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A kind of preparation method of water-soluble benzoxazine compound containing dopo

A technology for benzoxazine and compound, which is applied in the field of preparation of water-soluble benzoxazine compounds, can solve the problems of complicated synthesis steps, harm the environment, inconvenient for large-scale industrial production, etc., achieves good chemical stability and improves water solubility. properties, excellent flame retardancy

Inactive Publication Date: 2018-08-14
HUBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] The compound synthesized by the above synthetic method has cumbersome synthesis steps, the yield of the target product needs to be improved, and is not convenient for large-scale industrial production; at the same time, the target product synthesized does not have good water solubility, so it is still necessary to add organic solvents in the actual industrial use process As a diluent, it is harmful to the environment and threatens human health

Method used

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  • A kind of preparation method of water-soluble benzoxazine compound containing dopo
  • A kind of preparation method of water-soluble benzoxazine compound containing dopo
  • A kind of preparation method of water-soluble benzoxazine compound containing dopo

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Effect test

Embodiment 1

[0039] Take 24.32g (0.30mol formaldehyde) and 50ml dioxane in a reactor with a mass fraction of 37% formaldehyde solution, adjust the pH of the solution to 8 with triethylamine, add 9.01g (0.15mol) ethylenediamine dropwise, and Stir the reaction for 1 h, then add 12.21 g (0.10 mol) of p-hydroxybenzaldehyde, raise the temperature to 80 ° C, stir the reaction for 5 h, cool to room temperature, and distill off the dioxane under reduced pressure to obtain the crude product; dissolve the crude product in 50 ml of acetic acid ethyl ester, the resulting solution was washed 3 times with 1mol / L sodium hydroxide solution, and then washed with distilled water until the pH was neutral, and the resulting neutral solution was distilled off under reduced pressure to remove ethyl acetate under a vacuum of 0.09Mpa, and dried to obtain Refined benzoxazine product; get refined benzoxazine product in the reactor, add anhydrous dioxane and stir evenly, then add 21.6g (0.10mol) DOPO (9,10-dihydro-9-...

Embodiment 2

[0045] Take 16.62g (0.20mol formaldehyde) of 37% mass fraction of formaldehyde solution and 50ml ethanol in a reactor, adjust the pH of the solution to 9 with triethylamine, add dropwise 0.10mol (14.62g) triethylenetetramine, stir and react at low temperature for 2h, Then add 0.10mol (mass is 12.26g) p-Hydroxybenzaldehyde, heat up to 90°C, stir and react for 10h, cool to room temperature, and remove dioxane by distillation under reduced pressure to obtain the crude product, which is dissolved in 50ml ethyl acetate, The resulting solution was washed 3 times with 1mol / L sodium hydroxide solution, and then washed with distilled water until the pH was neutral. The resulting neutral solution was distilled off under reduced pressure to remove ethyl acetate and dried to obtain the refined benzo Oxazine product; take the refined benzoxazine product in the reactor, add anhydrous dioxane and stir evenly, then add 0.1mol (mass is 21.6g) DOPO (9,10-dihydro-9-oxa- 10-phosphaphenanthrene-10...

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Abstract

The invention discloses a preparation method of a water soluble benzoxazine resin containing DOPO, and belongs to the technical field of organic chemistry. The preparation method is used for solving problems that in application process of benzoxazine, environment pollution and health damage are caused by applications of toxic organic solvents such as benzene and methylbenzene as diluents. According to the preparation method, crude product benzoxazine is synthesized from a formaldehyde aqueous solution, a primary amine compound, and a phenol compound; benzoxazine is purified with ethyl acetate and a sodium hydroxide solution; and at last reaction with DOPO is carried out so as to obtain the water soluble benzoxazine resin containing DOPO. The preparation method comprises following steps: hydrophobicity of benzoxazine resin structure is improved, excellent water solubility is achieved, and using amount of toxic diluents is reduced; and in addition, DOPO groups are introduced into the obtained system, so that the water soluble benzoxazine resin containing DOPO possesses excellent flame resistance, is smoke-free, is nontoxic, is high in chemical stability, possesses permanent flame resistance, and is friendly to the environment.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and specifically relates to a preparation method of a DOPO-containing water-soluble benzoxazine compound. Background technique [0002] Benzoxazine resin is a new type of phenolic resin developed in recent years. It is generally prepared by condensation reaction of phenolic compounds, primary amine compounds and formaldehyde. Ring-opening polymerization can occur under heating conditions to form a network similar to phenolic resin. This type of resin not only maintains the high temperature resistance, flame retardancy, good electrical and mechanical properties of traditional phenolic resins, but also overcomes its shortcomings such as high brittleness, small molecule release during curing, strong acid catalyzed corrosion of equipment, and environmental pollution. In addition, the resin also has the characteristics of low water absorption, low dielectric constant and nearly zero volume shrinkage ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08K5/5313C08L63/00
CPCC07F9/657172C08K5/5313C08L2201/02C08L63/00
Inventor 邹其超李俊成张金枝柴仕淦王钊
Owner HUBEI UNIV
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