CN119331358A - A white food-grade EPDM rubber hose and preparation method thereof - Google Patents
A white food-grade EPDM rubber hose and preparation method thereof Download PDFInfo
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- 229920002943 EPDM rubber Polymers 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 229920001971 elastomer Polymers 0.000 claims abstract description 45
- 239000005060 rubber Substances 0.000 claims abstract description 45
- 239000000463 material Substances 0.000 claims abstract description 29
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000006229 carbon black Substances 0.000 claims abstract description 23
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 18
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 18
- KQPYUDDGWXQXHS-UHFFFAOYSA-N juglone Chemical compound O=C1C=CC(=O)C2=C1C=CC=C2O KQPYUDDGWXQXHS-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 13
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 11
- 239000011593 sulfur Substances 0.000 claims abstract description 11
- 239000005662 Paraffin oil Substances 0.000 claims abstract description 10
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000292 calcium oxide Substances 0.000 claims abstract description 10
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 9
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 9
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000008117 stearic acid Substances 0.000 claims abstract description 9
- 238000007599 discharging Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000001125 extrusion Methods 0.000 claims description 20
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 12
- 239000004408 titanium dioxide Substances 0.000 claims description 9
- VTHOKNTVYKTUPI-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyltetrasulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCSSSSCCC[Si](OCC)(OCC)OCC VTHOKNTVYKTUPI-UHFFFAOYSA-N 0.000 claims description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 3
- 239000005977 Ethylene Substances 0.000 claims description 3
- JFNLZVQOOSMTJK-KNVOCYPGSA-N norbornene Chemical compound C1[C@@H]2CC[C@H]1C=C2 JFNLZVQOOSMTJK-KNVOCYPGSA-N 0.000 claims description 3
- FBBATURSCRIBHN-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyldisulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCSSCCC[Si](OCC)(OCC)OCC FBBATURSCRIBHN-UHFFFAOYSA-N 0.000 claims description 3
- 239000001993 wax Substances 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims 3
- 239000003292 glue Substances 0.000 claims 2
- WUFRAKOFLITOHU-UHFFFAOYSA-N [SiH4].C(CCCCCCCCCCCCCCCCC)(=O)O Chemical compound [SiH4].C(CCCCCCCCCCCCCCCCC)(=O)O WUFRAKOFLITOHU-UHFFFAOYSA-N 0.000 claims 1
- 238000004073 vulcanization Methods 0.000 abstract description 45
- 238000005520 cutting process Methods 0.000 abstract description 3
- 238000000465 moulding Methods 0.000 abstract description 3
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 abstract 1
- DCXXMTOCNZCJGO-UHFFFAOYSA-N Glycerol trioctadecanoate Natural products CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 abstract 1
- 239000002131 composite material Substances 0.000 abstract 1
- 239000001038 titanium pigment Substances 0.000 abstract 1
- 239000011787 zinc oxide Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 20
- 235000013305 food Nutrition 0.000 description 18
- 235000019241 carbon black Nutrition 0.000 description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 239000012153 distilled water Substances 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 11
- 238000004821 distillation Methods 0.000 description 10
- 238000013329 compounding Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 238000003801 milling Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 230000002209 hydrophobic effect Effects 0.000 description 6
- 238000011056 performance test Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 230000000704 physical effect Effects 0.000 description 4
- 238000004513 sizing Methods 0.000 description 4
- 229910002012 Aerosil® Inorganic materials 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 239000002390 adhesive tape Substances 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 229910021485 fumed silica Inorganic materials 0.000 description 2
- 229920004482 WACKER® Polymers 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229910002011 hydrophilic fumed silica Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/16—Ethene-propene or ethene-propene-diene copolymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The application relates to the technical field of ethylene propylene diene monomer rubber, in particular to a white food-grade ethylene propylene diene monomer rubber tube and a preparation method thereof. The EPDM rubber comprises EPDM rubber, white carbon black, kaolin, paraffin oil, zinc oxide powder, calcium oxide powder, 1-2 parts of stearin, a silane coupling agent, titanium pigment, sulfur and a comprehensive accelerator. The preparation method comprises the steps of mixing EDPM rubber, zinc oxide and stearic acid, heating and mixing, adding white carbon black, kaolin and the like for continuous mixing, standing, adding sulfur and the like for mixing to obtain a pre-mixed rubber material, opening the pre-mixed rubber material, turning over the rubber material, discharging the rubber sheet, cutting a hanging rod, cooling at room temperature for standby, and extruding and molding the rubber sheet at normal temperature to obtain the product. According to the application, kaolin is additionally introduced into the raw materials, so that the moisture absorption can be reduced, and the composite accelerator compounded by Altermix BGL-70, HANSUN EG M-80GE and 5-hydroxy-1, 4-naphthoquinone is adopted, so that the vulcanization efficiency can be greatly improved, the time is shortened, the vulcanization temperature range is widened, and the process is more stable and controllable.
Description
Technical Field
The application relates to the technical field of ethylene propylene diene monomer rubber, in particular to a white food-grade ethylene propylene diene monomer rubber tube and a preparation method thereof.
Background
Ethylene Propylene Diene Monomer (EPDM) as a general purpose rubber material with excellent performance and superior cost performance shows a wide application potential in numerous fields, especially in the food and medical industries where extremely high requirements on material safety and durability are required. In these sensitive and critical industries, the quality of EPDM articles is directly related to the safety and reliability of the product. However, microwave vulcanization, a vital step in the preparation of EPDM extruded tubes, presents a significant challenge for food grade EPDM materials.
Specifically, food grade EPDM white compounds contain various fillers, such as white carbon black and calcium carbonate, which have extremely strong hygroscopicity. Once the compound absorbs too much moisture, it can have a significant adverse effect on the subsequent vulcanization. The existence of moisture not only can cause bubbles in the vulcanization process, thereby influencing the appearance quality and the internal structure stability of the product, but also can reduce the vulcanization efficiency, so that the product is difficult to meet the established performance standard.
In addition, food grade EPDM white compounds are also very demanding in terms of the choice of vulcanization accelerators. Since vulcanization accelerators are directly related to vulcanization speed and the quality of the vulcanization product, it is necessary to select vulcanization accelerators which meet the vulcanization speed requirements without jeopardizing the safety of the product. However, in practical applications, such vulcanization accelerators tend to have limited options and it is difficult to fully meet the rapid vulcanization conditions required for microwave vulcanization.
Disclosure of Invention
In order to solve the problems, the application provides a white food-grade ethylene propylene diene monomer and a preparation method thereof, which aim to overcome the difficult problem of microwave vulcanization caused by the hygroscopicity of a filler and the selection limitation of a vulcanization accelerator in the preparation process and realize the efficient and rapid production of a food-grade extrusion pipe.
In a first aspect, the application provides a white food-grade ethylene propylene diene monomer rubber tube, which adopts the following technical scheme:
the raw materials for preparing the white food-grade ethylene propylene diene monomer rubber pipe comprise the following components in parts by weight:
100 parts of EPDM rubber
20-40 Parts of white carbon black
100-150 Parts of kaolin
Paraffin oil 10-30 parts
3-5 Parts of zinc oxide powder
10-15 Parts of calcium oxide powder
Stearic acid 1-2 parts
1-3 Parts of silane coupling agent
5-10 Parts of titanium dioxide
0.5 To 1.5 portions of sulfur
3-5 Parts of comprehensive accelerator.
By adopting the technical scheme, the method optimizes the selection and the proportion of raw materials, effectively solves the difficult problem of microwave vulcanization caused by the hygroscopicity of the filler and the selection limit of the vulcanization accelerator in the preparation process, realizes the efficient and rapid production of the food-grade extrusion pipe, and ensures the safety and the reliability of the product.
Optionally, the raw materials for preparing the white food-grade ethylene propylene diene monomer rubber tube comprise the following components in parts by weight:
100 parts of EPDM rubber
30-40 Parts of white carbon black
130-150 Parts of kaolin
20-30 Parts of paraffin oil
3-5 Parts of zinc oxide powder
10-15 Parts of calcium oxide powder
Stearic acid 1-2 parts
1-3 Parts of silane coupling agent
5-8 Parts of titanium dioxide
0.5 To 1.5 portions of sulfur
3-5 Parts of comprehensive accelerator.
Further, optionally, the raw materials for preparing the white food-grade ethylene propylene diene monomer rubber tube are prepared from the following components in parts by weight:
100 parts of EPDM rubber
30 Parts of white carbon black
130 Parts of kaolin
20 Parts of paraffin oil
5 Parts of zinc oxide powder
10 Parts of calcium oxide powder
Stearic acid 1 part
3 Parts of silane coupling agent
Titanium dioxide 8 parts
0.5 Part of sulfur
5 Parts of comprehensive accelerator.
By adopting the technical scheme, the optimized preparation of the white food-grade ethylene propylene diene monomer rubber tube can be realized by precisely controlling the weight parts of the components, the performance, the safety and the production efficiency of the product are improved, and the requirements of the food and medical industry on high-quality rubber products are met.
Further optionally, the comprehensive promoter is a mixture prepared by compounding Altermix BGL-70, HANSUN EG, 6M-80GE and 5-hydroxy-1, 4-naphthoquinone according to the mass percent of 43% to 56% to 1%.
By adopting the technical scheme, the mixture prepared by compounding Altermix BGL-70, HANSUN EG6M-80GE and 5-hydroxy-1, 4-naphthoquinone according to a specific mass percentage is used as a comprehensive accelerator, so that the vulcanization process is optimized, the performance and the production efficiency of the product are improved, the safety and the reliability of the product are ensured, the compound composition has unique advantages and characteristics, and an efficient, environment-friendly and reliable solution is provided for the preparation of the white food-grade ethylene propylene diene monomer rubber tube;
the three components generate remarkable synergistic effect after being compounded, altermix BGL-70 and HANSUN EG M-80GE are used as main vulcanization accelerators, and respectively have different vulcanization active points and action mechanisms, and the compounding of the three components can widen the vulcanization temperature range, improve the vulcanization speed and reduce side effects in the vulcanization process.
The 5-hydroxy-1, 4-naphthoquinone has the key regulation function although the proportion is smaller, and can finely adjust the process of the vulcanization reaction, so that the vulcanization process is more stable, the phenomenon of oversulfiding or undersulfidation is avoided, and the cross-linking structure in the vulcanized product is more compact due to more sufficient and uniform vulcanization reaction, thereby reducing the generation of internal defects and bubbles, and further improving the overall quality of the product.
The compound composition can obviously improve the vulcanization efficiency, shorten the vulcanization time, quickly reach the required vulcanization temperature under the microwave vulcanization condition, and maintain the stable vulcanization rate, thereby accelerating the production flow and improving the production efficiency.
Further optionally, the silane coupling agent is selected from one or more of bis (triethoxysilylpropyl) disulfide, bis- (γ -triethoxysilylpropyl) tetrasulfide wax.
In a specific embodiment, the bis (triethoxysilylpropyl) disulfide can be one of SG-Si996, SG-Si 998, SG-Si 1589, the bis- (gamma-triethoxysilylpropyl) tetrasulfide can be KH-845-4 or SG-Si 1289, and the bis- (gamma-triethoxysilylpropyl) tetrasulfide wax can be Rsi-E.
Further alternatively, the EPDM rubber has an ethylene content of 70.0 to 70.5wt% and a norbornene content of 0.5 to 5.0wt%.
In a second aspect, the preparation method of the white food-grade ethylene propylene diene monomer rubber tube provided by the application adopts the following technical scheme:
a preparation method of a white food-grade ethylene propylene diene monomer rubber tube comprises the following preparation steps:
S1, banburying, namely adding EDPM rubber, zinc oxide powder and stearic acid, heating and mixing for 1-2min at a constant speed of 10-20 ℃ per min, adding white carbon black, kaolin, paraffin oil, silane coupling agent and titanium dioxide, continuously mixing for 5-8min until the temperature reaches 110-120 ℃, discharging rubber to obtain a crude rubber material, standing the crude rubber material at room temperature for 24h, mixing the rubber material with sulfur, a comprehensive accelerator and calcium oxide powder, mixing for 2-3min until the temperature reaches 110-120 ℃, and discharging rubber to obtain a pre-refined rubber material;
s2, open milling, namely open milling the pre-mixed rubber material at the speed of 30-40rpm/min, and turning rubber for 3-7min and then discharging tablets;
s3, preforming, namely cutting the film obtained after the film is discharged from the S2 into strips, hanging the strips, and naturally cooling the strips to below 25 ℃ at room temperature for later use;
And S4, extrusion molding, namely extruding and molding the normal-temperature adhesive tape obtained after cooling in the step S3 to obtain a product.
Further alternatively, the specific process of extrusion molding is extrusion molding by using a cold feed extruder, wherein the screw temperature is 50-60 ℃, the plasticizing temperature is 65-75 ℃, the head temperature is 75-85 ℃, and the extrusion speed is 15-25m/min.
By adopting the technical scheme, in the banburying step, the heating rate, mixing time and temperature are strictly controlled, so that the raw materials are fully mixed and uniformly dispersed, the problem of local overheating or insufficient mixing is avoided, meanwhile, the standing time of the crude sizing material is carefully set to ensure the full curing and stability of the crude sizing material, and in the open milling step, the open milling rate and the sizing material turning time are controlled, the fluidity and the plasticity of the sizing material are further optimized, and a good foundation is laid for the subsequent forming step;
In the extrusion molding step, a cold feed extruder is used, key parameters such as screw temperature, plasticizing temperature, machine head temperature, extrusion speed and the like are strictly controlled, smooth extrusion and molding of the rubber material are ensured, the production efficiency and the product quality are improved, the extrusion temperature is precisely controlled, the problem of insufficient degradation or crosslinking of the rubber material due to overhigh temperature in the extrusion process is avoided, and meanwhile, the dimensional stability and the surface quality of the rubber tube are ensured by reasonable extrusion speed.
The whole preparation process from banburying, open milling, preforming to extrusion molding is carefully designed and optimized, so that the smoothness and high efficiency of the production flow are ensured, the production efficiency is improved, and the production cost and the energy consumption are reduced.
In summary, the application has the following beneficial technical effects:
1. According to the application, kaolin is introduced into the raw materials for preparing the white food-grade ethylene propylene diene monomer rubber tube, and compared with the traditional white carbon black and calcium carbonate, the kaolin has lower hygroscopicity, so that the moisture absorbed by the rubber material in the preparation and storage processes is reduced, bubbles are avoided in the vulcanization process, and the appearance quality and the internal structural stability of the product are ensured;
2. The comprehensive accelerator in the raw materials for preparing the white food-grade ethylene propylene diene monomer rubber tube is prepared by compounding Altermix BGL-70, HANSUN EG, 6M-80GE and 5-hydroxy-1, 4-naphthoquinone according to a specific proportion, can obviously improve the vulcanization efficiency, shortens the vulcanization time, and widens the vulcanization temperature range after compounding, so that the vulcanization process is more stable and controllable.
Detailed Description
The present application will be described in further detail with reference to examples.
Performance test
The rubber tubes prepared in examples and comparative examples were tested for physical properties according to standard GB/T3512-2014, ISO 188:2011, and the test items were hardness (Shore A), tensile strength, elongation at break (%);
The rubber tubes prepared in examples and comparative examples were subjected to distilled water tests according to standard FDA 21 CFR 177.2600, and the residual amounts of 7 hours before distillation and 2 hours after distillation (residual amounts refer to the contents of distilled water and other unnecessary impurities) were measured, respectively.
Examples 1 to 4
A white food grade ethylene propylene diene monomer rubber tube comprises the following components and the amounts (kg) of the components are shown in the table.
TABLE 1 raw material conditions for preparing white food grade ethylene propylene diene monomer rubber tubes in examples 1-4
The white carbon black is AEROSIL R202 hydrophobic fumed silica, the kaolin is basf Metamax high-activity metakaolin, the silane coupling agent is SG-Si 1589 and Rsi-E, the proportion is 40-60%, the comprehensive accelerator is a mixture prepared by compounding Altermix BGL-70%, HANSUN EG M-80GE and 5-hydroxy-1, 4-naphthoquinone according to the mass percentage of 43-56-1%, the ethylene content of the EPDM rubber is 70.0-70.5wt% and the norbornene content of 0.5-5.0wt%;
the white food-grade ethylene propylene diene monomer rubber tube is prepared by the following preparation steps:
S1, banburying, namely adding a predetermined amount of EDPM rubber, zinc oxide powder and stearic acid, heating and mixing for 1min at a constant rate of 15 ℃ per min, adding white carbon black, kaolin, paraffin oil, a silane coupling agent and titanium dioxide, continuously mixing for 5min until the temperature reaches 115 ℃, discharging the rubber to obtain a crude rubber material, standing the crude rubber material at room temperature for 24h, mixing the rubber material with sulfur, a comprehensive accelerator and calcium oxide powder, mixing for 3min until the temperature reaches 120 ℃, and discharging the rubber to obtain a pre-refined rubber material;
S2, open milling, namely open milling the pre-mixed rubber material at the speed of 35rpm/min, and turning rubber for 5min and then discharging tablets;
S3, preforming, namely cutting the film obtained after the film is discharged from the S2 into strips, hanging the strips, and naturally cooling the strips to below 25 ℃ at room temperature for later use;
And S4, extrusion molding, namely using a cold feed extruder to extrude the normal-temperature adhesive tape obtained after cooling in the step S3, wherein the temperature of a screw is 55 ℃, the plasticizing temperature is 65 ℃, the extrusion temperature is 70 ℃, the temperature of a machine head is 80 ℃, the extrusion speed is 20m/min, so as to obtain a crude rubber pipe product, and then performing microwave vulcanization on the crude rubber pipe product through multiple sections of hot air, so as to obtain the white food-grade ethylene propylene diene monomer rubber pipe.
Examples 5 to 8
The only difference from example 2 is the white food grade ethylene propylene diene monomer hose, the amounts of the components being different, the components and their amounts (kg) being shown in the following table.
TABLE 2 raw materials for the preparation of white food grade ethylene propylene diene monomer rubber tubes of example 1 and examples 5-8
Each performance test was performed on the white food-grade ethylene propylene diene monomer rubber tubes prepared in examples 1 to 8 described above with reference to the aforementioned performance test, and the test results are shown in the following table.
TABLE 3 detection results of the performance of white food-grade ethylene propylene diene monomer rubber tubes of examples 1-8
As can be seen from the test data of the table, the rubber hoses prepared in the examples 1-8 have good physical properties and can meet the daily use requirements, but in the FDA distilled water test, the examples have different performances, wherein the residual quantity of 7 hours before distillation is within 1.6-22.4mg/in 2, only the example 6 fails the test requirement, the residual quantity of 2 hours after distillation is within 0.33-5.4mg/in 2, and only the example 2 passes the test requirement;
It follows that embodiment 2 may be the preferred embodiment among the above-described embodiments.
Examples 9 to 11
The white food grade ethylene propylene diene monomer rubber tube is different from the embodiment 2 only in that,
The white carbon black used in the preparation is different in use condition, and the specific conditions are shown in the table below.
TABLE 4 use cases of raw material white carbon black used for preparing white food grade ethylene propylene diene monomer rubber tubes of examples 9-11
Example 12
The white food grade ethylene propylene diene monomer rubber tube is different from the embodiment 2 only in that,
The kaolin used for preparation is Acti-Min RG.
Examples 13 to 16
The only difference from example 2 is the use of the synthetic accelerator used in the preparation.
TABLE 5 comprehensive promoter use cases in raw materials for preparing white food grade ethylene propylene diene monomer rubber tubes of examples 13-16
Comparative examples 1 to 3
The only difference from example 2 is the white food grade ethylene propylene diene monomer hose, which is prepared from different raw materials, in particular as shown in the following table.
TABLE 6 raw material conditions for preparing white food grade ethylene propylene diene monomer rubber tubes in comparative examples 1-3
The white food-grade ethylene propylene diene rubber hoses prepared in examples 9 to 16 and comparative examples 1 to 3 were subjected to various performance tests with reference to the performance test tests described above, and the test results are shown in the following table.
TABLE 7 results of the performance test of white food-grade ethylene propylene diene monomer rubber tubes of examples 1-8
As can be seen from the above table, the white food grade ethylene propylene diene monomer rubber tube prepared in examples 9-11 has a residual amount of 4.2-30.4mg/in 2 before distillation and a residual amount of 0.54-7.7mg/in 2 after distillation in FDA distilled water test;
In the index which cannot pass the FDA distilled water test in the embodiment 9, as AEROSIL20 hydrophilic fumed silica is adopted as the white carbon black in the embodiment 9, the surface of the white carbon black contains hydrophilic groups such as hydroxyl groups and the like, and the white carbon black is more likely to interact with water molecules;
In example 11, a mixture of two hydrophobic white carbon blacks was used in place of AEROSIL R202 in equal amounts, and there was still a gap in FDA distilled water testing compared to the test results of example 2, although the two hydrophobic white carbon blacks used alone performed well, their mixture may not have the same performance advantage, which may be a compromise or imbalance in performance caused by the interaction of the different types of hydrophobic white carbon blacks in the mixture.
In example 10, WACKER hydrophobic white carbon black HDK H20 was used to replace AEROSIL R202 hydrophobic fumed silica in equal amount, but the test result was still inferior to the white food grade ethylene propylene diene monomer rubber tube prepared in example 2.
In example 12, the 7 hour residue before distillation was 22.7mg/in 2 and the 2 hour residue after distillation was 5.6mg/in 2, an index that could not be calibrated by FDA distilled water test, which is probably that the high activity metakaolin of Pasteur Metamax had unique functional properties that make it perform well in rubber hoses, whereas the Acti-Min RG kaolin, while also being a good quality kaolin, may have properties that differ from Metamax, resulting in failure to achieve equivalent performance after replacement.
In examples 13-16, the residual amount of 7 hours before distillation is 5.4-9.8mg/in 2, the residual amount of 2 hours after distillation is 0.78-1.43mg/in 2, and examples 15 and 16 pass the index calibrated by the FDA distilled water test, when the comprehensive promoter is a mixture prepared by compounding Altermix BGL-70 and HANSUN EG M-80GE according to 50% by mass percent or a mixture prepared by compounding Actmix-75 EG3M-75GEF140, altermix BGL-70 and HANSUN EG M-80GE according to 20% by mass percent and 40% by mass percent, as shown by the performance detection results of examples 13 and 14, the index calibrated by the FDA distilled water test is not passed;
however, when 5-hydroxy-1, 4-naphthoquinone was included in the integrated accelerator, as shown in examples 13 and 14, there was a significant effect on the vulcanization efficiency and whether it could pass the FDA distilled water test, and the properties of the white food grade ethylene propylene diene monomer rubber tube prepared only when the integrated accelerator was a mixture of Altermix BGL-70, HANSUN EG M-80GE and 5-hydroxy-1, 4-naphthoquinone compounded at a mass percentage of 43% to 56% to 1% were optimal.
In addition, in comparative examples 1 to 3, an attempt was made to prepare white food-grade ethylene propylene diene monomer tubes using multiple rubber components instead of single EPDM rubber, and from the test results, although they exhibited good physical properties, they failed to reach the index calibrated by the FDA distilled water test, and there was a large gap from the calibration index.
Therefore, the raw material components are specially selected, so that the rubber material can reach the vulcanization temperature more quickly in the microwave vulcanization process, the vulcanization efficiency is improved, meanwhile, the vulcanization process is more stable and controllable due to the reduction of the adverse effect of moisture on the vulcanization process, the production efficiency and quality of the product are further improved, and all the components are mutually cooperated and matched, so that the prepared white food-grade ethylene propylene diene monomer rubber tube has excellent physical properties and chemical stability.
The above description is provided for the purpose of enabling those skilled in the art to make modifications and obvious technical teaching of the present embodiment without any creative contribution, as required, after reading the present specification, and is protected by patent law within the scope of the claims of the present application.
Claims (7)
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