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Preparation method and application of menthol derivative, mixture thereof and menthol derivative

A technology of menthol derivatives and mixtures, applied in mint substances and their preparation methods, and in the field of cultural relics reinforcement, can solve the problems of insufficient strength of reinforced cultural relics, difficulty in maintaining the shape of reinforced cultural relics, toxicity, etc., and achieve application Broad, controlled removal, high melting temperature effect

Active Publication Date: 2021-12-03
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] (2) Permeability
[0008] (3) Volatility
[0010] (5) toxicity
[0012] At present, menthol, a temporary reinforcement material used in China, has a melting point of 44°C and relatively high volatility. However, under high-heat climate conditions, due to its low melting point and fast volatilization, it is difficult to maintain the shape of reinforced cultural relics; Low melting point, menthol volatilizes quickly, insufficient strength for reinforcing cultural relics

Method used

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  • Preparation method and application of menthol derivative, mixture thereof and menthol derivative
  • Preparation method and application of menthol derivative, mixture thereof and menthol derivative
  • Preparation method and application of menthol derivative, mixture thereof and menthol derivative

Examples

Experimental program
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Effect test

Embodiment 1

[0042] In this embodiment, a method for preparing L-menthol lactic acid adopts a menthol esterification modification process to prepare menthol esterification-modified derivatives, including the following steps:

[0043] (1) Batching process: adopt menthol and L-lactic acid as raw materials, adopt cyclohexane as solvent, adopt p-toluenesulfonic acid as catalyst, take by weighing 85g of L-lactic acid whose mass percentage content is 90%, add cyclohexane 2L, Add 156g of menthol, 5g of p-toluenesulfonic acid, and mix menthol, L-lactic acid, cyclohexane and p-toluenesulfonic acid in the reactor to form a reactant system mixture;

[0044] (2) carry out menthol esterification reaction in reactor, control the reaction temperature of the reactant system mixture in said step (1) to be 95 ℃ above the solvent boiling point temperature, heat to reflux with water, and the reaction time is 6h; Embodiment Menthol esterification is carried out in solution;

[0045] (3) After the esterificati...

Embodiment 2

[0054] This embodiment is basically the same as Embodiment 1, especially in that:

[0055] In the present embodiment, a kind of preparation method of monomenthyl succinate adopts the menthol esterification modification process, prepares the menthol esterification modified derivative, comprises the following steps:

[0056] (1) batching process: adopt menthol and succinic anhydride as raw material, adopt chloroform as solvent, adopt DMAP as catalyst, take succinic anhydride 150g, add chloroform 1.5L, add 156g menthol, catalyst DMAP 12g, mix menthol, Succinic anhydride, chloroform and DMAP are mixed in a reactor to form a reactant system mixture;

[0057] (2) carry out menthol esterification reaction in reactor, control the reaction temperature of the reactant system mixture in described step (1) to be 80 ℃ above the solvent boiling point temperature, heat and reflux with water, and the reaction time is 12h; Embodiment Menthol esterification is carried out in solution;

[0058...

Embodiment 3

[0066] This embodiment is basically the same as the previous embodiment, and the special features are:

[0067] A kind of preparation method of menthyl benzoate adopts menthol esterification modification process, prepares the derivative of menthol esterification modification, comprises the steps:

[0068] (1) Ingredients process: using menthol, benzoyl chloride, NaHCO 3 As raw material, adopt DCM as solvent, adopt DMAP as catalyst, weigh the NaHCO of benzoyl chloride 155g and 74g 3 , add DCM to 1.5L, add 156g menthol, catalyst DMAP to 12g, menthol, benzoyl chloride, NaHCO 3 , DCM and DMAP are mixed in the reactor to form a reactant system mixture;

[0069] (2) carry out menthol esterification reaction in reactor, control the reaction temperature of the reactant system mixture in described step (1) to be 90 ℃, heat to reflux with water, the reaction time is 20h; Present embodiment menthol The esterification reaction is carried out in solution;

[0070] (3) After the esterif...

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Abstract

The invention discloses a preparation method and application of a menthol derivative, a mixture thereof, and a menthol derivative. Through esterification of menthol, molecular design is carried out, and mint with a specific molecular structure or a specific group is synthesized. Alcohol derivatives, through chemical structure modification, provide a new class of temporary reinforcement materials for cultural relics with higher melting point and lower volatility. The melting point of this series of compounds can form a gradient melting point, and the volatility is slower than menthol, which can achieve controllable removal and meet the requirements of the cultural relics protection department. The composite material of the present invention is used for temporary reinforcement of cultural relics at the excavation site of cultural relics, and is suitable for the temporary reinforcement of shedding painted paintings, fragments of stone cultural relics, murals of rock paintings, fragments of lacquerware cultural relics, fragments of wooden cultural relics, paper cultural relics, and cotton and hemp cultural relics. Extraction, widely used.

Description

technical field [0001] The invention relates to a temporary reinforcement material and its preparation method and its application in the protection of cultural relics, in particular to a mint-like material and its preparation method and its application in the field of cultural relics reinforcement, which are widely used in the technical field of cultural relics protection materials at archaeological sites. Background technique [0002] The protection of cultural relics on the archaeological site is a kind of cultural relics protection in special occasions. Compared with the conditions of the cultural relics protection laboratory, the conditions of the archaeological excavation site are not perfect in terms of reagents, medicines, instruments and materials, etc., which determines the protection of on-site protection. The character of the work can only be temporary, and sometimes even these measures are removed after arriving in the laboratory. Therefore, the technical means a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/68C07C69/40C07C69/78C07C69/38C07C69/42C07C69/60C07C67/08C07C67/14
CPCC07C69/38C07C69/40C07C69/42C07C69/60C07C69/68C07C69/78C07C2601/14
Inventor 米易晓邢菲菲周小安徐艺青姜标
Owner SHANGHAI UNIV
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