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Preparation method of low-acid-value phosphorus-containing reactive flame-retardant polyol

A reactive flame retardant and low acid value technology, applied in chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem of bubbles, affecting the mechanical properties of products, and not suitable for polyurethane materials and other problems, to achieve the effect of convenient post-processing, improved flame retardant performance, and simple experimental operation

Inactive Publication Date: 2020-07-07
SHANDONG INOV POLYURETHANE +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In addition, when the reactive phosphorus-based flame retardants in the prior art are used in polyurethane materials, due to their high acid value, bubbles will be generated during the reaction process, which will affect the mechanical properties of the product, and are not suitable for use in the preparation of polyurethane materials.

Method used

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  • Preparation method of low-acid-value phosphorus-containing reactive flame-retardant polyol
  • Preparation method of low-acid-value phosphorus-containing reactive flame-retardant polyol

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Embodiment 1

[0028] The preparation method of the described low-acid value phosphorus-containing reactive flame-retardant polyol consists of the following steps:

[0029] (1) Add 30g of 2-carboxyethylphenylphosphinic acid and 43.5g of ethylene glycol into a three-necked flask, then add 0.073g of antimony trioxide and 100μL of tetrabutyl titanate, raise the temperature to 100°C, and turn on the mechanical Stir to dissolve 2-carboxyethylphenylphosphinic acid completely. Under the protection of argon, perform esterification reaction at 100°C for 3h, then continue to heat up, and react at 160°C, 180°C and 200°C for 1.5h and 1h respectively and 1h, lower the temperature to 185°C, react under reduced pressure for 2h, and finally vacuum-dry the obtained product at 80°C to obtain an esterified intermediate with an acid value of 50mgKOH / g.

[0030] (2) Add 17.5931g of the esterification intermediate into the Erlenmeyer flask, and dissolve it completely with 30mL of acetonitrile, then add 6.49g of a...

Embodiment 2

[0032] The preparation method of the described low-acid value phosphorus-containing reactive flame-retardant polyol consists of the following steps:

[0033] (1) Add 30g of 2-carboxyethylphenylphosphinic acid and 26.1g of ethylene glycol into a three-necked flask, then add 0.056g of antimony trioxide and 100μL of tetrabutyl titanate, raise the temperature to 100°C, and turn on the mechanical Stir to completely dissolve 2-carboxyethylphenylphosphinic acid, react at 100°C for 3h under the protection of argon, then continue to heat up, and react at 160°C, 180°C, and 200°C for 1.5h, 1h, and 1h respectively , lower the temperature to 185°C, react under reduced pressure for 2h, and finally vacuum-dry the obtained product at 80°C to obtain an esterified intermediate with an acid value of 70mgKOH / g.

[0034] (2) Add 17.5931g of the esterification intermediate into the Erlenmeyer flask, and dissolve it completely with 30mL of acetonitrile, then add 6.49g of anhydrous potassium carbonat...

Embodiment 3

[0036] The preparation method of the described low-acid value phosphorus-containing reactive flame-retardant polyol consists of the following steps:

[0037] (1) The preparation method of the esterification intermediate is as in Example 2.

[0038] (2) 17.5931g of esterification intermediate was added to the conical flask, and it was completely dissolved with 30mL of N,N-dimethylformamide, then 6.49g of anhydrous potassium carbonate was added, and finally 3mL of methyl iodide was added, and Under the airtight condition of 20° C. protected from light, the reaction was carried out with magnetic stirring for 10 hours. After the reaction is complete, remove potassium carbonate by suction filtration, add copper powder to the filtrate, and distill off excess iodomethane and N,N-dimethylformamide under reduced pressure. After vacuum drying, the acid value of the product is 2.10 mgKOH / g, and the hydroxyl value is 174 mgKOH / g.

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Abstract

The invention belongs to the technical field of polymer chemical synthesis, and particularly relates to a preparation method of low-acid-value phosphorus-containing reactive flame-retardant polyol. The method comprises the following steps: (1) carrying out an esterification reaction on 2-carboxyethyl phenyl phosphinic acid and ethylene glycol to obtain an esterification intermediate, and concentrating and drying an esterification intermediate; and (2) reacting the dried esterification intermediate with a nucleophilic reagent in an organic solvent containing a basic catalyst, carrying out suction filtration, distilling in the presence of a reducing agent, filtering, and drying to obtain the low-acid-value phosphorus-containing reactive flame-retardant polyol, wherein the acid value of the low-acid-value phosphorus-containing reactive flame-retardant polyol ranges from 1.1 mgKOH / g to 2.1 mgKOH / g. The polyol prepared by the method can be used as a reactive flame retardant for polyurethanefoam, elastomers and other plastic products, enhances the flame retardancy of the high polymer material, and has the advantages of accessible materials, simple experimental operation and convenient post-treatment.

Description

technical field [0001] The invention belongs to the technical field of macromolecule chemical synthesis, and in particular relates to a method for preparing a low-acid value phosphorus-containing reactive flame-retardant polyol. Background technique [0002] Polyurethane, the full name of polyurethane, is composed of isocyanate and compounds containing active hydrogen (such as -OH, -NH 2 ) produced by nucleophilic addition reaction, is a general term for macromolecular compounds containing repeated carbamate groups (-NHCOO-) on the main chain. The preparation of polyurethane materials consumes less energy, and has various excellent properties such as light weight, easy processing, shock absorption, heat insulation, sound absorption, wear resistance, etc., and is widely used in automobile manufacturing, transportation, footwear, petrochemical, aviation, Medical, agricultural and many other fields. It is the only organic synthetic material among all kinds of polymer material...

Claims

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Application Information

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IPC IPC(8): C07F9/32C08G18/66C08G18/42C08G18/32C08G18/38
CPCC07F9/3229C07F9/3264C08G18/3206C08G18/388C08G18/4238C08G18/664
Inventor 徐军李爱香蔡昌辰陈淑海陈海良贾雪芹杨书刚
Owner SHANDONG INOV POLYURETHANE
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