CN115491038A - Halogen-free platinum flame retardant for silicone rubber and preparation method thereof - Google Patents

Halogen-free platinum flame retardant for silicone rubber and preparation method thereof Download PDF

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CN115491038A
CN115491038A CN202211131460.9A CN202211131460A CN115491038A CN 115491038 A CN115491038 A CN 115491038A CN 202211131460 A CN202211131460 A CN 202211131460A CN 115491038 A CN115491038 A CN 115491038A
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flame retardant
silicone rubber
halogen
parts
compound
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CN115491038B (en
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廖恺
胡怀东
祁航
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Guangzhou Siyou New Material Technology Co ltd
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Abstract

The invention relates to the field of flame retardants, and particularly discloses a halogen-free platinum flame retardant for silicone rubber and a preparation method thereof. The halogen-free platinum flame retardant for the silicone rubber comprises the following components: 55-75 parts of silicon rubber; 5-10 parts of a platinum catalyst; 3-5 parts of a nitrogen-containing compound; 0.5-1 part of phosphorus-containing compound; 12-30 parts of inorganic powder; 0-5 parts of alkynol compounds; 0.3-0.5 part of coupling agent; the preparation method comprises the following steps: step 1), putting silicon rubber, a coupling agent and inorganic powder into an internal mixer for mixing, heating to 150-152 ℃, and keeping the temperature for 90-95min; step 2), cooling to 50 ℃ or below, adding the rest components, and mixing for 60-65min. The invention has the advantage of further improving the flame retardant property of the silicon rubber.

Description

Halogen-free platinum flame retardant for silicone rubber and preparation method thereof
Technical Field
The invention relates to the field of flame retardants, in particular to a halogen-free platinum flame retardant for silicone rubber and a preparation method thereof.
Background
The main chain of the conventional polymer material is a carbon-carbon bond, and the main chain of the silicone rubber is a silicon-oxygen bond, so that the flame retardance is better than that of the conventional polymer material, but the requirement of high flame retardance of UL94V-0 cannot be met.
The conventional technical scheme is that inorganic fillers such as bromine, nitrogen and phosphorus flame retardants or aluminum hydroxide, magnesium hydroxide, zinc borate, zinc carbonate and the like are added into silicon rubber.
Among them, the brominated flame retardants are limited in many uses for environmental reasons; the nitrogen-phosphorus flame retardant has high cost, poor dispersibility in silica gel and relatively poor physical and mechanical properties; the cost of the inorganic flame retardant is low, and most of the flame-retardant silicone rubber in the market is the inorganic flame retardant used at present.
However, the inorganic filler has poor flame retardancy, and the flame retardant effect of UL94V0 with the thickness of 1-2 mm can be achieved only by adding a large amount (generally 100 parts of silicone rubber: more than 100 parts of inorganic filler), so that the physical and mechanical properties, rebound resilience and the like of the silicone rubber are seriously affected.
The platinum catalyst is used as an effective silicon rubber flame retardant aid, and the flame retardance of the silicon rubber can be effectively improved by adding a small amount of the platinum catalyst. However, even with the addition of a platinum catalyst, it is difficult to achieve a good flame retardant effect even with a high platinum addition amount, and therefore there is room for improvement.
Disclosure of Invention
In order to further improve the flame retardant property of the silicone rubber, the application provides a halogen-free platinum flame retardant for the silicone rubber and a preparation method thereof.
The halogen-free platinum flame retardant for the silicone rubber adopts the following technical scheme:
in a first aspect, the application provides a halogen-free platinum flame retardant for silicone rubber, which adopts the following technical scheme:
a halogen-free platinum flame retardant for silicone rubber comprises the following components in parts by weight:
55-75 parts of silicon rubber;
5-10 parts of a platinum catalyst;
3-5 parts of a nitrogen-containing compound;
0.5-1 part of phosphorus-containing compound;
12-30 parts of inorganic powder;
0-5 parts of alkynol compounds;
0.3-0.5 part of coupling agent;
the nitrogen-containing compound is one or more of benzotriazole, azodicarbonamide, tetramethyl ethylene diamine, tetraethyl ethylene diamine, dimethyl ethyl diamine, diethyl ethylene diamine, dibutyl ethylene diamine, dimethyl propane diamine and dibutyl butane diamine;
the phosphorus-containing compound is one or more of tricresyl phosphate, triphenyl phosphite, triisopropylphenyl phosphate, tributyl phosphate, trioctyl phosphate and cresyl diphenyl phosphate;
the alkynol compound is one or a compound of more of 1-ethynyl-1-cyclohexanol, 2-methyl-3-butyn-2-ol, 3-methyl-1-butyn-3-ol, 3, 5-dimethyl-1-hexyn-3-ol, 3,7, 11-trimethyldodecyn-3-ol, 3-methyl-1-dodecyn-3-ol, 3-phenyl-1-butyn-3-ol and 3-prop-1-butyn-3-ol;
the inorganic powder is one or a compound of more of nano titanium dioxide, nano cerium dioxide, zinc carbonate, glass powder and carbon black.
By adopting the technical scheme, the specific platinum catalyst, the nitrogen-containing compound and the phosphorus-containing compound inorganic powder are selected and compounded in a specific ratio, and the prepared flame retardant is added into the silicone rubber product in a ratio of 1-10%, so that the flame retardant property of the silicone rubber product is greatly improved, and a sample with the fire-retardant grade of UL94V-1 and the thickness of 0.5-2mm can reach the fire-retardant grade of UL94V-0 after being doped with 1-10% of the halogen-free platinum flame retardant for silicone rubber, so that the silicone rubber product is better applied to the field of high flame retardant property and has higher economic value.
By adding the specific alkynol compound, the platinum catalyst, the nitrogen-containing compound, the phosphorus-containing compound and the inorganic powder to be compounded in a specific ratio, the performance of the flame retardant can be further improved, and the flame retardant performance of the prepared silicone rubber product is further improved.
By adopting the silicon rubber as the base material, the prepared flame retardant has better compatibility with the silicon rubber, so that the flame retardant is easier to disperse uniformly in the silicon rubber, and the flame retardant property of a silicon rubber product is better improved.
By adding the coupling agent, the dispersion uniformity of each component in the silicon rubber base material is improved, and the prepared flame retardant has better quality.
Preferably, the silicone rubber can be raw or mixed methyl vinyl silicone rubber, and the mass parts of the silicone rubber can be 55 parts, 56 parts, 57 parts, 58 parts, 59 parts, 60 parts, 61 parts, 62 parts, 63 parts, 64 parts, 65 parts, 66 parts, 67 parts, 68 parts, 69 parts, 70 parts, 71 parts, 72 parts, 73 parts, 74 parts and 75 parts.
Preferably, the platinum catalyst may be present in an amount of 5 parts, 6 parts, 7 parts, 8 parts, 9 parts or 10 parts by mass.
Preferably, the nitrogen-containing compound may be present in an amount of 3 parts, 3.5 parts, 4 parts, 4.5 parts, or 5 parts by mass.
Preferably, the inorganic powder may be 12 parts, 14 parts, 16 parts, 18 parts, 20 parts, 22 parts, 24 parts, 26 parts, 28 parts or 30 parts by mass.
Preferably, the mass parts of the alkynol compound can be 0 part, 1 part, 2 parts, 3 parts, 4 parts and 5 parts.
Preferably, the coupling agent can be one or more of coupling agent A171, coupling agent A151, coupling agent KH570, coupling agent KH560 and coupling agent KH550.
Preferably, the platinum content in the platinum catalyst is 5000-20000ppm.
By adopting the technical scheme, the platinum catalyst is better matched with other components by specifically selecting the platinum content in the platinum catalyst, so that better flame retardant property is generated, a large amount of platinum is not needed, the cost can be better controlled, and the catalyst has excellent flame retardant property at lower cost.
Preferably, the platinum content of the platinum catalyst may be 5000ppm, 6000ppm, 7000ppm, 8000ppm, 9000ppm, 10000ppm, 11000ppm, 12000ppm, 13000ppm, 14000ppm, 15000ppm, 16000ppm, 17000ppm, 18000ppm, 19000ppm, 20000ppm.
Preferably, the nitrogen-containing compound is a compound of benzotriazole and azodicarbonamide.
By adopting the technical scheme, the flame retardant property can be better improved by specifically selecting the benzotriazole and the azodicarbonamide for compounding, and the prepared silicone rubber product has better flame retardant property.
Preferably, the mass ratio of the benzotriazole to the azodicarbonamide is 1:2.
by adopting the technical scheme, the matching effect is better by specifically selecting the mass ratio of the benzotriazole to the azodicarbonamide, and the effect of improving the flame retardant property of the silicone rubber product is further improved.
Preferably, the phosphorus-containing compound is triphenyl phosphite.
By adopting the technical scheme, triphenyl phosphite is specifically selected to be better matched with benzotriazole and azodicarbonamide, so that the flame retardant property of the silicone rubber product is better improved.
Preferably, the alkynol compound is a compound of 3-methyl-1-dodecyne-3-ol and 1-ethynyl-1-cyclohexanol.
By adopting the technical scheme, the 3-methyl-1-dodecyne-3-ol and the 1-ethynyl-1-cyclohexanol are specifically selected to be compounded, so that the flame retardant property of the silicone rubber product is further improved by better matching with benzotriazole, azodicarbonamide and triphenyl phosphite.
Preferably, the mass ratio of the 3-methyl-1-dodecyn-3-ol to the 1-ethynyl-1-cyclohexanol can be 1: 1. 2: 1. 1:2.
preferably, the inorganic powder is a compound of nano titanium dioxide, nano cerium dioxide, zinc carbonate, glass powder and carbon black.
By adopting the technical scheme, the nano titanium dioxide, the nano cerium dioxide, the zinc carbonate, the glass powder and the carbon black are specifically selected to be compounded, and the nano titanium dioxide, the nano cerium dioxide, the zinc carbonate, the glass powder and the carbon black are better matched with benzotriazole, azodicarbonamide, triphenyl phosphite, 3-methyl-1-dodecyne-3-ol and 1-ethynyl-1-cyclohexanol, so that the performance of the flame retardant is better improved, and the flame retardant performance of a silicon rubber product is further improved.
Preferably, the mass ratio of the nano titanium dioxide, the nano cerium dioxide, the zinc carbonate, the glass powder and the carbon black can be 1:1:1:1: 1. 1:2:3:4: 5. 1:3:2:2: 4. 2:4:3:5:6.
in a second aspect, the application provides a preparation method of a halogen-free platinum flame retardant for silicone rubber, which adopts the following technical scheme:
the preparation method of the halogen-free platinum flame retardant for the silicone rubber comprises the following steps:
step 1), putting silicon rubber, a coupling agent and inorganic powder into an internal mixer for mixing, heating to 150-152 ℃, and preserving heat for 90-95min;
step 2), cooling to 50 ℃ or below, adding the rest components, and mixing for 60-65min.
By adopting the technical scheme, all raw materials are uniformly dispersed in the silicone rubber by keeping the temperature of 150-152 ℃ for 90-95min, so that substances with smaller molecular weight in the silicone rubber and the powder are discharged, the dispersion uniformity of the silicone rubber and the powder is better improved, and the quality of the prepared flame retardant is better.
In summary, the present application has the following beneficial effects:
1. according to the application, a specific platinum catalyst, a nitrogen-containing compound and a phosphorus-containing compound inorganic powder are selected and compounded in a specific ratio, and the prepared flame retardant is added into the silicone rubber product in a ratio of 1-10%, so that the flame retardant property of the silicone rubber product is greatly improved, and a sample with the fire-retardant rating of UL94V-1 and the thickness of 0.5-2mm can reach the fire-retardant rating of UL94V-0 after being doped with 1-10% of the halogen-free platinum flame retardant for silicone rubber, so that the silicone rubber product is better applied to the field of high flame retardant property, and has higher economic value.
2. According to the application, the specific selection of nano titanium dioxide, nano cerium dioxide, zinc carbonate, glass powder, carbon black, benzotriazole, azodicarbonamide, triphenyl phosphite, 3-methyl-1-dodecyne-3-ol and 1-ethynyl-1-cyclohexanol is preferably adopted for matching, so that the performance of the flame retardant is better improved, and the flame retardant performance of the silicone rubber product is further improved.
3. According to the method, all raw materials are uniformly dispersed in the silicone rubber by keeping the temperature of 150-152 ℃ for 90-95min, so that substances with smaller molecular weight in the silicone rubber and the powder are discharged, the dispersion uniformity of the silicone rubber and the powder is better improved, and the quality of the prepared flame retardant is better.
Detailed Description
The present application will be described in further detail with reference to examples.
Example 1
A halogen-free platinum flame retardant for silicone rubber comprises the following components:
silicon rubber, a platinum catalyst, benzotriazole, azodicarbonamide, triphenyl phosphite, 3-methyl-1-dodecyne-3-ol, 1-ethynyl-1-cyclohexanol, nano titanium dioxide, nano cerium dioxide, zinc carbonate, glass powder, carbon black and a coupling agent.
Wherein the silicone rubber is 110 methyl vinyl silicone rubber crude rubber.
Wherein the platinum content of the platinum catalyst is 5000ppm.
Wherein the coupling agent is silane coupling agent KH550.
The preparation method of the halogen-free platinum flame retardant for the silicon rubber comprises the following steps:
step 1), 75kg of silicone rubber, 0.3kg of coupling agent, 1kg of nano titanium dioxide, 3kg of nano cerium dioxide, 2kg of zinc carbonate, 2kg of glass powder and 4kg of carbon black are put into an internal mixer, the rotating speed is 60r/min, the temperature is raised to 150 ℃ by means of plug pressing and mixing, the speed is changed, the temperature is controlled to be 150 +/-0.2 ℃, and the mixing time is 95min.
And 2), lifting the bolt, reducing the speed to 10r/min, adding 5kg of platinum catalyst, 1kg of benzotriazole, 2kg of azodicarbonamide, 0.5kg of triphenyl phosphite, 2kg of 3-methyl-1-dodecyne-3-ol and 2kg of 1-ethynyl-1-cyclohexanol when the glue temperature is reduced to 50 ℃, controlling the glue temperature to be lower than 50 ℃, mixing for 65min, and discharging the glue to obtain the halogen-free platinum flame retardant for the silicone rubber.
Example 2
A halogen-free platinum flame retardant for silicone rubber comprises the following components:
silicon rubber, a platinum catalyst, benzotriazole, azodicarbonamide, triphenyl phosphite, 3-methyl-1-dodecyne-3-ol, 1-ethynyl-1-cyclohexanol, nano titanium dioxide, nano cerium dioxide, zinc carbonate, glass powder, carbon black and a coupling agent.
Wherein the silicone rubber is 110 methyl vinyl silicone raw rubber.
Wherein the platinum content of the platinum catalyst is 10000ppm.
Wherein the coupling agent is a silane coupling agent KH550.
The preparation method of the halogen-free platinum flame retardant for the silicone rubber comprises the following steps:
step 1), putting 65kg of silicone rubber, 0.4kg of coupling agent, 2kg of nano titanium dioxide, 4kg of nano cerium dioxide, 3kg of zinc carbonate, 5kg of glass powder and 6kg of carbon black into an internal mixer, heating to 150 ℃ by means of plug pressing and mixing at a constant speed of 60r/min, mixing at a constant temperature of 150 +/-0.2 ℃ at a variable speed for 95min.
And step 2), lifting the suppository, reducing the speed to 10r/min, adding 8kg of platinum catalyst, 2kg of benzotriazole, 2kg of azodicarbonamide, 0.8kg of triphenyl phosphite, 2.2kg of 3-methyl-1-dodecyne-3-ol and 2.2kg of 1-ethynyl-1-cyclohexanol when the temperature of the rubber is reduced to 50 ℃, controlling the temperature of the rubber to be lower than 50 ℃, mixing for 65min, and discharging the rubber to obtain the halogen-free platinum flame retardant for the silicone rubber.
Example 3
A halogen-free platinum flame retardant for silicone rubber comprises the following components:
silicon rubber, a platinum catalyst, benzotriazole, azodicarbonamide, triphenyl phosphite, 3-methyl-1-dodecyne-3-ol, 1-ethynyl-1-cyclohexanol, nano titanium dioxide, nano cerium dioxide, zinc carbonate, glass powder, carbon black and a coupling agent.
Wherein the silicone rubber is 110 methyl vinyl silicone rubber crude rubber.
Wherein the platinum content of the platinum catalyst is 20000ppm.
Wherein the coupling agent is a silane coupling agent KH550.
The preparation method of the halogen-free platinum flame retardant for the silicone rubber comprises the following steps:
step 1), putting 55kg of silicone rubber, 0.5kg of coupling agent, 6kg of nano titanium dioxide, 6kg of nano cerium dioxide, 6kg of zinc carbonate, 6kg of glass powder and 6kg of carbon black into an internal mixer, heating to 152 ℃ by means of plug pressing and mixing at a constant speed of 60r/min, mixing at a constant temperature of 152 +/-0.2 ℃ at a variable speed for 90min.
And 2), lifting the bolt, reducing the speed to 10r/min, adding 10kg of platinum catalyst, 2kg of benzotriazole, 3kg of azodicarbonamide, 1kg of triphenyl phosphite, 2.5kg of 3-methyl-1-dodecyne-3-ol and 2.5kg of 1-ethynyl-1-cyclohexanol when the glue temperature is reduced to 50 ℃, controlling the glue temperature to be lower than 50 ℃, mixing for 60min, and discharging the glue to obtain the halogen-free platinum flame retardant for the silicone rubber.
Example 4
Compared with the example 1, the halogen-free platinum flame retardant for the silicon rubber is only different from the halogen-free platinum flame retardant for the silicon rubber in that:
tetramethyl ethylenediamine is used to replace benzotriazole in equivalent amount.
The azodicarbonamide was replaced with equal amounts of dimethylpropanediamine.
Example 5
Compared with the example 1, the halogen-free platinum flame retardant for the silicon rubber is only different from the halogen-free platinum flame retardant for the silicon rubber in that:
triphenyl phosphite was replaced with equal amounts of cresyl diphenyl phosphate.
Example 6
Compared with the example 1, the halogen-free platinum flame retardant for the silicon rubber is only different from the halogen-free platinum flame retardant for the silicon rubber in that:
2-methyl-3-butyne-2-ol is used for replacing 3-methyl-1-dodecyne-3-ol in equal amount.
3, 5-dimethyl-1-hexyn-3-ol replaces 1-ethynyl-1-cyclohexanol equivalently.
Example 7
A halogen-free platinum flame retardant for silicone rubber comprises the following components:
silicon rubber, a platinum catalyst, benzotriazole, azodicarbonamide, triphenyl phosphite, nano titanium dioxide, nano cerium dioxide, zinc carbonate, glass powder, carbon black and a coupling agent.
Wherein the silicone rubber is 110 methyl vinyl silicone raw rubber.
Wherein the platinum content of the platinum catalyst is 5000ppm.
Wherein the coupling agent is a silane coupling agent KH550.
The preparation method of the halogen-free platinum flame retardant for the silicon rubber comprises the following steps:
step 1), putting 75kg of silicon rubber, 0.3kg of coupling agent, 1kg of nano titanium dioxide, 3kg of nano cerium dioxide, 2kg of zinc carbonate, 2kg of glass powder and 4kg of carbon black into an internal mixer, rotating at 60r/min, carrying out bolt pressing and mixing, heating to 150 ℃, carrying out variable-speed constant-temperature mixing, controlling the rubber temperature to be 150 +/-0.2 ℃, and carrying out mixing for 95min.
And 2), lifting the bolt, reducing the bolt speed to 10r/min, adding 5kg of platinum catalyst, 1kg of benzotriazole, 2kg of azodicarbonamide and 0.5kg of triphenyl phosphite when the glue temperature is reduced to 50 ℃, controlling the glue temperature to be lower than 50 ℃, mixing for 60min, and discharging the glue to obtain the halogen-free platinum flame retardant for the silicon rubber.
Comparative example 1
Compared with the example 1, the halogen-free platinum flame retardant for the silicon rubber is only different from the halogen-free platinum flame retardant for the silicon rubber in that:
the nano-silica replaces the nano-titanium dioxide in equal amount.
Comparative example 2
Compared with the example 1, the halogen-free platinum flame retardant for the silicon rubber is only different from the halogen-free platinum flame retardant for the silicon rubber in that:
the nano silicon dioxide equally replaces the nano cerium dioxide.
Comparative example 3
Compared with the example 1, the halogen-free platinum flame retardant for the silicon rubber is only different in that:
the nano silicon dioxide equally replaces the zinc carbonate.
Comparative example 4
Compared with the example 1, the halogen-free platinum flame retardant for the silicon rubber is only different from the halogen-free platinum flame retardant for the silicon rubber in that:
the nano silicon dioxide equally replaces the glass powder.
Comparative example 5
Compared with the example 1, the halogen-free platinum flame retardant for the silicon rubber is only different in that:
the nano silica replaces the carbon black in equal amount.
Comparative example 6
Compared with the example 1, the halogen-free platinum flame retardant for the silicon rubber is only different from the halogen-free platinum flame retardant for the silicon rubber in that:
the preparation method of the halogen-free platinum flame retardant for the silicon rubber comprises the following steps:
step 1), putting 75kg of silicon rubber, 0.3kg of coupling agent, 1kg of nano titanium dioxide, 3kg of nano cerium dioxide, 2kg of zinc carbonate, 2kg of glass powder and 4kg of carbon black into an internal mixer, rotating at 60r/min, carrying out bolt pressing and mixing, heating to 150 ℃, carrying out variable-speed constant-temperature mixing, controlling the rubber temperature to be 150 +/-0.2 ℃, and carrying out mixing for 45min.
And step 2), lifting the suppository, reducing the speed to 10r/min, adding 5kg of platinum catalyst, 1kg of benzotriazole, 2kg of azodicarbonamide, 0.5kg of triphenyl phosphite, 2kg of 3-methyl-1-dodecyne-3-ol and 2kg of 1-ethynyl-1-cyclohexanol when the temperature of the silicone rubber is reduced to 50 ℃, controlling the temperature of the silicone rubber to be lower than 50 ℃, mixing for 30min, and discharging the silicone rubber to obtain the halogen-free platinum flame retardant for the silicone rubber.
Experiment 1
And (3) testing the fireproof performance:
the fire rating of the silicone rubber samples to which the flame retardants of each example and comparative example were added was determined using the UL94 standard.
The silicone rubber sample consisted of the following components:
silicon rubber, aluminum hydroxide, a dipenta-penta vulcanizing agent and a halogen-free platinum flame retardant for the silicon rubber.
The preparation method of the silicone rubber sample is as follows:
step 1), 550g of silicone rubber and 450g of aluminum hydroxide are put into an internal mixer for 40r/min, mixed until the rubber temperature reaches 150 ℃, and the rubber is discharged, so that master batch is obtained.
And 2) putting 1000g of master batch into an open mill for thin passing, adding 20g of halogen-free platinum flame retardant for silicon rubber and 12g of dipentane vulcanizing agent, and packaging for 10 times to obtain the final rubber.
And 3) putting the final rubber into a mold, and vulcanizing and molding the final rubber in a flat vulcanizing agent at 175 ℃ for 5min to obtain a silicon rubber sample, wherein the thickness of the silicon rubber sample is 0.5mm.
The control sample consisted of the following components:
silicon rubber, aluminum hydroxide and a dipenta vulcanizing agent.
The control sample was prepared as follows:
step 1), 550g of silicon rubber and 450g of aluminum hydroxide are put into an internal mixer for 40r/min, mixed until the rubber temperature reaches 150 ℃, and rubber is discharged to obtain the master batch.
And 2) putting 1000g of master batch into an open mill for thin passing, adding 12g of dipentane vulcanizing agent, and packaging in a triangular bag for 10 times to obtain the final rubber.
And 3) putting the final rubber into a mold, and vulcanizing and molding in a flat vulcanizing agent at 175 ℃ for 5min to obtain a reference sample, wherein the thickness of the reference sample is 0.5mm.
Experiment 2
And (3) testing physical properties:
the tensile strength and elongation at break of the silicone rubber samples to which the flame retardants of the examples and comparative examples were added were tested according to GB/T1701-2001, determination of tensile strength and elongation at break of hard rubber.
The tear strength of the silicone rubber samples to which the flame retardants of examples and comparative examples were added was tested in accordance with GB/T529-2008 "determination of tear strength of vulcanized rubber or thermoplastic rubber (pants, square, and crescentic samples), and the test was performed using the square samples.
The silicone rubber samples to which the flame retardants of examples and comparative examples were added were tested for resilience according to GB/T1681-2009 "determination of rebound resilience of vulcanized rubber", and the test was performed using standard samples.
The specific gravity of the silicone rubber samples added with the flame retardants of the examples and the comparative examples was tested according to GB/T533-2008 < determination of vulcanized rubber or thermoplastic rubber Density >, and the specific gravity was tested by the method A.
The preparation method of the silicon rubber sample comprises the following steps:
step 1), 550g of silicone rubber and 450g of aluminum hydroxide are put into an internal mixer for 40r/min, mixed until the rubber temperature reaches 150 ℃, and the rubber is discharged, so that master batch is obtained.
And step 2), putting 1000g of master batch into an open mill for thin passing, adding 20g of halogen-free platinum flame retardant for silicon rubber and 12g of dipenta vulcanizing agent, and packaging for 10 times in a triangular bag to obtain the final rubber.
And 3) putting the final rubber into a mold, and vulcanizing and molding in a flat vulcanizing agent at 175 ℃ for 5min to obtain the silicon rubber sample meeting the tensile strength test standard.
The control sample consisted of the following components:
silicon rubber, aluminum hydroxide and a dipenta vulcanizing agent.
The control samples were prepared as follows:
step 1), 550g of silicon rubber and 450g of aluminum hydroxide are put into an internal mixer for 40r/min, mixed until the rubber temperature reaches 150 ℃, and rubber is discharged to obtain the master batch.
And step 2), putting 1000g of master batch into an open mill for thin passing, adding 12g of dipentane vulcanizing agent, and packaging in a triangular bag for 10 times to obtain the final rubber.
And 3) putting the final rubber into a mold, and vulcanizing and molding in a flat vulcanizing agent at 175 ℃ for 5min to obtain a reference sample meeting the tensile strength test standard.
The specific detection data of experiments 1 and 2 are detailed in tables 1 and 2.
TABLE 1
Figure BDA0003850475030000131
Figure BDA0003850475030000141
TABLE 2
Figure BDA0003850475030000142
According to the data in the table 1-2, the specific nitrogen-containing compound, the specific phosphorus-containing compound, the specific inorganic powder and the specific platinum catalyst are adopted for compounding, so that the performance of the flame retardant is better, the fireproof grade of a sample with the fireproof grade of UL94V-1 and the thickness of 0.5mm is improved to UL94V-0 after 2% of the flame retardant is added, and the physical performance of the sample is not obviously changed.
When the flame retardant is compounded by a platinum catalyst, benzotriazole, azodicarbonamide, triphenyl phosphite, 3-methyl-1-dodecyne-3-ol, 1-ethynyl-1-cyclohexanol, nano titanium dioxide, nano cerium dioxide, zinc carbonate, glass powder and carbon black in a specific proportion, the fireproof grade of a sample with the fireproof grade of UL94V-1 and the thickness of 0.5mm is improved to UL945-VA after 2% of the flame retardant is added, the flame retardant performance is greatly improved, the addition amount of the flame retardant is low, the effect of greatly improving the flame retardant performance can be realized, the economic value is high, and the physical performance of a rubber product is not easily influenced.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.

Claims (8)

1. A halogen-free platinum flame retardant for silicone rubber is characterized in that: the composition comprises the following components in parts by mass:
55-75 parts of silicon rubber;
5-10 parts of a platinum catalyst;
3-5 parts of a nitrogen-containing compound;
0.5-1 part of a phosphorus-containing compound;
12-30 parts of inorganic powder;
0-5 parts of alkynol compound;
0.3-0.5 part of coupling agent;
the nitrogen-containing compound is one or more of benzotriazole, azodicarbonamide, tetramethyl ethylene diamine, tetraethyl ethylene diamine, dimethyl ethyl diamine, diethyl ethylene diamine, dibutyl ethylene diamine, dimethyl propane diamine and dibutyl butane diamine;
the phosphorus-containing compound is one or a compound of more of tricresyl phosphate, triphenyl phosphite, triisopropylphenyl phosphate, tributyl phosphate, trioctyl phosphate and cresyl diphenyl phosphate;
the alkynol compound is one or a plurality of compounds of 1-ethynyl-1-cyclohexanol, 2-methyl-3-butyn-2-ol, 3-methyl-1-butyn-3-ol, 3, 5-dimethyl-1-hexyn-3-ol, 3,7, 11-trimethyldodecyn-3-ol, 3-methyl-1-dodecyn-3-ol, 3-phenyl-1-butyn-3-ol and 3-prop-1-butyn-3-ol;
the inorganic powder is one or a compound of more of nano titanium dioxide, nano cerium dioxide, zinc carbonate, glass powder and carbon black.
2. The halogen-free platinum flame retardant for silicone rubber as claimed in claim 1, wherein: the platinum content in the platinum catalyst is 5000-20000ppm.
3. The halogen-free platinum flame retardant for silicone rubber as claimed in claim 1, wherein: the nitrogen-containing compound is the compound of benzotriazole and azodicarbonamide.
4. The halogen-free platinum flame retardant for silicone rubber as claimed in claim 3, wherein: the mass ratio of the benzotriazole to the azodicarbonamide is 1:2.
5. the halogen-free platinum flame retardant for silicone rubber according to claim 3, characterized in that: the phosphorus-containing compound is triphenyl phosphite.
6. The halogen-free platinum flame retardant for silicone rubber according to claim 5, wherein: the alkynol compound is the compound of 3-methyl-1-dodecyne-3-ol and 1-ethynyl-1-cyclohexanol.
7. The halogen-free platinum flame retardant for silicone rubber as claimed in claim 6, wherein: the inorganic powder is a compound of nano titanium dioxide, nano cerium dioxide, zinc carbonate, glass powder and carbon black.
8. The preparation method of the halogen-free platinum flame retardant for the silicone rubber according to any one of claims 1 to 7, characterized in that: the method comprises the following steps:
step 1), putting silicon rubber, a coupling agent and inorganic powder into an internal mixer for mixing, heating to 150-152 ℃, and preserving heat for 90-95min;
step 2), cooling to 50 ℃ or below, adding the rest components, and mixing for 60-65min.
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