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A kind of flame retardant and preparation method thereof, polycarbonate composite material and preparation method thereof

A polycarbonate and composite material technology, which is applied in the preparation of sulfonic acid amides, organic chemistry, etc., can solve the problems of poor water resistance of sulfonate flame retardants, great influence on the performance of PC materials, and high cost of silicon-based flame retardants. The effect of promoting PC cross-linking, small influence on mechanical properties, and high content of flame retardant elements

Inactive Publication Date: 2020-08-07
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In view of this, the present invention provides a flame retardant and a preparation method thereof, a polycarbonate composite material and a preparation method thereof, which are used to solve the problems of nitrogen-based flame retardants and phosphorus-based flame retardants in existing PC flame retardants. The large amount of addition in PC has a great impact on the performance of the PC material itself; the cost of silicon-based flame retardants is high, and generally needs to be used in combination; the water resistance of sulfonate flame retardants is poor, and the problem of agglomeration is prone to occur during processing

Method used

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  • A kind of flame retardant and preparation method thereof, polycarbonate composite material and preparation method thereof
  • A kind of flame retardant and preparation method thereof, polycarbonate composite material and preparation method thereof
  • A kind of flame retardant and preparation method thereof, polycarbonate composite material and preparation method thereof

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preparation example Construction

[0047] The present invention also provides a preparation method of flame retardant, comprising the following steps:

[0048] The 1,3,5,7-p-tetraphenylsulfonyl chloride adamantane is first reacted with ammonia water to obtain 1,3,5,7-p-tetraphenylsulfonamide adamantane;

[0049] Wherein, the structural formula of 1,3,5,7-tetraphenylsulfonamide adamantane is as shown in formula (I);

[0050]

[0051] In the present invention, the first reaction of 1,3,5,7-p-tetraphenylsulfonylchloroadamantane and ammonia specifically includes:

[0052] After dissolving 1,3,5,7-p-tetraphenylsulfonyl chloride adamantane in the first organic solvent, ammonia water is added, and the first reaction is carried out under stirring.

[0053] The mass ratio of 1,3,5,7-p-tetraphenylsulfonylchloroadamantane to ammonia water is 1:10-100, preferably 1:10-70, more preferably 1:10-50.

[0054] The mass ratio of 1,3,5,7-p-tetraphenylsulfonylchloroadamantane, the first organic solvent and ammonia water is 1:...

Embodiment 1

[0093] 1) Place 20 g (0.093 mol) of dry 1-bromoadamantane in a condensing reflux device and CaCl 2 In the 500mL three-necked flask of the drying tube, add 100mL (1.12mol) benzene and 26g (95mmol) tert-butyl bromide in sequence, slowly add 2.4g (9.04mmol) anhydrous aluminum trichloride under slow stirring, and heat up to 70°C , maintain a state of intense reflux, carry out Friedel-Crafts alkylation reaction, stop the reaction after 30 minutes of reaction, pour the mixture into an appropriate amount of ice-water mixture, then add an appropriate amount of ether, stir thoroughly, filter, and dry the obtained filter residue at 75°C for 12 hours , and then use chloroform as a solvent for Soxhlet extraction, and after one day of extraction, place the remaining solid at room temperature to dry to obtain a white powder, that is, 1,3,5,7-p-tetraphenyladamantane.

[0094] 2) Add 50mL (0.39mol) of dichloromethane to the 2 In a 150mL three-necked flask with a drying tube, 3.26g (7.41mmol)...

Embodiment 2

[0097] 1) Place 20 g (0.093 mol) of dry 1-bromoadamantane in a condensing reflux device and CaCl 2 In the 500mL three-necked flask of the drying tube, add 150mL (1.12mol) benzene and 26g (95mmol) tert-butyl bromide in sequence, slowly add 2.4g (9.04mmol) anhydrous aluminum trichloride under slow stirring, and heat up to 90°C , maintain a state of intense reflux, carry out Friedel-Crafts alkylation reaction, stop the reaction after 30 minutes of reaction, pour the mixture into an appropriate amount of ice-water mixture, then add an appropriate amount of ether, stir thoroughly, filter, and dry the obtained filter residue at 75°C for 12 hours , and then use chloroform as a solvent for Soxhlet extraction, and after one day of extraction, place the remaining solid at room temperature to dry to obtain a white powder, that is, 1,3,5,7-p-tetraphenyladamantane.

[0098] 2) Same as step 2) of Example 1.

[0099] 3) Same as step 3) of embodiment 1.

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Abstract

The invention belongs to the technical field of high polymer materials and particularly relates to a flame retardant, a preparation method thereof, a polycarbonate composite material and a preparationmethod thereof. The flame retardant is 1,3,5,7-p-tetraphenyl sulfonamide adamantane. The flame retardant uses the adamantane as a core and provides good lipid solubility and stability for flame retardant molecules. Four bridgehead displacements of the flame retardant can increase the content of flame retarding elements, SO2 produced through sulfur element decomposition can promote PC crosslinking, non-flammable gas produced through nitrogen element decomposition dilutes and isolates oxygen in a gas phase when a condensed phase plays an effect, and the working mechanism of the flame retardantmakes the flame retarding efficiency high while the condensed phase and the gas phase are formed. In addition, the polarity of amidogens of the flame retardant can improve the compatibility between the flame retardant molecules and PC. Furthermore, the flame retardant does not need compounding, the adding amount is small when the flame retardant is added to the PC to improve the flame retarding performance, and the influence on the mechanical properties of the PC material is small. Compared with a sulfonate flame retardant, the hygroscopicity of the flame retardant is low.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a flame retardant and a preparation method thereof, a polycarbonate composite material and a preparation method thereof. Background technique [0002] Relying on their high strength, high temperature resistance, corrosion resistance and other advantages, as well as the advantages of convenient material processing, engineering plastics can replace metal materials in some applications, and have been widely used in aerospace, electrical and electronics, vehicle engineering, office equipment, and energy-saving buildings. In industries such as plastics and other industries, there has been a material change trend of replacing steel with plastic and wood with plastic. Among them, polycarbonate (Polycarbonate, PC) has become one of the fastest-growing engineering plastics in the world due to its excellent performance. However, in terms of flame retardancy, although...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/435C08L69/00C07C303/38C07C311/16
CPCC07C311/16C07C2603/74C08K5/435C08L2201/02C08L69/00
Inventor 郭建维杨航锋崔亦华
Owner GUANGDONG UNIV OF TECH
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