High-ortho-position phenol-formaldehyde resin prepolymer and preparation method thereof

A technology of phenolic resin prepolymerization and high ortho position, which is applied in the fields of aldehyde/ketone condensation polymer adhesives, manufacturing tools, casting molding equipment, etc., and can solve the problem of limiting the application of high ortho phenolic resin and the methylol content of phenolic resin Low, to be developed and other issues, to achieve the effect of high adjacent to bit ratio, high positioning effect, low production cost

Inactive Publication Date: 2015-06-10
山东恒瑞磁电股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] It can be seen from the above-mentioned patent reports that phenolic resins with a high ortho-para position ratio can be prepared by selecting a suitable catalyst and a suitable molar ratio of formaldehyde to phenol, but there are still some shortcomings in the current research on high ortho-position phenolic resins. On the one hand, due to the low molar ratio of formaldehyde and phenol, the content of the methylol group in the prepared phenolic resin is low, which limits the application of high ortho-position phenolic resins in the field of wood adhesives; on the other hand, catalysts with efficient positioning effects system to be developed

Method used

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  • High-ortho-position phenol-formaldehyde resin prepolymer and preparation method thereof
  • High-ortho-position phenol-formaldehyde resin prepolymer and preparation method thereof
  • High-ortho-position phenol-formaldehyde resin prepolymer and preparation method thereof

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Embodiment -1

[0031] In a 500mL four-neck flask equipped with a thermometer and a reflux condenser, add 119.7g of formaldehyde solution (40% by mass fraction), mechanically stir, add 100.0g of phenol, and the molar ratio of phenol to formaldehyde is 1:1.5. After dissolving, add 0.5g zinc acetate, wherein zinc acetate is 0.5% of phenol mass, after zinc acetate dissolves completely, add catalyst 0.2g sodium hydroxide, wherein the amount of sodium hydroxide is 0.2% of phenol mass, stir and heat to 45 ℃ and kept at this temperature for 0.5 hours, heated to 100 ℃ and refluxed for 6 hours, cooled to 60 ℃ and dehydrated to a solid content of 65%. The prepared phenolic resin prepolymer had an ortho-to-para ratio of 4.1 .

Embodiment -2

[0033] In a 500mL four-neck flask equipped with a thermometer and a reflux condenser, add 109.4g of formaldehyde solution (mass fraction is 35%), mechanically stir, add 100.0g of phenol, the molar ratio of phenol to formaldehyde is 1:1.2, until the phenol is completely After dissolving, add 1.0g zinc acetate, wherein zinc acetate is 1.0% of phenol mass, after zinc acetate dissolves completely, add catalyst 0.4g sodium hydroxide, wherein the amount of sodium hydroxide is 0.4% of phenol mass, stir and heat to 50 ℃ and kept at this temperature for 0.75 hours, heated to 85 ℃ and refluxed for 5 hours, cooled to 50 ℃ and dehydrated to a solid content of 62%. The prepared phenolic resin prepolymer had an ortho-to-para ratio of 8.3 .

Embodiment -3

[0035] In a 500mL four-necked flask equipped with a thermometer and a reflux condenser, add 86.2g of formaldehyde solution (mass fraction is 37%), mechanically stir, add 100.0g of phenol, the molar ratio of phenol to formaldehyde is 1:1.0, until the phenol is completely After dissolving, add 2.0g zinc acetate, wherein zinc acetate is 2.0% of phenol mass, after zinc acetate dissolves completely, add catalyst 0.8g sodium hydroxide, wherein sodium hydroxide consumption is 0.8% of phenol mass, stir and heat to 60 ℃ and kept at this temperature for 1 hour, heated to 90 ℃ and refluxed for 6 hours, cooled to 45 ℃ and dehydrated to a solid content of 55%, the prepared phenolic resin prepolymer had an ortho-to-para ratio of 12.5.

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Abstract

The invention belongs to the field of phenol-formaldehyde resin wood adhesives and relates to a high-ortho-position phenol-formaldehyde resin prepolymer and a preparation method thereof. The method comprises the steps of (1) putting phenol and formaldehyde into a reaction kettle, and uniformly stirring; (2) respectively adding catalysts, namely zinc acetate and sodium hydroxide, then, heating to the temperature of 45-60 DEG C, and carrying out stirring reaction for 0.5-1 hour; (3) heating to the temperature of 85-100 DEG C, and carrying out reflux reaction for 4-6 hours; (4) cooling to the temperature of 45-60 DEG C, and dehydrating, thereby obtaining the high-ortho-position phenol-formaldehyde resin prepolymer with the solid content of 55-65%. According to the method, a zinc acetate and sodium hydroxide composite catalysis system is adopted, so that the high-ortho-position phenol-formaldehyde resin prepolymer can be prepared under the condition that the mole ratio of formaldehyde to phenol is relatively high. Besides, the method disclosed by the invention has the advantages that the reaction is relatively stable, the production cost is relatively low, and the obtained phenol-formaldehyde resin prepolymer is high in ortho-para ratio and good in fluidity and has a potential application value in the field of wood adhesives.

Description

technical field [0001] The invention belongs to the field of phenolic resin wood adhesives, and in particular relates to a high-ortho-position phenolic resin prepolymer and a preparation method thereof. Background technique [0002] In the application field of wood adhesives, two types of adhesives dominate and play a leading role, namely amino resin adhesives represented by urea and formaldehyde and phenolic resin adhesives represented by phenol and formaldehyde. Among them, phenolic resin adhesive is widely used as an adhesive for outdoor plywood because of its superior weather resistance, high temperature resistance, water resistance, especially boiling water resistance. [0003] The ortho-to-para ratio of phenolic resins prepared by traditional acid-catalyzed or base-catalyzed methods is relatively low, resulting in low activity of phenolic resins and long curing time, which limits the application of phenolic resins. In order to improve the ortho-to-para ratio of phenol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/10C08G12/40B22C1/22C09J161/10
Inventor 吕满庚张云飞杨成华李因文张蕊
Owner 山东恒瑞磁电股份有限公司
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