Fire retardant, preparation method thereof, composite polycarbonate material, and preparation method thereof
A technology of polycarbonate and composite materials, applied in the direction of sulfonic acid preparation, hydrocarbons, hydrocarbons, etc., can solve the problem that the flame retardant grade only reaches UL-94V-2, which is difficult to meet the requirements of polycarbonate composite materials, and cannot meet the requirements Flame retardant requirements and other issues, to achieve high flame retardant efficiency, high content of flame retardant elements, conducive to recovery and recycling effects
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[0048] The present invention also provides a preparation method of the above-mentioned flame retardant, comprising: S1) reacting haloadamantane and benzene through Friedel-Crafts alkylation to obtain 1,3,5,7-tetraphenyladamantane; S2) The 1,3,5,7-tetraphenyladamantane is reacted with chlorosulfonic acid to obtain 1,3,5,7-tetraphenylsulfonylchloroadamantane; then hydrolyzed to obtain 1,3,5,7 - adamantane tetra-p-benzenesulfonate; S3) react the 1,3,5,7-adamantane tetra-p-benzenesulfonate with the amino-containing compound shown in formula (II) to obtain the compound shown in formula (I) flame retardant;
[0049] R-NH 2 (II);
[0050] Wherein, R is selected from a C1-C5 substituted alkyl group, a C6-C10 substituted aryl group, a substituted five-membered heterocyclic group or a substituted six-membered heterocyclic group; the C1-C5 substituted alkyl group, C6-C10 The substituents in the substituted aryl group, substituted five-membered heterocyclic group or substituted six-...
Embodiment 1
[0085] 1.1 Synthesis of 1,3,5,7-tetraphenyladamantane
[0086] 5.0 g (23.2 mmol) of 1-bromoadamantane was placed in a condensing reflux device and CaCl 2 In the 150ml three-neck flask of the drying tube, add 50ml (0.56mol) benzene and 6.5g (47.5mmol) tert-butyl bromide in sequence, and slowly add 0.6g (4.52mmol) of anhydrous aluminum trichloride while stirring, and maintain a state of intense reflux After the reaction was stopped for 60 minutes, the mixture was poured into ice-water mixture, and an appropriate amount of ether was added, stirred, and filtered. The filter residue was dried at 75°C for 12 hours, and subjected to Soxhlet extraction with chloroform as a solvent. After one day of extraction, the residual insoluble solid was dried to obtain 8.6 g of 1,3,5,7-tetraphenyladamantane with a yield of 78.9%. Melting point m.p.>400°C.
[0087] 1.2 Synthesis of adamantane 1,3,5,7-tetra-p-benzenesulfonate
[0088] Suspend 1.63g (3.72mmol) of 1,3,5,7-tetraphenyladamantane in...
Embodiment 2
[0093] 2.1 Synthesis of 1,3,5,7-tetraphenyladamantane
[0094] 5.0 g (23.20 mmol) of 1-bromoadamantane was placed in a condensing reflux device and CaCl 2 In the 150ml three-necked flask of the drying tube, add 35ml (0.38mol) benzene and 9.5g (69.60mmol) tert-butyl bromide in sequence, slowly add anhydrous aluminum trichloride 0.77g (5.80mmol) under stirring, and maintain a state of intense reflux After the reaction was stopped for 40 minutes, the mixture was poured into ice-water mixture, and then an appropriate amount of ether was added, stirred, and filtered. The filter residue was dried at 75°C for 12 hours, and subjected to Soxhlet extraction with chloroform as a solvent. After one day of extraction, the residual insoluble solid was dried to obtain 8.5 g of 1,3,5,7-tetraphenyladamantane with a yield of 78.5%. Melting point m.p.>400°C.
[0095] 2.2 Synthesis of 1,3,5,7-tetra-p-benzenesulfonic acid adamantane
[0096] Suspend 1.63g (3.72mmol) of 1,3,5,7-tetraphenyladaman...
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