A kind of preparation method and application of phosphorus-containing polyether ester

A polyether ester and reactor technology, which is applied in the field of preparation of phosphorus-containing polyether ester, can solve the problems of not being able to meet the requirements at the same time, not being environmentally friendly, etc., and achieve the effects of excellent anti-dripping, low cost, and excellent corrosion resistance

Active Publication Date: 2016-08-24
BEIJING LIGONG FLAME RETARDATION TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, my country's fire retardant coatings have the following problems: (1) coatings with higher performance are almost all solvent-based, such as ultra-thin exterior steel structure fire retardant coatings, which are not environmentally friendly; (2) fire resistance, chemical resistance (corrosion resistance) ), physical and mechanical properties (mechanical properties), environmental protection and reasonable price, these four elements cannot meet the requirements at the same time

Method used

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  • A kind of preparation method and application of phosphorus-containing polyether ester
  • A kind of preparation method and application of phosphorus-containing polyether ester

Examples

Experimental program
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Effect test

Embodiment 1

[0048] Add 50kg of toluene to the reaction kettle, raise the temperature to 60°C while stirring, then add 103.2kg of D-33 into the reaction kettle while maintaining stirring and heating, stop heating until D-33 is completely dissolved, and cool down with cooling water To 25°C, control the temperature at 15-25°C and add 15.3 kg of phosphorus oxychloride dropwise to the reactor at a rate of about 5 kg / h, and the drop will be completed in about 3 hours. During this process, hydrogen chloride gas will escape from the reactor. , so that the escaped gas is passed into the lye tank, and the acid gas is absorbed with a sodium hydroxide solution with a mass concentration of 50% in the tank. The gas not absorbed by the lye tank is inert solvent vapor, which will be recovered by the condenser connected after the lye tank. After the dropwise addition of phosphorus oxychloride is completed, the temperature of the material in the reactor is raised to 110°C within 3 hours, so that the materi...

Embodiment 2

[0058] Add 50kg of toluene to the reaction kettle, raise the temperature to 70°C while stirring, then add 86kg of D-33 and 3.7kg of butanol into the reaction kettle successively while maintaining stirring and heating until D-33 is completely melted and stop Heating, passing cooling water to cool down to 15°C, and slowly adding 15.3kg of phosphorus oxychloride to the reactor at 15-25°C under control of the temperature. The lye tank uses a 10% sodium hydroxide solution to absorb acid gas in the tank. The gas not absorbed by the lye tank is inert solvent vapor, which will be recovered by the condenser connected after the lye tank. After the phosphorus oxychloride has been added dropwise, the temperature of the material in the reactor is raised to 130°C within 4 hours, so that the material in the kettle reaches a slight boiling state, and is kept in this state for 4 hours, and then the condenser, lye Vacuumize the tank and reactor, extract residual hydrogen chloride and all tolue...

Embodiment 3

[0067] Add 50kg of toluene to the reaction kettle, raise the temperature to 80°C while stirring, then add 86kg of D-33 and 2.3kg of absolute ethanol into the reaction kettle successively while maintaining stirring and heating until D-33 is completely dissolved Then stop heating, pass cooling water to cool down to 20°C, control the temperature at 15-25°C and slowly add 15.3kg of phosphorus oxychloride into the reactor dropwise, and drop it in about 3 hours. During this process, hydrogen chloride gas will be generated in the reactor Escape, make the escaped gas pass into the lye tank, and absorb the acid gas with a sodium hydroxide solution with a mass concentration of 30%. The gas not absorbed by the lye tank is inert solvent vapor, which will be recovered by the condenser connected after the lye tank. After the phosphorus oxychloride has been added dropwise, the temperature of the material in the reactor is raised to 120°C within 3.5 hours, so that the material in the kettle r...

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Abstract

The invention discloses a phosphorus-containing olyether ester preparation method, which belongs to the technical field of fireproof flame retardation material. According to the invention, D-33, monohydric alcohol and phosphorous oxychloride are employed for reacting in an inertia solvent, a by-product hydrogen chloride and a solvent are extracted by a vacuum-pumping and alkali absorption method and absorbing; when an acid-base value of products in a reactor reaches neutrality, the phosphorus-containing polyether ester is prepared; he phosphorus-containing polyether ester can be used as a hydroxy component of a polyurethane paint, can be cooperated with an isocyanate component, and can be a base material for preparing an aqueous (or solvent type) room-temperature solidification polyurethane flame retardation. The base material can be taken as a transparent flame retardation fireproof varnish in woodenware furniture field, and can be deeply processed to a paint for a steel-structure fireproof paint. The method has the advantages of wide raw material source, low cost, simple production technology, and flexible construction method, and has popularization application value.

Description

technical field [0001] The invention relates to a preparation method and application of phosphorus-containing polyether ester, belonging to the field of fire-resistant and flame-retardant materials. Background technique [0002] Fire-resistant and flame-retardant materials are a new type of functional material that can prevent or delay the occurrence, development, and expansion of fires. With the enhancement of public environmental protection awareness and national environmental protection regulations, two new issues have been proposed for fire-resistant and flame-retardant coatings. One is construction Environmental protection, that is, the content of volatile organic compounds in the coating should be as low as possible, especially without benzene, aldehydes, pungent odor, and strong toxicity solvents; on the other hand, the smoke produced by fire It must not contain toxic and harmful gases, because the cause of death in many fire incidents is smoke, not flame, so the coat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/09C08G18/32C09D175/04C09D5/18
Inventor 杨荣杰李文铎李定华王珂
Owner BEIJING LIGONG FLAME RETARDATION TECH
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