CN104592646A - Polystyrene flame-retardant resin and preparation method thereof - Google Patents
Polystyrene flame-retardant resin and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/14—Copolymers of propene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2603—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
- C08G65/2606—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
- C08G65/2609—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups containing aliphatic hydroxyl groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2650/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G2650/22—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the initiator used in polymerisation
- C08G2650/24—Polymeric initiators
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention provides a polystyrene flame-retardant resin which is prepared from the following components in parts by mass: 70-80 parts of polystyrene, 8-15 parts of char forming agent pentaerythritol, 10-15 parts of borax, 0.01-0.5 part of stabilizing agent, 20-30 parts of hexabromocyclododecane, 10.6 parts of French chalk, 18-25 parts of zinc borate, 4-8 parts of cosolvent, 20-40 parts of hydroxide, 0.6-1.8 parts of color master batch, 10-20 parts of flame-retardant polyether, 4-8 parts of antimony trioxide, 15-20 parts of expandable graphite, 0.1-0.5 part of coupling agent, 8-15 parts of wood meal, 8-12 parts of sucrose and 5-10 parts of rutile titanium white. The test result indicates that the polystyrene flame-retardant resin satisfies Grade A in Classification for Burning Behavior of Building Materials and Products GB 8624-2006 and Grade A in Chinese Code for Fire Prevention in Design of Interior Decoration of Building GB5022-95.
Description
Technical field
The invention belongs to fire retardant material field, be specifically related to a kind of fire-retardant organic polymer material composition and method of making the same.
Background technology
The copolymer rubber that poly-third ethene (PPE) is is basic monomer with ethene, propylene, is usually used in the manufacture of household supplies, Drug packing, building materials stopping composition or electrical equipment shell.The fire-protection rating of material of construction is directly connected to the life security of resident, provides the high macromolecular material of fire-protection rating to be the problem that material produce person must pay close attention to.
Poly-third ethene working temperature is usually below 80 DEG C, and its resistance to elevated temperatures, fire performance limit the scope of application.
The fire-resistance thermal insulation board that utility model patent CN2937735Y proposes, with poly-third ethene for stopping composition, upper layer is the flame-retardant layer that magnesium hydroxide and glass fiber mesh are made.Such material relies on upper layer to realize flame retardant properties, do not improve the fire-retardant fireproof performance of poly-third vinyl material itself.Patent CN00817915.8 proposes flame-proof polypropelene composition.From existing document, fire-retardant poly-third vinyl material was not also suggested.
Summary of the invention
For meeting market demand, the present invention proposes a kind of poly-third ethene flame-retarded resin.
Another object of the present invention is the preparation method proposing described poly-third ethene flame-retarded resin.
For the technical scheme realizing above-mentioned purpose of the present invention is:
A kind of poly-third ethene flame-retarded resin, is prepared from by the composition of following mass parts:
Poly-third ethene (PPE) 70-80, tetramethylolmethane 8-15, borax 10-15, stablizer 0.01-0.5, hexabromocyclododecane 20-30, talcum powder 10.6, zinc borate 18-25, solubility promoter 4-8, oxyhydroxide 20-40, look female 0.6-1.8, flame retarding polyether 10-20, antimonous oxide 4-8, expansible black lead 15-20, coupling agent 0.1-0.5, wood powder 8-15, sucrose 8-12, rutile titanium white powder 5-10.
Wherein, described solubility promoter is phthalic acid two (2-ethyl) ester or phthalic acid two (2-propylheptyl) ester, and described oxyhydroxide is the one in magnesium hydroxide, aluminium hydroxide, magnesium hydroxide and aluminium hydroxide equal amount of mixture; Described stablizer is barium stearate or lead stearate.Described talcum powder preferable particle size is 1250-2500 object talcum powder.
Wherein, described coupling agent is silane coupling agent, is selected from the one in vinyltriethoxysilane, vinyl trichloro silane, vinyl three (beta-methoxy-oxyethyl group) silane, γ-glycidylpropyl-Trimethoxy silane.
Preferably, described wood powder is the wood powder through water glass process, described water glass is treated to: after wood powder toasts 15-20 minute through 260-300 DEG C, add water glass saturated solution and soak 30-40 hour, ratio is wood powder 1-2 part: water glass 0.8-1.5 part, and then drying in nitrogen environment, pulverizing is 1250 order-2500 object particles.
Wherein, described flame retarding polyether adopts following methods preparation and obtains: mass fraction is respectively the fluorochemical of 1-2,0.5-0.8,1.4-2.3,1.5-3, butylene oxide ring, catalyzer, tetrafluoroethylene, is 500-700 in temperature, under pressure is 50 ~ 80MPa, voltage 1.2-2.0 ten thousand volts of reaction conditionss, was obtained by reacting through 2-4 hour;
Wherein said fluorochemical is one or more in Sodium Fluoride, Potassium monofluoride, rare earth fluoride, magnesium fluoride; Described catalyzer is the mixture of methyl alcohol 0.6-0.8 mass parts, silicone oil 0.4-0.7 mass parts, water glass 0.3-0.5 mass parts, sodium bicarbonate 0.1-0.3 mass parts.
Wherein, the reaction preparing flame retarding polyether is carried out in airtight reaction vessel, and described reaction vessel fills with non-oxidizing gas, and described non-oxidizing gas is the mixture of 100 parts of nitrogen or argon gas and 1-3 part (parts by volume) carbonic acid gas;
The microwave generator that frequency is 80GHz-140GHz is provided with in described reaction vessel.
The preparation of flame retarding polyether can be carried out in airtight reaction vessel, in reaction vessel, arrange arc generator, and microwave generator is arranged on the reactor wall.Before the reaction starts, first vacuumize, be then full of container with non-oxidizing gas, make container inner pressure be 50 ~ 80MPa.
The poly-third ethene flame-retarded resin that the present invention proposes, is preferably prepared from by the composition of following mass parts:
Poly-third ethene 75, char-forming agent tetramethylolmethane 10-12, borax 10-12, stablizer 0.04-0.08, hexabromocyclododecane 20-25, talcum powder 10.6, zinc borate 20-22, solubility promoter 5-6, oxyhydroxide 30-35, look female 0.6-1.8, flame retarding polyether 15-17, antimonous oxide 4-6, expansible black lead 15-20, coupling agent 0.1-0.2, wood powder 10-12, sucrose 8-10, rutile titanium white powder 6-8.
The preparation method of described poly-third ethene flame-retarded resin, comprises step:
1) hexabromocyclododecane, antimonous oxide, expansible black lead, zinc borate, oxyhydroxide, coupling agent, stablizer are put into high speed mixer mix and blend together;
2) flame retarding polyether and wood powder are puddled in heating stirrer, temperature 95-120 degree, time 8-15 minute; Then less than 80 degree are cooled to cold wind;
3) by step 1) and step 2) gained mixture mixes in mixer, stir 2-3 minute, then add char-forming agent, talcum powder, borax, look mother, sucrose, rutile titanium white powder successively, stirring 3-10 minute;
4) by step 3) gained mixture mixes with poly-third ethene, then adds solubility promoter stirring and evenly mixing.
Preferably, described step 1) in, material is mix and blend 2-5 minute in high speed mixer, and the temperature of mix and blend controls at 60-80 degree.
Wherein, described step 4) in, stir 2-5 minute after adding solubility promoter.
Beneficial effect of the present invention is:
The present invention has used expansible black lead undergoes rapid expansion 100-200 characteristic doubly when temperature more than 200 DEG C; formed on poly-third ethene (now surface volume expansion 3-5 doubly) surface do not fire, the porous protective layer of heat insulation, resistance oxygen, through special oxide treatment wood powder also rapidly carbonization form carburization zone that is fire-retardant, heat insulation, resistance oxygen.The speed that a large amount of heat energy slows down PPE decomposition is taken away in the carbonization of tetramethylolmethane 310 DEG C decomposition simultaneously, and carbide is attached to the density strengthening protective layer around graphite linings, charcoal layer cavity.The effective outside heat that intercepted is to the conduction of polymeric inner, convection current and radiation.Borax, sucrose, oxyhydroxide decomposition release crystal water absorbs a large amount of heat energy and thermolysis is not easily carried out.Also serve the effect of dilution combustable gas concentration simultaneously.
The self-control flame retarding polyether that the present invention proposes is reacted under the environment of microwave by fluorochemical, polyethers, catalyzer to make for 3 hours under high temperature, high atmospheric pressure, high-voltage.Now F ion is half unbound state running into 450 DEG C--discharge a large amount of F ion during 750 DEG C of high temperature and catch pyrolytic decomposition active group H
+, OH
-generate stable FH, this reaction is decomposed complete with PPE superpolymer always.The very effective concentration reducing inflammable gas, thus reach the object suppressing naked light to generate.
Embodiment
Following examples for illustration of the present invention, but should not be used for limiting the scope of the invention.In embodiment, if no special instructions, means used are this area routine techniques means.
Embodiment 1: the preparation of flame retarding polyether
2 meters high, the reaction vessel of cylindrical enclosure, in reaction vessel, arrange arc generator, reactor wall 1.5m At The Height arranges microwave generator.Before the reaction starts, vacuumize rear nitrogen and carbonic acid gas (volume ratio 100:1.5) is full of container, make container inner pressure be 75MPa.
Catalyzer is the mixture of methyl alcohol 0.8 mass parts, silicone oil 0.7 mass parts, water glass 0.5 mass parts, sodium bicarbonate 0.3 mass parts.
Mass fraction is respectively the rare earth fluoride of 1,0.8,2.3,3.0 (purchased from the new Willie one-tenth rare earth company limited in Yixing, 2000 orders), butylene oxide ring, catalyzer, tetrafluoroethylene be 560 DEG C in temperature, under pressure is 75MPa, voltage 1.5 ten thousand volts, microwave frequency 100GHz reaction conditions, be obtained by reacting through 3 hours.
Embodiment 2: the preparation of flame retarding polyether
Equipment and pressure-controlling are with embodiment 1.
Catalyzer is the mixture of methyl alcohol 0.7 mass parts, silicone oil 0.6 mass parts, water glass 0.5 mass parts, sodium bicarbonate 0.2 mass parts.
Mass fraction is respectively the rare earth fluoride of 1,0.5,2.0,2.0 (purchased from the new Willie one-tenth rare earth company limited in Yixing, 2000 orders), butylene oxide ring, catalyzer, tetrafluoroethylene be 550 DEG C in temperature, under pressure is 75MPa, voltage 1.5 ten thousand volts, microwave frequency 100GHz reaction conditions, be obtained by reacting through 3 hours.
Embodiment 3: the preparation of flame retarding polyether
Equipment and pressure-controlling are with embodiment 1.
Catalyzer is with embodiment 2.Lanthanum fluoride (becoming rare earth company limited purchased from new Willie, Yixing), butylene oxide ring, catalyzer, tetrafluoroethylene that mass fraction is respectively 1,0.5,2.0,1.5 are 550 DEG C in temperature, under pressure is 75MPa, voltage 1.5 ten thousand volts, microwave frequency 100GHz reaction conditions, were obtained by reacting through 3 hours.
The preparation of the poly-third ethene flame-retarded resin of embodiment 4
Composition of raw materials is:
Preparation technology:
1) hexabromocyclododecane, antimonous oxide, expansible black lead, zinc borate, magnesium hydroxide, coupling agent, aluminium hydroxide, barium stearate are put into together the mixed stirring of high speed mixer 3 minutes, temperature controls between 60-80 degree.
2) flame retarding polyether, molybdic oxide and the wood powder through special oxide treatment are puddled heating in mixer, temperature 105 degree, 10 minutes time; Then 80 degree are cooled to cold wind.
3) by step 1) and step 2) batch mixing that obtains to be placed in mixer mixed stirring 2 minutes, then add successively char-forming agent, talcum powder, borax, look mother, sucrose, rutile titanium white powder, stir 5 minutes;
4) by step 3) gained mixture and major ingredient PPE mix and add solubility promoter again and stir 5 minutes.Particulate material is extruded with screw extrusion press.
The preparation of the poly-third ethene flame-retarded resin of embodiment 5
Composition of raw materials is:
Preparation method is with embodiment 1.
The preparation of the poly-third ethene flame-retarded resin of embodiment 6
Composition of raw materials is:
Preparation method is with embodiment 1.
Experimental example: fire resistance is tested
The material that embodiment 4,5,6 is obtained, is pressed into the sheet material of different size, carries out following fire resistance test.
1 cut-off footpath 45mm, high 50mm plate sample, each embodiment two pieces, laboratory apparatus is JCB-2 building materials non-combustibility test stove, and test result is: 1. average temperature rising △ T≤50 DEG C in stove; 2, sample mean mass loss rate≤50%; 3, sample sustained combustion time tf≤20s.
2 get width 495mm, length 1500mm plate sample, each embodiment one piece, width 1000mm, length 1500mm plate sample, each embodiment one piece, through building material made monomer combustion testing apparatus (DT-1 type) test, result is 1, burning rate of increase index FIGRA≤120W/s; 2, flame laterally spreads length LFS=0m; 3, the total thermal discharge THR600s≤7.5MJ when time is 600s; 4, smoke-producing amount s1 level; 5, density flaming droplet/particulate d0 level.
3 get each three pieces of square sheet material 400mm by product smoke toxicity test device (JOD-3 type, English shellfish Tianjin measuring and controlling equipment company limited) test result is: produce smoke toxicity t0 level.
4 detect oxygen index for being respectively 39,38,42 through oxygen index tester, see the following form:
Table 1: sheet material flame retardant properties test result
| Combustion time s | Smoke density (GB-8624-1997 standard) | Oxygen index | |
| Embodiment 4 | 19 | 72 | 39 |
| Embodiment 5 | 18 | 70 | 38 |
| Embodiment 6 | 12 | 61 | 42 |
The A grade standard of existing People's Republic of China (PRC) GB 8624-2006 " material of construction and product burns grading performance " and the A level requirement of People's Republic of China (PRC) GB5022--95 " code for fire prevention design of interior decoration of buildings " is met completely by above test.
Although above the present invention has done detailed description, and on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (10)
1. a poly-third ethene flame-retarded resin, is characterized in that, be prepared from by the composition of following mass parts:
Poly-third ethene 70-80, char-forming agent tetramethylolmethane 8-15, borax 10-15, stablizer 0.01-0.5, hexabromocyclododecane 20-30, talcum powder 10.6, zinc borate 18-25, solubility promoter 4-8, oxyhydroxide 20-40, look female 0.6-1.8, flame retarding polyether 10-20, antimonous oxide 4-8, expansible black lead 15-20, coupling agent 0.1-0.5, wood powder 8-15, sucrose 8-12, rutile titanium white powder 5-10.
2. poly-third ethene flame-retarded resin according to claim 1, it is characterized in that, described solubility promoter is phthalic acid two (2-ethyl) ester or phthalic acid two (2-propylheptyl) ester, and described oxyhydroxide is the one in magnesium hydroxide, aluminium hydroxide, magnesium hydroxide and aluminium hydroxide equal amount of mixture; Described stablizer is barium stearate or lead stearate.
3. poly-third ethene flame-retarded resin according to claim 1, it is characterized in that, described coupling agent is silane coupling agent, is selected from the one in vinyltriethoxysilane, vinyl trichloro silane, vinyl three (beta-methoxy-oxyethyl group) silane, γ-glycidylpropyl-Trimethoxy silane.
4. poly-third ethene flame-retarded resin according to claim 1, it is characterized in that, described wood powder is the wood powder through water glass process, described water glass is treated to: after wood powder toasts 15-20 minute through 260-300 DEG C, add water glass saturated solution and soak 30-40 hour, ratio is wood powder 1-2 part: water glass 0.8-1.5 part, and then drying in nitrogen environment, pulverizing is 1250 order-2500 object particles.
5. according to the arbitrary described polyamide resin A level fire-retardant material of claim 1-4, it is characterized in that, described flame retarding polyether adopts following methods preparation and obtains: mass fraction is respectively the fluorochemical of 1-2,0.5-0.8,1.4-2.3,1.5-3, butylene oxide ring, catalyzer, tetrafluoroethylene, is 500-700 in temperature, under pressure is 50 ~ 80MPa, voltage 1.2-2.0 ten thousand volts of reaction conditionss, was obtained by reacting through 2-4 hour;
Wherein, described fluorochemical is one or more in Sodium Fluoride, Potassium monofluoride, rare earth fluoride, magnesium fluoride; Described catalyzer is the mixture of methyl alcohol 0.6-0.8 mass parts, silicone oil 0.4-0.7 mass parts, water glass 0.3-0.5 mass parts, sodium bicarbonate 0.1-0.3 mass parts.
6. polyamide resin A level fire-retardant material according to claim 5, it is characterized in that, the reaction preparing flame retarding polyether is carried out in airtight reaction vessel, described reaction vessel fills with non-oxidizing gas, and described non-oxidizing gas is the mixture of 100 parts of nitrogen or argon gas and 1-3 part, carbonic acid gas;
The microwave generator that frequency is 80GHz-140GHz is provided with in described reaction vessel.
7., according to the arbitrary described poly-third ethene flame-retarded resin of claim 1-6, it is characterized in that, be prepared from by the composition of following mass parts:
Poly-third ethene 75, char-forming agent tetramethylolmethane 10-12, borax 10-12, stablizer 0.04-0.08, hexabromocyclododecane 20-25, talcum powder 2000 order 10.6, zinc borate
20-22, solubility promoter 5-6, oxyhydroxide 30-35, look female 0.6-1.8, flame retarding polyether 15-17, antimonous oxide 4-6, expansible black lead 15-20, coupling agent 0.1-0.2, wood powder 10-12, sucrose 8-10, rutile titanium white powder 6-8.
8. prepare the method for the arbitrary described poly-third ethene flame-retarded resin of claim 1-7, it is characterized in that, comprise step:
1) hexabromocyclododecane, antimonous oxide, expansible black lead, zinc borate, oxyhydroxide, coupling agent, stablizer are put into high speed mixer mix and blend together;
2) flame retarding polyether and wood powder are puddled in heating stirrer, temperature 95-120 degree, time 8-15 minute; Then less than 80 degree are cooled to cold wind;
3) by step 1) and step 2) gained mixture mixes in mixer, stir 2-3 minute, then add char-forming agent, talcum powder, borax, look mother, sucrose, rutile titanium white powder successively, stirring 3-10 minute;
4) by step 3) gained mixture mixes with poly-third ethene, then adds solubility promoter stirring and evenly mixing.
9. method according to claim 8, is characterized in that, described step 1) in, material is mix and blend 2-5 minute in high speed mixer, and the temperature of mix and blend controls at 60-80 degree.
10. method according to claim 8 or claim 9, is characterized in that, described step 4) in, stir 2-5 minute after adding solubility promoter.
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