Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for synthesizing methyl (ethyl) gallate through catalysis of Cu-mordenite

A technology of methyl gallate and ethyl gallate, which is applied in the field of Cu-mordenite catalyzed synthesis of methyl gallate or ethyl gallate, can solve the problem of easily causing conjunctivitis, rhinitis, pharyngitis and respiratory tract inflammation, and complicated post-processing. , carcinogenic effects and other problems, to achieve the effect of high conversion rate and product purity, simple and easy process, less consumption and pollution

Active Publication Date: 2014-04-09
南京龙源天然多酚合成厂 +1
View PDF5 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are some obvious deficiencies in these synthetic methods, as: the raw material dimethyl sulfate that adopts has extremely strong toxicity, easily causes conjunctivitis, rhinitis, pharyngitis and respiratory tract inflammation, and has carcinogenic effect, and also needs to use alcohol as raw material Other toxic reagents, and in order to increase the yield need to consume a large amount of acidic catalysts and water-absorbing agents, the three wastes are serious, causing environmental pollution
In addition, the post-processing of traditional synthesis methods is relatively cumbersome.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for synthesizing methyl (ethyl) gallate through catalysis of Cu-mordenite
  • Method for synthesizing methyl (ethyl) gallate through catalysis of Cu-mordenite

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0013] The preparation of catalyst A was repeated except that the amount of copper nitrate dihydrate was 0.7 g. ICP spectroscopic analysis of the obtained Cu-mordenite showed that the Cu content was 0.4 wt%.

[0014] (3) Catalyst C:

[0015] The preparation of Catalyst A was repeated except that the amount of copper nitrate dihydrate was 1.0 g. The resulting Cu-mordenite was analyzed by ICP spectroscopy, which contained C u The amount is 1.8 wt%.

[0016] (4) Catalyst D:

[0017] The preparation of catalyst A was repeated except that the amount of copper nitrate dihydrate was 1.6 g. ICP spectroscopic analysis of the obtained Cu-mordenite showed that the Cu content was 4.3 wt%.

[0018] (5) Catalyst E:

[0019] The preparation of catalyst A was repeated except that the amount of copper nitrate dihydrate was 1.9 g. The resulting Cu-mordenite was analyzed by ICP spectroscopy, which contained C u The amount is 5.3 wt%.

[0020] Note: Mordenite is available from many c...

Embodiment 2

[0027] Example 2 Using recovered catalysts A, B, C, D, and E to catalyze the synthesis of methyl gallate

[0028] Using the recovered C in Example 1 u -Mordenite A, B, C, D, E are catalysts, repeat the reaction process of Example 1 respectively, just change the reaction pressure to 0.7 Mpa, and the reaction temperature to 115°C to obtain methyl gallate product.

Embodiment 3

[0029] Embodiment 3 Use catalyst A, B, C, D, E to catalyze the synthesis of ethyl gallate

[0030] Add 1 mol of gallic acid and 8 mol of diethyl carbonate into the reaction kettle, add 5.5 g of catalysts A, B, C, D, and E obtained above under stirring, pressurize to 0.4 MPa, and react at 120 °C for 12 h. After the reaction was monitored by HPLC, it was filtered and separated. The filter cake was first washed with 15 ml of diethyl carbonate, then washed with 100 ml of deionized water, then dried at 110 °C for 3 h, and then calcined in a muffle furnace at 500 °C for 4 h , recycling C u - Mordenite. The filtrate is combined with the diethyl carbonate washing solution for washing the catalyst, placed on a rotary evaporator, heated in a water bath at 80-85°C, evaporated under reduced pressure at -0.095Mpa, and the excess diethyl carbonate is evaporated and then condensed and recovered. Add 900 ml of deionized water to the residual solid in the bottle, raise the temperature to 95°...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
melting pointaaaaaaaaaa
melting pointaaaaaaaaaa
Login to View More

Abstract

The invention relates to a method for synthesizing methyl (ethyl) gallate through catalysis of Cu-mordenite. The method comprises the step: by taking gallic acid and dimethyl carbonate or diethyl carbonate as raw materials and Cu-mordenite as a catalyst, performing transesterification reaction under pressurization to obtain methyl gallate or ethyl gallate. As the green and environment-friendly dimethyl carbonate or diethyl carbonate are a methylating (ethylating) agent, the method is low in cost and environment-friendly, the yield of the synthesized technical products can achieve more than 98%, and the purity of the ethyl gallate product is greater than 99%.

Description

technical field [0001] The invention relates to a method for synthesizing methyl gallate or ethyl gallate, in particular to a method for catalyzing the synthesis of methyl gallate or ethyl gallate with Cu-mordenite. Background technique [0002] Methyl gallate or ethyl gallate are good antioxidants and important pharmaceutical intermediates, and are widely used in chemical industry, light industry and food industry. The classic synthesis method of gallic acid methyl (b) ester is to use sulfuric acid or p-toluenesulfonic acid and other protonic acids as catalysts to make gallic acid esterify with methanol and ethanol, and use water-absorbing agents such as anhydrous calcium chloride and molecular sieves at the same time Or with water agent to remove the water produced in the reaction process. In addition, there is also a process of using dimethyl sulfate to methylate gallic acid under the catalysis of potassium carbonate or sodium hydroxide. There are some obvious deficienc...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/84C07C67/11B01J29/24
CPCB01J29/24C07C67/11C07C69/84
Inventor 徐浩张宗和钱星黄嘉玲陶林徐斌陈文文
Owner 南京龙源天然多酚合成厂
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com