CN112795363A - Environment-friendly flame-retardant polysulfide sealant and production method thereof - Google Patents
Environment-friendly flame-retardant polysulfide sealant and production method thereof Download PDFInfo
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- CN112795363A CN112795363A CN202110047607.5A CN202110047607A CN112795363A CN 112795363 A CN112795363 A CN 112795363A CN 202110047607 A CN202110047607 A CN 202110047607A CN 112795363 A CN112795363 A CN 112795363A
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 239000003063 flame retardant Substances 0.000 title claims abstract description 110
- 239000004587 polysulfide sealant Substances 0.000 title claims abstract description 53
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 229920001971 elastomer Polymers 0.000 claims abstract description 33
- 229920001021 polysulfide Polymers 0.000 claims abstract description 33
- 239000005077 polysulfide Substances 0.000 claims abstract description 33
- 150000008117 polysulfides Polymers 0.000 claims abstract description 33
- 239000000945 filler Substances 0.000 claims abstract description 22
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 16
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000004014 plasticizer Substances 0.000 claims abstract description 16
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims abstract description 11
- 239000007822 coupling agent Substances 0.000 claims abstract description 11
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 11
- 239000012975 dibutyltin dilaurate Substances 0.000 claims abstract description 11
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 11
- 239000002131 composite material Substances 0.000 claims abstract description 6
- -1 silicon-phosphorus compound Chemical class 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims description 26
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 15
- 239000000565 sealant Substances 0.000 claims description 15
- 229910000077 silane Inorganic materials 0.000 claims description 15
- IRIAEXORFWYRCZ-UHFFFAOYSA-N Butylbenzyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCC1=CC=CC=C1 IRIAEXORFWYRCZ-UHFFFAOYSA-N 0.000 claims description 10
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 238000004898 kneading Methods 0.000 claims description 10
- 229920005989 resin Polymers 0.000 claims description 10
- 239000011347 resin Substances 0.000 claims description 10
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 5
- 239000005995 Aluminium silicate Substances 0.000 claims description 5
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical group CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 5
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 5
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 5
- 235000012211 aluminium silicate Nutrition 0.000 claims description 5
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 5
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- 239000006229 carbon black Substances 0.000 claims description 5
- 239000000084 colloidal system Substances 0.000 claims description 5
- 239000003822 epoxy resin Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 5
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 5
- 229920000647 polyepoxide Polymers 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 150000003505 terpenes Chemical class 0.000 claims description 5
- 235000007586 terpenes Nutrition 0.000 claims description 5
- 239000004408 titanium dioxide Substances 0.000 claims description 5
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 abstract description 8
- 239000001301 oxygen Substances 0.000 abstract description 8
- 239000000779 smoke Substances 0.000 abstract description 6
- 229910052736 halogen Inorganic materials 0.000 abstract description 5
- 150000002367 halogens Chemical class 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000006260 foam Substances 0.000 abstract description 3
- 238000009413 insulation Methods 0.000 abstract description 3
- 238000002955 isolation Methods 0.000 abstract description 3
- 231100000053 low toxicity Toxicity 0.000 abstract description 3
- 230000001629 suppression Effects 0.000 abstract description 3
- ZFOZVQLOBQUTQQ-UHFFFAOYSA-N Tributyl citrate Chemical compound CCCCOC(=O)CC(O)(C(=O)OCCCC)CC(=O)OCCCC ZFOZVQLOBQUTQQ-UHFFFAOYSA-N 0.000 description 6
- 238000002485 combustion reaction Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000012188 paraffin wax Substances 0.000 description 3
- 239000004590 silicone sealant Substances 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 229910000410 antimony oxide Inorganic materials 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 239000004588 polyurethane sealant Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J181/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur, with or without nitrogen, oxygen, or carbon only; Adhesives based on polysulfones; Adhesives based on derivatives of such polymers
- C09J181/04—Polysulfides
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention relates to an environment-friendly flame-retardant polysulfide sealant, which consists of the following components in percentage by mass: 25-60% of liquid polysulfide rubber, 5-20% of intumescent flame retardant, 1-20% of tackifier, 10-15% of plasticizer, 5-15% of 201 methyl silicone oil, 5-20% of dibutyltin dilaurate, 1-5% of cross-linking agent, 1-5% of coupling agent, 15-20% of filler and 5-10% of antioxidant, wherein the intumescent flame retardant is a silicon-phosphorus compound composite flame retardant. When the flame-retardant polysulfide sealant is heated, a uniform carbonaceous foam layer can be generated on the surface of the flame-retardant polysulfide sealant, and the flame-retardant polysulfide sealant has the functions of heat insulation, oxygen isolation and smoke suppression, and can prevent molten drops from being generated, so that the flame-retardant polysulfide sealant has good flame-retardant performance, accords with the development trend of the current flame retardant requiring less smoke and low toxicity, not only has good flame-retardant performance, but also improves the safety in use, and simultaneously accords with the requirement of environmental protection by the characteristic of no halogen.
Description
Technical Field
The invention relates to the technical field of sealants, in particular to an environment-friendly flame-retardant polysulfide sealant and a production method thereof.
Background
The elastic polysulfide rubber compound formed by vulcanization is widely used as a sealant in the industries of traffic, construction, petrochemical industry and the like. The known polysulfide sealant is a two-component sealing material prepared by taking polysulfide rubber as a matrix, adding a proper amount of filler, auxiliary agent and curing agent, and mechanically mixing.
In modern industrial production, particularly in the building industry and vehicle applications, sealants are required to have dual functions of sealing and bonding, and also to have good aging resistance, fatigue resistance, flexibility and the like. Silicone, polyurethane and polysulfide sealants are mostly used as known building, automobile and high-speed train sealants. The silicone sealant has general adhesive property and higher cost; the polyurethane sealant has poor solvent resistance and atmospheric aging resistance. The polysulfide sealant has the characteristics of reasonable cost, good bonding performance, good weather resistance, good solvent resistance and the like, and becomes an important sealant.
In the prior art, the polysulfide sealant is easy to combust in the air, has poor flame retardance, and easily causes certain potential safety hazard in the use process, so the production process of the polysulfide sealant in the aspect of flame retardance needs to be improved to obtain the environment-friendly flame-retardant polysulfide sealant.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the environment-friendly flame-retardant polysulfide sealant and the production method thereof, wherein the polysulfide sealant has good flame-retardant performance, and the safety in use is improved so as to meet the increasing demands of the market on the environment-friendly flame-retardant polysulfide sealant.
The above object of the present invention is achieved by the following technical solutions:
the environment-friendly flame-retardant polysulfide sealant comprises the following components in percentage by mass: 25-60% of liquid polysulfide rubber, 5-20% of intumescent flame retardant, 1-20% of tackifier, 10-15% of plasticizer, 5-15% of 201 methyl silicone oil, 5-20% of dibutyltin dilaurate, 1-5% of cross-linking agent, 1-5% of coupling agent, 15-20% of filler and 5-10% of antioxidant, wherein the intumescent flame retardant is a silicon-phosphorus compound composite flame retardant.
The present invention in a preferred example may be further configured to: the weight average molecular weight of the liquid polysulfide rubber is 4500.
The present invention in a preferred example may be further configured to: the tackifier is any one or a mixture of any more of rosin resin, terpene resin, epoxy resin and polyvinyl butyral.
The present invention in a preferred example may be further configured to: the plasticizer is any one or a mixture of any more of dibutyl phthalate, dioctyl phthalate, butyl benzyl phthalate and tributyl chloroparaffin citrate.
The present invention in a preferred example may be further configured to: the filler is any one or a mixture of any more of nano calcium carbonate, titanium dioxide, kaolin and carbon black.
The present invention in a preferred example may be further configured to: the antioxidant is 2, 6-di-tert-butyl-p-cresol.
A production method of an environment-friendly flame-retardant polysulfide sealant comprises the following steps: taking the raw materials for preparing the environment-friendly flame-retardant polysulfide sealant according to the sealant formula of any one of the claims 1 to 6:
s1: preparing silane modified polysulfide rubber, mixing liquid polysulfide rubber, a coupling agent and 201 methyl silicone oil according to a certain proportion, and carrying out mixing reaction at the temperature of 150 ℃ for 0.5h to obtain the silane modified polysulfide rubber;
s2: drying, namely drying the filler, the intumescent flame retardant and the antioxidant for 1.5 hours at the temperature of between 90 and 95 ℃;
s3: mixing, namely putting the dried filler, the intumescent flame retardant, the silane modified polysulfide rubber, the tackifier and the plasticizer into a vacuum kneading machine, heating and kneading uniformly, pouring into a double-planet stirring machine, adding the crosslinking agent and dibutyltin dilaurate according to the proportion, and mixing uniformly;
s4: grinding and dehydrating, grinding the paste obtained after mixing by a colloid mill, and dehydrating in a vacuum state by a reaction kettle to obtain the environment-friendly flame-retardant polysulfide sealant.
In conclusion, the beneficial technical effects of the invention are as follows:
1. the sealant contains a flame retardant, and the flame retardant can reduce the surface temperature of a combustion object, dilute the molecular concentration of the combustible object and cut off the supply of oxygen to achieve the flame retardant effect. The intumescent flame retardant is an environment-friendly flame retardant which develops very quickly, takes phosphorus and nitrogen as main active ingredients, does not contain halogen, and does not adopt antimony oxide as a synergist.
When the flame-retardant polysulfide sealant is heated, a uniform carbonaceous foam layer can be generated on the surface of the flame-retardant polysulfide sealant, and the flame-retardant polysulfide sealant has the functions of heat insulation, oxygen isolation and smoke suppression, and can prevent molten drops from being generated, so that the flame-retardant polysulfide sealant has good flame-retardant performance, accords with the development trend of the current flame retardant requiring less smoke and low toxicity, not only has good flame-retardant performance, but also improves the safety in use, and simultaneously accords with the requirement of environmental protection by the characteristic of no halogen.
2. The sealant has the advantages of wide viscosity adjusting range, good adhesiveness, easy construction and simple preparation process, ensures the performance, and avoids the inflammability in the air.
Drawings
FIG. 1 is a graph showing the effect of flame retardant amount on flame retardancy according to the present invention.
FIG. 2 is a schematic process flow diagram of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
The first embodiment is as follows:
the environment-friendly flame-retardant polysulfide sealant comprises the following components in percentage by mass: 25% of liquid polysulfide rubber, 5% of intumescent flame retardant, 1% of tackifier, 10% of plasticizer, 5% of 201 methyl silicone oil, 5% of dibutyltin dilaurate, 1% of cross-linking agent, 1% of coupling agent, 15% of filler and 5% of antioxidant, wherein the intumescent flame retardant is a silicon-phosphorus compound composite flame retardant.
Wherein the weight average molecular weight of the liquid polysulfide rubber is 4500, and the tackifier is any one or mixture of any several of rosin resin, terpene resin, epoxy resin and polyvinyl butyral. The plasticizer is any one or a mixture of any more of dibutyl phthalate, dioctyl phthalate, butyl benzyl phthalate and tributyl citrate chlorinated paraffin. The filler is any one or a mixture of any more of nano calcium carbonate, titanium dioxide, kaolin and carbon black, and the antioxidant is 2, 6-di-tert-butyl-p-cresol.
Referring to fig. 1, a method for producing an environment-friendly flame-retardant polysulfide sealant comprises the following steps: taking the raw materials for preparing the environment-friendly flame-retardant polysulfide sealant according to the sealant formula:
s1: preparing silane modified polysulfide rubber, mixing liquid polysulfide rubber, a coupling agent and 201 methyl silicone oil according to a certain proportion, and carrying out mixing reaction at the temperature of 150 ℃ for 0.5h to obtain the silane modified polysulfide rubber;
s2: drying, namely drying the filler, the intumescent flame retardant and the antioxidant for 1.5 hours at the temperature of between 90 and 95 ℃;
s3: mixing, namely putting the dried filler, the intumescent flame retardant, the silane modified polysulfide rubber, the tackifier and the plasticizer into a vacuum kneading machine, heating and kneading uniformly, pouring into a double-planet stirring machine, adding the crosslinking agent and dibutyltin dilaurate according to the proportion, and mixing uniformly;
s4: grinding and dehydrating, grinding the paste obtained after mixing by a colloid mill, and dehydrating in a vacuum state by a reaction kettle to obtain the environment-friendly flame-retardant polysulfide sealant.
Example two:
the environment-friendly flame-retardant polysulfide sealant comprises the following components in percentage by mass: 60% of liquid polysulfide rubber, 20% of intumescent flame retardant, 20% of tackifier, 15% of plasticizer, 15% of 201 methyl silicone oil, 20% of dibutyltin dilaurate, 5% of cross-linking agent, 5% of coupling agent, 20% of filler and 10% of antioxidant, wherein the intumescent flame retardant is a silicon-phosphorus compound composite flame retardant.
Wherein the weight average molecular weight of the liquid polysulfide rubber is 4500, and the tackifier is any one or mixture of any several of rosin resin, terpene resin, epoxy resin and polyvinyl butyral. The plasticizer is any one or a mixture of any more of dibutyl phthalate, dioctyl phthalate, butyl benzyl phthalate and tributyl citrate chlorinated paraffin. The filler is any one or a mixture of any more of nano calcium carbonate, titanium dioxide, kaolin and carbon black, and the antioxidant is 2, 6-di-tert-butyl-p-cresol.
Referring to fig. 1, a method for producing an environment-friendly flame-retardant polysulfide sealant comprises the following steps: taking the raw materials for preparing the environment-friendly flame-retardant polysulfide sealant according to the sealant formula:
s1: preparing silane modified polysulfide rubber, mixing liquid polysulfide rubber, a coupling agent and 201 methyl silicone oil according to a certain proportion, and carrying out mixing reaction at the temperature of 150 ℃ for 0.5h to obtain the silane modified polysulfide rubber;
s2: drying, namely drying the filler, the intumescent flame retardant and the antioxidant for 1.5 hours at the temperature of between 90 and 95 ℃;
s3: mixing, namely putting the dried filler, the intumescent flame retardant, the silane modified polysulfide rubber, the tackifier and the plasticizer into a vacuum kneading machine, heating and kneading uniformly, pouring into a double-planet stirring machine, adding the crosslinking agent and dibutyltin dilaurate according to the proportion, and mixing uniformly;
s4: grinding and dehydrating, grinding the paste obtained after mixing by a colloid mill, and dehydrating in a vacuum state by a reaction kettle to obtain the environment-friendly flame-retardant polysulfide sealant.
Example three:
the environment-friendly flame-retardant polysulfide sealant comprises the following components in percentage by mass: 42.5 percent of liquid polysulfide rubber, 12.5 percent of intumescent flame retardant, 10.5 percent of tackifier, 12.5 percent of plasticizer, 10 percent of 201 methyl silicone oil, 12.5 percent of dibutyltin dilaurate, 3 percent of cross-linking agent, 3 percent of coupling agent, 17.5 percent of filler and 7.5 percent of antioxidant, wherein the intumescent flame retardant is silicon-phosphorus compound composite flame retardant.
Wherein the weight average molecular weight of the liquid polysulfide rubber is 4500, and the tackifier is any one or mixture of any several of rosin resin, terpene resin, epoxy resin and polyvinyl butyral. The plasticizer is any one or a mixture of any more of dibutyl phthalate, dioctyl phthalate, butyl benzyl phthalate and tributyl citrate chlorinated paraffin. The filler is any one or a mixture of any more of nano calcium carbonate, titanium dioxide, kaolin and carbon black, and the antioxidant is 2, 6-di-tert-butyl-p-cresol.
Referring to fig. 1, a method for producing an environment-friendly flame-retardant polysulfide sealant comprises the following steps: taking the raw materials for preparing the environment-friendly flame-retardant polysulfide sealant according to the sealant formula:
s1: preparing silane modified polysulfide rubber, mixing liquid polysulfide rubber, a coupling agent and 201 methyl silicone oil according to a certain proportion, and carrying out mixing reaction at the temperature of 150 ℃ for 0.5h to obtain the silane modified polysulfide rubber;
s2: drying, namely drying the filler, the intumescent flame retardant and the antioxidant for 1.5 hours at the temperature of between 90 and 95 ℃;
s3: mixing, namely putting the dried filler, the intumescent flame retardant, the silane modified polysulfide rubber, the tackifier and the plasticizer into a vacuum kneading machine, heating and kneading uniformly, pouring into a double-planet stirring machine, adding the crosslinking agent and dibutyltin dilaurate according to the proportion, and mixing uniformly;
s4: grinding and dehydrating, grinding the paste obtained after mixing by a colloid mill, and dehydrating in a vacuum state by a reaction kettle to obtain the environment-friendly flame-retardant polysulfide sealant.
In order to make the disclosure of the specification more complete, the following experimental data for testing the flame retardant performance of the environment-friendly flame-retardant polysulfide sealant is provided, and refer to fig. 2, which is a data diagram of the influence of the amount of the flame retardant on the flame retardant performance.
As can be seen from figure 2, when the addition part of the flame retardant is not more than 50 parts, the flame retardant property of the sealant is obviously improved along with the increase of the flame retardant preparation amount. When the using amount of the flame retardant reaches 50 parts, the combustion oxygen index of the flame-retardant polysulfide sealant is 42, and the flame-retardant grade reaches FV-0; when the using amount of the flame retardant is more than 50 parts, the using amount is increased, and the rising trend of the flame retardant performance is slowed down.
When the combustion oxygen index is 24-28, the material has slight flame retardance; the material has flame retardance when the combustion oxygen index is 29-35. Therefore, as can be seen from table 2, the flame retardant silicone sealant is slightly flame retardant when the amount of the flame retardant is 30-40 parts; when the dosage of the flame retardant exceeds 40 parts, the flame-retardant polysulfide sealant has excellent flame retardance.
The implementation principle of the embodiment is as follows: the sealant contains a flame retardant, and the flame retardant can reduce the surface temperature of a combustion object, dilute the molecular concentration of the combustible object and cut off the supply of oxygen to achieve the flame retardant effect. The intumescent flame retardant is an environment-friendly flame retardant which develops very quickly, takes phosphorus and nitrogen as main active ingredients, does not contain halogen, and does not adopt antimony oxide as a synergist.
When the flame-retardant polysulfide sealant is heated, a uniform carbonaceous foam layer can be generated on the surface of the flame-retardant polysulfide sealant, and the flame-retardant polysulfide sealant has the functions of heat insulation, oxygen isolation and smoke suppression, and can prevent molten drops from being generated, so that the flame-retardant polysulfide sealant has good flame-retardant performance, accords with the development trend of the current flame retardant requiring less smoke and low toxicity, not only has good flame-retardant performance, but also improves the safety in use, and simultaneously accords with the requirement of environmental protection by the characteristic of no halogen.
The embodiments of the present invention are preferred embodiments of the present invention, and the scope of the present invention is not limited by these embodiments, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.
Claims (7)
1. An environment-friendly flame-retardant polysulfide sealant is characterized in that: the sealant consists of the following components in percentage by mass: 25-60% of liquid polysulfide rubber, 5-20% of intumescent flame retardant, 1-20% of tackifier, 10-15% of plasticizer, 5-15% of 201 methyl silicone oil, 5-20% of dibutyltin dilaurate, 1-5% of cross-linking agent, 1-5% of coupling agent, 15-20% of filler and 5-10% of antioxidant, wherein the intumescent flame retardant is a silicon-phosphorus compound composite flame retardant.
2. The environment-friendly flame-retardant polysulfide sealant as claimed in claim 1, characterized in that: the weight average molecular weight of the liquid polysulfide rubber is 4500.
3. The environment-friendly flame-retardant polysulfide sealant as claimed in claim 1, characterized in that: the tackifier is any one or a mixture of any more of rosin resin, terpene resin, epoxy resin and polyvinyl butyral.
4. The environment-friendly flame-retardant polysulfide sealant as claimed in claim 1, characterized in that: the plasticizer is any one or a mixture of any more of dibutyl phthalate, dioctyl phthalate, butyl benzyl phthalate and tributyl chloroparaffin citrate.
5. The environment-friendly flame-retardant polysulfide sealant as claimed in claim 1, characterized in that: the filler is any one or a mixture of any more of nano calcium carbonate, titanium dioxide, kaolin and carbon black.
6. The environment-friendly flame-retardant polysulfide sealant as claimed in claim 1, characterized in that: the antioxidant is 2, 6-di-tert-butyl-p-cresol.
7. The production method of the environment-friendly flame-retardant polysulfide sealant is characterized by comprising the following steps: the method comprises the following steps: taking the raw materials for preparing the environment-friendly flame-retardant polysulfide sealant according to the sealant formula of any one of the claims 1 to 6:
s1: preparing silane modified polysulfide rubber, mixing liquid polysulfide rubber, a coupling agent and 201 methyl silicone oil according to a certain proportion, and carrying out mixing reaction at the temperature of 150 ℃ for 0.5h to obtain the silane modified polysulfide rubber;
s2: drying, namely drying the filler, the intumescent flame retardant and the antioxidant for 1.5 hours at the temperature of between 90 and 95 ℃;
s3: mixing, namely putting the dried filler, the intumescent flame retardant, the silane modified polysulfide rubber, the tackifier and the plasticizer into a vacuum kneading machine, heating and kneading uniformly, pouring into a double-planet stirring machine, adding the crosslinking agent and dibutyltin dilaurate according to the proportion, and mixing uniformly;
s4: grinding and dehydrating, grinding the paste obtained after mixing by a colloid mill, and dehydrating in a vacuum state by a reaction kettle to obtain the environment-friendly flame-retardant polysulfide sealant.
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Application publication date: 20210514 |