CN103421129B - A kind of liquid phase production technique of natural rubber - Google Patents
A kind of liquid phase production technique of natural rubber Download PDFInfo
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Abstract
The invention provides a kind of liquid phase production technique of natural rubber.This production technique comprises the following steps: alkyl polyoxyethylene ether, promotor, zinc oxide, stearic acid, sulphur, anti-aging agent, dispersion agent, casein, water are mixed, obtain rubber ingredients; Or, alkyl polyoxyethylene ether, promotor, zinc oxide, stearic acid, sulphur, anti-aging agent, dispersion agent, carbon black or white carbon black, emulsifying agent, oily substance, casein, water are mixed, obtain rubber ingredients; Rubber ingredients mixed with water and carries out ball milling, then mix with latex and stir, obtaining latex mixed solution; After stirring, with microwave, Gel Treatment is carried out to the irradiation of latex mixed solution; Jel product is carried out granulation, dry, obtain liquid phase nanotube-natural rubber.The liquid phase production technique of natural rubber provided by the invention does not add acid gel agent, and product physicals is than improving a lot by the product performance of gelifying agent output.
Description
Technical field
The present invention relates to a kind of liquid phase production technique of natural rubber, belong to technical field of rubber preparation.
Background technology
At present, the complete processing of natural rubber mainly utilizes lower concentration formic acid to be prepared by gel, crepe, broken directly granulation and oven dry, also need repeatedly to plasticate with mixing when making rubber unvulcanizate, the mooney viscosity of the rubber unvulcanizate made so obviously reduces, sulfuration torque change is little, time of scorch slightly shortens, and vulcanization rate is accelerated; The hardness of cross-linked rubber and stress at definite elongation increase, tensile strength, elongation rate of tensile failure, rebound value, tear strength and break tension set and reduce, and flexible resistance and heat-resistant air aging property decline, and wear resisting property change is little; Number of times of plasticating is more, and the performance variation of rubber unvulcanizate and cross-linked rubber is larger, can not meet the needs of high-quality abrasive rubber.And repeatedly fragmentation, granulation and long oven dry not only waste manpower and time, also rubber molecular chain can be made to be interrupted by mechanical shear stress or destroy, rubber monomer (polyisoprene) polymerization degree is reduced, namely molecular weight reduces, directly affects the plasticity initial value of finished product, mooney viscosity and hardness like this, destroy the distinctive snappiness of rubber itself and physical and mechanical properties.
Therefore, developing a kind of novel rubber preparation technology is one of this area problem demanding prompt solution.
Summary of the invention
For solving the problems of the technologies described above, the object of the present invention is to provide a kind of liquid phase production technique of natural rubber, this liquid phase production technique can be cost-saving on the basis of improving rubber physical performance, enhance productivity, and effectively can avoid the appearance because of the situation making product performance generation difference with difference that is mixing and processing temperature of plasticating.
For achieving the above object, the invention provides a kind of liquid phase production technique of natural rubber, it comprises the following steps:
Alkyl polyoxyethylene ether 0.1-2 weight part, promotor 0.5-1.5 weight part, zinc oxide 1.5-10 weight part, stearic acid 0.1-5 weight part, sulphur 0.5-2 weight part, anti-aging agent 0.8-1.5 weight part, dispersion agent 0.1-2 weight part, casein 0.2-1 weight part, water 5-20 weight part are mixed, obtains rubber ingredients; Or, alkyl polyoxyethylene ether 0.1-2 weight part, promotor 0.5-1.5 weight part, zinc oxide 1.5-10 weight part, stearic acid 0.1-5 weight part, sulphur 0.5-2 weight part, anti-aging agent 0.8-1.5 weight part, dispersion agent 0.1-2 weight part, carbon black or white carbon black 5-120 weight part, emulsifying agent 0.5-5 weight part, oily substance 1-40 weight part, casein 0.2-1 weight part, water 5-150 weight part are mixed, obtains rubber ingredients;
By rubber ingredients with water by 1:(0.5-10) mass ratio mix and carry out ball milling, then with latex according to (1-20): the mass ratio of 100 mixes and stirs, and obtains latex mixed solution;
After stirring, with microwave, irradiation is carried out to latex mixed solution and carry out Gel Treatment;
Jel product is carried out granulation, then carries out microwave drying, obtain natural rubber.
In the liquid phase production technique of above-mentioned natural rubber, first the Synergist S-421 95 of the vulcanization of rubber makes emulsion, and then join in natural rubber latex, relative to pulverous Synergist S-421 95 being joined the technical scheme of going in solid rubber, adopt technical scheme of the present invention to avoid dust pollution.In the present invention, the latex adopted can be now conventional latex, such as revertex, undressed natural rubber latex etc.
In the liquid phase production technique of above-mentioned natural rubber, preferably, mass ratio when rubber ingredients mix with water is 1:1, and mixing the mass ratio being after ball milling with latex is 3:100.
In the liquid phase production technique of above-mentioned natural rubber, preferably, the promotor adopted is N-cyclohexyl-2-benzothiazole sulfonamide, tetramethyl-dithio thiuram, N-(oxidation diethylidene)-2-[4-morpholinodithio sulphenamide and 2, the combination of one or more in 2 '-dibenzothiazyl disulfide etc.
In the liquid phase production technique of above-mentioned natural rubber, preferably, the anti-aging agent adopted be 4,4 '-bis-a, a ' combination of one or more in-dimethyl benzyl pentanoic, N-Phenyl beta naphthylamine, N-phenyl-N`-cyclohexyl Ursol D etc.
In the liquid phase production technique of above-mentioned natural rubber, preferably, the dispersion agent adopted is sodium metnylene bis-naphthalene sulfonate salt
In the liquid phase production technique of above-mentioned natural rubber, preferably, the emulsifying agent adopted is the combination of one or more in OP-10, " two, tributyl phenol Soxylat A 25-7 ", styroyl phenol polyoxyethylene polyoxypropylene ether etc.
In the production technique of above-mentioned natural rubber, preferably, the oily substance adopted comprises the combination of one or more in No. 40 machine oil (i.e. existing N68 oil), Viscotrol C, epoxy soybean oil, lanolin, naphthenic oil and aromatic hydrocarbons wet goods.
In the liquid phase production technique of above-mentioned natural rubber, the microwave irradiation of Gel Treatment can adopt tunnel type micro wave stove to carry out, and preferably, in Gel Treatment process, the output rating of the microwave adopted is 55kW, and the temperature of Gel Treatment is not higher than 75 DEG C.
In the liquid phase production technique of above-mentioned natural rubber, preferably, the speed of ball milling is 100-400 rev/min, and Ball-milling Time is 4-10 hour.The diameter of the Synergist S-421 95 after ball milling can reach Nano grade, and Synergist S-421 95 can be made to be distributed to more equably in latex.
In the liquid phase production technique of above-mentioned natural rubber, preferably, after granulation, the output rating of the microwave that microwave drying adopts is 120kW, and dry temperature is no more than 85 DEG C.This drying treatment also can adopt tunnel type micro wave stove to carry out.In the production process of current rubber, main employing is that the method heating and ventilate carries out bake drying, the present invention can save time and the energy by adopting microwave method to carry out drying, temperature generally will be remained on 100 DEG C and continue 5-8 hour ability and dry by usual drying method, and adopts the mode of microwave drying provided by the present invention just can dry within the time of 0.5-1 hour.Rubber can cause the situation of thermal ageing to occur at high operating temperatures, and time longer thermal ageing situation is more obvious, and microwave drying can avoid the appearance of this situation well.
In above-mentioned liquid phase production technique, preferably, the speed of stirring is 60-200 rev/min, and the time of stirring is 1-2 hour.
According to specific embodiment of the invention scheme, preferably, above-mentioned liquid phase production technique can comprise following concrete steps:
By alkyl polyoxyethylene ether (paregal O) 0.1-2 weight part, N-cyclohexyl-2-benzothiazole sulfonamide (accelerant CZ) 0.5-1.5 weight part, zinc oxide 1.5-10 weight part, stearic acid 0.1-5 weight part, sulphur 0.5-2 weight part, 4,4 '-bis-a, a '-dimethyl benzyl pentanoic (anti-aging agent KY-405) 0.8-1.5 weight part, sodium metnylene bis-naphthalene sulfonate salt (dispersion agent NF) 0.1-2 weight part, casein 0.2-1 weight part, to mix, obtain rubber ingredients, or, by alkyl polyoxyethylene ether (paregal O) 0.1-2 weight part, N-cyclohexyl-2-benzothiazole sulfonamide (accelerant CZ) 0.5-1.5 weight part, zinc oxide 1.5-10 weight part, stearic acid 0.1-5 weight part, sulphur 0.5-2 weight part, 4, 4 '-bis-a, a '-dimethyl benzyl pentanoic (anti-aging agent KY-405) 0.8-1.5 weight part, sodium metnylene bis-naphthalene sulfonate salt (dispersion agent NF) 0.1-2 weight part, carbon black or white carbon black 5-120 weight part, OP-10(emulsifying agent) 0.5-5 weight part, No. 40 machine oil 1-40 weight parts, casein 0.2-1 weight part mixes, obtain rubber ingredients,
By rubber ingredients with water by 1:(0.5-10) mass ratio of (preferred 1:1) mixes and carries out ball milling, the speed of ball milling is 100-400 rev/min, Ball-milling Time is 4-10 hour, after ball milling with latex according to the preferred 3:100 of (1-20): 100() mass ratio mix and stir, the speed stirred is 60-200 rev/min, the time of stirring is 1-2 hour, obtains latex mixed solution;
After stirring, make latex mixed solution by microwave device (such as tunnel type micro wave stove), utilize microwave to carry out irradiation to latex mixed solution and carry out Gel Treatment, wherein, the output rating of microwave is 55kW, and the temperature of Gel Treatment is not higher than 75 DEG C;
Jel product is being carried out granulation (grain diameter that granulation obtains is at about 1cm) after cooling water washing, then microwave drying (tunnel type micro wave stove can be adopted to carry out) is carried out, obtain liquid phase nanotube-natural rubber, wherein, the output rating of microwave drying is 120kW, and dry temperature is not higher than 85 DEG C.
Present invention also offers a kind of natural rubber, it adopts above-mentioned liquid phase production technique to produce.
According to specific embodiment of the invention scheme, preferably, the tensile strength of above-mentioned natural rubber is 26-30MPa, and elongation at break is 780-830%, DIN wet-milling amount (rotary drum-type abrasion machine method) is 0.045-0.022g.
The liquid phase production technique of natural rubber provided by the invention does not add acid gel agent, the product performance of product physicals ratio gelifying agent output are improved a lot, carry out Gel Treatment by microwave and save a large amount of manpowers and time, wall scroll production line gel content per hour can reach 2 tons, and improve 20% by the rubber unvulcanizate that the rubber unvulcanizate physicals that the method is produced is produced than traditional technology, be the once innovation in rubber processing field.
Accompanying drawing explanation
The schematic flow sheet of the liquid phase production technique of the natural rubber that Fig. 1 adopts for embodiment 1.
Embodiment
In order to there be understanding clearly to technical characteristic of the present invention, object and beneficial effect, existing following detailed description is carried out to technical scheme of the present invention, but can not be interpreted as to of the present invention can the restriction of practical range.
Embodiment 1
The present embodiment provides a kind of liquid phase production technique of natural rubber, and as shown in Figure 1, this liquid phase production technique comprises the following steps its flow process:
Get CZ, 1.5g, ZnO, 5g, stearic acid, 1g, anti-aging agent KY-405,1g, sulphur, 1.5g, paregal O, 1g, dispersion agent NF, 1g, casein 0.2g, deionized water 11g mixes, and obtains rubber ingredients;
Rubber ingredients are put into ball mill 1 ball milling 10 hours, the speed of ball milling is 400 revs/min; Then, the revertex being 60% by rubber ingredients and 300g concentration mixes in stirrer 2, stirs obtain latex mixed solution in 2 hours with the speed of 180 revs/min;
Then the tunnel type micro wave stove 3 latex mixed solution being put into microwave output power 1KW carries out microwave irradiation to carry out Gel Treatment, forms gel after 4min;
Utilize and tear a machine 4 and the rubber after gel is made particle and after preliminary hydro-extraction, putting into microwave output power is the drying treatment that the tunnel type micro wave stove 5 of 1KW carries out 6min, obtains liquid phase nanotube-natural rubber, then directly carries out sulfuration;
Vulcanization adopts compression molding instrument to carry out mold pressing, and concrete curing parameter is 120 DEG C of sulfurations 40 minutes under the pressure of 8MPa.
Comparative example 1
This comparative example provides a kind of preparation technology of rubber, and it comprises the following steps:
Get CZ, 1.5g, ZnO, 5g, stearic acid, 1g, anti-aging agent KY-405,1g, sulphur, 1.5g mix and make Synergist S-421 95;
Get natural rubber 100g to plasticate on two roller mixing rolls after 5-10 time roll spacing is relaxed to 2mm, by above-mentioned join 5 mixture add carry out in the natural rubber of plasticating mixing, thin-pass after each 5 times of left and right cutter, roll spacing is adjusted to the thick triangle bag 5-6 of beating of 1mm, again roll spacing is adjusted to 2-3mm thick, clot slice is parked and is carried out sulfuration in 4 hours later;
Vulcanization adopts compression molding instrument to carry out mold pressing, and concrete curing parameter is 120 DEG C of sulfurations 40 minutes under the pressure of 8MPa.The performance comparison of the rubber after sulfuration is as shown in table 1.
Table 1
| Performance | Standard | Embodiment 1 | Comparative example 1 |
| Hardness | ISO48-1979 | 38IRHD | 38IRHD |
| Tensile strength | ISO37-1977 | 28MPa | 24MPa |
| Elongation at break | ISO37-1977 | 810% | 730% |
| Tension set | ISO2285-1981 | 8% | 12% |
| Tear strength | ISO37-1979 | 41N/mm | 36N/mm |
| Rebound resilience | BS.903：PART A8 | 76% | 72% |
| Proportion | 0.98 | 0.98 | |
| Temperature range | -40 DEG C to 70 DEG C | -40 DEG C to 70 DEG C | |
| Wear-resistant index (wetting) | The DIN53516 (wet type state) improved | 0.028 | 0.035 |
Illustrated by the Data Comparison in table 1, the every physical index of rubber that the preparation technology provided by embodiment 1 is produced all is better than the rubber that conventional machining process is produced.
DIN abrasion are a kind of rotary drum-type abrasion machine methods, general is all dry grinding, and the abrasive rubber of high elongation rate provided by the present invention, high strength is because elasticity is relatively good, hardness is not high, so can not dry grinding be adopted, mainly wet-milling, the DIN53516 (wet type state) of above-mentioned improvement refers to when carrying out wear-resisting preparation test, face arranges a water bath under the rollers, segment cylinder is immersed in the water, thus the state of a wet type is maintained when testing, simulate the environment for use of rubber item and test its wear(ing)value.
Embodiment 2
The present embodiment provides a kind of liquid phase production technique of natural rubber, and as shown in Figure 1, this liquid phase production technique comprises the following steps its flow process:
Get CZ, 1.5g, ZnO, 5g, stearic acid, 1g, anti-aging agent KY-405,1g, sulphur, 1.5g, paregal O, 1g, white carbon black, 15g, No. 40 machine oil, 5g, emulsifier op-10,1g, casein, 0.3g, dispersion agent NF, 2g, deionized water 34g mixes, and obtains rubber ingredients;
Rubber ingredients are put into ball mill 1 ball milling 10 hours, the speed of ball milling is 400 revs/min; Then, the revertex being 60% by rubber ingredients and 300g concentration mixes in stirrer 2, stirs obtain latex mixed solution in 2 hours with the speed of 180 revs/min;
Then the tunnel type micro wave stove 3 latex mixed solution being put into microwave output power 1KW carries out microwave irradiation to carry out Gel Treatment, forms gel after 4min;
Utilize and tear a machine 4 and the rubber after gel is made particle and after preliminary hydro-extraction, putting into microwave output power is the drying treatment that the tunnel type micro wave stove 5 of 1KW carries out 6min, obtains liquid phase nanotube-natural rubber, then directly carries out sulfuration;
Vulcanization adopts compression molding instrument to carry out mold pressing, and concrete curing parameter is 143 DEG C of sulfurations 25 minutes under the pressure of 8MPa.
Comparative example 2
This comparative example provides a kind of preparation technology of rubber, and it comprises the following steps:
Get CZ, 1.5g, ZnO, 5g, stearic acid, 1g, anti-aging agent KY-405,1g, sulphur, 1.5g, white carbon black, 15g, No. 40 machine oil, 5g mix and make Synergist S-421 95;
Get natural rubber 100g to plasticate on two roller mixing rolls after 5-10 time roll spacing is relaxed to 2mm, above-mentioned Synergist S-421 95 is added carry out in the natural rubber of plasticating mixing, thin-pass after each 5 times of left and right cutter, roll spacing is adjusted to the thick triangle bag 5-6 of beating of 1mm, again roll spacing is adjusted to 2-3mm thick, clot slice is parked and is carried out sulfuration in 4 hours later;
Vulcanization adopts compression molding instrument to carry out mold pressing, and concrete curing parameter is 143 DEG C of sulfurations 25 minutes under the pressure of 8MPa.The performance comparison of the rubber after sulfuration is as shown in table 2.
Table 2
| Performance | Standard | Embodiment 2 | Comparative example 2 |
| Hardness | ISO48-1979 | 42IRHD | 43IRHD |
| Tensile strength | ISO37-1977 | 30MPa | 26MPa |
| Elongation at break | ISO37-1977 | 750% | 690% |
| Tension set | ISO2285-1981 | 8% | 12% |
| Tear strength | ISO37-1979 | 64N/mm | 52N/mm |
| Rebound resilience | BS.903：PART A8 | 65% | 62% |
| Proportion | 0.99 | 0.99 | |
| Temperature range | -40 DEG C to 70 DEG C | -40 DEG C to 70 DEG C | |
| Wear-resistant index (wetting) | The DIN53516 (wet type state) improved | 0.039 | 0.042 |
Illustrated by the Data Comparison in table 2, the every physical index of rubber that the preparation technology provided by embodiment 2 is produced all is better than the rubber that conventional machining process is produced.
Claims (10)
1. a liquid phase production technique for natural rubber, it comprises the following steps:
Alkyl polyoxyethylene ether 0.1-2 weight part, promotor 0.5-1.5 weight part, zinc oxide 1.5-10 weight part, stearic acid 0.1-5 weight part, sulphur 0.5-2 weight part, anti-aging agent 0.8-1.5 weight part, dispersion agent 0.1-2 weight part, casein 0.2-1 weight part, water 5-20 weight part are mixed, obtains rubber ingredients; Or, alkyl polyoxyethylene ether 0.1-2 weight part, promotor 0.5-1.5 weight part, zinc oxide 1.5-10 weight part, stearic acid 0.1-5 weight part, sulphur 0.5-2 weight part, anti-aging agent 0.8-1.5 weight part, dispersion agent 0.1-2 weight part, carbon black or white carbon black 5-120 weight part, emulsifying agent 0.5-5 weight part, oily substance 1-40 weight part, casein 0.2-1 weight part, water 5-150 weight part are mixed, obtains rubber ingredients;
By rubber ingredients with water by 1:(0.5-10) mass ratio mix and carry out ball milling, then with latex according to (1-20): the mass ratio of 100 mixes and stirs, obtain latex mixed solution, wherein, described latex is revertex and/or undressed natural rubber latex;
After stirring, with microwave, irradiation is carried out to latex mixed solution and carry out Gel Treatment;
Jel product is carried out granulation, then carries out microwave drying, obtain described natural rubber.
2. liquid phase production technique according to claim 1, wherein, described promotor comprises N-cyclohexyl-2-benzothiazole sulfonamide, tetramethyl-dithio thiuram, N-(oxidation diethylidene)-2-[4-morpholinodithio sulphenamide and 2, the combination of one or more in 2 '-dibenzothiazyl disulfide.
3. liquid phase production technique according to claim 1, wherein, described anti-aging agent comprises 4,4 '-bis-a, a '-dimethyl benzyl pentanoic, N-Phenyl beta naphthylamine, the combination of one or more in N-phenyl-N`-cyclohexyl Ursol D.
4. liquid phase production technique according to claim 1, wherein, described dispersion agent is sodium metnylene bis-naphthalene sulfonate salt.
5. liquid phase production technique according to claim 1, wherein, described emulsifying agent is OP-10, two, tributyl phenol Soxylat A 25-7, the combination of one or more in styroyl phenol polyoxyethylene polyoxypropylene ether.
6. liquid phase production technique according to claim 1, wherein, described oily substance comprises the combination of one or more in No. 40 machine oil, Viscotrol C, epoxy soybean oil, lanolin, naphthenic oil and aromatic hydrocarbon oil.
7. liquid phase production technique according to claim 1, wherein, in Gel Treatment process, the temperature of Gel Treatment is not higher than 75 DEG C.
8. liquid phase production technique according to claim 1, wherein, the temperature of described microwave drying is no more than 85 DEG C.
9. the liquid phase production technique according to any one of claim 1-8, it comprises the following steps:
By alkyl polyoxyethylene ether 0.1-2 weight part, N-cyclohexyl-2-benzothiazole sulfonamide 0.5-1.5 weight part, zinc oxide 1.5-10 weight part, stearic acid 0.1-5 weight part, sulphur 0.5-2 weight part, 4,4 '-bis-a, a '-dimethyl benzyl pentanoic 0.8-1.5 weight part, sodium metnylene bis-naphthalene sulfonate salt 0.1-2 weight part, carbon black 5-120 weight part, OP-10 0.5-5 weight part, No. 40 machine oil 1-40 weight parts, casein 0.2-1 weight parts mix, and obtain rubber ingredients;
Rubber ingredients and water are mixed by the mass ratio of 1:1 and carries out ball milling, the speed of ball milling is 100-400 rev/min, Ball-milling Time is 4-10 hour, mix according to the mass ratio of 3:100 with latex after ball milling and stir, the speed stirred is 60-200 rev/min, and the time of stirring is 1-2 hour, obtains latex mixed solution, wherein, described latex is revertex and/or undressed natural rubber latex;
After stirring, make latex mixed solution by microwave device, utilize microwave to carry out irradiation to latex mixed solution and carry out Gel Treatment, wherein, the temperature of Gel Treatment is not higher than 75 DEG C;
Jel product is being carried out granulation after cooling water washing, is then carrying out microwave drying, obtaining described liquid phase nanotube-natural rubber, wherein, dry temperature is not higher than 85 DEG C.
10. a natural rubber, it is that the liquid phase production technique of the natural rubber adopted described in any one of claim 1-9 is produced; The tensile strength of this natural rubber is 26-30MPa, and elongation at break is 780-830%, DIN wet-milling amount is 0.045-0.022g.
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