New process for synthesizing 1-hydroxycyclohexanecarboxylic acid and application
A technology of hydroxycyclohexylcarboxylic acid and hydroxycyclohexyl, which is applied in the field of synthesizing 1-hydroxycyclohexylcarboxylic acid, can solve the problems of increasing the chance of meeting main and by-products, difficult temperature operation, large heat release of the system, etc., so as to reduce the chance of molecular collision , The effect of controlling the reaction temperature and reducing the reaction temperature
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[0029] Example 1
[0030] A new process for synthesizing 1-hydroxycyclohexyl carboxylic acid: Put 210kg of cyclohexanone cyanohydrin and 150kg of cyclohexanone into the acidification kettle successively, turn on the stirring and ventilate chlorine, heat is released during the chlorine venting process, and the temperature in the kettle reaches a maximum of 75 ℃, when the temperature starts to drop, stop the chlorine flow, turn on the reflux, and keep the reaction at 55℃ for 3h; after the temperature is finished, open the cooling water valve to cool the material. When the temperature drops to 30℃, the material will be centrifuged for ammonium chloride. The filtrate thrown out is 1-hydroxycyclohexyl carboxylic acid, and the centrifuged ammonium chloride is dried and sold as a by-product.
[0031] In this example, the yield of 1-hydroxycyclohexyl carboxylic acid was 87.21%, the purity was 97.11%, the purity of ammonium chloride was 99.21%, and the total yield of spirodiclofen obtained ...
Example Embodiment
[0032] Example 2
[0033] A new process for synthesizing 1-hydroxycyclohexyl carboxylic acid: Put 240kg of cyclohexanone cyanohydrin and 170kg of cyclohexanone into the acidification kettle in turn, turn on the stirring and ventilate chlorine, heat is released during the chlorination process, and the temperature in the kettle reaches a maximum of 75 ℃, when the temperature starts to drop, stop the flow of chlorine, turn on the reflux, and keep the temperature at 50℃ for 3.5h; after the temperature is finished, open the cooling water valve to cool the material. When the temperature drops to 25℃, the material is discharged, and the material is centrifuged for ammonium chloride. , The filtrate that is thrown out is 1-hydroxycyclohexyl carboxylic acid, and the centrifuged ammonium chloride is dried and sold as a by-product.
[0034] In this example, the yield of 1-hydroxycyclohexylcarboxylic acid was 87.08%, the purity was 97.26%, the purity of ammonium chloride was 99.07%, and the tot...
Example Embodiment
[0035] Example 3
[0036] A new process for synthesizing 1-hydroxycyclohexyl carboxylic acid: Put 180kg of cyclohexanone cyanohydrin and 120kg of cyclohexanone into the acidification kettle in turn, turn on the stirring and ventilate chlorine, heat is released during the chlorine venting process, and the temperature in the kettle reaches a maximum of 75 ℃, when the temperature starts to drop, stop the chlorine flow, turn on the reflux, and keep the reaction at 45℃ for 4h; after the temperature is finished, open the cooling water valve to cool the material. When the temperature drops to 35℃, the material is discharged, and the material is centrifuged for ammonium chloride. The filtrate thrown out is 1-hydroxycyclohexyl carboxylic acid, and the centrifuged ammonium chloride is dried and sold as a by-product.
[0037] In this example, the yield of 1-hydroxycyclohexyl carboxylic acid was 87.24%, the purity was 97.46%, the purity of ammonium chloride was 99.42%, and the total yield of s...
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