CN105461981A - Oxidization-resistant natural rubber material and preparation method thereof - Google Patents
Oxidization-resistant natural rubber material and preparation method thereof Download PDFInfo
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- CN105461981A CN105461981A CN201510952180.8A CN201510952180A CN105461981A CN 105461981 A CN105461981 A CN 105461981A CN 201510952180 A CN201510952180 A CN 201510952180A CN 105461981 A CN105461981 A CN 105461981A
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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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
- C08K3/34—Silicon-containing compounds
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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
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/11—Esters; Ether-esters of acyclic polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses an oxidization-resistant natural rubber material which comprises, by weight parts, 1-2 parts of antioxidant DSTP, 100-140 parts of natural rubber, 20-30 parts of kaolinite, 400-500 parts of dimethyl sulfoxide, 900-1000 parts of methanol, 70-80 parts of N-methylimidazole, 100-120 parts of bromoethane, 4-6 parts of nano silicon oxide, 1-1.6 parts of vulcanizing agent MOCA, 6-7 parts of dioctyl azelate, 2-3 parts of ammonium ferrous sulfate, 1-2 parts of anti-aging agent 688, 0.7-1 part of polybenzimidazole and 2-4 parts of medical stone powder. The rubber material has very good oxidization resistance and is long in service life and good in weather resistance.
Description
Technical field
The present invention relates to field of rubber technology, particularly relate to a kind of anti-oxidant natural rubber material and preparation method thereof.
Background technology
Kaolinite belongs to the kaolin (kaolinite of l: l type laminate structure, dickite, nakrite, one of halloysite etc.) clay mineral, to be superposed by 1: 1 by SiO4 tetrahedrallayer and AlO2 (OH) 4 octahedral layer and form asymmetric laminate structure, thus establish large folded dipole, interlayer is with (Al-O-H ... O-Si) hydrogen bond is connected, interlamellar spacing is about 072nm, isomorphous substitution is there is not in kaolinic lattice, interlamination region electric charge balances substantially, causing in its two-dimensional layer can not Liquidity limit, in addition, due to the interaction of the hydrogen bond force between layer and Van der Waals force, make it have sizable interior poly-, thus connect between crystal layer closely, stable performance, the organic guest molecule of its intercalation has more challenge compared to the montmorillonite of intercalation montmorillonite group.
However, the small molecules of some strong polarity, as dimethyl sulfoxide (DMSO), Potassium ethanoate, methane amide, urea, hydrazine etc. successfully as presoma to other organic molecules as pyridinium chloride, amino alcohol and pyridine carboxylic acid carry out further intercalation, along with going deep into of research, some other small molecules and macromole, as propylene glycol, polyacrylamide, polyoxyethylene glycol, polystyrene etc. also can enter interlayer by the mode of carrying secretly or replace kaolinite organic molecule mixture small molecular, the intercalated compound be substituted is called presoma, methyl alcohol also can be used as the intermediate of intercalated compound, under extreme temperature condition, fixing guest molecule is inserted in the alkyl imidazole clay processed, demonstrate excellent stability.
In addition, ionic liquid is inserted kaolinite interlayer and forms nanostructure by scholar, be widely used in electrode modification, catalyzer and detect the aspects such as negatively charged ion. ionic liquid intercalation kaolinite has good thermostability, specific conductivity and optical property, but kaolinic preparation method is single for external ionic liquid intercalation, and the cycle is longer, technique is loaded down with trivial details, by improving in the present invention, simplify experiment flow, shorten the reaction times, good intercalation effect can be obtained simultaneously.
Summary of the invention
The object of the invention is exactly the defect in order to make up prior art, provides a kind of anti-oxidant natural rubber material and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of anti-oxidant natural rubber material, it is made up of the raw material of following weight parts:
Oxidation inhibitor DSTP1-2, natural rubber 100-140, kaolinite 20-30, dimethyl sulfoxide (DMSO) 400-500, methyl alcohol 900-1000, N-Methylimidazole 70-80, monobromethane 100-120, nano silicon oxide 4-6, vulcanizing agent MOCA1-1.6, dioctyl azelate 6-7, ferrous ammonium sulphate 2-3, anti-aging agent 6881-2, polybenzimidazole 0.7-1, medical stone powder 2-4.
A preparation method for described anti-oxidant natural rubber material, comprises the following steps:
(1) kaolinite is worn into fine powder, join in its weight 1.6-2 distilled water doubly, add dimethyl sulfoxide (DMSO), with magnetic stirrer 70-72 hour under room temperature, suction filtration, filter cake is after absolute ethanol washing, dry 20-24 hour at 60-65 DEG C, obtains methyl kaolinite mixture;
(2) in above-mentioned methyl kaolinite mixture, add above-mentioned methyl alcohol, room temperature condition lower magnetic force stirs 20-30 hour, obtains methyl alcohol kaolinite mixture;
(3) join in the thermostatic mixer of 60-65 DEG C by above-mentioned N-Methylimidazole, drip monobromethane, dropwise rear insulated and stirred 40-50 hour, discharging, with ethyl acetate washing 3-4 time, dry 20-24 hour in the baking oven of 70-75 DEG C, obtains bromine salt ion body;
(4) above-mentioned medical stone powder is calcined 1-2 hour at 600-700 DEG C, join after cooling in its weight 10-13 times deionized water, add ferrous ammonium sulphate, insulated and stirred 4-7 minute at 80-90 DEG C, obtain stone flour solution;
(5) above-mentioned polybenzimidazole is joined in 3-4 times of dehydrated alcohol, stir;
(6) join in bromine salt ion body by above-mentioned methyl alcohol kaolinite mixture, magnetic agitation 20-23 hour, centrifugal, joined in above-mentioned stone flour solution by the solid precipitation obtained, stir, suction filtration, at 50-60 DEG C, dry 20-22 hour, obtains intercalated compound;
(7) joined by nano silicon oxide in its weight 20-25 chloroform soln doubly, ultrasonic disperse 3-5 minute is liquid a;
(8) above-mentioned intercalated compound is joined in its weight 4-6 chloroform soln doubly, ultrasonic disperse 1.6-2 minute, mix with above-mentioned liquid a, the dehydrated alcohol of mixed system weight 4-6% is added under agitation condition, stir, add the alcoholic solution of above-mentioned polybenzimidazole, suction filtration, by filter cake dry 2-3 hour in the vacuum drying oven of 100-106 DEG C, obtain modified filler;
(9) mixed with natural rubber by above-mentioned modified filler, send in Banbury mixer, banburying 40-50s at 65-90 DEG C, adds each raw material except vulcanizing agent MOCA, mixing 10-12 minute, binder removal, is cooled to less than 50 DEG C, drops in mill, add each raw material of residue, thin-pass 3-5 time, to obtain final product.
Advantage of the present invention is:
Rubber product of the present invention has good resistance toheat:
Of the present invention by monobromethane process N-Methylimidazole, obtain bromine salt ion body, stronger hydrogen bond can be produced with kaolinic internal surface hydroxyl after intercalation, new H-bonding capability is considerably beyond hydrogen bond in original kaolinic layer, thus improve kaolinic resistance toheat, and then improve the resistance of finished-product material to persistent high fever;
Rubber product of the present invention has good anti-ultraviolet property:
The present invention is through bromine salt ion body intercalation kaolin stone, stronger hydrogen bond can be produced by surface hydroxyl within it, the quantum yield of its fluorescence and chemical reaction more than without position between intramolecular hydrogen bond and para-isomeride low, there iing the occasion internal conversion of intramolecular hydrogen bond than without fast more than 100 times of hydrogen bond, the UV energy of absorption can be transformed into heat energy by the effect of hydrogen bond to disperse, thus play the effect of protection elastomeric material;
Rubber of the present invention has good antioxidant property, long service life, good weatherability.
Embodiment
A kind of anti-oxidant natural rubber material, it is made up of the raw material of following weight parts:
Oxidation inhibitor DSTP1, natural rubber 100, kaolinite 20, dimethyl sulfoxide (DMSO) 400, methyl alcohol 900, N-Methylimidazole 70, monobromethane 100, nano silicon oxide 4, vulcanizing agent MOCA1, dioctyl azelate 6, ferrous ammonium sulphate 2, anti-aging agent 6881, polybenzimidazole 0.7, medical stone powder 2.
A preparation method for described anti-oxidant natural rubber material, comprises the following steps:
(1) kaolinite is worn into fine powder, join in the distilled water of its weight 1.6 times, add dimethyl sulfoxide (DMSO), use magnetic stirrer 70 hours, suction filtration under room temperature, filter cake is after absolute ethanol washing, and at 60 DEG C, drying 20 hours, obtains methyl kaolinite mixture;
(2) in above-mentioned methyl kaolinite mixture, add above-mentioned methyl alcohol, room temperature condition lower magnetic force stirs 20 hours, obtains methyl alcohol kaolinite mixture;
(3) join in the thermostatic mixer of 60 DEG C by above-mentioned N-Methylimidazole, drip monobromethane, dropwise rear insulated and stirred 40 hours, discharging, wash 3 times by ethyl acetate, in the baking oven of 70 DEG C, drying 20 hours, obtains bromine salt ion body;
(4) calcined 1 hour at 600 DEG C by above-mentioned medical stone powder, join after cooling in its weight 10 times of deionized waters, add ferrous ammonium sulphate, at 80 DEG C, insulated and stirred 4 minutes, obtains stone flour solution;
(5) above-mentioned polybenzimidazole is joined in 3 times of dehydrated alcohols, stir;
(6) join in bromine salt ion body by above-mentioned methyl alcohol kaolinite mixture, magnetic agitation 20 hours, centrifugal, joined in above-mentioned stone flour solution by the solid precipitation obtained, stir, suction filtration, at 50 DEG C, drying 20 hours, obtains intercalated compound;
(7) being joined by nano silicon oxide in the chloroform soln of its weight 20 times, ultrasonic disperse 3 minutes, is liquid a;
(8) above-mentioned intercalated compound is joined in the chloroform soln of its weight 4 times, ultrasonic disperse 1.6 minutes, mix with above-mentioned liquid a, the dehydrated alcohol of mixed system weight 4% is added under agitation condition, stir, add the alcoholic solution of above-mentioned polybenzimidazole, suction filtration, by filter cake in the vacuum drying oven of 100 DEG C dry 2 hours, obtain modified filler;
(9) mixed with natural rubber by above-mentioned modified filler, send in Banbury mixer, banburying 40s at 65 DEG C, adds each raw material except vulcanizing agent MOCA, mixing 10 minutes, binder removal, was cooled to less than 50 DEG C, dropped in mill, add each raw material of residue, thin-pass 3 times, to obtain final product.
Performance test:
Tensile strength: 14.5Mpa;
Elongation at break: 435.1%;
70 DEG C × 22h × 20% compression set: 16.2%;
70 DEG C × 70h air oven aging test:
Tensile strength at yield reduced rate: 5.2%, elongation at break reduced rate: 8.5%.
Claims (2)
1. an anti-oxidant natural rubber material, is characterized in that, it is made up of the raw material of following weight parts:
Oxidation inhibitor DSTP1-2, natural rubber 100-140, kaolinite 20-30, dimethyl sulfoxide (DMSO) 400-500, methyl alcohol 900-1000, N-Methylimidazole 70-80, monobromethane 100-120, nano silicon oxide 4-6, vulcanizing agent MOCA1-1.6, dioctyl azelate 6-7, ferrous ammonium sulphate 2-3, anti-aging agent 6881-2, polybenzimidazole 0.7-1, medical stone powder 2-4.
2. a preparation method for anti-oxidant natural rubber material as claimed in claim 1, is characterized in that, comprise the following steps:
(1) kaolinite is worn into fine powder, join in its weight 1.6-2 distilled water doubly, add dimethyl sulfoxide (DMSO), with magnetic stirrer 70-72 hour under room temperature, suction filtration, filter cake is after absolute ethanol washing, dry 20-24 hour at 60-65 DEG C, obtains methyl kaolinite mixture;
(2) in above-mentioned methyl kaolinite mixture, add above-mentioned methyl alcohol, room temperature condition lower magnetic force stirs 20-30 hour, obtains methyl alcohol kaolinite mixture;
(3) join in the thermostatic mixer of 60-65 DEG C by above-mentioned N-Methylimidazole, drip monobromethane, dropwise rear insulated and stirred 40-50 hour, discharging, with ethyl acetate washing 3-4 time, dry 20-24 hour in the baking oven of 70-75 DEG C, obtains bromine salt ion body;
(4) above-mentioned medical stone powder is calcined 1-2 hour at 600-700 DEG C, join after cooling in its weight 10-13 times deionized water, add ferrous ammonium sulphate, insulated and stirred 4-7 minute at 80-90 DEG C, obtain stone flour solution;
(5) above-mentioned polybenzimidazole is joined in 3-4 times of dehydrated alcohol, stir;
(6) join in bromine salt ion body by above-mentioned methyl alcohol kaolinite mixture, magnetic agitation 20-23 hour, centrifugal, joined in above-mentioned stone flour solution by the solid precipitation obtained, stir, suction filtration, at 50-60 DEG C, dry 20-22 hour, obtains intercalated compound;
(7) joined by nano silicon oxide in its weight 20-25 chloroform soln doubly, ultrasonic disperse 3-5 minute is liquid a;
(8) above-mentioned intercalated compound is joined in its weight 4-6 chloroform soln doubly, ultrasonic disperse 1.6-2 minute, mix with above-mentioned liquid a, the dehydrated alcohol of mixed system weight 4-6% is added under agitation condition, stir, add the alcoholic solution of above-mentioned polybenzimidazole, suction filtration, by filter cake dry 2-3 hour in the vacuum drying oven of 100-106 DEG C, obtain modified filler;
(9) mixed with natural rubber by above-mentioned modified filler, send in Banbury mixer, banburying 40-50s at 65-90 DEG C, adds each raw material except vulcanizing agent MOCA, mixing 10-12 minute, binder removal, is cooled to less than 50 DEG C, drops in mill, add each raw material of residue, thin-pass 3-5 time, to obtain final product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510952180.8A CN105461981A (en) | 2015-12-17 | 2015-12-17 | Oxidization-resistant natural rubber material and preparation method thereof |
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| CN201510952180.8A CN105461981A (en) | 2015-12-17 | 2015-12-17 | Oxidization-resistant natural rubber material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107266724A (en) * | 2017-07-24 | 2017-10-20 | 陈登辉 | A kind of preparation method of hard hollow rubber material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381488A (en) * | 2008-11-04 | 2009-03-11 | 中国矿业大学(北京) | Kaolin/rubber nano compound material with strengthening and obstructing dual property |
| CN103787348A (en) * | 2013-12-27 | 2014-05-14 | 中国地质大学（武汉） | Preparation method of kaolin/1-butyl-3-methyl bromide imidazole intercalated nanocomposite |
-
2015
- 2015-12-17 CN CN201510952180.8A patent/CN105461981A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381488A (en) * | 2008-11-04 | 2009-03-11 | 中国矿业大学(北京) | Kaolin/rubber nano compound material with strengthening and obstructing dual property |
| CN103787348A (en) * | 2013-12-27 | 2014-05-14 | 中国地质大学（武汉） | Preparation method of kaolin/1-butyl-3-methyl bromide imidazole intercalated nanocomposite |
Non-Patent Citations (1)
| Title |
|---|
| 杜小龙等: "烷基咪唑离子液体插层高岭石复合物的制备与表征", 《功能材料》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107266724A (en) * | 2017-07-24 | 2017-10-20 | 陈登辉 | A kind of preparation method of hard hollow rubber material |
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