CN114316605A - Transparent flame-retardant silicone rubber and preparation method thereof - Google Patents
Transparent flame-retardant silicone rubber and preparation method thereof Download PDFInfo
- Publication number
- CN114316605A CN114316605A CN202111683439.5A CN202111683439A CN114316605A CN 114316605 A CN114316605 A CN 114316605A CN 202111683439 A CN202111683439 A CN 202111683439A CN 114316605 A CN114316605 A CN 114316605A
- Authority
- CN
- China
- Prior art keywords
- flame
- retardant
- silicone rubber
- parts
- transparent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 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 123
- 239000003063 flame retardant Substances 0.000 title claims abstract description 123
- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 98
- 239000004945 silicone rubber Substances 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000000463 material Substances 0.000 claims abstract description 37
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 33
- 239000003054 catalyst Substances 0.000 claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 claims description 24
- 238000009489 vacuum treatment Methods 0.000 claims description 13
- 238000004898 kneading Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 8
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 7
- 229920001971 elastomer Polymers 0.000 claims description 6
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000005060 rubber Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- -1 polydimethylsiloxane Polymers 0.000 claims description 5
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 claims description 5
- 239000006229 carbon black Substances 0.000 claims description 4
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 claims description 4
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 4
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 3
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- ZTOTXIJTXLDCFH-UHFFFAOYSA-N O(P(OCCCCCCCCCCCCCCCCCC)OP(O)O)CCCCCCCCCCCCCCCCCC.OCC(CO)(CO)CO Chemical compound O(P(OCCCCCCCCCCCCCCCCCC)OP(O)O)CCCCCCCCCCCCCCCCCC.OCC(CO)(CO)CO ZTOTXIJTXLDCFH-UHFFFAOYSA-N 0.000 claims description 2
- BGHBLQKNCVRIKV-UHFFFAOYSA-N OP(O)OP(O)O.OCC(CO)(CO)CO.C(C)(C)(C)C1=C(C=CC(=C1)C(C)(C)C)O.C(C)(C)(C)C1=C(C=CC(=C1)C(C)(C)C)O Chemical compound OP(O)OP(O)O.OCC(CO)(CO)CO.C(C)(C)(C)C1=C(C=CC(=C1)C(C)(C)C)O.C(C)(C)(C)C1=C(C=CC(=C1)C(C)(C)C)O BGHBLQKNCVRIKV-UHFFFAOYSA-N 0.000 claims description 2
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 2
- 239000003921 oil Substances 0.000 claims 2
- KUMNEOGIHFCNQW-UHFFFAOYSA-N diphenyl phosphite Chemical compound C=1C=CC=CC=1OP([O-])OC1=CC=CC=C1 KUMNEOGIHFCNQW-UHFFFAOYSA-N 0.000 claims 1
- 239000006082 mold release agent Substances 0.000 claims 1
- 238000002834 transmittance Methods 0.000 abstract description 6
- 230000000052 comparative effect Effects 0.000 description 9
- 238000004073 vulcanization Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- 229920002545 silicone oil Polymers 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- PZRWFKGUFWPFID-UHFFFAOYSA-N 3,9-dioctadecoxy-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane Chemical compound C1OP(OCCCCCCCCCCCCCCCCCC)OCC21COP(OCCCCCCCCCCCCCCCCCC)OC2 PZRWFKGUFWPFID-UHFFFAOYSA-N 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 3
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 3
- 239000012964 benzotriazole Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 3
- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NRLOQEQAWOKEJF-UHFFFAOYSA-N (6-methyl-1,1-diphenylheptyl) dihydrogen phosphite Chemical compound C=1C=CC=CC=1C(OP(O)O)(CCCCC(C)C)C1=CC=CC=C1 NRLOQEQAWOKEJF-UHFFFAOYSA-N 0.000 description 1
- DMWVYCCGCQPJEA-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane Chemical compound CC(C)(C)OOC(C)(C)CCC(C)(C)OOC(C)(C)C DMWVYCCGCQPJEA-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 1
- 239000008116 calcium stearate Substances 0.000 description 1
- 235000013539 calcium stearate Nutrition 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- JUWSSMXCCAMYGX-UHFFFAOYSA-N gold platinum Chemical compound [Pt].[Au] JUWSSMXCCAMYGX-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- UCNNJGDEJXIUCC-UHFFFAOYSA-L hydroxy(oxo)iron;iron Chemical compound [Fe].O[Fe]=O.O[Fe]=O UCNNJGDEJXIUCC-UHFFFAOYSA-L 0.000 description 1
- 239000012796 inorganic flame retardant Substances 0.000 description 1
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 description 1
- 235000019359 magnesium stearate Nutrition 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 238000010060 peroxide vulcanization Methods 0.000 description 1
- 150000008301 phosphite esters Chemical class 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a transparent flame-retardant silicone rubber which is prepared from the following materials in parts by weight: 100 parts of silicon rubber, 0.5-4 parts of platinum catalyst and 0.05-2 parts of flame-retardant synergist, wherein the flame-retardant synergist is prepared from 100 parts of basic silicon rubber and 0.5-6 parts of flame-retardant material. The transparent flame-retardant silicone rubber has good flame-retardant performance, and can keep excellent mechanical property and good light transmittance. The invention also provides a preparation method of the transparent flame-retardant silicone rubber.
Description
Technical Field
The invention relates to the technical field of silicone rubber, and particularly relates to transparent flame-retardant silicone rubber and a preparation method thereof.
Background
In recent years, the application of flame-retardant silicone rubber in various industries is more and more extensive. With the continuous progress of flame retardant technology, the requirements on flame retardant silicone rubber products are higher and higher. In some special application fields, the silicone rubber material is required to have excellent flame retardant property, and simultaneously, the silicone rubber material is required to have better transparency and mechanical property. The traditional halogen-free flame-retardant silicone rubber material is usually filled with environment-friendly inorganic flame-retardant fillers such as aluminum hydroxide, magnesium hydroxide and the like to improve the flame retardance, and has the defect that a good flame-retardant effect can be achieved only by filling a large amount of fillers. Therefore, the addition of aluminum hydroxide and magnesium hydroxide in large amounts can greatly reduce the mechanical properties of the silicone rubber material while improving the flame retardancy. By compounding a platinum catalyst and iron black or iron red, the using amount of the flame-retardant filler can be reduced, but the method cannot meet the requirement in the application field with color or transparency requirement.
At present, the method for preparing the transparent flame-retardant silicone rubber achieves the purposes of transparency and flame retardance by compounding a platinum catalyst and benzotriazole. However, the method has the limitation that the platinum catalyst is poisoned and fails under the action of benzotriazole, and cannot be applied to platinum sulfidation. For the application of adding the bis-tetrakissilica vulcanizing agent extrusion system, the active hydrogen in the benzotriazole can also influence the vulcanization of the bis-tetrakissilica vulcanizing agent. Therefore, the existing method for preparing the transparent flame-retardant silicone rubber is only suitable for products which are added with the double-two-five silica gel vulcanizing agent and are molded, and the application of the transparent flame-retardant silicone rubber in other fields is limited to a great extent.
Therefore, it is necessary to develop a transparent flame-retardant silicone rubber and a method for preparing the same to solve the above technical disadvantages.
Disclosure of Invention
The invention aims to provide transparent flame-retardant silicone rubber which has good flame-retardant performance and can keep excellent mechanical properties and good light transmittance.
The second purpose of the invention is to provide a preparation method of the transparent flame-retardant silicone rubber with wide application range.
In order to achieve the purpose, the invention discloses a transparent flame-retardant silicone rubber which comprises the following preparation materials in parts by weight: 100 parts of silicon rubber, 0.5-4 parts of platinum catalyst and 0.05-2 parts of flame-retardant synergist, wherein the flame-retardant synergist is prepared from 100 parts of basic silicon rubber and 0.5-6 parts of flame-retardant material.
Specifically, the transparent flame-retardant silicone rubber comprises the following preparation materials in parts by weight: 100 parts of silicone rubber, 1-3 parts of platinum catalyst and 0.1-1 part of flame-retardant synergist, wherein the preparation material of the flame-retardant synergist comprises 100 parts of base silicone rubber and 1-5 parts of flame-retardant material.
Preferably, the transparent flame-retardant silicone rubber is prepared from the following materials in parts by weight: 100 parts of silicon rubber, 1-3 parts of platinum catalyst and 0.4-0.8 part of flame retardant synergist.
Preferably, the silicone rubber comprises, by weight, 100 parts of methyl vinyl silicone rubber, 15-75 parts of white carbon black, 2-15 parts of a structure control agent and 0.1-3 parts of a release agent.
Preferably, the structure control agent is one or more selected from hexamethyldisilazane, hydroxy silicone oil, vinyl hydroxy silicone oil, dimethyl dimethoxy silane, dimethyl diethoxy silane and methoxy terminated polydimethylsiloxane (CAS: 68037-58-1).
Preferably, the flame retardant material is phosphite ester as the flame retardant material, which is selected from one or more of tris (2, 4-di-tert-butylphenyl) phosphite (antioxidant 168), bis (2, 4-di-tert-butylphenol) pentaerythritol diphosphite (antioxidant 626), pentaerythritol dioctadecyl diphosphite (antioxidant 618), poly (dipropylene glycol) phenyl phosphite (PDP), triphenyl phosphite (TPP) and diphenylisooctyl phosphite (DPIOP).
Preferably, the preparation method of the flame retardant synergist comprises the following steps:
(1) putting the base silicone rubber into a kneading machine and heating;
(2) kneading the heated base silicone rubber and adding a flame retardant material;
(3) and when the set temperature is reached, performing vacuum treatment to obtain the flame-retardant synergist.
Preferably, the temperature of the base silicone rubber in the step (1) is increased to 180-200 ℃; kneading for 8-15 minutes in the step (2), and adding a flame-retardant material; and (4) when the temperature of the mixed material of the basic silicone rubber and the flame retardant material in the step (3) reaches 145-155 ℃, performing vacuum treatment for 25-35 minutes to obtain the flame retardant synergist.
Correspondingly, the invention also provides a preparation method of the transparent flame-retardant silicone rubber, which comprises the following steps:
(1) uniformly mixing the silicon rubber and the flame-retardant synergist in proportion to obtain a base rubber;
(2) and adding a platinum catalyst into the base rubber, kneading into a cluster, and performing vacuum treatment to obtain the transparent flame-retardant silicone rubber.
Preferably, the mixing time in the step (1) is 3-6 minutes; and (3) performing vacuum treatment for 25-35 minutes in the step (2), wherein the temperature is controlled to be below 60 ℃ during the vacuum treatment.
Compared with the prior art, the invention has the following advantages:
(1) according to the invention, a platinum catalyst is used as a main flame retardant, the platinum catalyst has dual functions of catalysis and flame retardance at the same time, and the flame retardant synergist is compounded to realize flame retardant and transparent effects. The platinum catalyst can inhibit the decomposition of the silicone rubber to form flammable low molecular siloxane when the silicone rubber is burnt, and simultaneously improves the flame retardant property of the silicone rubber under the combined action of the catalytic action of the flame retardant synergist in a condensed phase and the capture of free radicals in a gas phase. And the silicone rubber can still keep excellent mechanical property and better light transmittance while improving the flame retardant property.
(2) The invention is suitable for peroxide vulcanization systems and platinum vulcanization systems, can solve the problem that the existing transparent flame-retardant adhesive cannot be vulcanized by platinum, and has wide application range.
(3) By the preparation method of the flame-retardant synergist, the flame-retardant synergist is prepared from the basic silicone rubber and the phosphite flame-retardant material, so that the problem that phosphite cannot be dispersed in the silicone rubber is solved, and the application range of phosphite is expanded.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Firstly, the components and contents of the material for preparing the transparent flame-retardant silicone rubber in the embodiment 1 and the preparation method of the transparent flame-retardant silicone rubber are as follows.
The transparent flame-retardant silicone rubber comprises the following preparation materials in parts by weight: 100 parts of silicon rubber, 1 part of platinum catalyst and 0.4 part of flame-retardant synergist, wherein the preparation material of the flame-retardant synergist comprises 100 parts of base silicon rubber and 2 parts of antioxidant 168.
In this example, the silicone rubber includes 100 parts of methyl vinyl silicone rubber, 30 parts of white carbon black, 4 parts of a structure-controlling agent, and 0.2 parts of a mold-releasing agent. In this example, the structure-controlling agent was a hydroxy silicone oil and the release agent was stearic acid. Specifically, the structure control agent can be one or more selected from hexamethyldisilazane, hydroxy silicone oil, vinyl hydroxy silicone oil, dimethyldimethoxysilane, dimethyldiethoxysilane and methoxy-terminated polydimethylsiloxane. The release agent can be one or more selected from methyl silicone oil, stearic acid, zinc stearate, calcium stearate and magnesium stearate. The weight portion of the methyl vinyl silicone rubber can be 100 portions, the weight portion of the white carbon black can be 15 portions, 30 portions, 45 portions, 60 portions and 75 portions, the weight portion of the structure control agent can be 2 portions, 4 portions, 6 portions, 9 portions, 13 portions and 15 portions, and the weight portion of the release agent can be 0.1 portion, 0.5 portion, 1 portion, 1.5 portions, 2 portions and 2.5 portions.
In addition, it is to be noted that the base silicone rubber and the silicone rubber are the same substance in the present invention.
The preparation method of the flame-retardant synergist comprises the following steps:
(1) adding the base silicone rubber into a kneader and heating to 195 ℃;
(2) kneading the heated basic silicone rubber for 10 minutes, and adding a flame-retardant material tris (2, 4-di-tert-butylphenyl) phosphite;
(3) and when the temperature reaches 150 ℃, performing vacuum treatment for 30 minutes to obtain the flame-retardant synergist.
Specifically, the base silicone rubber in step (1) may be heated to 180 ℃, 185 ℃, 190 ℃, 195 ℃, 200 ℃; the kneading time in the step (2) may be 8 minutes, 10 minutes, 12 minutes, 15 minutes; and (3) the temperature of the mixed material of the basic silicone rubber and the flame-retardant material in the step (3) can reach 145 ℃, 150 ℃ and 155 ℃, and the vacuum treatment time can be 25 minutes, 30 minutes and 35 minutes, so as to obtain the flame-retardant synergist.
The invention also provides a preparation method of the transparent flame-retardant silicone rubber, which comprises the following steps:
(1) mixing the silicon rubber and the flame-retardant synergist in a kneading machine for 5 minutes according to a proportion, and uniformly mixing to obtain a base rubber;
(2) adding a platinum catalyst into the base rubber, kneading into a cluster, and performing vacuum treatment at 55 ℃ for 30 minutes to obtain the transparent flame-retardant silicone rubber.
Secondly, the components and contents of the materials for preparing the transparent flame-retardant silicone rubber in examples 1 to 12 and comparative examples 1 to 3 and the preparation method of the transparent flame-retardant silicone rubber are as follows.
TABLE 1 Components and amounts of materials for preparing transparent flame-retardant silicone rubbers and Components and amounts of flame-retardant synergists in examples 1 to 13 and comparative examples 1 to 3
The rest of examples 2 to 12 are the same as example 1 and are not specifically described here.
And thirdly, testing the mechanical property, the flame retardant property and the light transmittance of the samples 1 to 12 and the comparative samples 1 to 3. Testing the mechanical properties according to GB/T528-; the flame retardant performance is tested according to UL94 flame retardant rating test standard and the light transmittance of the product is tested according to GB T2410-.
The vulcanization conditions are as follows: bis (dipentaerythritol) vulcanizing agent (2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane), the addition amount is 0.7 percent, and the molding conditions are as follows: temperature 175 ℃ for 5 minutes.
The transparent flame-retardant silicone rubbers prepared in examples 1 to 12 and comparative examples 1 to 3 were vulcanized by a dipentaerythritol vulcanizing agent and then subjected to a performance test, and the test results are shown in table 2.
The test items and the method are as follows:
table 2 performance test results of transparent flame-retardant silicone rubber
And (3) analyzing an experimental result:
as can be seen from the flame retardant performance data of comparative examples 1-3, the flame retardant performance of the silicone rubber is not improved by adding 1 part of the flame retardant synergist alone, and when 1 part of the platinum catalyst is added, the flame retardant performance of the prepared silicone rubber is improved, but the flame retardant level can not be reached, and the silicone rubber is not rated. However, by compounding the platinum catalyst and the flame retardant synergist, the flame retardant properties of the transparent flame retardant silicone rubber prepared in examples 1-12 are all improved to different degrees, reaching the UL94V 1 rating. Meanwhile, with the addition of the platinum catalyst and the flame-retardant synergist, the strength and the transparency of the transparent flame-retardant silicone rubber can still keep the level similar to that of the silicone rubber. The data of examples 1-4 show that the flame retardant rating of UL94V-1 can be achieved when the amount of the flame retardant synergist is between 0.4 and 1.0 while the amount of the platinum catalyst is kept unchanged. The data of examples 1 and 5-6 show that the flame retardant effect is similar when the flame retardant material content of the flame retardant synergist is similar in the whole silicone rubber system. However, as examples 1, 7 and 8, the flame retardant performance can be further improved as the amount of the platinum catalyst is increased. The test results of examples 9-10 show that the synergistic flame retardant effect of the antioxidant 626 and the antioxidant 618 is not obviously different from that of the antioxidant 168; the test results of example 4, example 11 and example 12 show that when the flame retardant synergist prepared from the antioxidant 168, the antioxidant 626 or the antioxidant 618 is used in an amount of more than 1 part, the flame retardant performance is reduced.
Fourthly, the examples 1 to 8 and the comparative example 3 are vulcanized by using a platinum vulcanizing agent under the following vulcanization conditions: the additive amount of the platinum vulcanizing agent A is 0.6 percent, and the additive amount of the platinum vulcanizing agent B is 1.5 percent; molding conditions are as follows: temperature 130 ℃ and time 5 minutes. The platinum vulcanizing agent is PTC-A/PTC-B9 platinum vulcanizing agent of Zi chemical industry (Zhongshan) Co. Table 3 below shows the performance data for platinum-gold vulcanized silicone rubbers of examples 1-8 and comparative example 3.
TABLE 3 Performance test results of transparent flame-retardant Silicone rubber
Note: comparative example 3 has no test data due to incomplete vulcanization.
At the vulcanization temperature of 130 ℃, when the comparative example 3 is vulcanized by using a platinum vulcanizing agent, the vulcanization is insufficient, which shows that the silicone rubber prepared by only adding the flame retardant synergist reduces the catalytic activity of the platinum catalyst, resulting in insufficient vulcanization. The data of examples 1-8 show that when the amount of the flame retardant synergist is less than 0.8 part and 1-3 parts of platinum catalyst is added, the transparent flame retardant silicone rubber can be normally subjected to platinum catalytic vulcanization at 130 ℃, and the strength and the light transmittance of the transparent flame retardant silicone rubber vulcanized rubber are kept at good levels.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the scope of the present invention, therefore, the present invention is not limited by the appended claims.
Claims (9)
1. The transparent flame-retardant silicone rubber is characterized by comprising the following preparation materials in parts by weight: 100 parts of silicone rubber, 0.5-4 parts of platinum catalyst and 0.05-2 parts of flame-retardant synergist, wherein the preparation material of the flame-retardant synergist comprises 100 parts of basic silicone rubber and 0.5-6 parts of flame-retardant material.
2. The transparent flame-retardant silicone rubber according to claim 1, wherein the preparation material comprises, in parts by weight: 100 parts of silicon rubber, 1-3 parts of platinum catalyst and 0.4-0.8 part of flame retardant synergist.
3. The transparent flame-retardant silicone rubber according to claim 1, wherein the silicone rubber comprises, by weight, 100 parts of methyl vinyl silicone rubber, 15 to 75 parts of white carbon black, 2 to 15 parts of a structure-controlling agent, and 0.1 to 3 parts of a mold release agent.
4. The transparent flame-retardant silicone rubber according to claim 1, wherein the structure-controlling agent is one or more selected from hexamethyldisilazane, hydroxysilicone oil, vinylhydroxysilicone oil, dimethyldimethoxysilane, dimethyldiethoxysilane, and methoxy-terminated polydimethylsiloxane.
5. The transparent flame-retardant silicone rubber according to claim 1, wherein the flame-retardant material is one or more selected from the group consisting of tris (2, 4-di-tert-butylphenyl) phosphite, bis (2, 4-di-tert-butylphenol) pentaerythritol diphosphite, pentaerythritol dioctadecyl diphosphite, poly (dipropylene glycol) phenyl phosphite, triphenyl phosphite, and diisooctyl diphenyl phosphite.
6. The transparent flame-retardant silicone rubber according to claim 1, wherein the preparation method of the flame-retardant synergist comprises the steps of:
(1) putting the base silicone rubber into a kneading machine and heating;
(2) kneading the heated base silicone rubber and adding a flame retardant material;
(3) and when the set temperature is reached, performing vacuum treatment to obtain the flame-retardant synergist.
7. The transparent flame-retardant silicone rubber according to claim 6, wherein in step (1), the base silicone rubber is heated to 180-200 ℃; kneading for 8-15 minutes in the step (2), and adding a flame-retardant material; and (4) when the temperature of the mixed material of the basic silicone rubber and the flame retardant material in the step (3) reaches 145-155 ℃, performing vacuum treatment for 25-35 minutes to obtain the flame retardant synergist.
8. A method for preparing the transparent flame-retardant silicone rubber according to any one of claims 1 to 7, comprising the steps of:
(1) uniformly mixing the silicon rubber and the flame-retardant synergist in proportion to obtain a base rubber;
(2) and adding a platinum catalyst into the base rubber, kneading into a cluster, and performing vacuum treatment to obtain the transparent flame-retardant silicone rubber.
9. The method for preparing transparent flame-retardant silicone rubber according to claim 8, wherein the mixing time in step (1) is 3 to 6 minutes; and (3) performing vacuum treatment for 25-35 minutes in the step (2), wherein the temperature is controlled to be below 60 ℃ during the vacuum treatment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111683439.5A CN114316605A (en) | 2021-12-31 | 2021-12-31 | Transparent flame-retardant silicone rubber and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111683439.5A CN114316605A (en) | 2021-12-31 | 2021-12-31 | Transparent flame-retardant silicone rubber and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114316605A true CN114316605A (en) | 2022-04-12 |
Family
ID=81023268
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111683439.5A Pending CN114316605A (en) | 2021-12-31 | 2021-12-31 | Transparent flame-retardant silicone rubber and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114316605A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115491038A (en) * | 2022-09-16 | 2022-12-20 | 广州市矽友新材料科技有限公司 | Halogen-free platinum flame retardant for silicone rubber and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07118536A (en) * | 1993-10-21 | 1995-05-09 | Shin Etsu Chem Co Ltd | Flame-reterdant silicone rubber composition |
| WO2017070893A1 (en) * | 2015-10-29 | 2017-05-04 | 国家纳米科学中心 | Ceramic silicone rubber, preparation method and use thereof |
| CN107903633A (en) * | 2017-11-27 | 2018-04-13 | 浙江新安化工集团股份有限公司 | A kind of melting silicone rubber and preparation method thereof |
| CN109504091A (en) * | 2018-10-24 | 2019-03-22 | 桂林裕天新材料有限公司 | A kind of low cigarette, flame-retardant silicone rubber rubber compound of high transparency and preparation method thereof |
| CN109880373A (en) * | 2019-01-21 | 2019-06-14 | 广州科系维新材料有限公司 | A kind of additive and preparation method thereof applied to transparent flame-retarding silicon rubber |
| CN112679959A (en) * | 2020-12-25 | 2021-04-20 | 浙江中特化工有限公司 | Transparent bi-component flame-retardant liquid silicone rubber filling material and preparation method thereof |
| JP2021127373A (en) * | 2020-02-12 | 2021-09-02 | 信越化学工業株式会社 | One-component millable type silicone rubber composition and cured product of the same |
-
2021
- 2021-12-31 CN CN202111683439.5A patent/CN114316605A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07118536A (en) * | 1993-10-21 | 1995-05-09 | Shin Etsu Chem Co Ltd | Flame-reterdant silicone rubber composition |
| WO2017070893A1 (en) * | 2015-10-29 | 2017-05-04 | 国家纳米科学中心 | Ceramic silicone rubber, preparation method and use thereof |
| CN107903633A (en) * | 2017-11-27 | 2018-04-13 | 浙江新安化工集团股份有限公司 | A kind of melting silicone rubber and preparation method thereof |
| CN109504091A (en) * | 2018-10-24 | 2019-03-22 | 桂林裕天新材料有限公司 | A kind of low cigarette, flame-retardant silicone rubber rubber compound of high transparency and preparation method thereof |
| CN109880373A (en) * | 2019-01-21 | 2019-06-14 | 广州科系维新材料有限公司 | A kind of additive and preparation method thereof applied to transparent flame-retarding silicon rubber |
| JP2021127373A (en) * | 2020-02-12 | 2021-09-02 | 信越化学工業株式会社 | One-component millable type silicone rubber composition and cured product of the same |
| CN112679959A (en) * | 2020-12-25 | 2021-04-20 | 浙江中特化工有限公司 | Transparent bi-component flame-retardant liquid silicone rubber filling material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115491038A (en) * | 2022-09-16 | 2022-12-20 | 广州市矽友新材料科技有限公司 | Halogen-free platinum flame retardant for silicone rubber and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TW201905056A (en) | Polyolefin composition | |
| US5164443A (en) | Electroconductive silicone composition | |
| CN109135299B (en) | Bi-component flame-retardant liquid silicone rubber for insulator and preparation method thereof | |
| CN111019358B (en) | Flame-retardant high-temperature-resistant radiation-resistant silicone rubber and preparation method thereof | |
| CN111363365B (en) | Ultra-high pressure and high temperature resistant mixed silicone rubber and preparation method thereof | |
| CA1152244A (en) | Flame resistant silicone rubber compositions and methods | |
| EP0180843A1 (en) | Silicone elastomer composition | |
| CN107548410A (en) | As polyolefin crosslinked with silicane solidification control additive through hydroxy-end capped PDMS | |
| CN108003628A (en) | Fire-retardant room temperature vulcanized silicone rubber and preparation method thereof | |
| CN114058189B (en) | Addition type flame-retardant high-temperature-resistant silicon rubber and preparation method and application thereof | |
| Zou et al. | Antioxidative behavior of a novel samarium complex in styrene-butadiene rubber/silica composites | |
| CN114316605A (en) | Transparent flame-retardant silicone rubber and preparation method thereof | |
| CN103834172B (en) | Low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubber and preparation method thereof | |
| CN109694523B (en) | Low-VOC low-odor polypropylene resin composition and preparation method thereof | |
| CN111647218A (en) | Ultra-soft low-smoke halogen-free flame-retardant polyolefin cable material and preparation method thereof | |
| CN111269488A (en) | Anti-cracking low-smoke halogen-free flame-retardant sheath material and preparation method thereof | |
| CN109054395B (en) | High-temperature-resistant halogen-free flame-retardant silicone rubber and preparation method thereof | |
| KR20090085680A (en) | Hot-vulcanisable polyorganosiloxane compositions essentially used in the production of electric wires or cables | |
| CN110204900B (en) | Flame-retardant organopolysiloxane composition and preparation method thereof | |
| CN114276604B (en) | High-insulation photovoltaic cable material and preparation method and application thereof | |
| JPH11140322A (en) | Flame resisting silicone gel composition | |
| CN115491038A (en) | Halogen-free platinum flame retardant for silicone rubber and preparation method thereof | |
| CN114231036B (en) | High-strength synergistic flame-retardant room temperature vulcanized silicone rubber and preparation method thereof | |
| JP5269405B2 (en) | Flame retardant silicone rubber composition | |
| CN113527800A (en) | Flame-retardant polyolefin composite material and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220412 |