Method for producing rosin ester and rosin ester

A manufacturing method and technology of rosin ester, which is applied in the field of rosin ester manufacturing, can solve problems such as the easy deterioration of color tone, and achieve the effect of excellent heating stability

Active Publication Date: 2017-11-24
ARAKAWA CHEM IND LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Meanwhile, rosin esters are generally yellow to yellowish-brown in co

Method used

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  • Method for producing rosin ester and rosin ester
  • Method for producing rosin ester and rosin ester
  • Method for producing rosin ester and rosin ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] In a four-necked eggplant-shaped flask with a capacity of 500 ml equipped with a water separator connected to a spherical condenser at the upper end, a stirrer, and a nitrogen introduction pipe, add Chinese gum rosin (WW grade: acid value 170.0, softening point 86.0 ° C, color tone 8+G, the following, same as "Chinese gum rosin") 300 parts, heated under nitrogen stream to melt. Subsequently, when the reaction system reached 160°C, 0.34 parts of heptylphosphonic acid, 0.07 parts of calcium hydroxide and a sulfur-based disproportionation catalyst (4,4'-thiobis(6-tert-butyl-3-methyl 1.2 parts of phenol) (trade name Sumiraizer WX-R, manufactured by Sumitomo Chemical Co., Ltd.), and 29.4 parts of pentaerythritol were added when the reaction system reached 180°C. Thereafter, the reaction system was brought to 275° C. over about 2 hours, and this time point was defined as the 0th hour, and sampling was performed from the 2nd hour (6 times in total), and the acid value of each ...

Embodiment 2～5

[0093] Using the raw materials shown in Table 1, rosin ester was produced by the same method as in Example 1, and the same sampling as in Example 1 was performed to evaluate the physical properties.

Embodiment 6

[0095] In the same reaction vessel as in Example 1, 200.0 parts of toluene and 46.8 parts of 2-ethylhexylphosphonic acid mono-2-ethylhexyl were charged, and 5.76 parts of calcium hydroxide were added little by little while stirring. After heating up for 1 hour to reflux, cool to room temperature and filter through filter paper. Subsequently, acetone, a poor solvent, was added to the filtrate at room temperature, and the precipitate was collected by filtration to obtain a white product. Thereafter, the white product was recrystallized to obtain 2-ethylhexylphosphonic acid mono-2-ethylhexyl calcium salt.

[0096] Subsequently, 300 parts of gum rosin was added to the same reaction vessel as in Example 1, and heated under nitrogen flow to melt it. Subsequently, at the point when the reaction system reached 160°C, 0.60 parts of the esterification catalyst shown in Table 1 (the aforementioned 2-ethylhexylphosphonic acid mono-2-ethylhexyl calcium salt) and Sumilaizer WX-R 1.2 29.4 ...

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Abstract

The present invention provides a method for producing a pastel rosin ester in high yield in a short period of time. The present inventors have found that by using a catalyst group that uses a phosphonic acid derivative having an alkaline earth metal compound and an alkyl group having a carbon number of at least 7 as a substituent or a reaction product of both (i.e., having a carbon atom number of at least a phosphonate and / or derivative of a phosphonic acid and / or a derivative of 7 and a salt of an alkaline earth metal compound) is used as a catalyst, and a rosin and an alcohol are reacted to produce a light-colored rosin ester in a short period of time with high efficiency .

Description

technical field [0001] The present invention relates to the manufacture method of rosin ester. According to the production method of the present invention, a light-colored rosin ester can be provided in a relatively short period of time. Background technique [0002] Rosin esters are reaction products of rosin and alcohol, and have been popular as additives and modifiers for adhesives, printing inks, road marking paints, rubber and plastics, etc. in the past. [0003] However, a long time is generally required in the manufacture of rosin esters. This is because the carboxyl group of the resin acid in the raw material rosin is bonded to a tertiary carbon, and lacks reactivity due to its steric hindrance. [0004] Meanwhile, rosin esters are generally yellow to yellowish brown, and, if exposed to high temperature, the color tone is easily deteriorated. This is because rosin acid has a conjugated double bond in the molecule among resin acids, and this part is easily oxidized...

Claims

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Application Information

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IPC IPC(8): C09F1/04
CPCC09F1/04
Inventor 山田幸治
Owner ARAKAWA CHEM IND LTD
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