NL2032626B1 - Device for producing flame-retardant expandable polystyrene by bulk polymerization - Google Patents
Device for producing flame-retardant expandable polystyrene by bulk polymerization Download PDFInfo
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- NL2032626B1 NL2032626B1 NL2032626A NL2032626A NL2032626B1 NL 2032626 B1 NL2032626 B1 NL 2032626B1 NL 2032626 A NL2032626 A NL 2032626A NL 2032626 A NL2032626 A NL 2032626A NL 2032626 B1 NL2032626 B1 NL 2032626B1
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- polymerization reactor
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- retardant
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 45
- 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 41
- 229920006248 expandable polystyrene Polymers 0.000 title claims abstract description 37
- 238000012662 bulk polymerization Methods 0.000 title claims description 12
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 59
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000005453 pelletization Methods 0.000 claims abstract description 17
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 claims abstract description 16
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 13
- 239000000155 melt Substances 0.000 claims abstract description 12
- ORYGKUIDIMIRNN-UHFFFAOYSA-N 1,2,3,4-tetrabromo-5-(2,3,4,5-tetrabromophenoxy)benzene Chemical compound BrC1=C(Br)C(Br)=CC(OC=2C(=C(Br)C(Br)=C(Br)C=2)Br)=C1Br ORYGKUIDIMIRNN-UHFFFAOYSA-N 0.000 claims abstract description 10
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004698 Polyethylene Substances 0.000 claims abstract description 6
- -1 polyethylene Polymers 0.000 claims abstract description 6
- 229920000573 polyethylene Polymers 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000004088 foaming agent Substances 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 8
- 239000004793 Polystyrene Substances 0.000 claims description 7
- 229920002223 polystyrene Polymers 0.000 claims description 7
- 239000002667 nucleating agent Substances 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 2
- 235000013539 calcium stearate Nutrition 0.000 claims description 2
- 239000008116 calcium stearate Substances 0.000 claims description 2
- 239000000498 cooling water Substances 0.000 claims description 2
- 238000007790 scraping Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims 1
- 238000007599 discharging Methods 0.000 abstract description 9
- 239000000047 product Substances 0.000 description 10
- 239000000725 suspension Substances 0.000 description 8
- 239000012530 fluid Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000010924 continuous production Methods 0.000 description 4
- 239000012736 aqueous medium Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000011324 bead Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1862—Stationary reactors having moving elements inside placed in series
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/91—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with propellers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/81—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles
- B01F33/811—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles in two or more consecutive, i.e. successive, mixing receptacles or being consecutively arranged
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
- B01F33/8362—Mixing plants; Combinations of mixers combining mixing with other treatments with chemical reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C44/00—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles
- B29C44/34—Auxiliary operations
- B29C44/3461—Making or treating expandable particles
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
- C08J9/141—Hydrocarbons
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/16—Making expandable particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
- B01F2101/2805—Mixing plastics, polymer material ingredients, monomers or oligomers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C44/00—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles
- B29C44/34—Auxiliary operations
- B29C44/3442—Mixing, kneading or conveying the foamable material
- B29C44/3446—Feeding the blowing agent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2025/00—Use of polymers of vinyl-aromatic compounds or derivatives thereof as moulding material
- B29K2025/04—Polymers of styrene
- B29K2025/06—PS, i.e. polystyrene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
Disclosed is a device for producing flame-retardant expandable polystyrene (EPS) by bulk 5 polymerization includes 2 polymerization reactors connected in series, wherein the polymerization reactors are connected with a heating devolatilizer via a discharging pump; a condenser and a vacuum collecting tank are connected at the upper end of the heating devolatilizer; a dynamic mixer, a melt heat exchanger, a pump and a high-pressure underwater pelletizing system are connected successively with the heating devolatilizer at the bottom via a pump. 92.0 kg of styrene, 10 5.0 kg of ethylbenzene, 1.0 kg of white oil, 0.5 kg of tributyl phosphate, 1.0 kg of low molecular weight polyethylene, 6.0 kg of pentane, and 0.9 kg of octabromodiphenyl ether (flame retardant) are preferred for the device. The obtained flame-retardant EPS has good impact resistance and tensile strength, with a particle diameter strictly controlled between 0.7 mm and 1.0 mm.
Description
DEVICE FOR PRODUCING FLAME-RETARDANT EXPANDABLE POLYSTYRENE BY BULK
POLYMERIZATION
The present invention relates to the technical field of expandable polystyrene resin, and in particular to a device for producing flame-retardant expandable polystyrene.
In the prior art, expandable polystyrene (EPS) is produced using styrene as the main raw material through a suspension batch polymerization process, including the following main steps: dispersing liquid styrene monomer in an aqueous medium by using a suspension dispersant, adding an initiator to initiate a polymerization reaction, and adding a foaming agent to complete the polymerization reaction when the conversion rate falls within a certain range; conducting washing, drying and sieving. CN105294041A discloses a homogeneous modified fireproof insulation board, wherein the diameter of beads obtained by this suspension technology varies widely from 0.1 mm to 4 mm; the incorporation of a nucleating agent and/or a flame retardant into beads is difficult, and may inhibit the polymerization reaction; the polymerization reaction is conducted in an aqueous medium, and a suspension dispersant requires to be added, resulting in a large amount of sewage and environmental protection problems; the product quality stability is poor.
In order to solve the above-mentioned technical problem, the present invention provides a device and method for producing flame-retardant EPS by bulk polymerization, so that the product obtained with a particle diameter of 0.7-1.0 mm, achieves the same flame-retarding effect as products prepared based on a suspension method when 0.9% of octabromodiphenyl ether (flame retardant) is used.
The present invention solves this technical problem through the following technical solution:
The present invention adopts a bulk polymerization process to produce flame-retardant
EPS, and the device used includes a polymerization reactor 1 and a polymerization reactor 2, wherein the polymerization reactor 1 and the polymerization reactor 2 are connected in series via a discharging pump; material inlets are arranged at upper heads of the polymerization reactors respectively, reaction stirrers are arranged in the middle parts of the upper heads respectively, and the upper heads are communicated with condensers respectively; the reaction stirrers are variable-frequency stirrers with rotational speeds adjusted depending on the viscosity of the materials; the lower end of the polymerization reactor 2 is connected with a heating devolatilizer via a discharging pump; a condenser is connected at the upper end of the heating devolatilizer, and the condenser is connected with a vacuum collecting tank; the bottom of the heating devolatilizer is connected with a dynamic mixer via a pump, and the dynamic mixer is connected with a melt heat exchanger; the melt heat exchanger is connected with a high-pressure underwater pelletizing system via a pump; a hole diameter of high-temperature die heads in the high-pressure underwater pelletizing system is 0.8 mm.
A connector for adding a molten flame retardant masterbatch is installed at the front end of the dynamic mixer; a material backflow preventer is arranged at the connector to prevent the materials from flowing back; the flame retardant masterbatch is melted by a screw extruder and injected into the mixer for mixing with a polystyrene foaming agent, so that a flame retardant is embedded in a molecular chain of polystyrene.
When the device is used to produce flame-retardant EPS, styrene, a solvent and an additive are added into the polymerization reactor 1 in proportion, the temperature of the materials in the polymerization reactor 1 is controlled at 120-150°C, the stirring speed is controlled at 40-80 rpm, and cooling is started for refluxing; the materials are polymerized in the polymerization reactor 1 for 1.5-2 h; then, the materials are delivered to the polymerization reactor 2 by the discharging pump, the temperature of the material in the polymerization reactor 2 is controlled at 180-180°C, cooling is started for refluxing, the stirring speed is controlled at 15-20 rpm, and the polymerization reaction is continued for 1.5-2 h. When a styrene conversion rate in the polymerization reactor 2 reaches 60-70%, the materials in the polymerization reactor 2 are delivered to the top of the heating devolatilizer via the discharging pump, the temperature of the heating devolatilizer is controlled at 220-250°C, the vacuum is controlled at -0.098 MPa, and flash evaporation is conducted; vapor containing the unreacted styrene, solvent and other light components is removed and delivered into the condenser for cooling and refluxing, and the condensate flows into the vacuum collecting tank and is recycled into the polymerization reactor 1 for polymerization reaction. A first fluid of polystyrene obtained through flash evaporation is delivered into the mixer via the pump; meanwhile, a second fluid of foaming agent and flame retardant is also delivered into the mixer via the connector; the two fluids are mixed uniformly and delivered into the melt heat exchanger, and the temperature of the material in the melt heat exchanger is controlled at 180-205°C; next, the materials are delivered into the high-pressure underwater pelletizing system via the pump, and flame-retardant EPS particles are obtained through pelletizing and drying.
The polymerization reaction time is a bottleneck for producing flame-retardant EPS by the bulk polymerization process. Therefore, the polymerization reactor 1 and the polymerization reactor 2 are connected in series, which can nearly double the overall capacity without adding other devices.
The materials delivered into the polymerization reactor 1 include the following components: 80-95 kg of styrene, 2-10 kg of solvent and 0.5-5 kg of additive. The materials delivered into the mixer also include: 3-8 kg of foaming agent; 0.5-4 kg of flame retardant.
Preferably, the styrene is 89-93 kg, and the ethylbenzene (solvent) is 5.0 kg; the additive contains one or more of white oil, tributyl phosphate, calcium stearate, MgO, and low molecular weight polyethylene (nucleating agent), amounting to 2.0-4.0 kg; the pentane (foaming agent) is 5.0-7.0 kg; the flame retardant contains one or more of brominated polystyrene, octabromo series flame retardant and tetrabromo series flame retardant, amounting to 0.7-1.0 kg.
Further preferably, 92.0 kg of styrene, 5.0 kg of ethylbenzene, 1.0 kg of white oil, 0.5 kg of tributyl phosphate, 1.0 kg of low molecular weight polyethylene, 6.0 kg of pentane, and 0.9 kg of octabromodiphenyl ether (flame retardant) are used. The obtained flame-retardant EPS has good impact resistance and tensile strength, with a particle diameter strictly controlled between 0.7 mm and 1.0 mm. Compared with ordinary EPS particle products, the product of the present invention merely requires 0.9% of octabromodiphenyl ether to satisfy national standard levels for flame retardance.
The present invention has the following features and advantages: 1. The device for producing flame-retardant EPS by bulk polymerization of the present invention enables the continuous production of flame-retardant EPS by bulk polymerization owing to mutual support and synergy of various components as well as operation methods and steps. Especially, the polymerization reactor 1 and the polymerization reactor 2 are connected in series, which can nearly double the capacity of the entire production line; a foundation is laid for the continuous production; the styrene conversion rate is controlled at 80-70% for discharging, mainly because the further increase in the styrene conversion rate is very slow and easily results in by-products, which is disadvantageous to product quality and production efficiency, the temperature and vacuum are controlled in the heating devolatilizer, which is advantageous to flash evaporation; vapor removed through flash evaporation enters the condenser for refluxing and recycling; the foaming agent and the flame retardant are mixed with polystyrene in the mixer, and the mixture is cooled by the melt heat exchanger, which facilitates quality stability; the flame-retardant EPS is obtained through cooling, pelletizing and drying in the high-pressure underwater pelletizing system, with a particle diameter strictly controlled between 0.7 mm and 1.0 mm, and merely requires 0.9% of octabromodiphenyl ether (flame retardant) to satisfy national standard levels for flame retardance, with favourable foaming performance, excellent appearance, and good flame retardance, impact resistance and tensile strength. 2. The continuous production of graphite-type EPS by the bulk polymerization requires no aqueous medium in the reaction process, generates less wastewater, and has good environmental protection effect.
FIG. 1 is a schematic diagram of a device for producing flame-retardant EPS by bulk polymerization.
The implementation of the technical solution of the present invention will be described below through specific embodiments.
FIG. 1 is a schematic diagram of a device for producing flame-retardant EPS by bulk polymerization of the present patent. In this specific embodiment, the device includes the following arrangements: a polymerization reactor (1-1) is connected in series with a polymerization reactor (1-2) via a discharging pump (4-1), material inlets are arranged at upper heads of the polymerization reactors (1-1) and (1-2) respectively, variable-frequency reaction stirrers (2-1) and (2-2) with adjustable rotational speeds are arranged in the middle parts of the upper heads respectively, and the upper heads are communicated with condensers (3-1) and (3-2) respectively; the lower end of the polymerization reactor (1-2) is connected with a heating devolatilizer (5) via a discharging pump (4-2), a condenser (7) is connected at the upper end of the heating devolatilizer (5), and the condenser (7) is connected with a vacuum collecting tank (8); the bottom of the heating devolatilizer (5) is connected with a dynamic mixer (9) via a pump (6), and the dynamic mixer (9) is connected with a melt heat exchanger (10); a flame retardant masterbatch connector (9-1) is arranged at the front end of the dynamic mixer (9), and a material backflow preventer is arranged at the connector (8-1); the melt heat exchanger (10) is connected with a high-pressure underwater pelletizing system (12) via a pump (11), and a hole diameter of high-temperature die heads in the high-pressure underwater pelletizing system (12) is 0.8 mm.
The following components are applied in the embodiment of the present invention: 92.0 kg of styrene, 5.0 kg of ethylbenzene, 1.0 kg of white oil, 0.5 kg of tributyl phosphate, 1.0 kg of low molecular weight polyethylene (nucleating agent), 6.0 kg of pentane (foaming agent), and 0.9 kg of octabromodiphenyl ether (flame retardant).
A method for producing flame-retardant EPS with the device includes the following steps:
First, a nucleating agent is prepared into a 10.0% solution by using styrene; styrene, an ethylbenzene solvent, white oil, tributyl phosphate and the nucleating agent are respectively measured with a flow meter and continuously delivered into the polymerization reactor (1-1), the temperature of the materials in the polymerization reactor (1-1) is controlled at 148°C, the rotational speed of the stirrer (2-1) is controlled at 40 rpm, and a polymerization reaction is conducted for 1.5 h; the condenser (3-1) is turned on, and vapor is cooled to flow into the polymerization reactor (1-1).
Then, the materials are delivered into the polymerization reactor (1-2) via the discharging pump (4-1), the temperature of the material is controlled at 168°C, the rotational speed of the stirrer (2-2) is controlled at 15 rpm, the condenser (3-2) is turned on, and vapor is cooled to flow back into the polymerization reactor (1-2); the polymerization reaction is continued for 1.5 h; the styrene conversion rate is 70.0% at this moment, the materials are delivered from the polymerization reactor (1-2) to the top of the heating devolatilizer (5) via the discharge pump (4-
2), the temperature of the heating devolatilizer (5) is controlled at 240°C, flash evaporation is completed within 1 min, the unreacted styrene, solvent and other light components are removed into the condenser (7) for cooling, the vacuum is controlled at -0.098 MPa, and the condensate flows into the vacuum collecting tank (8); the condensate is recycled into the polymerization 5 reactors (1) for the polymerization reaction, which can reduce monomer residues in EPS particles, lower costs and satisfy food-grade requirements.
A first fluid of polystyrene obtained through flash evaporation is delivered into the dynamic mixer (9) via the pump (8); meanwhile, a second fluid of pentane (foaming agent) and octabromodiphenyl ether is accurately measured and delivered into the dynamic mixer (9) via the connector (9-1), and the two fluids are uniformly mixed through high-speed shearing in the dynamic mixer (9).
The two fluids are mixed uniformly, and the temperature of the uniform mixture is decreased to 185°C by the melt heat exchanger (10).
Next, the materials are delivered into the high-pressure underwater pelletizing system (12) via the pump (11), wherein 60 high-temperature die heads with a hole diameter of 0.8 mm are arranged in the high-pressure underwater pelletizing system (12); the materials are scraped by blades into small particles of 0.7-1.0 mm, wherein both die heads and scraping blades are immersed in high-pressure cooling water at 40°C; and the finished product, i.e., EPS particles, is obtained through cooling, pelletizing and drying.
Through testing, the obtained flame-retardant EPS has an oxygen index of 32, satisfying requirements for class B1 fireproof materials. Data of EPS prepared by this method and EPS prepared by the suspension method are compared and analysed. Production consumption data are as shown in Table 1 and product performance test data are as shown in Table 2.
Table 1 Production consumption data
Material Unit Test data of producing Data of producing flame-
EPS by the method of the | retardant EPS by suspension rn mw omeerees | 0 | 8
Ki ehr | Fofov ofS | 8 | ow wd | Twonoes | 0 | wm
Table 2 Product performance test data
Index Test data of EPS prepared Data of EPS prepared by by the embodiment suspension method
Molecular weight (number-average 188,000 55,000 molecular weight)
Molecular weight (weight-average 396,000 molecular weight)
Particle size (mm) 0.80+0.05 0.3-4.5, multilevel particle diameters
It can be seen from Table 1 and Table 2 that the flame-retardant EPS with the equivalent flame-retarding effect can be obtained by adding 0.9% of octabromodiphenyl ether (flame retardant) through the bulk polymerization in the present invention, and the consumption of raw materials and the discharge of wastewater and waste gas are reduced. The continuous production by bulk polymerization is realized, so that production cost is reduced, and the product performance is greatly improved.
Claims (5)
Applications Claiming Priority (1)
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