CN114753152A - Titanate modified polypropylene fiber, preparation method and application thereof, heat-shrinkage-resistant sealing ring and preparation method thereof - Google Patents

Titanate modified polypropylene fiber, preparation method and application thereof, heat-shrinkage-resistant sealing ring and preparation method thereof Download PDF

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Publication number
CN114753152A
CN114753152A CN202210400973.9A CN202210400973A CN114753152A CN 114753152 A CN114753152 A CN 114753152A CN 202210400973 A CN202210400973 A CN 202210400973A CN 114753152 A CN114753152 A CN 114753152A
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parts
sealing ring
polypropylene fiber
rubber
titanate
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Inventor
宋增胜
任晓龙
孟令彦
马丽霞
张雨
苏金龙
宋金环
侯敏
苏俊英
闫婷婷
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Hebei Xinerte Rubber And Plastic Sealing Co ltd
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Hebei Xinerte Rubber And Plastic Sealing Co ltd
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Priority to CN202210400973.9A priority Critical patent/CN114753152A/en
Publication of CN114753152A publication Critical patent/CN114753152A/en
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
    • D06M13/503—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms without bond between a carbon atom and a metal or a boron, silicon, selenium or tellurium atom
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08L27/18—Homopolymers or copolymers or tetrafluoroethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
    • C08L2205/16—Fibres; Fibrils
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Sealing Material Composition (AREA)

Abstract

The invention provides a titanate modified polypropylene fiber, a preparation method and application thereof, a heat-shrinkable sealing ring and a preparation method thereof, and belongs to the technical field of sealing rings. According to the invention, the fluoroether rubber and the polyacrylate rubber are adopted as main materials, and the fluoroether rubber and the polyacrylate rubber have excellent high temperature resistance and aging resistance, so that the sealing ring has good high temperature resistance, and the sealing ring can still have good mechanical properties after being subjected to high temperature treatment; the sodium gluconate can improve the dimensional stability of the sealing ring; the titanate modified polypropylene fiber is used for improving the dimensional stability of the sealing ring and improving the shrinkage resistance of the sealing ring; the double-end vinyl silicone oil is used for improving the toughness of rubber and improving the sealing performance of the sealing ring; the polyallylamine hydrochloride can improve the mechanical stability of the sealing ring, so that the sealing ring has excellent anti-shrinkage performance. Experimental results show that the heat-resistant and oil-resistant sealing ring has excellent anti-shrinkage performance, mechanical performance and other performances.

Description

Titanate modified polypropylene fiber, preparation method and application thereof, heat-shrinkage-resistant sealing ring and preparation method thereof
The application is a divisional application with application date of 2019, 12 and 29, application number of 201911386801.5 and invention name of 'a heat-shrinkable sealing ring and a preparation method thereof'.
Technical Field
The invention belongs to the field of sealing rings, and particularly relates to a titanate modified polypropylene fiber, a preparation method and application thereof, a heat-shrinkable sealing ring and a preparation method thereof.
Background
The sealing element generally comprises a movable ring, a static ring and a sealing ring; wherein the sealing ring plays an essential role in the sealing effect of the sealing element. The sealing ring is applied to various industries and is fixed in the gap to form elastic separation, so that the sealing ring plays a role in separation and sealing. The seal ring generally satisfies the following conditions: the product is rich in elasticity and resilience; suitable mechanical strength including tensile strength, elongation, tear strength, and the like; the material is stable, is not easy to swell in a medium, and has small thermal contraction effect (Joule effect); the processing and the forming are easy, and the precise size can be kept; does not corrode the contact surface and does not pollute the medium, etc.
At present, sealing elements are divided into NBR nitrile rubber sealing rings, HNBR hydrogenated nitrile rubber sealing rings, FLS fluorosilicone rubber sealing rings, CR chloroprene rubber sealing rings and the like according to materials, and although the sealing elements can basically meet production requirements, the heat shrinkage resistance of the sealing elements in certain specific environments is difficult to meet the production requirements.
Disclosure of Invention
The invention provides a titanate modified polypropylene fiber, a preparation method and application thereof, a heat-shrinkable sealing ring and a preparation method thereof, and the titanate modified polypropylene fiber has excellent heat-shrinkable performance and mechanical property.
The invention provides a preparation method of titanate modified polypropylene fiber, which comprises the following steps: adding isopropyl tri (dioctyl pyrophosphoric acid acyloxy) titanate into a dimethylacetamide solvent, uniformly stirring, adding polypropylene fibers, soaking at 40-50 ℃ for 10-15 h, and drying at room temperature to obtain titanate modified polypropylene fibers;
the weight average molecular weight of the polypropylene fiber is 50000, 8000 or 10000;
the mass ratio of the isopropyl tri (dioctyl pyrophosphato acyloxy) titanate to the polypropylene fiber is 0.1: 1. 0.15: 1 or 0.2: 1.
the invention also provides the titanate modified polypropylene fiber prepared by the preparation method in the scheme, wherein the diameter of the titanate modified polypropylene fiber is 10-41 mu m, and the length of the titanate modified polypropylene fiber is 5-6 mm.
The invention also provides application of the titanate modified polypropylene fiber in the scheme in a heat shrinkage resistant sealing ring.
The invention also provides a heat-shrinkage-resistant sealing ring which comprises the following raw materials in parts by weight:
50-70 parts of fluoroether rubber, 20-30 parts of polyacrylate rubber, 30-40 parts of carbon black, 1-2 parts of vulcanizing agent, 3-5 parts of microcrystalline glass, 10-20 parts of heavy calcium carbonate, 3-4 parts of p-hydroxybenzene sulfonic acid, 2-3 parts of sodium gluconate, 10-15 parts of titanate modified polypropylene fiber, 4-7 parts of double-ended vinyl silicone oil, 5-10 parts of polyallylamine hydrochloride and 5-10 parts of dipropylene glycol monoethyl ether;
the vulcanizing agents are sulfur and tetramethyl thiuram disulfide;
the viscosity of the double-end vinyl silicone oil is 10000mPa & s-50000 mPa & s;
the microcrystalline glass has a coefficient of thermal expansion of (0.5 to 1) × 10-7/℃；
The weight average molecular weight of the polyacrylate rubber is 5000-10000;
the weight average molecular weight of the polyallylamine hydrochloride is 10000-15000;
the mass ratio of the sulfur to the tetramethyl thiuram disulfide is 1: (0.3 to 0.4);
the titanate modified polypropylene fiber is the titanate modified polypropylene fiber in the scheme.
The invention also provides a preparation method of the anti-heat shrinkage sealing ring, which comprises the following steps:
1) feeding fluoroether rubber, polyacrylate rubber, carbon black, a vulcanizing agent, microcrystalline glass, heavy calcium carbonate, p-hydroxyphenylsulfonic acid, sodium gluconate, titanate modified polypropylene fiber, double-end vinyl silicone oil, polyallylamine hydrochloride and dipropylene glycol monoethyl ether into an internal mixer, and carrying out internal mixing for 8-10 min at 90-110 ℃ to obtain mixed rubber;
2) mixing the mixed rubber by an open mill for molding, putting the molded rubber into a molding die of vulcanization equipment, and vulcanizing at 150-160 ℃ for 100-150 s;
3) trimming the vulcanized product to obtain the anti-heat shrinkage sealing ring.
The invention provides a heat-shrinkage-resistant sealing ring and a preparation method thereof, wherein fluoroether rubber and polyacrylate rubber are used as main materials, and the main materials have excellent high-temperature resistance and aging resistance, so that the sealing ring has good high-temperature resistance, and can still have good mechanical properties after being subjected to high-temperature treatment; the sodium gluconate can improve the dimensional stability of the sealing ring; the titanate modified polypropylene fiber is used for improving the dimensional stability of the sealing ring and the shrinkage resistance of the sealing ring; the double-end vinyl silicone oil is used for improving the toughness of rubber and improving the sealing performance of the sealing ring; the polyallylamine hydrochloride can improve the mechanical stability of the sealing ring, so that the sealing ring has excellent anti-shrinkage performance. Experimental results show that the heat-resistant and oil-resistant sealing ring has excellent anti-shrinkage performance, mechanical performance and other performances. The preparation method is simple, and the prepared anti-heat-shrinkage sealing ring has excellent anti-heat-shrinkage performance and mechanical property.
Detailed Description
The invention provides a heat-shrinkage-resistant sealing ring which comprises the following raw materials in parts by weight:
50-70 parts of fluoroether rubber, 20-30 parts of polyacrylate rubber, 30-40 parts of carbon black, 1-2 parts of vulcanizing agent, 3-5 parts of microcrystalline glass, 10-20 parts of heavy calcium carbonate, 3-4 parts of p-hydroxybenzene sulfonic acid, 2-3 parts of sodium gluconate, 10-15 parts of titanate modified polypropylene fiber, 4-7 parts of double-ended vinyl silicone oil, 5-10 parts of polyallylamine hydrochloride and 5-10 parts of dipropylene glycol monoethyl ether.
According to the invention, the fluoroether rubber and the polyacrylate rubber are adopted as main materials, and the fluoroether rubber and the polyacrylate rubber have excellent high temperature resistance and aging resistance, so that the sealing ring has good high temperature resistance, and the sealing ring can still have good mechanical properties after being subjected to high temperature treatment; the sodium gluconate can improve the dimensional stability of the sealing ring; the titanate modified polypropylene fiber is used for improving the dimensional stability of the sealing ring and improving the shrinkage resistance of the sealing ring; the double-end vinyl silicone oil is used for improving the toughness of rubber and improving the sealing performance of the sealing ring; the polyallylamine hydrochloride can improve the mechanical stability of the sealing ring, so that the sealing ring has excellent anti-shrinkage performance. Experimental results show that the heat-resistant and oil-resistant sealing ring has excellent anti-shrinkage performance, mechanical performance and other performances.
The fluoroether rubber has excellent aging resistance, so that the sealing ring can keep high mechanical property at high temperature, and the sealing ring has high heat shrinkage resistance. Preferably, the weight part of the fluoroether rubber is 50-70 parts; more preferably, the weight part of the fluoroether rubber is 55 to 65 parts.
The polyacrylate rubber can enable the sealing ring to have good high-temperature resistance, and can ensure that the sealing ring still has good mechanical properties after being subjected to high-temperature treatment. Preferably, the weight part of the polyacrylate rubber is 20-30 parts; more preferably, the weight part of the polyacrylate rubber is 20-25 parts.
Preferably, the weight part of the carbon black is 30-40 parts; more preferably, the weight part of the carbon black is 35 to 40 parts. In the present invention, the source of carbon black is not limited, and carbon black commercially available in the art may be used, and the type of carbon black is N326, N660 or N539.
The vulcanizing agent is used for improving the mechanical property, the high temperature resistance and the aging resistance of the high temperature resistant rubber. In an embodiment of the invention, the vulcanizing agents are sulfur and tetramethylthiuram disulfide. The mass ratio of the sulfur to the tetramethylthiuram disulfide is 1: (0.3-0.4).
Preferably, the vulcanizing agent is 1-2 parts by weight; more preferably, the vulcanizing agent is 1.4-1.7 parts by weight.
Preferably, the weight part of the microcrystalline glass is 3-5 parts; more preferably, the weight part of the microcrystalline glass is 3.5-4.5 parts. In the embodiment of the invention, the thermal expansion coefficient of the microcrystalline glass is (0.5-1) × 10-7/℃。
Preferably, the weight part of the heavy calcium carbonate is 10-20 parts; more preferably, the weight part of the heavy calcium carbonate is 13 to 17 parts.
Preferably, the weight portion of the p-hydroxybenzene sulfonic acid is 3-4; more preferably, the weight portion of the p-hydroxybenzene sulfonic acid is 3.2-3.4 portions.
Preferably, the weight part of the sodium gluconate is 2-3 parts; more preferably, the weight part of the sodium gluconate is 2.3-2.6 parts.
The titanate modified polypropylene fiber is used for improving the dimensional stability of the sealing ring and improving the shrinkage resistance of the sealing ring. Preferably, the weight part of the titanate modified polypropylene fiber is 10-15 parts; more preferably, the weight part of the titanate modified polypropylene fiber is 12-13 parts. In the embodiment of the invention, the diameter of the titanate modified polypropylene fiber is 10-41 μm, and the length is 5-6 mm. Wherein the titanate modified polypropylene fiber is a titanate modified polypropylene fiber; the preparation method of the titanate modified polypropylene fiber comprises the following steps: adding isopropyl tri (dioctyl pyrophosphato acyloxy) titanate into a dimethylacetamide solvent, uniformly stirring, adding polypropylene fiber, soaking at 40-50 ℃ for 10-15 h, and drying at room temperature to obtain the isopropyl tri (dioctyl pyrophosphato acyloxy) titanate modified polypropylene fiber.
The double-end vinyl silicone oil is used for improving the toughness of rubber and improving the sealing performance of the sealing ring. Preferably, the weight part of the double-end vinyl silicone oil is 4-7 parts; more preferably, the weight part of the double-end vinyl silicone oil is 5-6 parts. The viscosity of the vinyl-terminated silicone oil is 10000 mPas-50000 mPas.
The polyallylamine hydrochloride can improve the mechanical stability of the sealing ring, so that the sealing ring has excellent anti-shrinkage performance. Preferably, the weight part of the polyallylamine hydrochloride is 5-10 parts; more preferably, the weight part of the polyallylamine hydrochloride is 7-8 parts. In the embodiment of the invention, the polyallylamine hydrochloride has a weight average molecular weight of 10000-15000.
Preferably, the weight part of the dipropylene glycol monoethyl ether is 5-10 parts; more preferably, the weight part of the dipropylene glycol monoethyl ether is 8-10 parts.
The invention also provides a preparation method of the anti-heat shrinkage sealing ring, which comprises the following steps:
1) feeding fluoroether rubber, polyacrylate rubber, carbon black, a vulcanizing agent, microcrystalline glass, heavy calcium carbonate, p-hydroxyphenylsulfonic acid, sodium gluconate, titanate modified polypropylene fiber, double-end vinyl silicone oil, polyallylamine hydrochloride and dipropylene glycol monoethyl ether into an internal mixer, and carrying out internal mixing for 8-10 min at 90-110 ℃ to obtain mixed rubber;
2) mixing the mixed rubber by an open mill for molding, putting the molded rubber into a molding die of vulcanization equipment, and vulcanizing at 150-160 ℃ for 100-150 s;
3) trimming the vulcanized product to obtain the anti-heat shrinkage sealing ring.
The fluoroether rubber, polyacrylate rubber, carbon black, a vulcanizing agent, microcrystalline glass, heavy calcium carbonate, p-hydroxyphenylsulfonic acid, sodium gluconate, titanate-modified polypropylene fiber, double-ended vinyl silicone oil, polyallylamine hydrochloride and dipropylene glycol monoethyl ether are the same as those described above, and are not described herein again.
The preparation method is simple, and the prepared anti-heat-shrinkage sealing ring has excellent anti-heat-shrinkage performance and mechanical property.
In order to further illustrate the present invention, the following will describe in detail an anti-heat-shrinkable sealing ring and a method for manufacturing the same in accordance with the examples, which should not be construed as limiting the scope of the present invention.
Example 1
The titanate modified polypropylene fiber is titanate modified polypropylene fiber, and the preparation method of the titanate modified polypropylene fiber comprises the following steps:
adding isopropyl tri (dioctyl pyrophosphato acyloxy) titanate into a dimethylacetamide solvent, uniformly stirring, adding polypropylene fiber, soaking at 40 ℃ for 15h, and drying at room temperature to obtain isopropyl tri (dioctyl pyrophosphato acyloxy) titanate modified polypropylene fiber with the diameter of 10 mu m and the length of 5 mm; the weight average molecular weight of the polypropylene fiber is 50000;
the mass ratio of the isopropyl tri (dioctyl pyrophosphato acyloxy) titanate to the polypropylene fiber is 0.1: 1.
example 2
The titanate modified polypropylene fiber is titanate modified polypropylene fiber, and the preparation method of the titanate modified polypropylene fiber comprises the following steps:
adding isopropyl tri (dioctyl pyrophosphato acyloxy) titanate into a dimethylacetamide solvent, uniformly stirring, adding polypropylene fiber, soaking at 50 ℃ for 10h, and drying at room temperature to obtain isopropyl tri (dioctyl pyrophosphato acyloxy) titanate modified polypropylene fiber with the diameter of 41 mu m and the length of 6 mm; the weight average molecular weight of the polypropylene fiber is 100000;
the mass ratio of the isopropyl tri (dioctyl pyrophosphato acyloxy) titanate to the polypropylene fiber is 0.2: 1.
example 3
The titanate modified polypropylene fiber is titanate modified polypropylene fiber, and the preparation method of the titanate modified polypropylene fiber comprises the following steps:
adding isopropyl tri (dioctyl pyrophosphato acyloxy) titanate into a dimethylacetamide solvent, stirring uniformly, adding polypropylene fiber, soaking at 45 ℃ for 12h, and drying at room temperature to obtain isopropyl tri (dioctyl pyrophosphato acyloxy) titanate modified polypropylene fiber with the diameter of 25 mu m and the length of 5.5 mm; the weight average molecular weight of the polypropylene fiber is 80000;
the mass ratio of the isopropyl tri (dioctyl pyrophosphato acyloxy) titanate to the polypropylene fiber is 0.15: 1.
example 4
The heat shrinkage resistant sealing ring comprises the following raw materials in parts by weight:
50 parts of fluoroether rubber, 20 parts of polyacrylate rubber with the weight-average molecular weight of 5000, 30 parts of carbon black, 1 part of vulcanizing agent and 3 parts of rubber with the thermal expansion coefficient of 0.5 multiplied by 10-7/° c microcrystalline glass, 10 parts of ground calcium carbonate, 3 parts of p-hydroxybenzene sulfonic acid, 2 parts of sodium gluconate, 10 parts of the titanate-modified polypropylene fiber prepared in example 1, 4 parts of terminal vinyl silicone oil having a viscosity of 10000mPa · s, 5 parts of polyallylamine hydrochloride having a weight average molecular weight of 10000, and 5 parts of dipropylene glycol monoethyl ether;
the vulcanizing agent is prepared from the following components in percentage by mass: 0.3 of sulfur and tetramethylthiuram disulfide.
The preparation method of the anti-heat shrinkage sealing ring comprises the following steps:
1) feeding fluoroether rubber, polyacrylate rubber, carbon black, a vulcanizing agent, microcrystalline glass, heavy calcium carbonate, p-hydroxyphenylsulfonic acid, sodium gluconate, titanate modified polypropylene fiber, double-end vinyl silicone oil, polyallylamine hydrochloride and dipropylene glycol monoethyl ether into an internal mixer, and internally mixing for 8min at 90 ℃ to obtain mixed rubber;
2) the mixed rubber is subjected to open mixing molding through an open mill, and the molded rubber is placed into a molding die of vulcanization equipment and is vulcanized for 100s at the temperature of 150 ℃;
3) trimming the vulcanized product to obtain the O-shaped anti-heat shrinkage sealing ring with the inner diameter of 40mm, the wire diameter of 3.55mm, the inner diameter of a groove of 37.1mm, the outer diameter of the groove of 47.1mm, the depth of 2.75mm and the width of the groove of 5 mm.
Example 5
The heat shrinkage resistant sealing ring comprises the following raw materials in parts by weight:
70 parts of fluoroether rubber, 30 parts of polyacrylate rubber with the weight-average molecular weight of 8000, 40 parts of carbon black, 2 parts of vulcanizing agent and 5 parts of rubber with the thermal expansion coefficient of 0.6 multiplied by 10-7Per DEG C microcrystalline glass, 20 parts of ground calcium carbonate, 4 parts of p-hydroxybenzene sulfonic acid, 3 parts of sodium gluconate, 15 parts of the titanate-modified polypropylene fiber prepared in example 1, 7 parts of double-ended vinyl silicone oil with the viscosity of 40000mPa & s,10 parts of polyallylamine hydrochloride having a weight-average molecular weight of 15000 and 10 parts of dipropylene glycol monoethyl ether;
the vulcanizing agent is prepared from the following components in percentage by mass: 0.4 sulfur and tetramethylthiuram disulfide.
The preparation method of the anti-heat shrinkage sealing ring comprises the following steps:
1) feeding fluoroether rubber, polyacrylate rubber, carbon black, a vulcanizing agent, microcrystalline glass, heavy calcium carbonate, p-hydroxyphenylsulfonic acid, sodium gluconate, titanate modified polypropylene fiber, double-end vinyl silicone oil, polyallylamine hydrochloride and dipropylene glycol monoethyl ether into an internal mixer, and internally mixing for 9min at 100 ℃ to obtain mixed rubber;
2) mixing the mixed rubber by an open mill for molding, putting the molded rubber into a molding die of vulcanization equipment, and vulcanizing at 155 ℃ for 130 s;
3) and trimming the vulcanized product to obtain the O-shaped anti-heat shrinkage sealing ring with the inner diameter of 40mm, the wire diameter of 3.55mm, the inner diameter of the groove of 37.1mm, the outer diameter of the groove of 47.1mm, the depth of 2.75mm and the width of the groove of 5 mm.
Example 6
The heat shrinkage resistant sealing ring comprises the following raw materials in parts by weight:
55 parts of fluoroether rubber, 22 parts of polyacrylate rubber having a weight average molecular weight of 7000, 35 parts of carbon black, 1.4 parts of a vulcanizing agent, and 3.5 parts of a rubber having a coefficient of thermal expansion of 0.7X 10-7Per DEG C microcrystalline glass, 13 parts of heavy calcium carbonate, 3.2 parts of p-hydroxybenzene sulfonic acid, 2.3 parts of sodium gluconate, 12 parts of the titanate-modified polypropylene fiber prepared in example 2, 5 parts of double-ended vinyl silicone oil having a viscosity of 50000 mPa.s, 7 parts of polyallylamine hydrochloride having a weight-average molecular weight of 10000 and 8 parts of dipropylene glycol monoethyl ether;
the vulcanizing agent is a mixture of 1: 0.32 sulfur and tetramethylthiuram disulfide.
The preparation method of the anti-heat shrinkage sealing ring comprises the following steps:
1) feeding fluoroether rubber, polyacrylate rubber, carbon black, a vulcanizing agent, microcrystalline glass, heavy calcium carbonate, p-hydroxyphenylsulfonic acid, sodium gluconate, titanate modified polypropylene fiber, double-end vinyl silicone oil, polyallylamine hydrochloride and dipropylene glycol monoethyl ether into an internal mixer, and internally mixing for 10min at 90 ℃ to obtain mixed rubber;
2) mixing the mixed rubber by an open mill for molding, putting the molded rubber into a molding die of vulcanization equipment, and vulcanizing at 160 ℃ for 120 s;
3) and trimming the vulcanized product to obtain the O-shaped anti-heat shrinkage sealing ring with the inner diameter of 40mm, the wire diameter of 3.55mm, the inner diameter of the groove of 37.1mm, the outer diameter of the groove of 47.1mm, the depth of 2.75mm and the width of the groove of 5 mm.
Example 7
The heat shrinkage resistant sealing ring comprises the following raw materials in parts by weight:
65 parts of fluoroether rubber, 20 parts of polyacrylate rubber with the weight-average molecular weight of 10000, 40 parts of carbon black, 1.7 parts of vulcanizing agent and 4.5 parts of rubber with the thermal expansion coefficient of 1 multiplied by 10-7V. microcrystalline glass, 17 parts of ground calcium carbonate, 3.4 parts of p-hydroxybenzene sulfonic acid, 2.6 parts of sodium gluconate, 13 parts of the titanate-modified polypropylene fiber obtained in example 3, 6 parts of a double-terminal vinyl silicone oil having a viscosity of 20000 mPas, 8 parts of polyallylamine hydrochloride having a weight-average molecular weight of 13000 and 10 parts of dipropylene glycol monoethyl ether;
the vulcanizing agent is prepared from the following components in percentage by mass: 0.36 sulfur and tetramethylthiuram disulfide.
The preparation method of the anti-heat shrinkage sealing ring comprises the following steps:
1) feeding fluoroether rubber, polyacrylate rubber, carbon black, a vulcanizing agent, microcrystalline glass, heavy calcium carbonate, p-hydroxyphenylsulfonic acid, sodium gluconate, titanate modified polypropylene fiber, double-end vinyl silicone oil, polyallylamine hydrochloride and dipropylene glycol monoethyl ether into an internal mixer, and internally mixing for 10min at 110 ℃ to obtain mixed rubber;
2) the mixed rubber is subjected to open mixing molding through an open mill, and the molded rubber is placed into a molding die of vulcanization equipment and is vulcanized for 150 seconds at the temperature of 155 ℃;
3) and trimming the vulcanized product to obtain the O-shaped anti-heat shrinkage sealing ring with the inner diameter of 40mm, the wire diameter of 3.55mm, the inner diameter of the groove of 37.1mm, the outer diameter of the groove of 47.1mm, the depth of 2.75mm and the width of the groove of 5 mm.
Example 8
The heat shrinkage resistant sealing ring comprises the following raw materials in parts by weight:
60 parts of fluoroether rubber, 22 parts of polyacrylate rubber with the weight-average molecular weight of 8000, 37 parts of carbon black, 1.5 parts of vulcanizing agent and 4 parts of rubber with the thermal expansion coefficient of 0.8 multiplied by 10-7V. microcrystalline glass, 15 parts of ground calcium carbonate, 3.3 parts of p-hydroxybenzene sulfonic acid, 2.5 parts of sodium gluconate, 12.5 parts of the titanate-modified polypropylene fiber obtained in example 3, 5.5 parts of a double-terminal vinyl silicone oil having a viscosity of 30000 mPas, 7.8 parts of polyallylamine hydrochloride having a weight-average molecular weight of 12000 and 9 parts of dipropylene glycol monoethyl ether;
the vulcanizing agent is a mixture of 1: 0.35 sulfur and tetramethylthiuram disulfide.
The preparation method of the anti-heat shrinkage sealing ring comprises the following steps:
1) feeding fluoroether rubber, polyacrylate rubber, carbon black, a vulcanizing agent, microcrystalline glass, heavy calcium carbonate, p-hydroxyphenylsulfonic acid, sodium gluconate, titanate modified polypropylene fiber, double-end vinyl silicone oil, polyallylamine hydrochloride and dipropylene glycol monoethyl ether into an internal mixer, and internally mixing for 9min at 100 ℃ to obtain mixed rubber;
2) mixing the mixed rubber by an open mill for molding, putting the molded rubber into a molding die of vulcanization equipment, and vulcanizing at 160 ℃ for 150 s;
3) and trimming the vulcanized product to obtain the O-shaped anti-heat shrinkage sealing ring with the inner diameter of 40mm, the wire diameter of 3.55mm, the inner diameter of the groove of 37.1mm, the outer diameter of the groove of 47.1mm, the depth of 2.75mm and the width of the groove of 5 mm.
Comparative example 1
The heat shrinkage resistant sealing ring comprises the following raw materials in parts by weight:
60 parts of fluoroether rubber, 22 parts of polyacrylate rubber with the weight-average molecular weight of 8000, 37 parts of carbon black, 1.5 parts of vulcanizing agent and 4 parts of thermal expansion coefficientIs 0.8X 10-7V. microcrystalline glass, 15 parts of heavy calcium carbonate, 3.3 parts of p-hydroxybenzene sulfonic acid, 2.5 parts of sodium gluconate, 12.5 parts of polypropylene fiber, 5.5 parts of double-ended vinyl silicone oil with the viscosity of 30000mPa & s, 7.8 parts of polyallylamine hydrochloride with the weight-average molecular weight of 12000 and 9 parts of dipropylene glycol monoethyl ether; the diameter of the polypropylene fiber is 25 μm, and the length is 5.5 mm; the weight average molecular weight of the polypropylene fiber is 80000;
the vulcanizing agent is prepared from the following components in percentage by mass: 0.35 sulfur and tetramethylthiuram disulfide.
The preparation method of the anti-heat shrinkage sealing ring comprises the following steps:
1) feeding fluoroether rubber, polyacrylate rubber, carbon black, a vulcanizing agent, microcrystalline glass, heavy calcium carbonate, p-hydroxybenzene sulfonic acid, sodium gluconate, polypropylene fiber, double-end vinyl silicone oil, polyallylamine hydrochloride and dipropylene glycol monoethyl ether into an internal mixer, and internally mixing for 9min at 100 ℃ to obtain mixed rubber;
2) the mixed rubber is subjected to open mixing molding through an open mill, and the molded rubber is placed into a molding die of vulcanization equipment and is vulcanized for 150 seconds at 160 ℃;
3) and trimming the vulcanized product to obtain the O-shaped anti-heat shrinkage sealing ring with the inner diameter of 40mm, the wire diameter of 3.55mm, the inner diameter of the groove of 37.1mm, the outer diameter of the groove of 47.1mm, the depth of 2.75mm and the width of the groove of 5 mm.
Comparative example 2
The heat shrinkage resistant sealing ring comprises the following raw materials in parts by weight:
60 parts of fluoroether rubber, 22 parts of polyacrylate rubber with the weight-average molecular weight of 8000, 37 parts of carbon black, 1.5 parts of sulfur and 4 parts of thermal expansion coefficient of 0.8 multiplied by 10-7V. microcrystalline glass, 15 parts of ground calcium carbonate, 3.3 parts of p-hydroxybenzene sulfonic acid, 2.5 parts of sodium gluconate, 12.5 parts of the titanate-modified polypropylene fiber obtained in example 3, 5.5 parts of a double-terminal vinyl silicone oil having a viscosity of 30000 mPas, 7.8 parts of polyallylamine hydrochloride having a weight-average molecular weight of 12000 and 9 parts of dipropylene glycol monoethyl ether;
the preparation method of the anti-heat shrinkage sealing ring comprises the following steps:
1) feeding fluoroether rubber, polyacrylate rubber, carbon black, a vulcanizing agent, microcrystalline glass, heavy calcium carbonate, p-hydroxyphenylsulfonic acid, sodium gluconate, titanate modified polypropylene fiber, double-end vinyl silicone oil, polyallylamine hydrochloride and dipropylene glycol monoethyl ether into an internal mixer, and internally mixing for 9min at 100 ℃ to obtain mixed rubber;
2) mixing the mixed rubber by an open mill for molding, putting the molded rubber into a molding die of vulcanization equipment, and vulcanizing at 160 ℃ for 150 s;
3) and trimming the vulcanized product to obtain the O-shaped anti-heat shrinkage sealing ring with the inner diameter of 40mm, the wire diameter of 3.55mm, the inner diameter of the groove of 37.1mm, the outer diameter of the groove of 47.1mm, the depth of 2.75mm and the width of the groove of 5 mm.
The seal rings obtained in examples 4 to 8 and comparative examples 1 to 2 were tested for tensile strength, tensile elongation and shrinkage, and the results are shown in table 1.
Wherein the tensile strength and tensile elongation are tested according to GBT 528-2009;
the heat shrinkage rate is calculated by the formula: c ═ [ (L11-L21)/L11+ (L12-L22)/L12+ (L13-L23)/L13+ (L14-L24)/L14+ (L15-L25)/L15+ (L16-L26)/L16] ÷ 4 × 100%, wherein L11 is the inner diameter of the sealing ring at 100 ℃, and L21 is the inner diameter of the sealing ring at 30 ℃; l11 is the inner diameter of the sealing ring at 100 ℃, and L21 is the inner diameter of the sealing ring at 30 ℃; l12 is the linear diameter size of the sealing ring at 100 ℃, and L22 is the linear diameter size of the sealing ring at 30 ℃; l13 is the inner diameter of the groove of the sealing ring at 100 ℃, and L23 is the inner diameter of the groove of the sealing ring at 30 ℃; l14 is the outer diameter of the groove of the sealing ring at 100 ℃, and L24 is the outer diameter of the groove of the sealing ring at 30 ℃; l15 is the depth of the sealing ring at 100 ℃, and L25 is the depth of the sealing ring at 30 ℃; l16 is the groove width dimension of the seal ring at 100 ℃ and L26 is the groove width dimension of the seal ring at 30 ℃.
TABLE 1 test results of examples 4 to 8 and comparative examples 1 to 2
Figure BDA0003600147940000111
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, it is possible to make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention.

Claims (5)

1. A preparation method of titanate modified polypropylene fiber comprises the following steps: adding isopropyl tri (dioctyl pyrophosphoric acid acyloxy) titanate into a dimethylacetamide solvent, uniformly stirring, adding polypropylene fibers, soaking at 40-50 ℃ for 10-15 h, and drying at room temperature to obtain titanate modified polypropylene fibers;
the weight average molecular weight of the polypropylene fiber is 50000, 8000 or 10000;
the mass ratio of the isopropyl tri (dioctyl pyrophosphato acyloxy) titanate to the polypropylene fiber is 0.1: 1. 0.15: 1 or 0.2: 1.
2. the titanate-modified polypropylene fiber prepared by the preparation method of claim 1,
the diameter of the titanate modified polypropylene fiber is 10-41 mu m, and the length of the titanate modified polypropylene fiber is 5-6 mm.
3. Use of the titanate-modified polypropylene fiber of claim 2 in heat-shrink resistant seals.
4. The heat-shrinkable sealing ring is characterized by comprising the following raw materials in parts by weight:
50-70 parts of fluoroether rubber, 20-30 parts of polyacrylate rubber, 30-40 parts of carbon black, 1-2 parts of vulcanizing agent, 3-5 parts of microcrystalline glass, 10-20 parts of heavy calcium carbonate, 3-4 parts of p-hydroxybenzene sulfonic acid, 2-3 parts of sodium gluconate, 10-15 parts of titanate modified polypropylene fiber, 4-7 parts of double-ended vinyl silicone oil, 5-10 parts of polyallylamine hydrochloride and 5-10 parts of dipropylene glycol monoethyl ether;
the vulcanizing agents are sulfur and tetramethyl thiuram disulfide;
the viscosity of the double-end vinyl silicone oil is 10000mPa & s-50000 mPa & s;
the microcrystalline glass has a coefficient of thermal expansion of (0.5 to 1) × 10-7/℃；
The weight average molecular weight of the polyacrylate rubber is 5000-10000;
the weight average molecular weight of the polyallylamine hydrochloride is 10000-15000;
the mass ratio of the sulfur to the tetramethyl thiuram disulfide is 1: (0.3 to 0.4);
the titanate-modified polypropylene fiber of claim 2.
5. The method for producing an anti-heat-shrinkable seal ring according to claim 4, comprising the steps of:
1) feeding fluoroether rubber, polyacrylate rubber, carbon black, a vulcanizing agent, microcrystalline glass, heavy calcium carbonate, p-hydroxyphenylsulfonic acid, sodium gluconate, titanate modified polypropylene fiber, double-end vinyl silicone oil, polyallylamine hydrochloride and dipropylene glycol monoethyl ether into an internal mixer, and internally mixing for 8-10 min at 90-110 ℃ to obtain mixed rubber;
2) mixing the mixed rubber by an open mill for molding, putting the molded rubber into a molding die of vulcanization equipment, and vulcanizing at 150-160 ℃ for 100-150 s;
3) and trimming the vulcanized product to obtain the anti-heat shrinkage sealing ring.
CN202210400973.9A 2019-12-29 2019-12-29 Titanate modified polypropylene fiber, preparation method and application thereof, heat-shrinkage-resistant sealing ring and preparation method thereof Pending CN114753152A (en)

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