CN109280230A - A kind of ageing-resistant sealant - Google Patents
A kind of ageing-resistant sealant Download PDFInfo
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- CN109280230A CN109280230A CN201811098472.XA CN201811098472A CN109280230A CN 109280230 A CN109280230 A CN 109280230A CN 201811098472 A CN201811098472 A CN 201811098472A CN 109280230 A CN109280230 A CN 109280230A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L7/00—Compositions of natural rubber
- C08L7/02—Latex
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/325—Calcium, strontium or barium phosphate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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
Abstract
The invention discloses a kind of ageing-resistant sealants, belong to field of compound material.The present invention is using the montmorillonite of natural nano stratified material as raw material, it is mixed with polymerized monomer, oxidation processes are carried out to sodium alginate, obtain the oxidized sodium alginate with two aldehyde structures, and processing is blended with natural emulsion and multiple emulsion, it is more advantageous to the inoxidizability and weatherability for playing other ingredients, is conducive to provide extrusion stress, neutralizing applied external force bring damage；The present invention is handled nanometer hydroxyapatite surface using silane coupling agent; its surface hydroxyl groups is replaced with into active amine groups; it reduces oxygen and free radical chain reaction occurs with rubber molecule in sealant; fracture or excessively crosslinking occur for strand, and protection sealant performance avoids being destroyed.The present invention solves the problems, such as that the ageing-resistant performance for commonly using ageing-resistant sealant at present is poor.
Description
Technical field
The invention belongs to field of compound material, and in particular to a kind of ageing-resistant sealant.
Background technique
According to statistics, building energy consumption accounts for about the 35%~40% of social total energy consumption at present, and for whole building, pass through
The energy of door and window loss accounts for the 50% of building energy consumption, and the door and window heat loss of poor sealing is 5~6 times of wall heat loss, so
The key of building energy conservation is exactly door and window energy conservation, and one of energy-efficient key factor of door and window is exactly sealant.
Sealant is to guide to deform with sealing surface shape, is not easy to trickle, there is the sealing material of certain caking property.Be for
Filling configuration gap, the adhesive to play sealing function.Have the effects that anti-leak, waterproof, vibration proof and sound insulation, heat-insulated.
Usually using the dope of the stemness such as pitch object, natural resin or synthetic resin, natural rubber or synthetic rubber or non-dry as base
Material, the inert fillers such as cooperation talcum powder, carclazyte, carbon black, titanium dioxide and asbestos, adds plasticizer, solvent, curing agent, promotion
Agent etc. is made.
Sealant is also known as hydraulic seal pad, compared with sealed solid (such as steel pad, paper washer), has easy to use, sealing
Property good advantage, sealant is that a kind of flowing or crowded indefinite form material can be relied on embedded with filling up a closed joint
Dry, temperature change, solvent volatilization is chemically crosslinked the stability and bond of material, and gradually by solid gum, viscoelastic sexual behaviour or
Elaxtic seal molding.
Sealant on the market is mainly ethylene propylene diene rubber and plasticised polyvinyl chloride material at present.Ethylene propylene diene rubber tool
There is excellent low-temperature characteristics, most of vulcanized articles are also softer under the conditions of -50 DEG C, and its density is small, almost
Than lightest one kind in all synthetic rubber.Butyl rubber is low under the action of catalyst by isobutene and a small amount of isoprene
A kind of rubber product made from warm cationic polymerization, its feature are that gas permeability is small, flexible resistance is excellent.Not with economy
Disconnected development, the rapid development of automobile industry have higher requirement for automobile interior decoration etc., and sealant is excellent due to its
Performance, be widely used in the sealing and adhesion of automobile, become gradually one kind can not substituted product, there have to be unlimited
Development potentiality.But although sealant leakproofness on the market is relatively good at present, can high temperature resistant ageing-resistant performance it is poor, make
It is shorter with the service life.Therefore a kind of ageing-resistant sealant that the ageing-resistant performance strong service life is long need to be developed.
Summary of the invention
The technical problems to be solved by the invention: for the poor problem of the ageing-resistant performance of current common sealant,
A kind of ageing-resistant sealant is provided.
In order to solve the above technical problems, the present invention is using technical solution as described below:
A kind of ageing-resistant sealant, including following component: 6 ~ 10 parts of nitrile rubbers, 3 ~ 6 parts of epoxy resin, 2 ~ 5 parts of auxiliary agents, 3 ~ 7
Part antioxidant, 2 ~ 5 parts of promotors, 1 ~ 4 part of plasticizer, further includes: 30 ~ 50 parts of composite modified natural emulsions, 15 ~ 30 parts it is compound
Modified hydroxylapatite material.
The preparation method of the composite modified natural emulsion, includes the following steps:
(1) 10 ~ 15:1:30 in mass ratio takes sodium alginate, sodium metaperiodate, deionized water to be mixed, and is stored at room temperature, and sea is added
The ethylene glycol of mosanom quality 4 ~ 8% is mixed, and obtains mixed reaction solution, mixed reaction solution 20 ~ 25:1:30 in mass ratio is taken to add
Enter NaCl, dehydrated alcohol mixing, stands, filter, take filter residue to be freeze-dried, obtain dried object, it is spare；
(2) 1:2 ~ 5:3:20 ~ 40 take neopelex, emulsifier, montmorillonite, deionized water mixing in mass ratio, lead to
Nitrogen protection, stirring obtain just mixed object, are warming up to 75 ~ 85 DEG C, and the intercalation monomer of first mixed amount of substance 7 ~ 12% is added, just mixes amount of substance
4 ~ 8% azodiisobutyronitrile mixing, obtains multiple emulsion；
(3) it takes multiple emulsion 5 ~ 8:1:3 in mass ratio that spare dried object, natural emulsion mixing is added, adjusts pH, shearing point
It dissipates, refrigerates to get composite modified natural emulsion.
Emulsifier in the step (1): in mass ratio 1:3 ~ 6 take Tween-80, oleic acid polyoxyethylene mixing to get
Emulsifier.
Intercalation monomer in the step (1): 1:3 ~ 5 take methyl methacrylate, methacrylic acid different pungent in mass ratio
Ester mixes to get intercalation monomer.
The preparation of the composite modified hydroxy-apatite building stones: in 25 ~ 40 DEG C, 15 ~ 25:3 in mass ratio takes acetone, nanometer hydroxyl
The stirring of base apatites mixed, obtains suspension, is warming up to 70 ~ 85 DEG C, and the silane coupling agent mixing that suspension quality 2 ~ 5% is added is stirred
It mixes, keeps the temperature, obtain surface grafting apatite, add the isopropanol of suspension quality 1 ~ 4%, the sad fourth of suspension quality 3 ~ 7%
The lactide mixing of ester, suspension quality 18 ~ 30%, obtains modified hydroxylapatite-polylactic acid mixing, takes modified hydroxyl phosphorus
Butyl titanate is added in lime stone-polylactic acid mixing 10 ~ 15:3:0.1 in mass ratio, glacial acetic acid is mixed to get composite modified
Hydroxy-apatite building stones.
The silane coupling agent: any one in silane resin acceptor kh-550, KH-560, KH-570.
The auxiliary agent: 5:0.1:1 ~ 3 take white carbon black, sulphur, microcrystalline wax mixing to get auxiliary agent in mass ratio.
The antioxidant: 5 ~ 8:0.1 in mass ratio takes tert-butylhydroquinone, sodium metasulfite mixing to get antioxygen
Agent.
The promotor: 3 ~ 6:8 in mass ratio takes ferric trichloride, triethanolamine mixing to get promotor.
The plasticizer: 6 ~ 10:3 in mass ratio takes triethyl citrate, di-n-octyl phthalate mixing to get increasing
Mould agent.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention is mixed using the montmorillonite of natural nano stratified material as raw material with polymerized monomer, and aliphatic organic modifiers expand
It dissipates and enters between cheating engaging layer, increase its interlamellar spacing, so that the ingredients such as oxidized sodium alginate are able to enter interlayer, increase two-phase
Interfacial area generates excellent weatherability and high temperature resistance, carries out oxidation processes to sodium alginate, obtains having two aldehyde structures
Oxidized sodium alginate, antioxygenic property is provided, and processing is blended with natural emulsion and multiple emulsion, with the monomeric ester of introducing
The compatibility of the increase of side chain, obtained polymer and natural emulsion is also improved, and latex molecule polymerize with long ester side chain
Object mutually diffuses to form entanglement point, improves internal workability, montmorillonite layer evenly dispersed formation physics in rubber rubber
Crosslinking points are more advantageous to the inoxidizability and weatherability for playing other ingredients, and the monomer between cheating engaging layer can generate volume
Bigger polymer is broken down into the particle of smaller size, is fixed on system, favorably so that removing even cracks montmorillonite
In providing extrusion stress, neutralizing applied external force bring is damaged；
(2) present invention is handled nanometer hydroxyapatite surface using silane coupling agent, its surface hydroxyl groups is replaced
For active amine groups, ring-opening polymerisation then occurs, obtains the hydroxyapatite of surface grafting, then using isopropanol as initiator,
Stannous octoate is catalyst, causes the ring-opening polymerization of lactide, and modified apatite-polylactic acid compound material is made, and is had good
Good biocompatibility provides good workability for colloid, stablizes the ageing-resistant effect of performance, butyl titanate partial hydrolysis,
So that system has part TiO2, oxygen radical can be eliminated, oxygen is reduced and free radical chain lock occurs with rubber molecule in sealant
Fracture or excessively crosslinking occur for reaction, strand, and protection sealant performance avoids being destroyed.
Specific embodiment
Emulsifier: 1:3 ~ 6 take Tween-80, oleic acid polyoxyethylene mixing to get emulsifier in mass ratio.
Plasticizer: 6 ~ 10:3 in mass ratio takes triethyl citrate, di-n-octyl phthalate mixing to get plasticising
Agent.
Promotor: 3 ~ 6:8 in mass ratio takes ferric trichloride, triethanolamine mixing to get promotor.
Antioxidant: 5 ~ 8:0.1 in mass ratio takes tert-butylhydroquinone, sodium metasulfite mixing to get antioxidant.
Silane coupling agent: any one in silane resin acceptor kh-550, KH-560, KH-570.
Auxiliary agent: 5:0.1:1 ~ 3 take white carbon black, sulphur, microcrystalline wax mixing to get auxiliary agent in mass ratio.
Intercalation monomer: 1:3 ~ 5 take methyl methacrylate, isooctyl methacrylate mixing to get intercalation in mass ratio
Monomer.
The preparation method of composite modified natural emulsion, includes the following steps:
(1) 10 ~ 15:1:30 in mass ratio takes sodium alginate, sodium metaperiodate, deionized water mixing, with 400 ~ 600r/min magnetic force
1 ~ 3h is stirred, it is stored at room temperature 20 ~ for 24 hours, the ethylene glycol mixing of sodium alginate quality 4 ~ 8% is added, with 300 ~ 500r/min stirring 25
~ 50min, obtains mixed reaction solution, takes mixed reaction solution 20 ~ 25:1:30 in mass ratio that NaCl, dehydrated alcohol mixing is added
It is even, 1 ~ 3h is stood, is filtered, takes filter residue in -40 DEG C of freeze driers freezing 20 ~ for 24 hours, obtains dried object, it is spare；
(2) 1:2 ~ 5:3:20 ~ 40 take neopelex, emulsifier, montmorillonite, deionized water mixing in mass ratio, lead to
Nitrogen protection stirs 1 ~ 3h in room temperature with 500 ~ 800r/min, obtains just mixed object, is warming up to 75 ~ 85 DEG C, be added just mixed amount of substance 7 ~
The azodiisobutyronitrile mixing of 12% intercalation monomer, just mixed amount of substance 4 ~ 8%, obtains multiple emulsion；
(3) take multiple emulsion 5 ~ 8:1:3 in mass ratio that spare dried object, natural emulsion mixing is added, with concentration 0.1mol/L
Ammonium hydroxide adjust pH to 10 ~ 11 after, with 2000 ~ 3000r/min shear dispersion 15 ~ 25min after, move to 1 ~ 4 DEG C of refrigerator cold-storage 12 ~
16h is to get composite modified natural emulsion.
The preparation of composite modified hydroxy-apatite building stones: in 25 ~ 40 DEG C, 15 ~ 25:3 in mass ratio takes acetone, nano hydroxyapatite
Lime stone mixing stirs 40 ~ 60min with 350 ~ 600r/min, obtains suspension, be warming up to 70 ~ 85 DEG C, suspension quality 2 ~ 5% is added
Silane coupling agent be mixed, keep the temperature 40 ~ 60min, obtain surface grafting apatite, add the isopropyl of suspension quality 1 ~ 4%
The lactide mixing of alcohol, the butyl caprylate of suspension quality 3 ~ 7%, suspension quality 18 ~ 30%, is stirred with 400 ~ 800r/min magnetic force
Mix 40 ~ 60min, obtain modified hydroxylapatite-polylactic acid mixing, take modified hydroxylapatite-polylactic acid mixing in mass ratio 10 ~
Butyl titanate, glacial acetic acid mixing is added in 15:3:0.1, stirs 1 ~ 3h with 500 ~ 800r/min to get composite modified hydroxy-apatite
Building stones.
A kind of ageing-resistant sealant, according to the mass fraction, including following component: 6 ~ 10 parts of nitrile rubbers, 3 ~ 6 parts of asphalt mixtures modified by epoxy resin
Rouge, 2 ~ 5 parts of auxiliary agents, 3 ~ 7 parts of antioxidants, 2 ~ 5 parts of promotors, 1 ~ 4 part of plasticizer, 30 ~ 50 parts of composite modified natural emulsions, 15
~ 30 parts of composite modified hydroxy-apatite building stones.
A kind of preparation method of ageing-resistant sealant, includes the following steps:
(1) according to the mass fraction, take 6 ~ 10 parts of nitrile rubbers, 3 ~ 6 parts of epoxy resin, 2 ~ 5 parts of auxiliary agents, 3 ~ 7 parts of antioxidants, 2 ~
5 parts of promotors, 1 ~ 4 part of plasticizer, 30 ~ 50 parts of composite modified natural emulsions, 15 ~ 30 parts of composite modified hydroxy-apatite building stones；
(2) first take nitrile rubber, composite modified hydroxy-apatite building stones, composite modified natural emulsion in mixer, in 170 ~ 190 DEG C
25 ~ 40min of mixing is cooled to 130 ~ 150 DEG C, and auxiliary agent, antioxidant, promotor, plasticizer, epoxy resin mixing is added, close
30 ~ 45min is refined, discharging, natural cooling is to get ageing-resistant sealant.
Embodiment 1
Emulsifier: 1:3 in mass ratio takes Tween-80, oleic acid polyoxyethylene mixing to get emulsifier.
Plasticizer: 6:3 in mass ratio takes triethyl citrate, di-n-octyl phthalate mixing to get plasticizer.
Promotor: 3:8 in mass ratio takes ferric trichloride, triethanolamine mixing to get promotor.
Antioxidant: 5:0.1 in mass ratio takes tert-butylhydroquinone, sodium metasulfite mixing to get antioxidant.
Silane coupling agent: silane resin acceptor kh-550.
Auxiliary agent: 5:0.1:1 in mass ratio takes white carbon black, sulphur, microcrystalline wax mixing to get auxiliary agent.
Intercalation monomer: 1:3 in mass ratio takes methyl methacrylate, isooctyl methacrylate mixing to get intercalation list
Body.
The preparation method of composite modified natural emulsion, includes the following steps:
(2) 10:1:30 in mass ratio takes sodium alginate, sodium metaperiodate, deionized water mixing, with 400r/min magnetic agitation 1h,
It is stored at room temperature 20h, the ethylene glycol mixing of sodium alginate quality 4% is added, 25min is stirred with 300r/min, obtains mixed reaction solution,
It takes mixed reaction solution 20:1:30 in mass ratio addition NaCl, dehydrated alcohol to be mixed evenly, stands 1h, filter, take filter residue
20h is freezed in -40 DEG C of freeze driers, obtains dried object, it is spare；
(2) 1:2:3:20 in mass ratio takes neopelex, emulsifier, montmorillonite, deionized water mixing, leads to nitrogen and protects
Shield obtains in room temperature with 500r/min stirring 1h and just mixes object, be warming up to 75 DEG C, is added and just mixes the intercalation monomer of amount of substance 7%, just mixes
The azodiisobutyronitrile of amount of substance 4% mixes, and obtains multiple emulsion；
(3) take multiple emulsion 5:1:3 in mass ratio that spare dried object, natural emulsion mixing is added, with concentration 0.1mol/L's
After ammonium hydroxide adjusts pH to 10, after shearing dispersion 15min with 2000r/min, 1 DEG C of refrigerator cold-storage 12h is moved to get composite modified day
Right latex.
The preparation of composite modified hydroxy-apatite building stones: in 25 DEG C, 15:3 in mass ratio takes acetone, nanometer hydroxyapatite mixed
It closes, 40min is stirred with 350r/min, obtains suspension, is warming up to 70 DEG C, the silane coupling agent mixing that suspension quality 2% is added is stirred
It mixes, keeps the temperature 40min, obtain surface grafting apatite, add the isopropanol of suspension quality 1%, the sad fourth of suspension quality 3%
The lactide mixing of ester, suspension quality 18%, with 400r/min magnetic agitation 40min, obtains modified hydroxylapatite-polylactic acid
Mixing takes modified hydroxylapatite-polylactic acid mixing 10:3:0.1 in mass ratio that butyl titanate, glacial acetic acid mixing is added, with
500r/min stirs 1h to get composite modified hydroxy-apatite building stones.
A kind of ageing-resistant sealant, according to the mass fraction, including following component: 6 parts of nitrile rubbers, 3 parts of epoxy resin, 2
Part auxiliary agent, 3 parts of antioxidants, 2 parts of promotors, 1 part of plasticizer, 30 parts of composite modified natural emulsions, 15 parts of composite modified hydroxyls
Apatite material.
A kind of preparation method of ageing-resistant sealant, includes the following steps:
(1) according to the mass fraction, 6 parts of nitrile rubbers, 3 parts of epoxy resin, 2 parts of auxiliary agents, 3 parts of antioxidants, 2 parts of promotors, 1 are taken
Part plasticizer, 30 parts of composite modified natural emulsions, 15 parts of composite modified hydroxy-apatite building stones；
(2) first take nitrile rubber, composite modified hydroxy-apatite building stones, composite modified natural emulsion in mixer, in 170 DEG C of mixings
25min is cooled to 130 DEG C, and auxiliary agent, antioxidant, promotor, plasticizer, epoxy resin is added and mixes, mixing 30min, out
Material, natural cooling is to get ageing-resistant sealant.
Embodiment 2
Emulsifier: 1:5 in mass ratio takes Tween-80, oleic acid polyoxyethylene mixing to get emulsifier.
Plasticizer: 8:3 in mass ratio takes triethyl citrate, di-n-octyl phthalate mixing to get plasticizer.
Promotor: 4:8 in mass ratio takes ferric trichloride, triethanolamine mixing to get promotor.
Antioxidant: 6:0.1 in mass ratio takes tert-butylhydroquinone, sodium metasulfite mixing to get antioxidant.
Silane coupling agent: silane coupling agent KH-560.
Auxiliary agent: 5:0.1:2 in mass ratio takes white carbon black, sulphur, microcrystalline wax mixing to get auxiliary agent.
Intercalation monomer: 1:4 in mass ratio takes methyl methacrylate, isooctyl methacrylate mixing to get intercalation list
Body.
The preparation method of composite modified natural emulsion, includes the following steps:
(3) 13:1:30 in mass ratio takes sodium alginate, sodium metaperiodate, deionized water mixing, with 500r/min magnetic agitation 2h,
It is stored at room temperature 22h, the ethylene glycol mixing of sodium alginate quality 6% is added, 40min is stirred with 400r/min, obtains mixed reaction solution,
It takes mixed reaction solution 23:1:30 in mass ratio addition NaCl, dehydrated alcohol to be mixed evenly, stands 2h, filter, take filter residue
22h is freezed in -40 DEG C of freeze driers, obtains dried object, it is spare；
(2) 1:4:3:30 in mass ratio takes neopelex, emulsifier, montmorillonite, deionized water mixing, leads to nitrogen and protects
Shield obtains in room temperature with 600r/min stirring 2h and just mixes object, be warming up to 79 DEG C, is added and just mixes the intercalation monomer of amount of substance 9%, just mixes
The azodiisobutyronitrile of amount of substance 6% mixes, and obtains multiple emulsion；
(3) take multiple emulsion 6:1:3 in mass ratio that spare dried object, natural emulsion mixing is added, with concentration 0.1mol/L's
After ammonium hydroxide adjusts pH to 10.5, after shearing dispersion 20min with 2500r/min, 3 DEG C of refrigerator cold-storage 14h are moved to get composite modified
Natural emulsion.
The preparation of composite modified hydroxy-apatite building stones: in 30 DEG C, 20:3 in mass ratio takes acetone, nanometer hydroxyapatite mixed
It closes, 50min is stirred with 400r/min, obtains suspension, is warming up to 75 DEG C, the silane coupling agent mixing that suspension quality 4% is added is stirred
It mixes, keeps the temperature 50min, obtain surface grafting apatite, add the isopropanol of suspension quality 3%, the sad fourth of suspension quality 5%
The lactide mixing of ester, suspension quality 20%, with 600r/min magnetic agitation 50min, obtains modified hydroxylapatite-polylactic acid
Mixing takes modified hydroxylapatite-polylactic acid mixing 13:3:0.1 in mass ratio that butyl titanate, glacial acetic acid mixing is added, with
600r/min stirs 2h to get composite modified hydroxy-apatite building stones.
A kind of ageing-resistant sealant, according to the mass fraction, including following component: 8 parts of nitrile rubbers, 5 parts of epoxy resin, 4
Part auxiliary agent, 5 parts of antioxidants, 4 parts of promotors, 3 parts of plasticizer, 40 parts of composite modified natural emulsions, 15 ~ 30 parts of composite modified hydroxyls
Base apatite material.
A kind of preparation method of ageing-resistant sealant, includes the following steps:
(1) according to the mass fraction, 8 parts of nitrile rubbers, 5 parts of epoxy resin, 4 parts of auxiliary agents, 4 parts of antioxidants, 4 parts of promotors, 3 are taken
Part plasticizer, 40 parts of composite modified natural emulsions, 20 parts of composite modified hydroxy-apatite building stones；
(2) first take nitrile rubber, composite modified hydroxy-apatite building stones, composite modified natural emulsion in mixer, in 180 DEG C of mixings
30min is cooled to 140 DEG C, and auxiliary agent, antioxidant, promotor, plasticizer, epoxy resin is added and mixes, mixing 40min, out
Material, natural cooling is to get ageing-resistant sealant.
Embodiment 3
Emulsifier: 1:6 in mass ratio takes Tween-80, oleic acid polyoxyethylene mixing to get emulsifier.
Plasticizer: 10:3 in mass ratio takes triethyl citrate, di-n-octyl phthalate mixing to get plasticizer.
Promotor: 6:8 in mass ratio takes ferric trichloride, triethanolamine mixing to get promotor.
Antioxidant: 8:0.1 in mass ratio takes tert-butylhydroquinone, sodium metasulfite mixing to get antioxidant.
Silane coupling agent: Silane coupling reagent KH-570.
Auxiliary agent: 5:0.1:3 in mass ratio takes white carbon black, sulphur, microcrystalline wax mixing to get auxiliary agent.
Intercalation monomer: 1:5 in mass ratio takes methyl methacrylate, isooctyl methacrylate mixing to get intercalation list
Body.
The preparation method of composite modified natural emulsion, includes the following steps:
(4) 15:1:30 in mass ratio takes sodium alginate, sodium metaperiodate, deionized water mixing, with 600r/min magnetic agitation 3h,
It is stored at room temperature the ethylene glycol mixing that sodium alginate quality 8% is added for 24 hours, 50min is stirred with 500r/min, obtains mixed reaction solution,
It takes mixed reaction solution 25:1:30 in mass ratio addition NaCl, dehydrated alcohol to be mixed evenly, stands 3h, filter, take filter residue
For 24 hours in -40 DEG C of freeze drier freezings, dried object is obtained, it is spare；
(2) 1:5:3:40 in mass ratio takes neopelex, emulsifier, montmorillonite, deionized water mixing, leads to nitrogen and protects
Shield stirs 3h in room temperature with 800r/min, obtains just mixed object, is warming up to 85 DEG C, and the just intercalation monomer of mixed amount of substance 12%, just is added
The azodiisobutyronitrile mixing of mixed amount of substance 8%, obtains multiple emulsion；
(3) take multiple emulsion 8:1:3 in mass ratio that spare dried object, natural emulsion mixing is added, with concentration 0.1mol/L's
After ammonium hydroxide adjusts pH to 11, after shearing dispersion 25min with 3000r/min, 4 DEG C of refrigerator cold-storage 16h are moved to get composite modified day
Right latex.
The preparation of composite modified hydroxy-apatite building stones: in 40 DEG C, 25:3 in mass ratio takes acetone, nanometer hydroxyapatite mixed
It closes, 60min is stirred with 600r/min, obtains suspension, is warming up to 85 DEG C, the silane coupling agent mixing that suspension quality 5% is added is stirred
It mixes, keeps the temperature 60min, obtain surface grafting apatite, add the isopropanol of suspension quality 4%, the sad fourth of suspension quality 7%
The lactide mixing of ester, suspension quality 30%, with 800r/min magnetic agitation 60min, obtains modified hydroxylapatite-polylactic acid
Mixing takes modified hydroxylapatite-polylactic acid mixing 15:3:0.1 in mass ratio that butyl titanate, glacial acetic acid mixing is added, with
800r/min stirs 3h to get composite modified hydroxy-apatite building stones.
A kind of ageing-resistant sealant, according to the mass fraction, including following component: 10 parts of nitrile rubbers, 6 parts of epoxy resin, 5
Part auxiliary agent, 7 parts of antioxidants, 5 parts of promotors, 4 parts of plasticizer, 50 parts of composite modified natural emulsions, 30 parts of composite modified hydroxyls
Apatite material.
A kind of preparation method of ageing-resistant sealant, includes the following steps:
(1) according to the mass fraction, take 10 parts of nitrile rubbers, 6 parts of epoxy resin, 5 parts of auxiliary agents, 7 parts of antioxidants, 5 parts of promotors,
4 parts of plasticizer, 50 parts of composite modified natural emulsions, 30 parts of composite modified hydroxy-apatite building stones；
(2) first take nitrile rubber, composite modified hydroxy-apatite building stones, composite modified natural emulsion in mixer, in 190 DEG C of mixings
40min is cooled to 150 DEG C, and auxiliary agent, antioxidant, promotor, plasticizer, epoxy resin is added and mixes, mixing 45min, out
Material, natural cooling is to get ageing-resistant sealant.
Comparative example 1: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking composite modified natural emulsion.
Comparative example 2: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking composite modified hydroxy-apatite
Building stones.
Comparative example 3: the ageing-resistant sealant of Wuxi City company production.
Embodiment is tested with ageing-resistant sealant obtained by comparative example by JC/T 914-2003 requirement, the master of test
Want performance indicator as shown in the table.
Table 1:
It can be seen that the performance change of ageing-resistant sealant of the invention before ageing and after aging is few, have good resistance to old
Change performance, mechanical property is good, and anti-ultraviolet property is excellent, and high temperature resistance is good, is worth promoting.
Claims (10)
1. a kind of ageing-resistant sealant, according to the mass fraction, including following component: 6 ~ 10 parts of nitrile rubbers, 3 ~ 6 parts of asphalt mixtures modified by epoxy resin
Rouge, 2 ~ 5 parts of auxiliary agents, 3 ~ 7 parts of antioxidants, 2 ~ 5 parts of promotors, 1 ~ 4 part of plasticizer, which is characterized in that further include: 30 ~ 50 parts
Composite modified natural emulsion, 15 ~ 30 parts of composite modified hydroxy-apatite building stones.
2. a kind of ageing-resistant sealant according to claim 1, which is characterized in that the preparation of the composite modified natural emulsion
Method includes the following steps:
(1) 10 ~ 15:1:30 in mass ratio takes sodium alginate, sodium metaperiodate, deionized water to be mixed, and is stored at room temperature, and sea is added
The ethylene glycol of mosanom quality 4 ~ 8% is mixed, and obtains mixed reaction solution, mixed reaction solution 20 ~ 25:1:30 in mass ratio is taken to add
Enter NaCl, dehydrated alcohol mixing, stands, filter, take filter residue to be freeze-dried, obtain dried object, it is spare；
(2) 1:2 ~ 5:3:20 ~ 40 take neopelex, emulsifier, montmorillonite, deionized water mixing in mass ratio, lead to
Nitrogen protection, stirring obtain just mixed object, are warming up to 75 ~ 85 DEG C, and the intercalation monomer of first mixed amount of substance 7 ~ 12% is added, just mixes amount of substance
4 ~ 8% azodiisobutyronitrile mixing, obtains multiple emulsion；
(3) it takes multiple emulsion 5 ~ 8:1:3 in mass ratio that spare dried object, natural emulsion mixing is added, adjusts pH, shearing point
It dissipates, refrigerates to get composite modified natural emulsion.
3. a kind of ageing-resistant sealant according to claim 2, which is characterized in that the emulsifier in the step (1): pressing matter
Amount takes Tween-80, oleic acid polyoxyethylene mixing to get emulsifier than 1:3 ~ 6.
4. a kind of ageing-resistant sealant according to claim 2, which is characterized in that the intercalation monomer in the step (1): press
Mass ratio 1:3 ~ 5 take methyl methacrylate, isooctyl methacrylate mixing to get intercalation monomer.
5. a kind of ageing-resistant sealant according to claim 1, which is characterized in that the composite modified hydroxy-apatite building stones
Preparation: in 25 ~ 40 DEG C, 15 ~ 25:3 in mass ratio takes acetone, nanometer hydroxyapatite to be mixed, and obtains suspension, is warming up to 70
~ 85 DEG C, the silane coupling agent that suspension quality 2 ~ 5% is added is mixed, and heat preservation obtains surface grafting apatite, adds suspension
The lactide mixing of the isopropanol of liquid quality 1 ~ 4%, the butyl caprylate of suspension quality 3 ~ 7%, suspension quality 18 ~ 30%,
Modified hydroxylapatite-polylactic acid mixing is obtained, modified hydroxylapatite-polylactic acid mixing 10 ~ 15:3:0.1 in mass ratio is taken to add
Enter butyl titanate, glacial acetic acid is mixed to get composite modified hydroxy-apatite building stones.
6. a kind of ageing-resistant sealant according to claim 5, which is characterized in that the silane coupling agent: silane coupling agent
Any one in KH-550, KH-560, KH-570.
7. a kind of ageing-resistant sealant according to claim 1, which is characterized in that the auxiliary agent: 5:0.1:1 ~ 3 in mass ratio
Take white carbon black, sulphur, microcrystalline wax mixing to get auxiliary agent.
8. a kind of ageing-resistant sealant according to claim 1, which is characterized in that the antioxidant: in mass ratio 5 ~ 8:
0.1 takes tert-butylhydroquinone, sodium metasulfite mixing to get antioxidant.
9. a kind of ageing-resistant sealant according to claim 1, which is characterized in that the promotor: 3 ~ 6:8 takes in mass ratio
Ferric trichloride, triethanolamine mixing are to get promotor.
10. a kind of ageing-resistant sealant according to claim 1, which is characterized in that the plasticizer: 6 ~ 10:3 in mass ratio
Take triethyl citrate, di-n-octyl phthalate mixing to get plasticizer.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109929465A (en) * | 2019-03-29 | 2019-06-25 | 广州掘策机械设备有限公司 | A kind of machine components protection wax and preparation method thereof |
| CN110655895A (en) * | 2019-10-08 | 2020-01-07 | 成都新柯力化工科技有限公司 | Anti-aging polyurethane sealant and preparation method thereof |
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| CN109929465A (en) * | 2019-03-29 | 2019-06-25 | 广州掘策机械设备有限公司 | A kind of machine components protection wax and preparation method thereof |
| CN110655895A (en) * | 2019-10-08 | 2020-01-07 | 成都新柯力化工科技有限公司 | Anti-aging polyurethane sealant and preparation method thereof |
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