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Polypropylene-based dimethyl phosphate flame retardant and preparation method thereof

A technology of polypropylene-based dimethyl phosphate and propylene-based dimethyl phosphate, used in textiles, papermaking, fiber processing, etc., can solve the problems of harsh reaction conditions and complicated processes, and achieve high flame retardant efficiency and durability. Flame retardant effect, good flame retardant effect

Inactive Publication Date: 2012-07-11
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the flame retardant effect of the flame retardant is better, the synthesis of the flame retardant needs to be carried out in a reactor, and nitrogen gas needs to be fed continuously to prevent oxidation, and anhydrous AlCl 3 As a catalyst, the process is complicated and the reaction conditions are relatively harsh

Method used

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  • Polypropylene-based dimethyl phosphate flame retardant and preparation method thereof
  • Polypropylene-based dimethyl phosphate flame retardant and preparation method thereof
  • Polypropylene-based dimethyl phosphate flame retardant and preparation method thereof

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specific Embodiment approach 1

[0017] Implement the preparation method of a kind of polypropylene base dimethyl phosphate flame retardant of the present invention, this method is to react propenyl alcohol and phosphorus oxychloride, diethyl ether or ethyl acetate are solvent, take triethylamine or pyridine as acid-binding agent , at 0°C, stirred and reacted for 6 hours, then added dropwise a mixture of methanol and triethylamine, reacted for another 3 hours, filtered and evaporated to obtain propenyl dimethyl phosphate monomer; then propenyl dimethyl Phosphate monomer and potassium persulfate react in aqueous solution or emulsion, and the reaction mass ratio is propylene dimethyl phosphate monomer: potassium persulfate: Span-60: deionized water = 40~45: 2~10: 0~10: 40~45, adjust the pH value to 5~7, microwave radiation, power: 220~700W, control temperature: 65~95℃, reaction time: 3~10 minutes, get the filtrate by suction filtration, separate Remove the supernatant, and then distill to obtain polypropylene-b...

specific Embodiment approach 2

[0018] Implement the preparation method of a kind of polypropylene base dimethyl phosphate flame retardant of the present invention, its concrete method is to carry out according to the following steps:

[0019] (1) Add diethyl ether and phosphorus oxychloride into the reaction kettle, the molar ratio is 4:1, diethyl ether is used as solvent;

[0020] (2) Add a mixture of propenol and triethylamine with a molar ratio of 1:1 to the reaction kettle dropwise, stir and react for 6 hours, control the temperature at 0°C, and obtain the compound (1) as shown in the reaction formula (1) ):

[0021]

[0022] Reaction formula (1) Compound (1)

[0023] (3) React the mixture of compound (1) with methanol and triethylamine through reaction formula (2) for 3-6 hours; let stand for 12 hours, filter with suction to obtain the filtrate, and evaporate at 50-70°C to obtain compound (2) - propenyl dimethyl phosphate;

[0024]

[0025] Reaction formula (2) Compound (...

Embodiment 1

[0034] (1) Add 4 mol of ether and 1 mol of phosphorus oxychloride into a three-necked flask, and use ether as a solvent;

[0035] (2) Add a mixture of 1 mol of allyl alcohol and 1 mol of triethylamine dropwise into the reaction kettle, stir and react for 6 hours, and control the temperature at 0°C;

[0036] (3) After the reaction is completed, add dropwise a mixture of 2.2 mol methanol and 2 mol triethylamine, react for 3 hours, and let stand for 12 hours;

[0037] (4) The filtrate was obtained by suction filtration, and was evaporated by a rotary evaporator to obtain propenyl dimethyl phosphate, and the rotary evaporation temperature was 50°C;

[0038] (5) Put 45 parts by mass of propenyl dimethyl phosphate, 45 parts of water, 6 parts of Span-60, and 4 parts of persulfate into the beaker. The reaction temperature is controlled at 80°C, and the pH value is adjusted with formic acid 7. Heating by microwave, set the power to 400W, and the reaction time is 6 minutes;

[0039] (...

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Abstract

The invention discloses a polypropylene-based dimethyl phosphate flame retardant and a preparation method thereof. The preparation method comprises the following steps of: reacting allyl alcohol with phosphorus oxychloride, performing stirring reaction at the temperature of 0 DEG C by using triethylamine or pyridine as an acid capturer, dripping methanol to react with the triethylamine mixed solution, filtering, evaporating to obtain an allyl dimethyl phosphate monomer, reacting with potassium persulfate, regulating the pH value, performing graft polymerization reaction by microwave irradiation, filtering, separating the supernate, distilling, and thus obtaining the polypropylene-based dimethyl phosphate flame retardant. The flame retardant does not contain halogen, and is good in thermal stability and easy and convenient to synthesize; the phosphorus content of the flame retardant reaches 18.7 percent; and the flame retardant has a good lasting flame-retardant effect, and is suitable for flame-retardant finishing of fibers of hemp, hair, silk and the like and plastics.

Description

technical field [0001] The invention relates to a phosphorus-based flame retardant and a preparation method thereof, and further relates to a polypropylene-based dimethyl phosphate flame retardant and a preparation method thereof. Background technique [0002] The existing halogen flame retardants have good flame retardant effect and less addition amount, but when they burn, they release a large amount of poisonous gas and smoke, pollute the environment, and affect people's health. Therefore, halogen-free flame retardants are the hotspot of current research. Existing phosphoric acid ester flame retardants can replace halogenated flame retardants, so that the flame retardant can be completely halogen-free. Phosphate ester flame retardants containing vinyl functional groups are single-molecule flame retardants, which are used to flame-retardant textiles by chemical initiation, electron irradiation, and plasma initiation. However, the unimolecular flame retardant is prone to ...

Claims

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Application Information

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IPC IPC(8): D06M15/356C08F130/02C08F2/46
Inventor 魏丽乔王灿灿李全红晏泓高向华王慧芳
Owner TAIYUAN UNIV OF TECH
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