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A kind of preparation method of green high-purity thermoplastic phenolic resin

A phenolic resin and thermoplastic technology, applied in the field of green high-purity thermoplastic phenolic resin preparation, can solve the problems of high-concentration phenol-containing waste water, excessive free phenol, difficult to obtain thermoplastic phenolic resin, etc., achieving less free phenol content and reducing free phenol. , the effect of high yield

Inactive Publication Date: 2016-11-16
HUAINAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to solve the problem of high-concentration phenol-containing wastewater caused by excessive phenol in the synthesis stage of thermoplastic phenolic resin in the master's degree thesis of Northwestern Polytechnical University "Research on New Green Production Process of Thermoplastic Phenolic Resin", a new selective catalyst and new process were used to synthesize Produce thermoplastic phenolic resin, so that the molar ratio of phenol and formaldehyde reaches 1:1 during synthesis. This method theoretically solves the problem of excess free phenol, but it is not easy to obtain thermoplastic phenolic resins with different molecular weights and different molecular weight distributions.

Method used

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  • A kind of preparation method of green high-purity thermoplastic phenolic resin
  • A kind of preparation method of green high-purity thermoplastic phenolic resin
  • A kind of preparation method of green high-purity thermoplastic phenolic resin

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Embodiment 1

[0053] A kind of preparation method of green high-purity thermoplastic phenolic resin of the present embodiment, its steps are as follows:

[0054] Take 0.5 moles of phenol as an example to prepare other raw materials used for high-purity thermoplastic phenolic resin and the preparation method comprises the following steps:

[0055] (1), ingredients

[0056] Take 47g of phenol, 9.76g of paraformaldehyde, 15.75g of water, and 0.12g of acetic acid, mix them in a reaction kettle, and stir evenly, that is, the molar ratio of phenol to aldehyde compounds, water, and organic acids is 1:0.65:1.75:0.004; Paraformaldehyde is a low molecular weight polyoxymethylene with a degree of polymerization of 8-100.

[0057] (2), chemical reaction

[0058] The reactant was heated to 90° C. under stirring, and reacted at constant temperature for 4 hours.

[0059] (3), dehydration and granulation of phenolic resin

[0060] Step (2) After the reaction is completed, the reaction product is dehydr...

Embodiment 2

[0074] Take 0.5 moles of phenol as an example to prepare other raw materials used for high-purity thermoplastic phenolic resin and the preparation method comprises the following steps:

[0075] In the batching process step (1) in Example 1, take 47g of phenol, 20.29g of formaldehyde with a mass concentration of 37%, 0g of water, and 0.18g of hydrochloric acid and mix them in the reactor, stir evenly, that is, phenol and aldehyde compounds , water, and inorganic acid in a molar ratio of 1:0.5:0:0.01. Other processing steps are identical with embodiment 1, the productive rate of the thermoplastic phenolic resin recorded, softening point, free phenol, molecular weight Mw and the waste water volatile phenol in the production process are: productive rate: 96.8%, softening point: 63 ℃, free Phenol: 0.1%, molecular weight Mw: 908, waste water volatile phenol: 0.5mg / L.

Embodiment 3

[0077] Take m-cresol 0.5 mole as an example to prepare other raw materials used for high-purity thermoplastic phenolic resin and the preparation method comprises the following steps:

[0078] In the batching process step (1) among the embodiment 1, get m-cresol 54g, paraformaldehyde 14.26g, water 2.7g, organic acid be any one in oxalic acid or maleic acid or citric acid to be catalyst, phenol and Aldehyde compounds, water, and organic acids are mixed in a molar ratio of 1:0.95:0.3:0.050, respectively placed in a reactor and stirred evenly, and reacted separately. The other processing steps were the same as in Example 1 to obtain 3 kinds of thermoplastic phenolic resins. The yield, softening point, free phenol, molecular weight Mw and waste water volatile phenol in the production process of the thermoplastic phenolic resin prepared with oxalic acid as a catalyst are: yield: 109.7%, softening point: 99 ° C, free phenol: 0.1%, Molecular weight Mw: 3108, waste water volatile phen...

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Abstract

The invention discloses a preparation method of green high-purity thermoplastic phenolic resin, belonging to the technical field of phenolic resin materials. The preparation method comprises the following steps: (1) weighing phenol, aldehyde and acid catalysts; (2) heating reactants to 60-120 DEG C in a stirring state, and reacting for 1-6 hours at normal pressure and constant temperature; (3) performing normal pressure drying at 100-160 DEG C, and then pelletizing; and (4) conveying a phenolic resin particle material into a super-critical carbon dioxide extraction tower, and adding alcohol or ketone extracting agents which account for 0-20% of the mass of the resin to perform dephenolization treatment for 5-30 minutes to obtain a required product under the conditions that the extraction temperature is 31-50 DEG C, the extraction pressure is 8-20Mpa and the separation pressure is 5-7Mpa. By adopting the preparation method disclosed by the invention, free phenol can be effectively separated from the thermoplastic phenolic resin, the emission of phenolic wastewater can be reduced, the yield of the product can be improved, and the continuous production without pollution can be achieved, so that the preparation method is suitable for the production of various thermoplastic phenolic resins.

Description

technical field [0001] The invention belongs to the technical field of phenolic resin materials, and in particular relates to a preparation method of a green high-purity thermoplastic phenolic resin. Background technique [0002] Phenolic resin has heat resistance, insulation, high temperature resistance, corrosion resistance and good mechanical processing properties. It can be used in the manufacture of molding compounds, laminated plastics, foam plastics, etc., and can also be used as paint raw materials, adhesives, anti-corrosion cement and other Phenolic resin-based ion exchange resins can also be used as adhesives for grinding wheels, brake pads, and coated sand. In the defense industry, phenolic resins have also been widely used. [0003] At present, the method of producing thermoplastic phenolic resin internationally or domestically is to use various production processes under the catalysis of organic acid and inorganic acid to make phenol and aldehyde react. In orde...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/10C08G8/08
CPCY02P20/54
Inventor 梁铣魏亦军王凤武张晓艳
Owner HUAINAN NORMAL UNIV
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