Method for preparing hinokitiol metal compound and complex

A metal compound and tarry alcohol technology, which is applied in the field of preparation of organic compounds, can solve the problems of incapability of uniform and sufficient compounding of cyperol and metal ions, the property of being easily decomposed in the presence of light is not fundamentally improved, and the material quality is greatly different, and the like. Avoid waste water treatment and pollution load, improve visible photolysis, get results quickly

Inactive Publication Date: 2020-09-04
INST OF ENVIRONMENT & SUSTAINABLE DEV IN AGRI CHINESE ACADEMY OF AGRI SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the Japanese published patent JP flat 1-53855 (manufacturing method of water-soluble cypress alcohol) drops the cypress alcohol solution dissolved in the lower alcohol into the powdered salt compound constantly stirred and mixed to prepare the cypress alcohol metal Compound, although improved to a certain extent the unstable characteristics of cypress alcohol that is easy to decompose when exposed to light, it does not sufficiently suspend and evenly disperse the cypress alcohol organic solvent solution, causing the cypress alcohol solution to be added dropwise to powdery salts When compounding, the material quantity contrast difference is huge, thus, the homogeneous property difference of product is greatly affected by stirring and mixing and the grinding of powdery salt compounds, etc., and can not make cypress alcohol and metal ion fully compounded evenly, and its exposure to light The characteristics of easy decomposition have not been fundamentally improved
In CN101396021A, acid solution is used in the preparation process of cypress alcohol metal compound, which causes costs such as waste water treatment and environmental load, which is not conducive to industrialization promotion

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Weigh 5.8 g of NaCl and 16ml of water to prepare a saturated or high-concentration aqueous solution with a solution temperature of 35°C~50°C, dissolve 16.4g of cypress alcohol in 5~15ml of acetone, and measure 1 / 4 of the volume of NaCl solution in deionized water , under the condition of high-speed shear homogeneity, the measured deionized water is quickly added to the cypress alcohol acetone solution, fully dispersed to form a stable suspended self-emulsifying solution, and under the condition of continuous rapid shear homogeneity, Quickly add high-concentration NaCl solution, continue to shear and homogenize and fully compound for 20-60 minutes, and cool in the temperature range of -2°C to 5°C to promote the rapid crystallization of cypressoyl alcohol-Na. The mass ratio is 1:1. centrifuge to separate the cypresseyl alcohol-Na crystalline compound, and wash it with deionized water at a temperature of 0°C to 5°C to prepare the cypressetyl alcohol-Na crystalline compound...

Embodiment 2

[0047] Weigh 11.1 g CaCl 2 Prepare a saturated or high-concentration aqueous solution with a solution temperature of 35°C~50°C with 10ml of water, dissolve 24.6 g of cedaryl alcohol in 10~20ml of ethanol, and measure CaCl 2 1 / 3 of the solution volume deionized water, under the condition of high-speed shear homogeneity, quickly add the measured deionized water into the cypress alcohol ethanol solution, fully disperse to form a stable suspended self-emulsifying solution, and continuously Under the condition of rapid shear homogeneity, add high concentration CaCl quickly 2 The solution is continuously sheared and homogeneously fully compounded for 20 to 60 minutes, and cooled in the temperature range of -2°C to 5°C to promote the rapid crystallization of cypresseyl alcohol-Ca. Among them, CaCl 2 The molar mass ratio of cypressyl alcohol is 1:1.5. centrifuge to separate the cypress alcohol-Ca crystalline compound, and wash it with deionized water at a temperature of 0°C to 5°C t...

Embodiment 3

[0050] Weigh 16.2 g FeCl 3 Prepare a saturated or high-concentration aqueous solution with 10ml of water at a temperature of 35°C~50°C, dissolve 49.2 g of cedaryl alcohol in 20~30ml of acetone, and measure FeCl 3 Solution equal volume of deionized water, under the condition of high-speed shear homogeneity, quickly add the measured deionized water into the cypress alcohol acetone solution, fully disperse to form a stable suspension self-emulsifying solution, and continuously and rapidly shear Under the condition of cutting homogeneity, add high concentration FeCl quickly 3 The solution is continuously sheared and homogenized, fully compounded for 20-60 minutes, and cooled in the temperature range of -2°C to 5°C to promote the rapid crystallization of cypresseyl alcohol-Fe. Among them, FeCl 3 The molar mass ratio of cypress and cypress alcohol is 1:3. centrifuge to separate the cypress alcohol-Fe crystalline compound, and further wash it with deionized water at a temperature o...

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Abstract

The invention provides a method for preparing a hinokitiol metal compound or a hinokitiol ammonium compound. The method comprises the following steps: dissolving hinokitiol in a water-soluble organicsolvent to obtain a hinokitiol solution with a hinokitiol concentration of 6-25 mol/L; fully mixing and reacting the obtained hinokitiol solution with an aqueous solution of water-soluble metal salt or ammonium salt at room temperature, wherein the water-soluble metal salt is selected from metal salt with solubility not lower than 35 g/100ml at room temperature, or the concentration of the aqueoussolution of the water-soluble metal salt or ammonium salt is not lower than 25% at room temperature, and the aqueous solution of the water-soluble metal salt or ammonium salt is further preferably asaturated solution of the water-soluble metal salt at 30-50 DEG C; and controlling the molar ratio of the water-soluble metal salt or ammonium salt to the hinokitiol to be 1: (0.9-5) to prepare a hinokitiol metal compound or hinokitiol ammonium compound solution. The method provided by the invention can fundamentally improve the instability characteristic that the hinokitiol is easy to decompose when meeting light, and avoids environmental pollution load and treatment cost of wastewater caused by the use of an acid solution.

Description

technical field [0001] The invention relates to a method for preparing an organic compound, in particular to a method for preparing a cypress alcohol metal compound and a compound. Background technique [0002] Hinokitiol, also known as hinokitiol, hinokitiol or hinokitiol, has good broad-spectrum antibacterial properties, moisture retention and pest repelling effects. It is a high-safety raw material for the preparation of antibacterial agents and insect repellents. Surrounding that cypress alcohol has broad-spectrum antibacterial and antifungal properties, inhibits ALDH activity and self-renewal ability in glioma stem cells, inhibits carcinogenicity in vitro, inhibits tyrosinase, inhibits plant production of ethylene, and has the properties of imparting cell activity, etc. People apply it in the development of many products such as medicine development, hygiene products, cosmetics, hair care, food preservation, etc. [0003] Cinnamon alcohol has a minimum inhibitory conce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/61C07C45/81C07C49/717
CPCC07C45/61C07C45/81C07C49/717
Inventor 宋吉青刘家磊何文清
Owner INST OF ENVIRONMENT & SUSTAINABLE DEV IN AGRI CHINESE ACADEMY OF AGRI SCI
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