CN113698706A - Low-creep waterstop material and preparation method thereof - Google Patents
Low-creep waterstop material and preparation method thereof Download PDFInfo
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- CN113698706A CN113698706A CN202110878221.9A CN202110878221A CN113698706A CN 113698706 A CN113698706 A CN 113698706A CN 202110878221 A CN202110878221 A CN 202110878221A CN 113698706 A CN113698706 A CN 113698706A
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- 239000000463 material Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 229920002943 EPDM rubber Polymers 0.000 claims abstract description 43
- 239000012763 reinforcing filler Substances 0.000 claims abstract description 29
- 239000002270 dispersing agent Substances 0.000 claims abstract description 22
- 239000013543 active substance Substances 0.000 claims abstract description 21
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 20
- 239000004014 plasticizer Substances 0.000 claims abstract description 19
- BOXSVZNGTQTENJ-UHFFFAOYSA-L zinc dibutyldithiocarbamate Chemical compound [Zn+2].CCCCN(C([S-])=S)CCCC.CCCCN(C([S-])=S)CCCC BOXSVZNGTQTENJ-UHFFFAOYSA-L 0.000 claims abstract description 18
- DUBNHZYBDBBJHD-UHFFFAOYSA-L ziram Chemical compound [Zn+2].CN(C)C([S-])=S.CN(C)C([S-])=S DUBNHZYBDBBJHD-UHFFFAOYSA-L 0.000 claims abstract description 18
- 238000001125 extrusion Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims description 42
- 239000000203 mixture Substances 0.000 claims description 40
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 claims description 22
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 20
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 229920001971 elastomer Polymers 0.000 claims description 14
- 235000021355 Stearic acid Nutrition 0.000 claims description 13
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 13
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 13
- 239000008117 stearic acid Substances 0.000 claims description 13
- 239000002202 Polyethylene glycol Substances 0.000 claims description 12
- 229920001223 polyethylene glycol Polymers 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 11
- CPGFMWPQXUXQRX-UHFFFAOYSA-N 3-amino-3-(4-fluorophenyl)propanoic acid Chemical compound OC(=O)CC(N)C1=CC=C(F)C=C1 CPGFMWPQXUXQRX-UHFFFAOYSA-N 0.000 claims description 10
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 10
- 238000004073 vulcanization Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 239000011787 zinc oxide Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 239000011593 sulfur Substances 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 3
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 3
- 239000000194 fatty acid Substances 0.000 claims description 3
- 229930195729 fatty acid Natural products 0.000 claims description 3
- -1 fatty acid ester Chemical class 0.000 claims description 3
- 229960002447 thiram Drugs 0.000 claims description 3
- 239000005662 Paraffin oil Substances 0.000 claims description 2
- 239000012190 activator Substances 0.000 claims description 2
- WITDFSFZHZYQHB-UHFFFAOYSA-N dibenzylcarbamothioylsulfanyl n,n-dibenzylcarbamodithioate Chemical compound C=1C=CC=CC=1CN(CC=1C=CC=CC=1)C(=S)SSC(=S)N(CC=1C=CC=CC=1)CC1=CC=CC=C1 WITDFSFZHZYQHB-UHFFFAOYSA-N 0.000 claims description 2
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 claims description 2
- 239000004971 Cross linker Substances 0.000 claims 1
- 239000006185 dispersion Substances 0.000 claims 1
- DEQZTKGFXNUBJL-UHFFFAOYSA-N n-(1,3-benzothiazol-2-ylsulfanyl)cyclohexanamine Chemical compound C1CCCCC1NSC1=NC2=CC=CC=C2S1 DEQZTKGFXNUBJL-UHFFFAOYSA-N 0.000 claims 1
- 239000000454 talc Substances 0.000 claims 1
- 229910052623 talc Inorganic materials 0.000 claims 1
- 238000000748 compression moulding Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 6
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 4
- 230000000630 rising effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 239000012936 vulcanization activator Substances 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- DKVNPHBNOWQYFE-UHFFFAOYSA-N carbamodithioic acid Chemical compound NC(S)=S DKVNPHBNOWQYFE-UHFFFAOYSA-N 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000000109 continuous material Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000012990 dithiocarbamate Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- STSDHUBQQWBRBH-UHFFFAOYSA-N n-cyclohexyl-1,3-benzothiazole-2-sulfonamide Chemical compound N=1C2=CC=CC=C2SC=1S(=O)(=O)NC1CCCCC1 STSDHUBQQWBRBH-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- NRINZBKAERVHFW-UHFFFAOYSA-L zinc;dicarbamate Chemical class [Zn+2].NC([O-])=O.NC([O-])=O NRINZBKAERVHFW-UHFFFAOYSA-L 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—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D29/00—Producing belts or bands
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a low-creep waterstop material and a preparation method thereof, wherein the material is prepared from the following raw materials: 100 parts of EPDM, 4-10 parts of active agent, 3-15 parts of dispersant, 80-150 parts of reinforcing filler, 40-80 parts of softening plasticizer, 0.5-1.5 parts of zinc dimethyldithiocarbamate, 1-2.5 parts of zinc dibutyldithiocarbamate and 4-8 parts of cross-linking agent; the preparation method is extrusion molding. The waterstop material has excellent low creep property, the efficiency can be improved by 3-4 times compared with compression molding by improving the preparation method, the appearance is smooth, no connecting mark exists, and the length of a product can be cut according to requirements.
Description
Technical Field
The invention relates to the field of waterstop materials, in particular to a low-creep waterstop material and a preparation method thereof.
Background
The waterproof and anti-seepage principle of the structural joint in underground concrete projects such as subways, tunnels, culverts, dams and the like in the prior art is to make up for the change of the structural joint by depending on the elasticity of a water stop belt, so that the waterproof and anti-seepage effects are achieved. Because the rubber material has creep property, the high-creep waterstop causes leakage phenomenon along with the change of time, and in order to improve the safety of engineering, a low-creep waterstop material needs to be developed. Meanwhile, most of the existing water stops are molded into lines, and the molded water stops have the problems of uneven appearance, obvious connecting marks, low production efficiency, incapability of meeting the requirement of any length and the like, so that an improved preparation method is urgently needed.
Disclosure of Invention
In order to solve the technical problems, the invention provides a low-creep water stop belt material, which takes ethylene propylene diene monomer as a main component, and the water stop belt material has low creep property by improving the component distribution ratio, can keep good elasticity in long-term use, and thus improves the safety of an engineering structure. The specific technical scheme is that the low-creep water stop belt material comprises the following components in parts by weight: the composition is characterized by comprising the following raw materials in parts by mass: 100 parts of EPDM, 4-10 parts of activator, 3-15 parts of dispersant, 80-150 parts of reinforcing filler, 40-80 parts of softening plasticizer, 0.5-1.5 parts of zinc dimethyldithiocarbamate, 1-2.5 parts of zinc dibutyldithiocarbamate and 4-8 parts of cross-linking agent.
The EPDM is ethylene propylene diene monomer.
The active agent is at least one of zinc oxide and stearic acid.
The reinforcing filler is at least one of carbon black N550, N660, talcum powder and superfine calcium carbonate.
The softening plasticizer is paraffin oil.
The dispersant is at least one of polyethylene glycol and fatty acid ester.
The cross-linking agent is at least one of sulfur, 2-mercaptobenzothiazole, dipentamethylenethiuram tetrasulfide, tetrabenzylthiuram disulfide, tetramethylthiuram disulfide and N-cyclohexyl-2-benzothiazole sulfonamide.
The invention finds that although the zinc dimethyldithiocarbamate and the zinc dibutyldithiocarbamate are both dithiocarbamate vulcanization activators, the two zinc carbamates are compounded according to a certain proportion and then used, so that a synergistic effect can be achieved, the creep property of the EPDM can be further reduced, and the creep resistance effect of the EPDM is better than that of the EPDM which is singly used.
Meanwhile, the invention also provides an extrusion molding method of the low-creep waterstop material, which can obtain a continuous material with a smooth appearance, and the method specifically comprises the following steps:
the first step is as follows: firstly, putting ethylene propylene diene monomer rubber into an internal mixer to break rubber for 60-120 seconds;
the second step is that: adding an active agent and a dispersing agent into ethylene propylene diene monomer rubber in mixing, and mixing for 60-120 seconds to obtain a mixture I;
the third step: adding 2/3 reinforcing filler into the mixture prepared in the step two, mixing for 120-180 seconds, adding softener and the rest reinforcing filler, discharging rubber when the temperature of an internal mixing chamber reaches 130 +/-5 ℃, and then cooling the lower piece of an open mill to room temperature to form a mixture two;
the fourth step: carrying out two-stage mixing on the mixture II prepared in the step 3, adding a vulcanizing agent in the mixing process, after the mixing is finished, removing rubber, cooling the lower piece to the room temperature, and standing for at least 16 hours to form a mixture III;
the fifth step: and cutting the mixture III into a film with the width of 30-40 cm, filling the film into an extruder, forming a product shape through an extrusion mouth, and vulcanizing through a high-temperature microwave production line to obtain the water stop product.
In the second step, after the active agent and the dispersing agent are added, the mixture is continuously mixed to 40-50 ℃ and/or the mixing time is maintained within 100-120 seconds;
in the third step, 2/3 reinforcing filler is added, the mixture is mixed for 180 seconds, then softener and the rest reinforcing filler are added, the mixture is pressurized and mixed to 105 +/-5 ℃, the internal mixer carries out plug rising for one time, the mixture is turned over for one time, then the mixture is pressurized and mixed again to 130 +/-5 ℃, and finally the sheet is taken down and cooled by the open mill;
in the fourth step, the mixture II is mixed in an internal mixer for 110-120 seconds, and the mixture II is pressurized and internally mixed to 80-90 ℃ after the vulcanizing agent is added, and the mixing is completed;
in the fifth step, the temperature of the extruder is controlled to be 35-50 ℃, the temperature of the high-temperature microwave vulcanization is controlled to be 190-210 ℃, and the running speed of the microwave vulcanizing machine is 3-4 m/min.
The invention has the beneficial effects that:
by adding zinc dimethyldithiocarbamate and zinc dibutyldithiocarbamate into the EPDM rubber material according to a certain proportion, the two materials have synergistic effect as vulcanization activators, so that a vulcanization system can be activated, the two materials can act with other vulcanizing agents to form a complex with good solubility in rubber, an accelerator and sulfur are activated, the vulcanization efficiency is improved, the vulcanization crosslinking density is improved, the low-temperature creep property of a product is further improved, and the safety of a structure is enhanced.
The waterstop product adopts extrusion moulding, vulcanizes through high temperature microwave production line, for compression molding, extrusion moulding production process is continuous, production efficiency is high, the rejection rate is low, and the outward appearance is leveled, does not have the connection trace, and the length of product can be tailor as required.
Detailed Description
The invention will be further illustrated with reference to specific examples, but the scope of the invention is not limited thereto.
Example 1:
the low-creep waterstop material is prepared from the following raw materials in parts by weight: 100 parts of EPDM (ethylene-propylene-diene monomer), 7 parts of an active agent (5 parts of zinc oxide and 2 parts of stearic acid), 5 parts of a dispersing agent (polyethylene glycol), 120 parts of a reinforcing filler (carbon black N550), 65 parts of a softening plasticizer, 5 parts of a cross-linking agent (sulfur), 0.9 part of zinc dimethyldithiocarbamate and 1.8 parts of zinc dibutyldithiocarbamate.
The water stop is prepared by the following method:
the first step is as follows: firstly, 100 parts of ethylene propylene diene monomer rubber is put into an internal mixer to break rubber for 100 seconds;
the second step is that: adding an active agent (5 parts of zinc oxide and 2 parts of stearic acid) and a dispersing agent into ethylene propylene diene monomer rubber in mixing, and mixing for 80 seconds to obtain a first mixture;
the third step: adding 2/3 reinforcing filler into the mixture prepared in the step two in the mixing process, mixing for 160 seconds, adding softening plasticizer and the rest reinforcing filler, pressurizing and internally mixing to 105 ℃, carrying out once plug rising by an internal mixer to turn the mixing once, then pressurizing and internally mixing again to 130 ℃, and finally cooling the lower sheet of the open mill to room temperature to form a mixture two;
the fourth step: carrying out two-stage mixing on the mixture II prepared in the step III, mixing for 120 seconds by using an internal mixer, adding a crosslinking agent, zinc dimethyldithiocarbamate and zinc dibutyldithiocarbamate in the mixing process, pressurizing and mixing the mixture II to 80 ℃ after adding a vulcanization crosslinking agent, finishing mixing, discharging rubber, cooling to room temperature, standing for at least 16 hours, and forming a mixture III;
the fifth step: and cutting the mixture III into a rubber sheet with the width of 40cm, filling the rubber sheet into an extruder, forming a product shape through an extrusion mouth, and vulcanizing through a high-temperature microwave production line to obtain a water stop product. The temperature of the extruder is controlled at 50 ℃, the temperature of the high-temperature microwave vulcanization is controlled at 190 ℃, and the running speed of the microwave vulcanizing machine is 3 m/min.
Example 2:
the low-creep waterstop material comprises the following materials in parts by weight: 100 parts of EPDM (ethylene-propylene-diene monomer), 6 parts of an active agent (6 parts of zinc oxide), 10 parts of a dispersing agent (10 parts of polyethylene glycol), 100 parts of a reinforcing filler (50 parts of N660 and 50 parts of talcum powder), 65 parts of a softening plasticizer, 5 parts of a cross-linking agent (2-mercaptobenzothiazole), 1.5 parts of zinc dimethyldithiocarbamate and 1 part of zinc dibutyldithiocarbamate.
The water stop is prepared by the following method:
the first step is as follows: firstly, 100 parts of ethylene propylene diene monomer rubber is put into an internal mixer to break the rubber for 120 seconds;
the second step is that: adding an active agent and a dispersing agent into ethylene propylene diene monomer rubber in mixing, and then continuously mixing to 50 ℃ to obtain a mixture I;
the third step: adding 2/3 reinforcing filler into the mixture prepared in the step two in the mixing process, mixing for 180 seconds, adding softening plasticizer and the rest reinforcing filler, pressurizing and internally mixing to 105 ℃, carrying out once plug rising by an internal mixer to turn the mixing once, then pressurizing and internally mixing again to 130 ℃, and finally cooling the lower sheet of the open mill to room temperature to form a mixture two;
the fourth step: carrying out two-stage mixing on the mixture II prepared in the step 3, mixing for 110 seconds by using an internal mixer, adding a crosslinking agent, zinc dimethyldithiocarbamate and zinc dibutyldithiocarbamate in the mixing process, pressurizing and mixing the mixture II to 90 ℃ after adding a vulcanization crosslinking agent, finishing mixing, discharging rubber, cooling to room temperature, standing for at least 16 hours, and forming a mixture III;
the fifth step: and cutting the mixture III into a film with the width of 30cm, filling the film into an extruder, forming a product shape through an extrusion mouth, and vulcanizing through a high-temperature microwave production line to obtain the water stop product. The temperature of the extruder is controlled at 40 ℃, the temperature of the high-temperature microwave vulcanization is controlled at 200 ℃, and the running speed of the microwave vulcanizing machine is 4 m/min.
Example 3:
the low-creep waterstop material comprises the following materials in parts by weight: 100 parts of EPDM (ethylene-propylene-diene monomer), 5 parts of an active agent (3 parts of zinc oxide and 2 parts of stearic acid), 7 parts of a dispersing agent (7 parts of polyethylene glycol), 100 parts of a reinforcing filler (50 parts of N660 and 50 parts of talcum powder), 70 parts of a softening plasticizer, 5 parts of a crosslinking agent (2 parts of 2-mercaptobenzothiazole and 3 parts of dipentamethylenethiuram tetrasulfide), 1.0 part of zinc dimethyldithiocarbamate and 2.0 parts of zinc dibutyldithiocarbamate.
The preparation method was the same as in example 1.
Example 4:
the low-creep waterstop material comprises the following materials in parts by weight: 100 parts of EPDM (ethylene-propylene-diene monomer), 8 parts of an active agent (8 parts of stearic acid), 10 parts of a dispersing agent (10 parts of polyethylene glycol), 100 parts of a reinforcing filler (50 parts of N660 and 50 parts of superfine calcium carbonate), 70 parts of a softening plasticizer, 5 parts of a crosslinking agent (2 parts of 2-mercaptobenzothiazole and 3 parts of dipentamethylenethiuram tetrasulfide), 0.7 part of zinc dimethyldithiocarbamate and 1.8 parts of zinc dibutyldithiocarbamate.
The preparation method was the same as in example 1.
Example 5:
the low-creep waterstop material comprises the following materials in parts by weight: 100 parts of EPDM (ethylene-propylene-diene monomer), 10 parts of an active agent (7 parts of zinc oxide and 3 parts of stearic acid), 10 parts of a dispersing agent (10 parts of polyethylene glycol), 120 parts of a reinforcing filler (80 parts of N660 and 40 parts of superfine calcium carbonate), 70 parts of a softening plasticizer, 5 parts of a crosslinking agent (5 parts of dipentamethylenethiuram tetrasulfide), 0.8 part of zinc dimethyldithiocarbamate and 2.5 parts of zinc dibutyldithiocarbamate.
The preparation method was the same as in example 1.
Example 6:
the low-creep waterstop material comprises the following materials in parts by weight: 100 parts of EPDM (ethylene-propylene-diene monomer), 4 parts of an active agent (4 parts of stearic acid), 5 parts of a dispersing agent (5 parts of polyethylene glycol), 80 parts of a reinforcing filler (80 parts of superfine calcium carbonate), 70 parts of a softening plasticizer, 5 parts of a crosslinking agent (2 parts of 2-mercaptobenzothiazole and 3 parts of dipentamethylenethiuram tetrasulfide), 0.9 part of zinc dimethyldithiocarbamate and 1.5 parts of zinc dibutyldithiocarbamate.
The preparation method was the same as in example 2.
Example 7:
the low-creep waterstop material comprises the following materials in parts by weight: 100 parts of EPDM (ethylene-propylene-diene monomer), 8 parts of an active agent (4 parts of zinc oxide and 4 parts of stearic acid), 10 parts of a dispersing agent (10 parts of polyethylene glycol), 100 parts of a reinforcing filler (50 parts of talcum powder and 50 parts of superfine calcium carbonate), 50 parts of a softening plasticizer, 8 parts of a crosslinking agent (5 parts of 2-mercaptobenzothiazole and 3-tetramethyl thiuram disulfide), 1.5 parts of zinc dimethyldithiocarbamate and 1.8 parts of zinc dibutyldithiocarbamate.
The preparation method was the same as in example 2.
Example 8:
the low-creep waterstop material comprises the following materials in parts by weight: 100 parts of EPDM (ethylene-propylene-diene monomer), 10 parts of an active agent (10 parts of stearic acid), 8 parts of a dispersing agent (8 parts of fatty acid ester), 100 parts of a reinforcing filler (50 parts of N660 and 50 parts of superfine calcium carbonate), 70 parts of a softening plasticizer, 5 parts of a crosslinking agent (2 parts of 2-mercaptobenzothiazole and 3 parts of dipentamethylenethiuram tetrasulfide), 0.5 part of zinc dimethyldithiocarbamate and 1 part of zinc dibutyldithiocarbamate.
The preparation method was the same as in example 2.
Comparative example 1:
the low-creep waterstop material comprises the following materials in parts by weight: 100 parts of EPDM (ethylene-propylene-diene monomer), 8 parts of an active agent (8 parts of stearic acid), 10 parts of a dispersing agent (10 parts of polyethylene glycol), 100 parts of a reinforcing filler (50 parts of N660 and 50 parts of superfine calcium carbonate), 70 parts of a softening plasticizer, 5 parts of a crosslinking agent (2 parts of 2-mercaptobenzothiazole and 3 parts of dipentamethylenethiuram tetrasulfide) and 3 parts of zinc dimethyldithiocarbamate.
The preparation method was the same as in example 2.
Comparative example 2:
the low-creep waterstop material comprises the following materials in parts by weight: 100 parts of EPDM (ethylene-propylene-diene monomer), 8 parts of an active agent (8 parts of stearic acid), 10 parts of a dispersing agent (10 parts of polyethylene glycol), 100 parts of a reinforcing filler (50 parts of N660 and 50 parts of superfine calcium carbonate), 70 parts of a softening plasticizer, 5 parts of a crosslinking agent (2 parts of 2-mercaptobenzothiazole and 3 parts of dipentamethylenethiuram tetrasulfide) and 3.5 parts of zinc dibutyl dithiocarbamate.
The preparation method was the same as in example 2.
Comparative example 3:
the low-creep waterstop material comprises the following materials in parts by weight: 100 parts of EPDM (ethylene-propylene-diene monomer), 8 parts of an active agent (8 parts of stearic acid), 10 parts of a dispersing agent (10 parts of polyethylene glycol), 100 parts of a reinforcing filler (50 parts of N660 and 50 parts of superfine calcium carbonate), 70 parts of a softening plasticizer, 5 parts of a crosslinking agent (2 parts of 2-mercaptobenzothiazole and 3 parts of dipentamethylenethiuram tetrasulfide), 0.3 part of zinc dimethyldithiocarbamate and 0.5 part of zinc dibutyldithiocarbamate.
The preparation method was the same as in example 2.
The physical and mechanical property testing experiments and related data of the above examples 1-8 and comparative examples 1-3 of the present invention are shown in table 1, and the testing equipment: a servo control computer tension tester AI-7000M, a 401A type aging test box, a UTM5105 electronic universal tester and the like.
TABLE 1 results of physical Properties
As can be seen from Table 1, the tensile strength and the elongation at break of the water stop material of the invention are equivalent to or slightly lower than those of the water stop material of the comparative example, but the performance meets the standard requirement, but the compression set (low-temperature creep performance) is more superior than that of the water stop material of the comparative example, and the pressure-variable performance is far lower than that of the standard requirement.
The production efficiency of the extrusion molding waterstop is (180-240) m/h, and the production efficiency of the compression molding waterstop is (50-60) m/h, so that the efficiency can be improved by 3-4 times by changing the production mode, the extrusion molding appearance is smooth and free of connecting marks, the extrusion molding is continuous production, and the length of a product can be cut according to requirements.
Claims (12)
1. The low-creep waterstop material is characterized by comprising the following raw materials in parts by mass: 100 parts of EPDM, 4-10 parts of an active agent, 3-15 parts of a dispersing agent, 80-150 parts of a reinforcing filler, 40-80 parts of a softening plasticizer, 0.5-1.5 parts of zinc dimethyldithiocarbamate, 1-2.5 parts of zinc dibutyldithiocarbamate and 4-8 parts of a cross-linking agent, wherein the EPDM is ethylene propylene diene monomer.
2. The low creep waterstop material of claim 1, wherein the active agent is at least one of zinc oxide and stearic acid.
3. The low creep waterstop material of claim 2, wherein the reinforcing filler is at least one of carbon black N550, N660, talc, ultrafine calcium carbonate.
4. The low creep waterstop material of claim 3, wherein the softening plasticizer is paraffin oil.
5. The low creep waterstop material of claim 4, wherein the dispersant is at least one of polyethylene glycol and fatty acid ester.
6. The low creep waterstop material of claim 5, wherein the crosslinker is one or more of sulfur, 2-mercaptobenzothiazole, dipentamethylenethiuram tetrasulfide, tetrabenzylthiuram disulfide, tetramethylthiuram disulfide, N-cyclohexyl-2-benzothiazolesulfenamide.
7. The low-creep waterstop material according to any one of claims 1 to 6, wherein the raw material components comprise the following materials in parts by mass: 100 parts of EPDM, 7 parts of an active agent, 5 parts of a dispersion aid, 120 parts of a reinforcing filler, 65 parts of a softening plasticizer, 5 parts of a cross-linking agent, 0.9 part of zinc dimethyldithiocarbamate and 1.8 parts of zinc dibutyldithiocarbamate.
8. A method for preparing a low creep waterstop material according to any one of claims 1 to 7, characterized by comprising the following steps:
the first step is as follows: firstly, putting ethylene propylene diene monomer rubber into an internal mixer to break rubber for 60-120 seconds;
the second step is that: adding an active agent and a dispersing agent into ethylene propylene diene monomer rubber in mixing, and mixing for 60-120 seconds to obtain a mixture I;
the third step: adding 2/3 reinforcing filler into the mixture prepared in the step two, mixing for 120-180 seconds, adding softener and the rest reinforcing filler, discharging rubber when the temperature of an internal mixing chamber reaches 130 +/-5 ℃, and then cooling the lower piece of an open mill to room temperature to form a mixture two;
the fourth step: carrying out two-stage mixing on the mixture II prepared in the step 3, adding a vulcanizing agent in the mixing process, after the mixing is finished, removing rubber, cooling the lower piece to the room temperature, and standing for at least 16 hours to form the mixture II;
the fifth step: and cutting the mixture III into a film with the width of 30-40 cm, filling the film into an extruder, forming a product shape through an extrusion mouth, and vulcanizing through a high-temperature microwave production line to obtain the water stop product.
9. The method as claimed in claim 8, wherein in step two, the mixing is continued to 40-50 ℃ after the activator and the dispersant are added and/or the mixing time is maintained within 120 seconds of 100-.
10. The method for preparing a low-creep waterstop material as claimed in claim 9, wherein in the third step, 2/3 reinforcing filler is added, the mixture is mixed for 120-180 seconds, then softener and the rest reinforcing filler are added, the mixture is pressurized and mixed to 105 ± 5 ℃, the internal mixer is used for one plug lifting, the mixture is turned over once, then the mixture is pressurized and mixed again to 130 ± 5 ℃, and finally the lower sheet of the open mill is cooled.
11. The method for preparing a low-creep waterstop material as claimed in claim 10, wherein in the fourth step, the second mixture is mixed in an internal mixer for 110-120 seconds, and the second mixture is pressurized and mixed to 80-90 ℃ after the vulcanizing agent is added.
12. The method for preparing a low-creep waterstop material as claimed in claim 11, wherein in the fifth step, the temperature of the extruder is controlled to be 35-50 ℃, the temperature of the high-temperature microwave vulcanization is controlled to be 190 ℃ and 210 ℃, and the running speed of the microwave vulcanization machine is 3-4 m/min.
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| CN116376177A (en) * | 2023-03-31 | 2023-07-04 | 马鞍山宏力橡胶制品有限公司 | Microwave heating continuous vulcanization extrusion type rubber water stop and preparation method thereof |
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| CN107573600A (en) * | 2017-09-06 | 2018-01-12 | 北京化工大学 | A kind of railway tunnel special (purpose) rubber water stop rubber and its preparation technology |
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