Preparation method of oligomerization phosphate polyalcohol

A technology of oligomeric phosphate and polyol, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problems of reducing the aging time of flame retardancy, poor safety, and the risk of skin burns, etc. problem, to achieve the effect of durable flame retardant performance and high safety

Active Publication Date: 2010-12-01
山东兄弟科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The adverse effect brought by this kind of alkyl monophosphate is that, because it does not contain terminal hydroxyl groups, it cannot be chemically combined with polyurethane materials, and it is easy to separate out, which affects the use environment and reduces the flame retardant aging; and the ethylene oxide used in this method , chemically unstable, under certain conditions, easy to decompose or polymerize to release a lot of heat, forming an explosion
It has a low boiling point, is a gas at room temperature, and has a wide range of explosion when mixed with air; phosphorus pentoxide is very easy to absorb moisture, emits a lot of heat, and has a risk of burns when it comes into contact with the skin, and has poor safety.

Method used

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  • Preparation method of oligomerization phosphate polyalcohol
  • Preparation method of oligomerization phosphate polyalcohol
  • Preparation method of oligomerization phosphate polyalcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1, 1 mol and 153.5 g of phosphorus oxychloride were dissolved in 200 mL of dichloromethane, and then added to a four-necked flask equipped with stirring, thermometer, reflux condenser and liquid dropping device. Start stirring, slowly add 1 mol of methanol with a mass of 32g, cool down in a water bath during the dropwise addition, and control the reaction temperature at 30±5°C, absorb the hydrogen chloride gas generated during the dropwise addition with water, after the dropwise addition, keep warm and reflux for 4h until No hydrogen chloride gas escaped, and a reaction solution containing monoalkyl dichlorophosphate was obtained. Then add 2 mol of acid-binding agent triethylamine with a mass of 202 g and 0.31 g of catalyst aluminum trichloride to the reaction solution, control the reaction temperature at 20±5°C, slowly add 1.1 mol of ethylene glycol with a mass of 68.3 g After the addition, reflux for 10 hours until no hydrogen chloride gas escapes to obtain a ...

Embodiment 2

[0038] Example 2, 1 mol of phosphorus oxychloride with a mass of 153.5 g was dissolved in 200 mL of dichloromethane, and then added to a four-necked flask equipped with stirring, thermometer, reflux condenser and liquid dropping device. Start stirring, slowly add 1 mol of absolute ethanol with a mass of 46g, cool down in a water bath during the dropwise addition, and control the reaction temperature at 30±5°C, absorb the hydrogen chloride gas generated during the dropwise addition with water, and keep warm and reflux for 4 hours after the dropwise addition , until no hydrogen chloride gas escapes to obtain a reaction solution containing monoalkyl dichlorophosphate. Add 2 mol and 202 g of acid-binding agent triethylamine and 0.23 g of catalyst aluminum trichloride to the reaction solution, control the reaction temperature at 20±5° C., slowly add 1.5 mol of ethylene glycol with a quality of 93.1 g, add After completion of the reflux reaction for 16 hours, until no hydrogen chlor...

Embodiment 3

[0039] Example 3, 1 mol and 153.5 g of phosphorus oxychloride were dissolved in 200 mL of dichloromethane, and then added to a four-necked flask equipped with stirring, thermometer, reflux condenser and liquid dropping device. Start stirring, slowly add 1 mol of n-propanol with a mass of 60.1g, cool down in a water bath during the dropwise addition, and control the reaction temperature at 30±5°C, absorb the hydrogen chloride gas generated during the dropwise addition with water, after the dropwise addition, keep warm and reflux 5h, until no hydrogen chloride gas escapes, the reaction solution containing monoalkyl dichlorophosphate is obtained. In the reaction solution, add 2mol, a quality of 202g acid-binding agent triethylamine and 0.28g catalyst aluminum trichloride, control the reaction temperature 20±5°C, slowly add 1.9mol of ethylene glycol with a mass of 117.9g, and then reflux for 20h until no hydrogen chloride gas escapes to obtain oligomeric phosphate polyol, triethyla...

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Abstract

The invention relates to a preparation method of oligomerization phosphate polyalcohol. Dissolvent and phosphorus oxychloride are put into an agitated reactor; monohydric alcohol is dropwise added; after the monohydric alcohol is dropwise added, heat preservation and backflow are carried out to obtain reaction liquid; acid binding agent and catalyst are added into reaction liquid; dihydric alcohol is slowly dropwise added; after the dihydric alcohol is dropwise added, backflow reaction is carried out to obtain mixture; the mixture is filtered, heated and distilled to obtain solvent; oligomerization phosphate polyalcohol is obtained, and oligomerization phosphate polyalcohol containing hydroxy terminal is synthesized; the oligomerization phosphate polyalcohol contains no halogen, protects environment, has no toxin and belongs to reaction type fire retardant. Because of the contained hydroxy terminal, the oligomerization phosphate polyalcohol can replace parts of polyether glycol or polyester polyol and reacts with isocyanate to produce polyurethane, i.e. the oligomerization phosphate polyalcohol can be combined into polyurethane material; and when being heated, the oligomerization phosphate polyalcohol does not move and is not separated out, and so that the material has enduring flame retardant property.

Description

technical field [0001] The invention relates to a method for preparing a phosphorus-based flame retardant, in particular to a method for preparing an oligophosphate polyol. Background technique [0002] Polyurethane foam is one of the most commonly used plastic varieties at present, and is widely used in industries such as furniture, automobiles, cushions, petrochemical pipelines and equipment manufacturing. However, polyurethane foam is extremely flammable in the air, and produces a large amount of toxic gas and smoke when burned. Therefore, great attention has been paid to the flame retardancy of polyurethane foam at home and abroad. [0003] The flame retardants currently used in polyurethane foam are mainly liquid halogen-containing phosphates, such as tris (2-chloroisopropyl) phosphate (TCPP), tris (2,2'-dichloroisopropyl) phosphate ( TDCPP) Tris(2-chloroethyl)phosphate (TCEP). However, these halogen-containing flame retardants are easy to precipitate from the polyur...

Claims

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Application Information

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IPC IPC(8): C08G79/04C07F9/11C08G18/64C08G18/32
Inventor 张玉梅贾宝泉
Owner 山东兄弟科技股份有限公司
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