compound by the second-stage vulcanizing, simplifies the preparation process of the existing natural rubber foaming rubber compound, omits plastication of raw rubber, reduces the processing cost, is beneficial to large-scale production of modern mixing plants, and the prepared foaming material has uniform pore diameter, good elasticity and high foaming ratio.
Description
Technical Field
The invention belongs to the technical field of natural rubber foaming, and particularly relates to a high-Mooney natural rubber foaming rubber compound and a preparation method thereof.
Background
The natural rubber foaming material has the characteristics of damping, sound insulation, light weight, good elasticity and the like, and is widely applied to various production and living fields. However, the traditional natural rubber foaming rubber compound requires low mooney viscosity of raw rubber and extremely high plastication cost, is not beneficial to field management and is not suitable for continuous production of modern mixing plants.
Poor stability of the rubber compound causes unstable performance of the natural rubber foamed product, and the rubber compound has low Mooney viscosity and low strength and is difficult to meet the production of thin foamed products which are continuously rolled out of sheets. Therefore, the development of the rubber compound which is convenient and simple to produce, low in cost, stable in product and wide in application range and can be suitable for continuous production in modern mixing plants and the preparation method have important significance.
Disclosure of Invention
The invention aims to provide a high-Mooney natural rubber foaming rubber compound and a preparation method thereof, which solve the problems of high plastication cost, low Mooney viscosity of raw rubber, inconvenience for field management, unsuitability for continuous production of modern mixing plants and instability of foaming products in the traditional process by reasonably selecting raw materials and proportion and optimizing the preparation process.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention relates to a high-Mooney natural rubber foaming rubber compound which comprises the following raw materials in parts by weight:
100 parts of natural rubber, 10-15 parts of an active agent, 1.5-4.5 parts of an anti-aging agent, 20-40 parts of a softening agent, 1.5-4 parts of a vulcanizing agent, 3.5-5 parts of an accelerator, 0.5-3 parts of a dispersing agent, 200-260 parts of a filler, 4-6 parts of a foaming agent and 4-4 parts of a foaming auxiliary agent BK 2.
Preferably, the feed comprises the following raw materials in parts by weight: 100 parts of natural rubber, 10 parts of an active agent, 1.5 parts of an anti-aging agent, 30 parts of a softener, 3.5 parts of a vulcanizing agent, 3.5 parts of an accelerator, 2 parts of a dispersant, 215 parts of a filler, 5 parts of a foaming agent and 2 parts of a foaming auxiliary agent BK.
Preferably, the softener is a mixture of white mineral oil and white factice, wherein the white mineral oil accounts for 20 parts, and the white factice accounts for 10 parts.
Preferably, the foaming agent is foaming agent H, wherein the foaming agent H is 5 parts.
Preferably, the filler is heavy calcium carbonate, fine tire rubber powder and carbon black, wherein the heavy calcium carbonate is 190 parts, the fine tire rubber powder is 20 parts, and the carbon black is 5 parts.
A preparation method of a high-Mooney natural rubber foaming rubber compound comprises the following steps:
step 1, batching: selecting the components in parts and preparing raw materials within the range of the mixture ratio of the raw materials;
step 2, first-stage mixing: adding filler and natural rubber into an internal mixer at the same time, heating the mixture to 120 ℃ at a ram pressure of 60bar and a rotation speed of 45r/min, adding an active agent, an anti-aging agent, a softening agent and a dispersing agent, reducing the rotation speed to 25r/min, heating to 155 ℃ of the mixture, and discharging rubber for 6-9 min to obtain a primary rubber;
step 3, parking: standing the prepared primary masterbatch for 4-24 hours at the temperature of not less than 15 ℃;
step 4, two-stage mixing: adding the parked primary rubber into an internal mixer, heating the mixture to 80 ℃ at a plug loading pressure of 50bar and a rotating speed of 25r/min, adding a vulcanizing agent, an accelerator, a foaming agent and a foaming auxiliary agent, heating to the mixture temperature of 100 ℃, and discharging rubber to obtain the natural rubber foaming rubber compound.
The invention has the following beneficial effects:
1. the filler and the natural rubber are simultaneously put into the internal mixer, the internal mixing chamber can be effectively filled due to the fact that the filler is added in a large amount, the filler is mostly heavy calcium carbonate which is a hard material, and therefore the rotor, the filler and the natural rubber interact at the initial stage of mixing to effectively plasticate the crude rubber, the Mooney viscosity of a section of the crude rubber is still 15-25 unit values higher than that of the crude rubber in the traditional process, and the Mooney viscosity of a terminal rubber is 10-20 unit values higher than that of the traditional process;
2. the Mooney viscosity of the terminal rubber compound is higher, a faster vulcanization system is not beneficial to foaming, T10 is prolonged by controlling the selection and the using amount of the accelerator, the time is 2-2.5 times of the time of T10 in the traditional process, and sufficient softening time is reserved for the rubber compound before the product is foamed and formed in an oven;
3. by controlling the dosage of the foaming agent and the foaming auxiliary agent, the decomposition temperature of the foaming agent is slightly increased, so that the foaming agent is matched with a vulcanization system, and simultaneously, the foaming rate is reduced, and the foaming pore diameter is more uniform;
compared with the prior art, the invention saves plastication of raw rubber, reduces processing cost and is beneficial to large-scale production of modern mixing factories; the vulcanization speed and the foaming rate are optimized, so that the foaming aperture is more uniform while the foaming ratio is ensured; the rubber compound has higher Mooney viscosity and higher strength, and can meet the production of thin foamed products which are continuously calendered into sheets; the molecular chain of the natural rubber is broken without fully plasticating, so that the molecular chain is relatively longer, and the prepared foamed product has good elasticity.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
Detailed Description
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 only a part of the embodiments of the present invention, and not all of the 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.
Comparative example:
the common natural rubber foaming rubber compound comprises the following components in parts by weight: 100 parts of natural rubber, 10 parts of an active agent, 1.5 parts of an anti-aging agent, 30 parts of a softener, 4 parts of a vulcanizing agent, 3.8 parts of an accelerator, 2 parts of a dispersant, 200 parts of a filler, 4 parts of a foaming agent H and 4 parts of a foaming auxiliary agent BK.
The rubber mixing process of the rubber compound specifically comprises the following steps:
step 1, batching: accurately configuring the component parts according to the parts by weight;
step 2, plasticating: under the condition of room temperature, repeatedly thinly passing the prepared natural rubber in an open mill until the Mooney viscosity ML100 ℃ (1+4) is 20-25 to obtain natural rubber A;
step 3, parking: standing the natural rubber A at room temperature (not lower than 15 ℃) for 12-24 hours;
step 4, first-stage mixing: adding the parked natural rubber A into an internal mixer, raising the temperature to 80 ℃ at a ram-up pressure of 60bar and a rotation speed of 45r/min, increasing the rotation speed to 25r/min, sequentially adding an active agent, an anti-aging agent, a dispersing agent, a filler and a softening agent, heating to the mixture temperature of 130 ℃, and discharging rubber for 6-9 min to obtain a section of master batch B;
step 5, parking: standing the prepared primary masterbatch B at room temperature (not lower than 15 ℃) for 4-24 h;
step 6, two-stage mixing: and adding the parked section of master batch B into an internal mixer, heating the mixture to 80 ℃ at the top plug pressure of 50bar and the rotating speed of 25r/min, adding a vulcanizing agent, an accelerator, a foaming agent and a foaming auxiliary agent, heating to the mixture temperature of 100 ℃, and discharging rubber to obtain the natural rubber foaming rubber compound.
The existing natural rubber foaming rubber compound is prepared by plasticating through an open mill, controlling the Mooney viscosity of raw rubber to be 100ML (1+4) to be 20-25, and then preparing master batch and terminal rubber compound in an internal mixer, and is characterized in that the rubber compound has low viscosity and low strength, the T10 speed is shorter, and the T10 measured at 150 ℃ in the traditional process is generally 50-80 s.
The first embodiment is as follows:
a high-Mooney natural rubber foaming rubber compound comprises the following components in parts by weight: 100 parts of natural rubber, 10 parts of an active agent, 1.5 parts of an anti-aging agent, 30 parts of a softener, 3.5 parts of a vulcanizing agent, 3.5 parts of an accelerator, 2 parts of a dispersant, 215 parts of a filler, 5 parts of a foaming agent H (the foaming agent H is dinitrosopentamethylenetetramine) and 2 parts of a foaming auxiliary agent BK;
the preparation method of the high-Mooney natural rubber foaming rubber compound comprises the following steps:
step 1, batching: preparing raw materials accurately according to 100 parts of natural rubber, 10 parts of an active agent, 1.5 parts of an anti-aging agent, 30 parts of a softener, 3.5 parts of a vulcanizing agent, 3.5 parts of an accelerator, 2 parts of a dispersing agent, 215 parts of a filler, 5 parts of a foaming agent H and 2 parts of a foaming auxiliary agent BK;
step 2, first-stage mixing: adding a filler and natural rubber into an internal mixer, heating the mixture to 120 ℃ at a ram-up pressure of 60bar and a rotation speed of 45r/min, sequentially adding an active agent, a dispersing agent, an anti-aging agent and a softening agent, reducing the rotation speed to 25r/min, heating to 155 ℃ of the mixture, and discharging rubber for 6-9 min to obtain a primary rubber;
step 3, parking: standing the prepared primary masterbatch for 4-24 h at room temperature (not lower than 15 ℃);
step 4, two-stage mixing: and adding the parked primary rubber into an internal mixer, heating the mixture to 80 ℃ at a plug loading pressure of 50bar and a rotating speed of 25r/min, sequentially adding a vulcanizing agent, an accelerator, a foaming agent and a foaming auxiliary agent, heating to the mixture temperature of 100 ℃, and discharging rubber to obtain the natural rubber foaming rubber compound.
The second embodiment is as follows:
a high-Mooney natural rubber foaming rubber compound comprises the following components in parts by weight: 100 parts of natural rubber, 10 parts of an active agent, 1.5 parts of an anti-aging agent, 40 parts of a softener, 3.5 parts of a vulcanizing agent, 3.3 parts of an accelerator, 2 parts of a dispersing agent, 260 parts of a filler, 6 parts of a foaming agent H and 2 parts of a foaming auxiliary agent BK.
The preparation method of the high-Mooney natural rubber foaming rubber compound comprises the following steps:
step 1, batching: preparing raw materials accurately according to 100 parts of natural rubber, 10 parts of an active agent, 1.5 parts of an anti-aging agent, 40 parts of a softening agent, 3.5 parts of a vulcanizing agent, 3.3 parts of an accelerator, 2 parts of a dispersing agent, 260 parts of a filler, 6 parts of a foaming agent and 2 parts of a foaming auxiliary agent BK;
step 2, first-stage mixing: adding a filler and natural rubber into an internal mixer, heating the mixture to 120 ℃ at a ram-up pressure of 60bar and a rotation speed of 45r/min, sequentially adding an active agent, a dispersing agent, an anti-aging agent and a softening agent, reducing the rotation speed to 25r/min, heating to 155 ℃ of the mixture, and discharging rubber for 6-9 min to obtain a primary rubber;
step 3, parking: standing the prepared primary masterbatch for 4-24 h at room temperature (not lower than 15 ℃);
step 4, two-stage mixing: and adding the parked primary rubber into an internal mixer, heating the mixture to 80 ℃ at a plug loading pressure of 50bar and a rotating speed of 25r/min, sequentially adding a vulcanizing agent, an accelerator, a foaming agent and a foaming auxiliary agent, heating to the mixture temperature of 100 ℃, and discharging rubber to obtain the natural rubber foaming rubber compound.
Molding: and (3) discharging the mixed rubber on a calender into a sheet, placing the sheet into an oven, and carrying out pressureless free foaming molding at the hot air temperature of 155-165 ℃, wherein the vulcanization speed is determined according to the vulcanization speed of the mixed rubber and the sheet discharging thickness of the mixed rubber.
The foaming and vulcanizing time of the product in an oven is T90+50s, and the MDR test conditions are as follows: the performances of the rubber mixtures of the comparative example, the first specific example and the second specific example and the conditions of the foamed products are shown in the following table one:
watch 1
The filler and the natural rubber are simultaneously put into the internal mixer, the internal mixing chamber can be effectively filled due to the fact that the filler is added in a large amount, the filler is mostly heavy calcium carbonate which is a hard material, and therefore the rotor, the filler and the natural rubber interact at the initial stage of mixing to effectively plasticate the crude rubber, the Mooney viscosity of a section of the crude rubber is still 15-25 unit values higher than that of the crude rubber in the traditional process, and the Mooney viscosity of a terminal rubber is 10-20 unit values higher than that of the traditional process; the Mooney viscosity of the terminal rubber compound is higher, a faster vulcanization system is not beneficial to foaming, T10 is prolonged by controlling the selection and the using amount of the accelerator, the time is 2-2.5 times of the time of T10 in the traditional process, and sufficient softening time is reserved for the rubber compound before the product is foamed and formed in an oven; by controlling the dosage of the foaming agent and the foaming auxiliary agent, the decomposition temperature of the foaming agent is slightly increased, so that the foaming agent is matched with a vulcanization system, the foaming rate is reduced, and the foaming pore diameter is more uniform. In conclusion, compared with the prior art, the invention omits the plastication of raw rubber, reduces the processing cost and is beneficial to the large-scale production of modern mixing plants; the vulcanization speed and the foaming rate are optimized, so that the foaming aperture is more uniform while the foaming ratio is ensured; the rubber compound has higher Mooney viscosity and higher strength, and can meet the production of thin foamed products which are continuously calendered into sheets; the molecular chain of the natural rubber is broken without fully plasticating, so that the molecular chain is relatively longer, and the prepared foamed product has good elasticity.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (6)
1. The high-Mooney natural rubber foaming rubber compound is characterized by comprising the following raw materials in parts by weight:
100 parts of natural rubber, 10-15 parts of an active agent, 1.5-4.5 parts of an anti-aging agent, 20-40 parts of a softening agent, 1.5-4 parts of a vulcanizing agent, 3.5-5 parts of an accelerator, 0.5-3 parts of a dispersing agent, 200-260 parts of a filler, 4-6 parts of a foaming agent and 2-4 parts of a foaming auxiliary agent BK.
2. The high-Mooney natural rubber foaming mix as claimed in claim 1, which comprises the following raw materials in parts by weight:
100 parts of natural rubber, 10 parts of an active agent, 1.5 parts of an anti-aging agent, 30 parts of a softener, 3.5 parts of a vulcanizing agent, 3.5 parts of an accelerator, 2 parts of a dispersant, 215 parts of a filler, 5 parts of a foaming agent and 2 parts of a foaming auxiliary agent BK.
3. The high-Mooney natural rubber foaming mix as claimed in claim 2, wherein the softener is a mixture of white mineral oil and white ointment, wherein the white mineral oil is 20 parts and the white ointment is 10 parts.
4. The high-Mooney natural rubber foaming mix as claimed in claim 2, wherein the foaming agent is foaming agent H, wherein the foaming agent H is 5 parts.
5. The high-Mooney natural rubber foaming rubber compound as claimed in claim 2, wherein the filler is ground calcium carbonate, fine tire rubber powder and carbon black, wherein the ground calcium carbonate is 190 parts, the fine tire rubber powder is 20 parts, and the carbon black is 5 parts.
6. The method for preparing a high-Mooney natural rubber foaming compound as claimed in any one of claims 1 to 5, comprising the steps of:
step 1, batching: selecting the components in parts and preparing raw materials within the range of the mixture ratio of the raw materials;
step 2, first-stage mixing: adding filler and natural rubber into an internal mixer at the same time, heating the mixture to 120 ℃ at a ram pressure of 60bar and a rotation speed of 45r/min, adding an active agent, an anti-aging agent, a softening agent and a dispersing agent, reducing the rotation speed to 25r/min, heating to 155 ℃ of the mixture, and discharging rubber for 6-9 min to obtain a primary rubber;
step 3, parking: standing the prepared primary masterbatch for 4-24 hours at the temperature of not less than 15 ℃;
step 4, two-stage mixing: adding the parked primary rubber into an internal mixer, heating the mixture to 80 ℃ at a plug loading pressure of 50bar and a rotating speed of 25r/min, adding a vulcanizing agent, an accelerator, a foaming agent and a foaming auxiliary agent, heating to the mixture temperature of 100 ℃, and discharging rubber to obtain the natural rubber foaming rubber compound.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114133631A (en) * | 2021-12-07 | 2022-03-04 | 江苏冠联新材料科技股份有限公司 | Environment-friendly health-care rubber pad mixed compound and preparation method thereof |
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| CN1687206A (en) * | 2005-04-21 | 2005-10-26 | 上海交通大学 | Technique for producing freerise foaming material of rubber |
| CN107200872A (en) * | 2016-03-16 | 2017-09-26 | 青岛科技大学 | A kind of wear-resisting microcellular foam material |
| CN109370065A (en) * | 2018-10-15 | 2019-02-22 | 浙江仙通橡塑股份有限公司 | A kind of weather strip for automobile rubber compound of one-step method continuous mixing and preparation method thereof |
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2019
- 2019-12-30 CN CN201911391779.3A patent/CN111154150A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1687206A (en) * | 2005-04-21 | 2005-10-26 | 上海交通大学 | Technique for producing freerise foaming material of rubber |
| CN107200872A (en) * | 2016-03-16 | 2017-09-26 | 青岛科技大学 | A kind of wear-resisting microcellular foam material |
| CN109370065A (en) * | 2018-10-15 | 2019-02-22 | 浙江仙通橡塑股份有限公司 | A kind of weather strip for automobile rubber compound of one-step method continuous mixing and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114133631A (en) * | 2021-12-07 | 2022-03-04 | 江苏冠联新材料科技股份有限公司 | Environment-friendly health-care rubber pad mixed compound and preparation method thereof |
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