CN102977607A - Flame-retardant liquid silicone rubber of high tear resistance - Google Patents
Flame-retardant liquid silicone rubber of high tear resistance Download PDFInfo
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Abstract
The invention discloses a flame-retardant liquid silicone rubber of high tear resistance. The silicone rubber comprises in parts by weight the following components: 100-150 parts of MQ silicone resin, 50-100 parts of reactive diluent, which uses linear phenyl vinyl siloxane, 5-10 parts of cross-linking agent, which uses linear phenyl hydrosiloxane, 5-20 parts of reinforcing agent, which uses fumed silica, and 0.01-0.15 part of thermosensitive inhibitor, which uses dimethyl fumarate. Phenyl group is applied to pre-modifying the reactive diluent and the cross-linking agent in the preparation process of the reactive diluent and the cross-linking agent to greatly improve the flame retardant performance, the high temperature resistance and the volume resistance of the product. By combining the MQ-based silicone resin and the fumed silica in the preparation process of the silicone rubber, the prepared silicone rubber has a better physical performance and excellent tear strength.
Description
Technical field
The present invention relates to silicone resin, especially relate to a kind of anti-tear liquid silicone resin of fire-retardant height for material surface coatings such as fiberglass sleeve, silicone tube, glasscloths.
Background technology
Silicone resin is the thermoset polysiloxane polymer with highly cross-linked structure.Early stage product is (such as MeSiCl by organochlorosilane
3, Me
2SiCl
2, MePhSiCl
2, PhSiCl
3, Ph
2SiCl
2) via hydrolytic condensation and rearrangement, make active siloxane prepolymer stable under the room temperature.During application, hard or the less solid silicon resin of elasticity can be contracted and be cross-linked into to its further heating.Silicone resin has good electrical insulation property, the effect of heatproof and waterproof.And weathering resistance is better than general organic resin.Therefore, in the coating on heatproof, heat-resisting and anti-wet treatment protection top layer, be all desirable material.
Silicone resin molecule side group mainly is methyl, introduces phenyl and can improve thermo-elasticity and cementability, and the compatibility of improvement and organic polymer and pigment is introduced ethyl, propyl group or chain alkyl and can be improved organic affinity, and improves hydrophobic nature; Introduce vinyl and hydrogen base, can use platinum catalytic addition reaction and superoxide to cause crosslinking reaction; Introduce the carbon official can machine then can with more organic compound reactions, improve cementability to base material.
The add-on type silicone resin is different from condensed type or superoxide initiation type silicone resin is curing mechanism.Add-on type silicone resin curing mechanism system is by having ≡ Si-CH=CH
2The siloxanes of group with contain the siloxanes (linking agent) of ≡ Si-H group, the hydrosilylation reaction occurs under the platinum catalyst effect and crosslinked.Addition type liquid silicon resin has and does not contain solvent, and condition of cure is gentle, the characteristics such as emits without low molecule by product, is used for the dipping of various coils, and insulativity, flame retardant resistance, thermotolerance and the tear strength of coil excellence is provided.
Silicone resin is a kind of heat cured plastics, and one of performance that it is the most outstanding is excellent thermo-oxidative stability.250 ℃ of heating are after 24 hours, and silicone resin weightlessness only is 2～8%.Another outstanding performance of silicone resin is excellent electrical insulation capability, and it all can keep its good insulating property in wide temperature and range of frequency.Silicone resin is broadly divided into several large classes such as organic silicon insulating varnish, organosilicon coating, silicone plastics and silicone adhesive by its main application and crosslinking method.Silicone resin has good resistance to elevated temperatures and outstanding dielectricity.It has good anti-corona, arc resistance, and dielectric loss angle tangent is low, these be other synthetic resins can't be obtained.Silicone resin can be made anti-180 ℃ electric motor insulating material, such as varnished glass cloth, glass cloth laminated board, mica tape, impregnating varnish, enamel paint etc.Both can be made into anti-500 ℃ of life-time service, the anti-1000 ℃ high-temperature coatings of instantaneous use after adding aluminium powder afterwards, are used for the jet nozzle of application, metal chimney etc.With the moulding compound that glass fibre or asbestos reinforcement are made, can be used as the material of making anti-strong current, high-tension anti-arc switch.Silicone resin (being commonly called as silicone glass resin) so that methyl trialkoxysilane makes can in order to treatment paper, plastics, metallic surface, make it that good brightness and wear resistance be arranged.Silicone resin can be used as the good outdoor use coating of weathering resistance after modification (as with Synolac etc.).
Because silicone resin raw materials for production, technique difference cause the silicone resin kind numerous and diverse.Such as Chinese patent 98101493.3 with regard to manufacture method of disclosed a kind of transparent liquid silicone resin and products thereof, selecting the organic oxirane that contains unsaturated alkyl, poly-diorganosiloxane and Diphenylsilanediol is raw material, its mole ratio is 1: 1 ~ 5: 5 ~ 1, adding anionic catalyst is 0.005 ~ 0.04% of raw material gross weight, be the polycondensation 1 ~ 3 hour of reducing pressure under 140 ~ 180 ℃ the condition in temperature, generate transparent liquid solvent-free silicone resin.A kind of organosilicon resin composition is disclosed such as Chinese patent 200710027914.7.By: methyl vinyl silicon kautschuk, methylvinyl-polysiloxane, methyl ethylene silicone resin, linking agent, catalyzer and inhibitor mixed form, and its mass ratio is: 100 parts of methyl vinyl silicon kautschuks, 50～400 parts of methylvinyl-polysiloxane, 50～400 parts of methyl ethylene silicone resins, 5 ~ 50 parts of linking agents, 0.1～2 part of catalyzer, 0.05～2 part in inhibitor; Manufacture craft and flow process be, first methyl vinyl silicon kautschuk, methylvinyl-polysiloxane, methyl ethylene silicone resin, linking agent and inhibitor added mixing and stirring in proportion, then adds catalyzer and stir to get final product.A kind of nano solidifiable silicone impression material is disclosed such as Chinese patent 200910305628.1, formed by basic paste and catalyzer paste two portions, the basis paste comprise 0.2% ethenyl blocking polydimethylsiloxane, have at least 3 SiH base polymethyl hydrogen siloxane polydimethylsiloxanes, polyethet surfactant, diameter less than nano silicon, the coloring agent of 30nm, superfine talcum powder, light calcium carbonate, inhibitor 3-methyl isophthalic acid-butine-3-alcohol; The component of catalyzer paste comprises polydimethylsiloxane, the polydimethylsiloxane of 0.2% ethenyl blocking, platinum catalyst, the nano silicon of ethylene methacrylic radical siloxane coordination.Basis paste and catalyzer paste two portions are take volume ratio as 1:1 or after the mediation of 5:1, are cured as silicone elastomer under room temperature in 3 ~ 5 minutes.
Dow corning company adopts bulk polymerization to prepare add-on type silicone resin trade mark DC-996, and this product contains high phenyl content, has excellent flame retardant properties.It also is a kind of add-on type silicone resin that Japan chemical company of SHIN-ETSU HANTOTAI adopts the trade mark KR-255 that produces.
This shows that the How to choose suitable feedstock also generates translucent liquid silicone resin by new technique, product is not only wanted excellent property, and shelf-stable; Technique has short, power savings advantages of time spent; With its product of making or processing have not xanthochromia, do not ftracture, shrinking percentage is little, and preferably pliability, intensity, glossiness are arranged, self-extinguishing and dielectricity are good.These all are the directions of from now on silicone resin research and development.
Summary of the invention
The purpose of this invention is to provide the anti-tear liquid silicone resin of a kind of fire-retardant height, solve the especially flame retardant properties of the liquid silicone resin existence that has material surface coatings such as being used for fiberglass sleeve, silicone tube, glasscloth now and the problem that tear resistance is excellent not, storage is stable not.
The technical solution adopted for the present invention to solve the technical problems is:
Provide a kind of fire-retardant height anti-tear liquid silicone resin, in weight part, comprise that 100 ~ 150 parts of MQ silicone resin, reactive thinner select 50 ~ 100 parts of line style phenyl vinyl siloxanes, linking agent to select 5 ~ 10 parts of the phenyl modified hydrogen-containing siloxanes of line style, strengthening agent to select 5 ~ 20 parts of fumed silicas, temperature sensitive inhibitor to select 0.01 ~ 0.15 part of dimethyl fumarate.
Preferably, the ratio of M chain link and Q chain link is 0.6 ~ 0.8 in the described MQ silicone resin.
Preferably, the specific surface area of described fumed silica is at 160 ~ 300m
2/ g.
Described line style phenyl vinyl siloxanes comprises the steps to make: drop into 150 ~ 200 parts of 50 ~ 120 parts of two (methyl phenyl vinyl) sily oxide and dimethoxydiphenylsilanes in the reactor, be warmed up to 85 ℃ ~ 100 ℃, add 6 ~ 8 parts of 30 ~ 40 parts in an amount of water and catalyzer concentrated hydrochloric acids, reaction 4 ~ 8h namely gets line style phenyl vinyl siloxanes with 2.5 ~ 5 parts of alkali sodium hydroxide neutralizations.
The phenyl modified hydrogen-containing siloxane of described line style comprises the steps to make: in weight part, drop into the polymerization degree 60 ~ 80 parts of 70 ~ 100 parts of Methyl Hydrogen Polysiloxane Fluids 80 below and 10 ~ 15 parts of vinyl toluenes and solvent Virahols, be warmed up to 80 ℃ ~ 95 ℃, add 0.001 ~ 0.005 part of platinum catalyst Platinic chloride-divinyl tetramethyl disiloxane, reaction 6 ~ 8h, reactant becomes clear gradually by muddiness, transparent rear continuation reaction 2 ~ 4h time, then solvent is deviate from decompression, and cooling normal temperature namely gets the phenyl modified hydrogen-containing siloxane of line style.
Described Platinic chloride-divinyl tetramethyl disiloxane catalyzer comprises the steps to make: weight part platinum content 33% is H
2PtCl
66H
232 ~ 40 parts of the O aqueous solution are dissolved in the Virahol with 210 ~ 260 parts of divinyl tetramethyl disiloxane, then add 15 ~ 20 parts NaHCO in this solution
3, in there-necked flask, descending stirring 30min. that the isopropyl alcohol and water is evaporated under reduced pressure 1.667kPa at 70 ~ 80 ℃ suspension and remove, the elimination solids component gets platiniferous network and divinyl tetramethyl disiloxane solution.
The anti-tear liquid silicone resin of described arbitrary fire-retardant height makes by being prepared as follows method steps:
1) partly measure MQ silicone resin and the silicon-dioxide with gross weight drops into kneader, adds line style phenyl vinyl siloxanes, the phenyl modified hydrogen-containing siloxane of line style, water, stearic acid again, mediates 2 hours must sizing material;
2) kneaded sizing material is heated up in vacuum Banbury mixer banburying, material temperature is controlled at 130 ~ 200 ° of C degree, vacuumizes when 150 ° of C, adds the MQ silicone resin again, banburying 6 ~ 8h, the banburying material was placed 12 ~ 24 hours to get in discharging;
3) banburying material physicals detect qualified after, grind and remove its block material, add again the inhibitor dimethyl fumarate, the phenyl modified hydrogen-containing siloxane of linking agent line style stirs 2h, after the press filtration liquid silicone resin.
Beneficial effect of the present invention: owing in preparation reactive thinner and linking agent, all used phenyl that it is carried out in advance modification, the flame retardant properties, resistance to elevated temperatures that has greatly improved product with and volume resistance.In the preparation silicone resin, adopt MQ base silicon resin to combine with Meteorological Act silicon-dioxide, made the silicone resin of preparation have better physicals, had excellent tearing toughness.
Below with reference to embodiment, the present invention is described in detail.
Embodiment
Embodiment 1, the anti-tear liquid silicone resin preparation of a kind of fire-retardant height
The anti-tear liquid silicone resin of a kind of fire-retardant height, in weight part, comprise that 100 parts of MQ silicone resin, reactive thinner select 50 parts of line style phenyl vinyl siloxanes, linking agent to select 5 parts of the phenyl modified hydrogen-containing siloxanes of line style, strengthening agent to select 5 parts of fumed silicas, temperature sensitive inhibitor to select 0.01 part of dimethyl fumarate.
The ratio of M chain link and Q chain link is 0.6 in the above-mentioned MQ silicone resin.
The specific surface area of above-mentioned fumed silica is at 160m
2/ g.
Described line style phenyl vinyl siloxanes comprises the steps to make: drop into 150 parts of 50 parts of two (methyl phenyl vinyl) sily oxide and dimethoxydiphenylsilanes in the reactor, be warmed up to 85 ℃, add 6 parts of 30 parts in an amount of water and catalyzer concentrated hydrochloric acids, reaction 4h namely gets line style phenyl vinyl siloxanes with 2.5 parts of alkali sodium hydroxide neutralizations.
The phenyl modified hydrogen-containing siloxane of described line style comprises the steps to make: in weight part, drop into the polymerization degree 60 parts of 70 parts of Methyl Hydrogen Polysiloxane Fluids 80 below and 10 parts of vinyl toluenes and solvent Virahols, be warmed up to 80 ℃, add 0.001 part of platinum catalyst Platinic chloride-divinyl tetramethyl disiloxane, reaction 6h, reactant becomes clear gradually by muddiness, the transparent rear continuation reaction 2h time, then solvent is deviate from decompression, and cooling normal temperature namely gets the phenyl modified hydrogen-containing siloxane of line style.
Described Platinic chloride-divinyl tetramethyl disiloxane catalyzer comprises the steps to make: weight part platinum content 33% is H
2PtCl
66H
232 parts of the O aqueous solution are dissolved in the Virahol with 210 parts of divinyl tetramethyl disiloxane, then add 15 parts NaHCO in this solution
3, in there-necked flask, descending stirring 30min. that the isopropyl alcohol and water is evaporated under reduced pressure 1.667kPa at 70 ℃ suspension and remove, the elimination solids component gets platiniferous network and divinyl tetramethyl disiloxane solution.
The above-mentioned anti-tear liquid silicone resin of fire-retardant height makes by being prepared as follows method steps:
1) partly measure MQ silicone resin and the silicon-dioxide with gross weight drops into kneader, adds line style phenyl vinyl siloxanes, the phenyl modified hydrogen-containing siloxane of line style, water, stearic acid again, mediates 2 hours must sizing material;
2) kneaded sizing material is heated up in vacuum Banbury mixer banburying, material temperature is controlled at 130 ° of C degree, vacuumizes when 150 ° of C, adds the MQ silicone resin again, banburying 6h, the banburying material was placed 12 hours to get in discharging;
3) banburying material physicals detect qualified after, grind and remove its block material, add again the inhibitor dimethyl fumarate, the phenyl modified hydrogen-containing siloxane of linking agent line style stirs 2h, after the press filtration liquid silicone resin.
Embodiment 2, the anti-tear liquid silicone resin preparation of a kind of fire-retardant height
The anti-tear liquid silicone resin of a kind of fire-retardant height, in weight part, comprise that 150 parts of MQ silicone resin, reactive thinner select 100 parts of line style phenyl vinyl siloxanes, linking agent to select 10 parts of the phenyl modified hydrogen-containing siloxanes of line style, strengthening agent to select 20 parts of fumed silicas, temperature sensitive inhibitor to select 0.15 part of dimethyl fumarate.
The ratio of M chain link and Q chain link is 0.8 in the above-mentioned MQ silicone resin.
The specific surface area of above-mentioned fumed silica is at 300m
2/ g.
Described line style phenyl vinyl siloxanes comprises the steps to make: drop into 200 parts of 120 parts of two (methyl phenyl vinyl) sily oxide and dimethoxydiphenylsilanes in the reactor, be warmed up to 100 ℃, add 8 parts of 40 parts in an amount of water and catalyzer concentrated hydrochloric acids, reaction 8h namely gets line style phenyl vinyl siloxanes with 5 parts of alkali sodium hydroxide neutralizations.
The phenyl modified hydrogen-containing siloxane of described line style comprises the steps to make: in weight part, drop into the polymerization degree 80 parts of 100 parts of Methyl Hydrogen Polysiloxane Fluids 80 below and 15 parts of vinyl toluenes and solvent Virahols, be warmed up to 95 ℃, add 0.005 part of platinum catalyst Platinic chloride-divinyl tetramethyl disiloxane, reaction 8h, reactant becomes clear gradually by muddiness, the transparent rear continuation reaction 4h time, then solvent is deviate from decompression, and cooling normal temperature namely gets the phenyl modified hydrogen-containing siloxane of line style.
Described Platinic chloride-divinyl tetramethyl disiloxane catalyzer comprises the steps to make: weight part platinum content 33% is H
2PtCl
66H
240 parts of the O aqueous solution are dissolved in the Virahol with 260 parts of divinyl tetramethyl disiloxane, then add 20 NaHCO in this solution
3, in there-necked flask, descending stirring 30min. that the isopropyl alcohol and water is evaporated under reduced pressure 1.667kPa at 80 ℃ suspension and remove, the elimination solids component gets platiniferous network and divinyl tetramethyl disiloxane solution.
The above-mentioned anti-tear liquid silicone resin of fire-retardant height makes by being prepared as follows method steps:
1) partly measure MQ silicone resin and the silicon-dioxide with gross weight drops into kneader, adds line style phenyl vinyl siloxanes, the phenyl modified hydrogen-containing siloxane of line style, water, stearic acid again, mediates 2 hours must sizing material;
2) kneaded sizing material is heated up in vacuum Banbury mixer banburying, material temperature is controlled at 200 ° of C degree, vacuumizes when 150 ° of C, adds the MQ silicone resin again, banburying 8h, the banburying material was placed 24 hours to get in discharging;
3) banburying material physicals detect qualified after, grind and remove its block material, add again the inhibitor dimethyl fumarate, the phenyl modified hydrogen-containing siloxane of linking agent line style stirs 2h, after the press filtration liquid silicone resin.
Embodiment 3, the anti-tear liquid silicone resin preparation of a kind of fire-retardant height
The anti-tear liquid silicone resin of a kind of fire-retardant height, in weight part, comprise that 120 parts of MQ silicone resin, reactive thinner select 80 parts of line style phenyl vinyl siloxanes, linking agent to select 6 parts of the phenyl modified hydrogen-containing siloxanes of line style, strengthening agent to select 10 parts of fumed silicas, temperature sensitive inhibitor to select 0.08 part of dimethyl fumarate.
The ratio of M chain link and Q chain link is 0.7 in the above-mentioned MQ silicone resin.
The specific surface area of above-mentioned fumed silica is at 240m
2/ g.
Described line style phenyl vinyl siloxanes comprises the steps to make: drop into 180 parts of 70 parts of two (methyl phenyl vinyl) sily oxide and dimethoxydiphenylsilanes in the reactor, be warmed up to 95 ℃, add 7 parts of 32 parts in an amount of water and catalyzer concentrated hydrochloric acids, reaction 6h namely gets line style phenyl vinyl siloxanes with 4 parts of alkali sodium hydroxide neutralizations.
The phenyl modified hydrogen-containing siloxane of described line style comprises the steps to make: in weight part, drop into the polymerization degree 70 parts of 85 parts of Methyl Hydrogen Polysiloxane Fluids 80 below and 12 parts of vinyl toluenes and solvent Virahols, be warmed up to 90 ℃, add 0.003 part of platinum catalyst Platinic chloride-divinyl tetramethyl disiloxane, reaction 7h, reactant becomes clear gradually by muddiness, the transparent rear continuation reaction 3h time, then solvent is deviate from decompression, and cooling normal temperature namely gets the phenyl modified hydrogen-containing siloxane of line style.
Described Platinic chloride-divinyl tetramethyl disiloxane catalyzer comprises the steps to make: weight part platinum content 33% is H
2PtCl
66H
238 parts of the O aqueous solution are dissolved in the Virahol with 240 parts of divinyl tetramethyl disiloxane, then add 18 NaHCO in this solution
3, in there-necked flask, descending stirring 30min. that the isopropyl alcohol and water is evaporated under reduced pressure 1.667kPa at 80 ℃ suspension and remove, the elimination solids component gets platiniferous network and divinyl tetramethyl disiloxane solution.
The above-mentioned anti-tear liquid silicone resin of fire-retardant height makes by being prepared as follows method steps:
1) partly measure MQ silicone resin and the silicon-dioxide with gross weight drops into kneader, adds line style phenyl vinyl siloxanes, the phenyl modified hydrogen-containing siloxane of line style, water, stearic acid again, mediates 2 hours must sizing material;
2) kneaded sizing material is heated up in vacuum Banbury mixer banburying, material temperature is controlled at 180 ° of C degree, vacuumizes when 150 ° of C, adds the MQ silicone resin again, banburying 7h, the banburying material was placed 18 hours to get in discharging;
3) banburying material physicals detect qualified after, grind and remove its block material, add again the inhibitor dimethyl fumarate, the phenyl modified hydrogen-containing siloxane of linking agent line style stirs 2h, after the press filtration liquid silicone resin.
Embodiment 4, the anti-tear liquid silicone resin preparation of a kind of fire-retardant height
The anti-tear liquid silicone resin of a kind of fire-retardant height, in weight part, comprise that 130 parts of MQ silicone resin, reactive thinner select 80 parts of line style phenyl vinyl siloxanes, linking agent to select 8 parts of the phenyl modified hydrogen-containing siloxanes of line style, strengthening agent to select 16 parts of fumed silicas, temperature sensitive inhibitor to select 0.12 part of dimethyl fumarate.
The ratio of M chain link and Q chain link is 0.8 in the above-mentioned MQ silicone resin.
The specific surface area of above-mentioned fumed silica is at 200m
2/ g.
Described line style phenyl vinyl siloxanes comprises the steps to make: drop into 150 parts of 80 parts of two (methyl phenyl vinyl) sily oxide and dimethoxydiphenylsilanes in the reactor, be warmed up to 85 ℃, add 6 parts of 30 parts in an amount of water and catalyzer concentrated hydrochloric acids, reaction 8h namely gets line style phenyl vinyl siloxanes with 5 parts of alkali sodium hydroxide neutralizations.
The phenyl modified hydrogen-containing siloxane of described line style comprises the steps to make: in weight part, drop into the polymerization degree 60 parts of 100 parts of Methyl Hydrogen Polysiloxane Fluids 80 below and 15 parts of vinyl toluenes and solvent Virahols, be warmed up to 80 ℃, add 0.005 part of platinum catalyst Platinic chloride-divinyl tetramethyl disiloxane, reaction 8h, reactant becomes clear gradually by muddiness, the transparent rear continuation reaction 4h time, then solvent is deviate from decompression, and cooling normal temperature namely gets the phenyl modified hydrogen-containing siloxane of line style.
Described Platinic chloride-divinyl tetramethyl disiloxane catalyzer comprises the steps to make: weight part platinum content 33% is H
2PtCl
66H
240 parts of the O aqueous solution are dissolved in the Virahol with 260 parts of divinyl tetramethyl disiloxane, then add 20 NaHCO in this solution
3, in there-necked flask, descending stirring 30min. that the isopropyl alcohol and water is evaporated under reduced pressure 1.667kPa at 80 ℃ suspension and remove, the elimination solids component gets platiniferous network and divinyl tetramethyl disiloxane solution.
The above-mentioned anti-tear liquid silicone resin of fire-retardant height makes by being prepared as follows method steps:
1) partly measure MQ silicone resin and the silicon-dioxide with gross weight drops into kneader, adds line style phenyl vinyl siloxanes, the phenyl modified hydrogen-containing siloxane of line style, water, stearic acid again, mediates 2 hours must sizing material;
2) kneaded sizing material is heated up in vacuum Banbury mixer banburying, material temperature is controlled at 200 ° of C degree, vacuumizes when 150 ° of C, adds the MQ silicone resin again, banburying 8h, the banburying material was placed 24 hours to get in discharging;
3) banburying material physicals detect qualified after, grind and remove its block material, add again the inhibitor dimethyl fumarate, the phenyl modified hydrogen-containing siloxane of linking agent line style stirs 2h, after the press filtration liquid silicone resin.
Embodiment 5, silicate resinous product performance perameter detect and compare
Each parameter adopts standard " GB/T1303.8-2009 is electric with thermosetting resin industry rigid laminate the 8th part: the silicone resin rigid laminate ", standard " JB/T7093-1993 silicone resin glass fibre is from clipper tube ", standard " DIN VDE0250-502-1985 insulating power wire. the wiring of heat-resisting silicone resin lamp holder ", standard " the mensuration Ka Er. Fei Xiufa of NF T77-105-1985 industrial silicon resin water-content ", standard " mensuration of NFT77-101-1985 industrial silicon resin density " and standard " BS EN2261-1995 silicone rubber (VMQ). hardness: 70IRHD (international rubber hardness degree) " described method detection.Detected result such as following table:
Silicate resinous product performance perameter comparison sheet:
As can be seen from the table, the parameters inspection reflects the embodiment product better performance, and especially tear strength/kNm surpasses the Japanese KR-255 of SHIN-ETSU HANTOTAI, Dow corning 3-1953.
Claims (7)
1. anti-tear liquid silicone resin of fire-retardant height, it is characterized in that: in weight part, comprise that 100 ~ 150 parts of MQ silicone resin, reactive thinner select 50 ~ 100 parts of line style phenyl vinyl siloxanes, linking agent to select 5 ~ 10 parts of the phenyl modified hydrogen-containing siloxanes of line style, strengthening agent to select 5 ~ 20 parts of fumed silicas, temperature sensitive inhibitor to select 0.01 ~ 0.15 part of dimethyl fumarate.
2. the anti-tear liquid silicone resin of fire-retardant height as claimed in claim 1, it is characterized in that: the ratio of M chain link and Q chain link is 0.6 ~ 0.8 in the described MQ silicone resin.
3. the anti-tear liquid silicone resin of fire-retardant height as claimed in claim 1, it is characterized in that: the specific surface area of described fumed silica is at 160 ~ 300m
2/ g.
4. the anti-tear liquid silicone resin of fire-retardant height as claimed in claim 1, it is characterized in that: described line style phenyl vinyl siloxanes comprises the steps to make: drop into 150 ~ 200 parts of 50 ~ 120 parts of two (methyl phenyl vinyl) sily oxide and dimethoxydiphenylsilanes in the reactor, be warmed up to 85 ℃ ~ 100 ℃, add 6 ~ 8 parts of 30 ~ 40 parts in an amount of water and catalyzer concentrated hydrochloric acids, reaction 4 ~ 8h namely gets line style phenyl vinyl siloxanes with 2.5 ~ 5 parts of alkali sodium hydroxide neutralizations.
5. the anti-tear liquid silicone resin of fire-retardant height as claimed in claim 1, it is characterized in that: the phenyl modified hydrogen-containing siloxane of described line style comprises the steps to make:
In weight part, drop into the polymerization degree 60 ~ 80 parts of 70 ~ 100 parts of Methyl Hydrogen Polysiloxane Fluids 80 below and 10 ~ 15 parts of vinyl toluenes and solvent Virahols, be warmed up to 80 ℃ ~ 95 ℃, add 0.001 ~ 0.005 part of platinum catalyst Platinic chloride-divinyl tetramethyl disiloxane, reaction 6 ~ 8h, reactant becomes clear gradually by muddiness, transparent rear continuation reaction 2 ~ 4h time, then solvent is deviate from decompression, and cooling normal temperature namely gets the phenyl modified hydrogen-containing siloxane of line style.
6. the anti-tear liquid silicone resin of fire-retardant height as claimed in claim 5, it is characterized in that: described Platinic chloride-divinyl tetramethyl disiloxane catalyzer comprises the steps to make:
Be H with weight part platinum content 33%
2PtCl
66H
232 ~ 40 parts of the O aqueous solution are dissolved in the Virahol with 210 ~ 260 parts of divinyl tetramethyl disiloxane, then add 15 ~ 20 parts NaHCO in this solution
3, in there-necked flask, descending stirring 30min. that the isopropyl alcohol and water is evaporated under reduced pressure 1.667kPa at 70 ~ 80 ℃ suspension and remove, the elimination solids component gets platiniferous network and divinyl tetramethyl disiloxane solution.
7. such as the anti-tear liquid silicone resin of the described arbitrary fire-retardant height of claim 1 ~ 6, make by being prepared as follows method steps:
1) partly measure MQ silicone resin and the silicon-dioxide with gross weight drops into kneader, adds line style phenyl vinyl siloxanes, the phenyl modified hydrogen-containing siloxane of line style, water, stearic acid again, mediates 2 hours must sizing material;
2) kneaded sizing material is heated up in vacuum Banbury mixer banburying, material temperature is controlled at 130 ~ 200 ° of C degree, vacuumizes when 150 ° of C, adds the MQ silicone resin again, banburying 6 ~ 8h, the banburying material was placed 12 ~ 24 hours to get in discharging;
3) banburying material physicals detect qualified after, grind and remove its block material, add again the inhibitor dimethyl fumarate, the phenyl modified hydrogen-containing siloxane of linking agent line style stirs 2h, after the press filtration liquid silicone resin.
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| CN104140535A (en) * | 2013-11-06 | 2014-11-12 | 郑州中原应用技术研究开发有限公司 | Phenyl-containing MQ silicon resin and preparation method thereof |
| CN105585957A (en) * | 2014-10-22 | 2016-05-18 | 株洲时代新材料科技股份有限公司 | Silicone impregnating varnish, and preparing method and applications thereof |
| CN107446352A (en) * | 2017-08-10 | 2017-12-08 | 深圳市铂科新材料股份有限公司 | A kind of silicones |
| CN111205767A (en) * | 2020-02-26 | 2020-05-29 | 科顺防水科技股份有限公司 | Super-hydrophobic coating for corrosion prevention and freeze-thaw resistance of concrete and preparation method thereof |
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| CN104140535A (en) * | 2013-11-06 | 2014-11-12 | 郑州中原应用技术研究开发有限公司 | Phenyl-containing MQ silicon resin and preparation method thereof |
| CN104140535B (en) * | 2013-11-06 | 2016-08-31 | 郑州中原应用技术研究开发有限公司 | A kind of MQ silicones containing phenyl and preparation method thereof |
| CN103694948A (en) * | 2013-11-18 | 2014-04-02 | 江苏国豪耐火科技有限公司 | Adhesive material with characteristics of high performance, reversibility, temperature resistance and corrosion resistance, and preparation method thereof |
| CN103694948B (en) * | 2013-11-18 | 2015-06-24 | 江苏国豪耐火科技有限公司 | Adhesive material with characteristics of high performance, reversibility, temperature resistance and corrosion resistance, and preparation method thereof |
| CN105585957A (en) * | 2014-10-22 | 2016-05-18 | 株洲时代新材料科技股份有限公司 | Silicone impregnating varnish, and preparing method and applications thereof |
| CN105585957B (en) * | 2014-10-22 | 2017-12-15 | 株洲时代新材料科技股份有限公司 | Silicone impregnating varnish and its preparation method and application |
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| CN111254712A (en) * | 2020-01-17 | 2020-06-09 | 江西赛欧特科新材料有限公司 | Fluorine-free waterproof breathable fabric and preparation method thereof |
| CN111205767A (en) * | 2020-02-26 | 2020-05-29 | 科顺防水科技股份有限公司 | Super-hydrophobic coating for corrosion prevention and freeze-thaw resistance of concrete and preparation method thereof |
| CN111205767B (en) * | 2020-02-26 | 2022-02-01 | 科顺防水科技股份有限公司 | Super-hydrophobic coating for corrosion prevention and freeze-thaw resistance of concrete and preparation method thereof |
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