Classifications

• • 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
  • C08G64/00—Macromolecular compounds obtained by reactions forming a carbonic ester link in the main chain of the macromolecule
  • C08G64/04—Aromatic polycarbonates
  • C08G64/06—Aromatic polycarbonates not containing aliphatic unsaturation
  • C08G64/08—Aromatic polycarbonates not containing aliphatic unsaturation containing atoms other than carbon, hydrogen or oxygen
  • C08G64/10—Aromatic polycarbonates not containing aliphatic unsaturation containing atoms other than carbon, hydrogen or oxygen containing halogens
• • 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
  • C08K5/00—Use of organic ingredients
  • C08K5/04—Oxygen-containing compounds
  • C08K5/10—Esters; Ether-esters
  • C08K5/109—Esters; Ether-esters of carbonic acid, e.g. R-O-C(=O)-O-R
• • 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
  • C08K5/00—Use of organic ingredients
  • C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
  • C08K5/41—Compounds containing sulfur bound to oxygen
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
  • C09K21/00—Fireproofing materials
  • C09K21/06—Organic materials
  • C09K21/08—Organic materials containing halogen

Definitions

• the present invention relates to a method for producing a particulate flame retardant comprising a halogenated carbonate compound having excellent workability, workability and heat resistance.
• polybutylene terephthalate ⁇ ABS resin Due to its excellent properties, polybutylene terephthalate ⁇ ABS resin is widely used in electrical, electronic, mechanical, automotive and other applications. However, since such a thermoplastic resin is inherently flammable, its field of use is limited. Therefore, halogenated polycarbonate oligomers have been proposed as these flame retardants.
• thermoplastic resin flame-retardant As a method of making a thermoplastic resin flame-retardant, it is difficult to mix and extrude a pellet-shaped thermoplastic resin with a flame retardant and, if necessary, other additives, and melt-extrude it using an extruder. Flammable thermoplastic resin pellets are obtained.
• the above-mentioned flame retardant is an extremely fine powder, it is uniformly dispersed due to poor workability such as poor layer separation and bridge formation in the hopper of the extruder and poor penetration into the screw. And has the drawback of lowering the quality of the final product obtained.
• the workability is poor, such as the flame retardant itself becoming dusty and significantly deteriorating the work environment.
• the flame retardant contains a considerable amount of a solvent (methylene chloride) used in the production thereof, and there is a concern that this may adversely affect the quality of the final product.
• Japanese Patent Application Laid-Open No. Sho 62-1499738 discloses a granulation method of cold-compacting an orifice hydrocarbon flame retardant. Has been proposed. However, in order to granulate the halogenated polycarbonate oligomer by the granulation method of cold compaction, a high pressure of 1000 to 200 O kgZcm 2 is required, and further obtained. Granules have a disadvantage that they are easily broken down during transportation or work.
• An object of the present invention is to provide a method for producing a particulate flame retardant comprising a parogenated carbonate compound having excellent workability, workability and heat resistance.
• the present inventors have conducted intensive studies to achieve the above-mentioned object.
• a halogenated carbonate compound having a specific specific viscosity can be easily granulated by melt-extruding with an extruder and immediately cutting it.
• the present invention was found to be possible, and that the amount of solvent in the obtained particulate matter could be reduced to a level that did not cause any problem.
• the present invention provides the following general formula (i):
• X is a bromine atom or a chlorine atom
• R 1 is an alkylene group having 1 to 4 carbon atoms, an alkylidene group or 1 S 0 2 —.
• the halogenated carbonate compound used in the present invention has the general formula (i) And a halogenated bisphenol which is a constituent of this unit is 2,2-bis (3,5-dibromo-14-hydroxyphenyl) propane, 2,2-bis ( 3,5-dichloro-1-hydroxypropenyl, propane, bis (3,5-dibromo-1-hydroxyphenyl) methane, 1,1-bis (3,5-dibromo-1-hydroxyphenyl) ethane And bis (3,5-dibromo-14-hydroxyphenyl) sulfone.
• 2,2-bis (3,5-dibromo-14-hydroxyphenyl) propane which is called tetrabromobisphenol A, is preferred.
• halogenated bisphenols such as 2,2-bis (4-hydroxyphenyl) pulp bread, bis (4-hydroxyphenyl) sulfone, and bis (4-hydroxyphenyl) Methane or the like can be used in combination.
• a non-halogenated bisphenol it is usually preferable to use an amount of 40 mol% or less of the total bisphenol, and in this case, a carbonate composed of non-halogenated bisphenol It may contain one or more of them.
• the halogenated carbonate compound used in the present invention has a specific viscosity of 0.1.
• halogenated carbonate compounds include, for example, halogenated bisphenols. It is produced by reacting phenol with phenol and a carbonate precursor such as phosgene. At this time, a terminal blocking agent can be used.
• Preferred end-capping agents are aromatic monohydroxy compounds that are substituted or unsubstituted with halogen atoms or organic groups.
• the halogenated carbonate compound may include, for example, a flame retardant aid, an antioxidant, a heat stabilizer, an ultraviolet absorber, a lubricant, a release agent, a dye and a pigment within a range not to impair the object of the present invention.
• a flame retardant aid such as an antioxidant, a heat stabilizer, an ultraviolet absorber, a lubricant, a release agent, a dye and a pigment within a range not to impair the object of the present invention.
• One or more additives such as a coloring agent and a nucleating agent can be added as necessary.
• the temperature of the melt is usually in the range of 10 ° C to 60 ° C higher than its melting point. It is preferable to use Any single-screw or twin-screw extruder can be used, but a twin-screw extruder is preferred, and a twin-screw extruder with a vent is particularly preferred.
• the extruded melt is cut into granules immediately after extrusion.
• the granular material of the halogenated carbonate compound obtained by the present invention has good processability and is uniformly dispersed, does not cause deterioration in the quality of the final resin product obtained, and has good workability and improves the working environment. It does not worsen. In addition, the amount of solvent in the resulting granules has been reduced to an acceptable level. ⁇ Best mode for carrying out the invention>
• Melting point Shows the temperature at which about half the amount was melted by a trace melting point measuring instrument, from the melting point.
• 3 Methylene chloride content 3 g of a sample is precisely weighed, heated at 250 ° C for 2 hours, gas is collected for 1 l, analyzed by gas chromatography, and determined by the calibration curve.
• Each of the fine powders A to H of the finely divided halogenated carbonate compound described in Table 1 is melt-extruded at the cylinder temperature shown in the table using a twin screw extruder of 30 ⁇ , and is immediately cut into granules and sprayed with compressed air. The mixture was cooled to obtain granules.
• Table 1 shows the physical properties of the fine powder used, the temperature of the melt during melt extrusion, and the physical properties of the obtained granular material.
• the fine powders A to H described in the table are as follows.
• A, D, F, G, H Brominated carbonate compounds obtained from tetrabromobisphenol A, phosgene and tert-butyl phenol (end capping agent).
• A Brominated carbonate compound obtained from tetrabromobisphenol A, bisphenol A (50 mol% based on tetrabromobisphenol A), phosgene and tetrabromophenol (terminal blocking agent).
• Example 1 A 0.46 230 to 240 2480 447 240 275 0.0447 228 to 238 340 451 Almost colorless Example 2 A 0.0046 230 to 240 2480 447 240 275 Yes 0.048 230 to 240 150 452 Almost colorless Difficult 3 B 0.046 230 to 240 2480 447 240 280 Yes 0.049 227 to 237 160 455 Almost colorless 4 C 0.018 175-180 1050 438 180 220 0.001 018 173 ⁇ 178 210 445 Almost colorless Example 5 D 0.032 210 ⁇ 215 1600 448 210 240 0.033 210 ⁇ 215 410 453 Almost colorless 0.030 215 to 222 3700 467 220 250 Yes 0.032 213 to 220 100 476 Almost colorless Example 7 F 0.072 255 to 275 1850 441 250 290 m

Landscapes

• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Health & Medical Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Medicinal Chemistry (AREA)
• Polymers & Plastics (AREA)
• Engineering & Computer Science (AREA)
• Materials Engineering (AREA)
• Compositions Of Macromolecular Compounds (AREA)
• Fireproofing Substances (AREA)
• Polyesters Or Polycarbonates (AREA)

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Publications (1)

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Cited By (2)

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Citations (2)

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• 1990
  • 1990-02-14 JP JP2033349A patent/JPH0819412B2/ja not_active Expired - Lifetime
• 1991
  • 1991-02-14 DE DE4190245A patent/DE4190245C2/de not_active Expired - Lifetime
  • 1991-02-14 DE DE19914190245 patent/DE4190245T/de not_active Expired - Lifetime
  • 1991-02-14 WO PCT/JP1991/000174 patent/WO1991012295A1/ja active Application Filing
  • 1991-02-14 US US07/768,193 patent/US5180525A/en not_active Expired - Lifetime

Patent Citations (2)

Non-Patent Citations (1)

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