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Method for preparing epoxy fatty acid methyl ester

A technology of epoxy fatty acid methyl ester and fatty acid methyl ester, which is applied in the field of preparation of plasticizer epoxy fatty acid methyl ester, can solve problems such as low level of equipment and self-control, inability to realize continuous production, backward synthesis process, etc., to avoid Effects of by-product generation, good operability, and easy preparation process

Inactive Publication Date: 2010-11-24
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing problems are mainly manifested in: ① small output; ② backward synthesis process, large acid water discharge, inaccurate temperature control; ③ low level of equipment and automatic control
④Intermittent operation, unable to achieve continuous production

Method used

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  • Method for preparing epoxy fatty acid methyl ester
  • Method for preparing epoxy fatty acid methyl ester
  • Method for preparing epoxy fatty acid methyl ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 30% hydrogen peroxide and formic acid are mixed according to the molar ratio of hydrogen peroxide and formic acid as 1.2:1, 5% sulfuric acid catalyst is added in the mixed solution, the stabilizer is 1% urea, and the dihydrogen peroxide in formic acid and fatty acid methyl ester is respectively mixed. The molar ratio of the number of bonds is 1.0:1 and injected into a micro-mixing reactor with temperature control at 50° C. through a high-pressure pump. The micro-mixer is a T-shaped curved channel glass micro-mixer (T-mixer, Mixcrogalss, Germany), the channel size (μm) is 50×210000 (diameter×length), and the residence time is 4.94ms; the inner diameter is 1mm, the length is 3.2m polytetrafluorocapillary, and the residence time is 0.5min. Submerge in an ice-water bath to terminate the reaction. Collect reaction product, product solution has obtained the product containing epoxidized fatty acid methyl ester through liquid separation, washing, drying, and its titration obta...

Embodiment 2

[0029] Mix 45% hydrogen peroxide and formic acid according to the molar ratio of hydrogen peroxide and formic acid at 1.0:1, add 1.0% sulfuric acid catalyst in the mixed solution, stabilizer is 1.5% EDTA, respectively press the double bond in formic acid and fatty acid methyl ester The molar ratio of the number is 1.2:1 and injected into the micro-mixing reactor with temperature control at 75 °C through a high-pressure pump. The micro-mixer is a T-shaped curved channel glass micro-mixer (T-mixer, Mixcrogalss, Germany ), the channel size (μm) is 50×210000 (diameter×length), and the residence time is 4.10ms; followed by a PTFE capillary with an inner diameter of 1mm and a length of 8m, and the PTFE tube is immersed in an ice-water bath to terminate reaction with a residence time of 1 min. Collect reaction product, product solution has obtained the product containing epoxidized fatty acid methyl ester through liquid separation, washing, drying, and iodine value is 9.3g I 2 / 100g...

Embodiment 3-8

[0031] Using the same reaction conditions as in Example 1 and Example 2, the micro-mixer is changed into a small size stainless steel tee (inner diameter is 1.0mm) or a cross-toed micro-mixer (HPIMM, IMM, Germany), and its channel size (μm) It is 25×21×37, or V2 (IMM, Germany), and the residence time in the micro-mixer and the microchannel reactor are 2.1 ms and 10 min, respectively. The iodine value and epoxy value of the obtained epoxidized fatty acid methyl ester product are shown in Table 1.

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Abstract

The invention relates to a method for preparing epoxy fatty acid methyl ester. The method comprises the following specific steps of: mixing hydrogen peroxide and formic acid or acetic acid; adding a catalyst and a stabilizer into mixed liquor; pumping fatty acid methyl ester into a microstructure reactor; separating the epoxy fatty acid methyl ester from a reacted material; introducing a reaction product into a separator; standing to delaminate lower layer water solution; washing an upper layer organic phase with water; and drying the washed upper layer organic phase to obtain the epoxy fatty acid methyl ester. In the entire process of the method, a strong exothermic reaction is performed, and a peroxy acid synthesis reaction is performed together with an epoxidation reaction, so that the epoxy fatty acid methyl ester is synthesized in situ at one time. The production process has the advantages of high safety, low energy consumption, continuity and high product quality by adopting micro-reaction production technology of the invention.

Description

technical field [0001] The invention relates to a method for preparing epoxy fatty acid methyl ester, in particular to a method for preparing plasticizer epoxy fatty acid methyl ester in a microstructure reactor using hydrogen peroxide, formic acid (or acetic acid) and fatty acid methyl ester as raw materials. Background technique [0002] Epoxy plasticizers are organic compounds with epoxy groups in their molecular structure. Compared with traditional ortho-phthalic plasticizers, they have the advantages of non-toxicity, good heat resistance and light resistance. With the improvement of environmental protection awareness in various countries in the world, plastic products such as medicine and food packaging, daily necessities, toys, etc. have put forward higher purity and hygiene requirements for the main plasticizer dioctyl phthalate (DOP). Epoxy plasticizers mainly include epoxy oil and epoxy fatty acid ester. In addition to the advantages of epoxy oil, epoxy fatty acid e...

Claims

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Application Information

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IPC IPC(8): C07D303/42C07D301/16
Inventor 张利雄姚型军王重庆徐南平
Owner NANJING UNIV OF TECH
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