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Method for synthesizing o-cresol novolac resin

A technology of novolak resin and o-cresol, applied in the field of synthesizing o-cresol series novolak resin

Active Publication Date: 2010-12-08
LUCKY HUAGUANG GRAPHICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

As for the method of synthesizing ortho-cresol novolac resin with two reaction devices separated in space, especially the alkali-acid step-by-step catalysis of a double-layer reaction device, no reports have been seen in patents or papers

Method used

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  • Method for synthesizing o-cresol novolac resin
  • Method for synthesizing o-cresol novolac resin
  • Method for synthesizing o-cresol novolac resin

Examples

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Synthetic example

[0068] The synthesis examples and comparative examples of the present invention are described below. It must be pointed out that there are many synthetic examples of the present invention that have application value and can be implemented, and only a part of representative examples are listed here.

Synthetic example 1

[0070]Get 216kg (2kmol) of o-cresol, 37% by weight of aqueous formaldehyde solution 162.2kg (2kmol) and 0.864kg of sodium hydroxide and join in the upper layer enamel reactor of double-layer reactor, and this upper layer enamel reactor adopts steam heating and is equipped with Vertical and horizontal condensers and water collection tanks. The temperature was raised to 70°C with stirring and maintained for 5 hours, and then maintained at 80°C, 90°C, and the reflux temperature of the reaction system for 1 hour, respectively. Then heat up the effluent, when the effluent reaches about 1 / 3 of the total effluent, cool down to 80~90 ℃, neutralize the reaction system to pH value 5 with concentrated hydrochloric acid solution, then add oxalic acid 2.16 % based on the total phenolic amount of 1% by weight kg, then the temperature was raised to the reflux temperature of the reaction system in about 1 hour, and the temperature was further increased to produce water, and then the temperatu...

Synthetic example 2

[0072] 162.2 kg of 37 wt % formaldehyde aqueous solution in Synthesis Example 1 was changed to 154.2 kg of 37 wt % formaldehyde aqueous solution (1.9 kmol), and the others were completely the same as Synthetic Example 1. The crude product P-2 was obtained in 98% yield. The general physicochemical properties of the resin as well as the formaldehyde and phenol content in the wastewater and the free phenol content in the resin are listed in Table 1, and the imaging properties are listed in Table 2.

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Abstract

The invention relates to a method for synthesizing o-cresol novolac resin, comprising the following steps of (1) reacting o-cresol with formaldehyde under the temperature of 65 DEGC to the reflux temperature of a reaction system with the existence of an alkaline catalyst for 6-14 hours in a first reaction area, then heating and discharging water, cooling to the temperature of 80-90 DEG C when effluent water accounts for 1 / 4-1 / 3 of the total effluent water, adjusting the pH to 4.5-5.5 by adding acid which is used as the neutralizer, then adding an acidic catalyst of 0.5-2 percent of the total weight of phenol monomer, subsequently heating to the temperature of 140-145 DEG C, wherein water is discharged continuously in the process for 4-4.5 hours from starting water discharging to the temperature of 140-145 DEG C; and (2) transferring a reaction mixture obtained from step (1) to a second reaction area which is preheated to the temperature of 180-185 DEG C, heating to the temperature of 190-195 DEG C within 2-2.5 hours, and then decompressing and vacuumizing to obtain the o-cresol novolac resin. The o-cresol novolac resin synthesized by using the method has high Mw, trace contents of monomer and diplocaryon, extreme lower content of monomer in waste gas and waste water and less environment pollution.

Description

technical field [0001] The present invention relates to a kind of method for synthesizing o-cresol series novolac resin, more particularly, to a kind of synthesizing o-cresol series novolac resin under the action of basic catalyst and acidic catalyst in two reaction zones successively Methods. Background technique [0002] Phenolic resins are synthetic resins with the longest history and very densely documented related patent documents. The situation prior to the 1950s The present inventors rely solely on the general conclusions made on phenolic resins in the book Phenolic Resins, edited by Robitschek P and Lewin A (Londan: Iliffe & Sons, Ltd., 1950), which discusses Various phenol monomers pointed out: "It is impossible to synthesize high molecular weight novolac resin with o-cresol monomer". The inventor has systematically checked the synthesis methods of phenolic novolak resins from the 1950s to 1985, and found that the conclusions about o-cresol novolak resins are basi...

Claims

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Application Information

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IPC IPC(8): C08G8/12C08G8/24G03F7/004
Inventor 余尚先丛培军邵永智杨金瑞顾江楠王大伟邵正春
Owner LUCKY HUAGUANG GRAPHICS
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