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Polyborosiloxane fire retardant for polycarbonate and preparing method thereof

A polysilaboroxane and polycarbonate technology, which is applied in the field of flame retardants and their preparation, can solve the problems of uneven dispersion and difficult compounding of compositions, and achieves high transparency, good mechanical properties, and no environment and human body. harmful effect

Inactive Publication Date: 2007-09-12
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention provides a synthetic route of polysiloxane flame retardant for polycarbonate, in which boron is chemically bonded with siloxane to form a copolymer, and B and Si are on the same molecular chain The synergistic flame retardant effect solves the problem of difficult compounding and uneven dispersion of the composition caused by the addition of boron compounds and siloxanes to polycarbonate in the form of physical mixing

Method used

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  • Polyborosiloxane fire retardant for polycarbonate and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 70g of water and a small amount of acetic acid in a 500ml three-necked flask. Pour the mixture of 0.2 mol of diphenyldimethoxysilane and 0.1 mol of methyltrimethoxysilane into the constant pressure dropping funnel, add drop by drop into the above flask, finish the drop within 10 minutes, adjust the pH value to 3.0, control the temperature at 80°C, and react for 2 hours to obtain the intermediate product silanol. Then the synthesized silanol was dissolved in 70g of xylene, allowed to stand to separate layers, and the water layer was removed. The silanol xylene solution was then reacted with 7g of boric acid at 100°C for 7 hours, and the solvent xylene was distilled off under reduced pressure. Finally, a white solid is obtained, which is polysiloxane flame retardant.

[0016] Its infrared spectrum is shown in Figure 1, and its specific structure is as follows: 3421cm -1 It is the stretching vibration peak of O-H; 3071cm -1 、1592cm -1 They are the stretching vibrat...

Embodiment 2

[0018] Add 80g of water and a small amount of acetic acid in a 500ml three-necked flask. Pour a total of 0.225mol of diphenyldimethoxysilane and 0.075mol of dimethyldimethoxysilane into the constant pressure dropping funnel, add dropwise to the above flask, and complete the dropwise addition within 10 minutes, adjust the pH value to 4.5, the temperature was controlled at 85°C, and the reaction was carried out for 1.5 hours to obtain the intermediate product silanol. Then the synthesized silanol was dissolved in 60g xylene, left to stand for stratification, and the water layer was removed, the silanol xylene solution continued to react with 6g boric acid for 7 hours, and the solvent xylene was distilled off under reduced pressure to finally obtain a white solid, i.e. Polysilaboroxane flame retardant.

Embodiment 3

[0020] Add 80g of water and a small amount of acetic acid in a 500ml three-necked flask. Pour the mixture of 0.18mol dimethyldimethoxysilane and 0.12mol diphenyldimethoxysilane into the constant pressure dropping funnel, add it dropwise to the above flask, complete the dropwise addition within 10min, and control the temperature at 80 °C, adjust the pH value to 2.8, and react for 2 hours to obtain the intermediate product silanol. Then dissolve the synthesized silanol in 70g of toluene, let the layers stand, remove the water layer, continue to react the silanol toluene solution with 7g of boric acid for 8.5 hours, distill off the solvent toluene under reduced pressure, and finally get a white solid, namely polysilicon boron Oxygen flame retardants.

[0021] The flame retardant and polycarbonate obtained in this example were added into a high-speed mixer at a weight ratio of 1:20 and mixed at a high speed for 15 minutes at 70° C., and then melted and extruded on a twin-screw ex...

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Abstract

The invention discloses a flame retardant of boron polysiloxane, including the following steps: (1)adding acetic acid or hydrochloric acid into water, adjusting pH from 1.8 to 5.0, then adding silane mixture which molar ratio with water is 1:3~20, stirring for hydrolysis at 60~90deg.C for 0.5~5 hours, generating silicon alcohol, adding solvent for extraction to separate the organic phase, (2)adding boric acid into the organic phase for reaction at 70~110deg.C for 2~16 hours, conducting vacuum distillation to remove solvent to obtain the flame retardant of boron polysiloxane, in which, the molar ratio of oxygen in silanol and boric in boric acid is 1:0.3~3.0. Adding 3% to 5% of this fire retardant into polycarbonate can raise the flame retardant level of UL94 to V0, and the flame-retardant polycarbonate has good mechanical properties, high transparency, brushing tolerance, non-corrosive, without harm to the environment.

Description

technical field [0001] The present invention relates to a flame retardant and its preparation method, in particular to a preparation method of a polysilaboroxane flame retardant containing a B-O-Si structural unit and a polycarbonate polycarbonate prepared according to the method. Siloboroxane flame retardant. Background technique [0002] Silicone flame retardant has high heat resistance and maintains a high degree of safety when burning without producing harmful gases. As an emerging flame retardant, it can not only endow the substrate with excellent flame retardancy, but also Improve other properties of the substrate, such as processing performance, mechanical properties, heat resistance, etc., eco-friendly, showing the characteristics of halogen-free, low smoke, low toxicity or non-toxic, etc., it is a kind of flame retardant with great development and application potential agent. [0003] 文献号为CN1724591、CN1556273、CN1631942、CN1724591、CN1280597、CN1675305、CN1737058、CN1426...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L69/00C08G77/56
Inventor 周文君
Owner HANGZHOU NORMAL UNIVERSITY
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