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Organic silicon phosphate and preparation method thereof

A technology of organosilicon phosphate and alkyl, which is applied in the field of organosilicon phosphate and its preparation, and can solve the problems of low molecular weight, high composition, pollution, and easy volatility.

Inactive Publication Date: 2011-08-10
GRAND TEK ADVANCE MATERIAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Early phosphorus-based flame retardants were mainly monomeric, such as triphenyl phosphate (TPP) or tricresyl phosphate (tricresyl phosphate, TCP). , began to develop condensed phosphoric ester

Method used

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  • Organic silicon phosphate and preparation method thereof
  • Organic silicon phosphate and preparation method thereof
  • Organic silicon phosphate and preparation method thereof

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preparation example Construction

[0032] The present invention also provides a method for preparing organosilicon phosphate, which includes the following steps (a) to (c). First carry out step (a), the phenol (phenol) of formula (III) and phosphorus oxychloride (phosphoryl chloride, POCl 3 ) reacts with the ratio of molar ratio 2: (1-1.2), and its reaction formula is as follows:

[0033]

[0034] (III) Intermediate 1 Intermediate 2

[0035] where R 1 and R 2 for the same or different C 1 ~C 5 Alkyl (alkyl); R 3 for hydrogen or C 1 ~C5 Alkyl (alkyl).

[0036] After the reaction, intermediate product 1 and intermediate product 2 can be obtained, wherein intermediate product 1 is the main product, accounting for 80%-90% of the product. Hydrogen chloride (HCl) gas generated during the reaction process can be recycled through water under normal pressure or reduced pressure.

[0037] The above-mentioned phenols include dimethylphenol (dimethylphenol), diethylphenol (diethylphenol), 2-methyl-3-ethylphenol...

Embodiment 1

[0060] In a 1000mL four-necked flask equipped with a mechanical stirrer, a thermometer, a condensation tube connected to a hydrogen chloride gas absorption device, and a dropping funnel, add 244g (2.00mol) of 2,6-dimethylphenol (2,6-dimethylphenol), 7.03g (0.07mol) anhydrous magnesium chloride (anhydrous magnesiumchloride), 160g (1.04mol) phosphorus oxychloride (phosphoryl chloride, POCl 3 ) and 10g of xylene (xylene) were mixed and heated. Gradually raise the temperature to 110°C to generate a large amount of hydrogen chloride gas, react at 110°C for 2 hours, then raise the temperature to 130°C for 2 hours, then raise the temperature to 155°C for 6 hours, and then reduce the pressure to 150mmHg for 4 hours.

[0061] After the reaction mixture was cooled to 100°C, 61g (0.55mol) of resorcinol (m-bisphenol), 1.5g (0.01mol) of anhydrous aluminum chloride (anhydrous aluminum chloride) and 10g of xylene (xylene) were added, and the temperature was raised After reacting at 120°C fo...

Embodiment 2

[0064] In a 1000mL four-neck flask equipped with a mechanical stirrer, a thermometer, a condenser tube connected to a hydrogen chloride gas absorption device, and a dropping funnel, add 244g (2.00mol) of 2,6-dimethylphenol, 7.05g (0.07mol) of Magnesium chloride hydrate, 160g (1.04mol) phosphorus oxychloride (phosphoryl chloride, POCl 3 ) and 10g of xylene (xylene) were mixed and heated. Gradually raise the temperature to 110°C to generate a large amount of hydrogen chloride gas, react at 110°C for 2 hours, then raise the temperature to 130°C for 2 hours, then raise the temperature to 155°C for 6 hours, and then reduce the pressure to 150mmHg for 4 hours.

[0065] After the reaction mixture was cooled to 100°C, 110g (1.00mol) of resorcinol (m-bisphenol), 3.3g (0.02mol) of anhydrous aluminum chloride and 10g of xylene (xylene) were added, and the temperature was raised to 120°C for reaction 12 After one hour, add 70g (0.33mol) of phenyltrichlorosilane (phenyltrichlorosilane) in...

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Abstract

The invention provides organic silicon phosphate and a preparation method thereof. The organic silicon phosphate has a structure shown as the following formula, wherein R1 and R2 are same or different C1-C5 alkyl groups; R3 and R4 are same or different hydrogen or C1-C5 alkyl groups; R5 is an aryl group or C1-C5 alkyl groups; Y is a connecting key which comprises -CH2-, -C(CH3)2-, -S-, -SO2-, -O-, -CO- or -N=N-; m is an integer from 0 to 4; n is 0 or 1; and k is an integer from 0 to 9.

Description

technical field [0001] The invention relates to phosphate ester compounds, in particular to an organosilicon phosphate ester and a preparation method thereof. Background technique [0002] Flame retardants (flame retardant) can be divided into inorganic type and organic type. Among them, the inorganic type usually needs a higher addition amount to achieve the flame retardant effect. However, when the addition amount is too high, it will cause The physical properties of the resin are reduced, and the organic type is divided into two types: halogen-based and phosphorus-based. Among them, the halogen-based flame retardant will produce hydrogen halide gas and a large amount of smoke when burned, which will cause harm to the human body. Therefore, the current organic type flame retardant Phosphorus-based flame retardants are the main axis of development. [0003] The flame retardant effect of phosphorus-based flame retardants depends on the phosphorus content in the phosphide. F...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F19/00C09K21/12
Inventor 汤上慰林学佐陈冠青锺迪克
Owner GRAND TEK ADVANCE MATERIAL SCI
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