Method for preparing high-ortho thermoplastic phenolic resin

A phenolic resin and thermoplastic technology, which is applied in the field of preparation of high-ortho-position thermoplastic phenolic resins, can solve the problems of unfavorable industrial production of thermoplastic high-ortho-position phenolic resins, increase production costs, and high requirements for equipment conditions, and achieve high-temperature reactions and easy gelation Curing, reducing the requirements for production equipment, and stabilizing the reaction process

Active Publication Date: 2010-11-10
SHANDONG SHENGQUAN NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The normal pressure reaction has the disadvantages of long time consumption, easy gel solidification and difficult control in the later stage; there are reports in the literature that high-ortho thermoplastic phenolic resins are produced using high-pressure reactors, and the use of high-pressure reactors can enable the reaction to be carried out at a higher temperature. The high temperature of 180°C is conducive to the breakage of ether bonds and prevents the resin gel from curing. However, high pressure conditions require high equipment conditions and increase production costs, which is not conducive to the industrial production of thermoplastic high-ortho phenolic resins.

Method used

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  • Method for preparing high-ortho thermoplastic phenolic resin
  • Method for preparing high-ortho thermoplastic phenolic resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Put phenol and formaldehyde into the reactor according to the molar ratio of 1:0.72, add the catalyst zinc acetate according to 0.7% of the mass of phenol, then add the catalyst oxalic acid, the mass of oxalic acid is 0.3% of the phenol, stir and heat to 70°C and at this temperature Keep it under low temperature for 1 hour, then heat up to 100°C and boil and reflux for 5 hours; start distillation and dehydration after the reaction is completed, and continue heating and heating after the temperature rises to 110°C to stabilize for 1.5 hours, and finally vacuum dehydration at 150°C ~ 160°C Phenol, when the negative pressure reaches 0.97MPa, it can be discharged after 1 hour of dephenolization.

[0027] According to HG5 1342, measure the free phenol content in the phenolic resin, the free phenol content of the thermoplastic resin obtained by the above method is 2.1% after testing; the resin molecular weight (Mw) is 4415; the ortho-to-para ratio obtained from the infrared tr...

Embodiment 2

[0029] Put phenol and formaldehyde into the reaction kettle according to the molar ratio of 1:0.70, add catalyst zinc acetate according to 0.7% of the mass of phenol, then add catalyst oxalic acid, the mass of oxalic acid is 0.3% of phenol, stir and heat to 70°C Keep at low temperature for 1 hour, then heat up to 100°C and boil and reflux for 3 hours; start distillation and dehydration after the reaction is completed, and heat up after the temperature rises to 120°C to stabilize for 1 hour. When the temperature reaches 150°C-160°C, vacuum dehydration Phenol, when the negative pressure reaches 0.97MPa, it can be discharged after 1 hour of dephenolization.

[0030] According to HG5 1342, the free phenol content in the phenolic resin is measured, and the free phenol content of the thermoplastic resin obtained by the above method is about 2.3% after testing; the molecular weight of the resin is 3951; the ortho-to-para ratio obtained from the infrared transmission spectrum is 6: 1; ...

Embodiment 3

[0032] Put phenol and formaldehyde into the reactor according to the molar ratio of 1:0.68, add the catalyst zinc acetate according to 0.7% of the mass of phenol, then add the catalyst oxalic acid, the mass of oxalic acid is 0.3% of the phenol, stir and heat to 70°C and at this temperature Keep it under low temperature for 1 hour, then heat up to 100°C and boil and reflux for 4 hours; start distillation and dehydration after the reaction is completed, when the temperature rises to 130°C, stabilize the temperature for 0.5 hours and then heat up, when the temperature reaches 150°C, vacuum dephenolization can be done , When the negative pressure reaches 0.97MPa, it can be discharged after 0.5 hours of dephenolization.

[0033] Measure free phenol content in phenolic resin according to HG5 1342, the free phenol content of the thermoplastic resin obtained by the above method is about 2.1% after testing; the resin molecular weight is 3320; the ortho-para ratio obtained from infrared ...

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Abstract

The invention discloses a method for preparing high-ortho thermoplastic phenolic resin. The method comprises the following steps of: (1) feeding phenol and formaldehyde into a reaction kettle in a proportion of 1:0.6-0.8, and uniformly stirring; (2) adding a weak acid salt catalyst with divalent metal ions into the reaction kettle, and then adding a weak acid catalyst, wherein the weak acid salt catalyst with divalent metal ions accounts for 0.5%-1% of the weight of the phenol, and the weight of the weak acid catalyst accounts for 0.2-0.4% of the weight of the phenol; raising temperature to 60 DEG C - 80 DEG C, and stirring to react for 0.5-2 hours; (3) heating, and boiling to reflux for 3-5 hours; and (4) dewatering, and removing excessive phenol. By adopting the composite catalyst system of zinc acetate and oxalic acid, the invention is difficult to gel and cure in the reaction process, and has no need of high-pressure condition, and the yield of the resin achieves more than 95%. The high-ortho thermoplastic phenolic resin prepared by the method has good flowability, high gelling and curing speed, and great application value in the coated sand and injection moulding process.

Description

technical field [0001] The invention relates to the field of phenolic resins, in particular to a preparation method of high ortho-position thermoplastic phenolic resins. Background technique [0002] The biggest feature of high ortho phenolic resin is its fast polymerization speed, which can make the resin cure faster under the condition of adding appropriate hexamethylenetetramine. At the same time, the high-ortho resin also has the characteristics of a relatively low softening point, so it has good coating performance in the application of coated sand, and can make the coated sand reach an appropriate room temperature tensile strength with a relatively low amount of resin added. And higher thermal tensile strength, and significantly reduce the gas generation of coated sand, which is unmatched by ordinary phenolic resin coated sand. In addition, in terms of phenolic resin injection molding process, the ideal injection molding material should have good fluidity in the machi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/10
Inventor 唐路林焦峰姜广锋邢介名李枝芳
Owner SHANDONG SHENGQUAN NEW MATERIALS CO LTD
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