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Method for preparing salicylonitrile by salicylamide continuous method

A technology of salicylamide and salicylonitrile, which is applied in the field of preparation of nitrile compounds, can solve the problems of increasing the difficulty of the separation and purification process, increasing the complexity of equipment, and low yield, so as to improve selectivity and yield and reduce reaction Energy consumption, effect of simplifying the separation process

Active Publication Date: 2021-04-13
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The temperature of the gasification furnace is 270°C, and the salicylamide in the furnace will inevitably undergo a thermal decomposition reaction to produce by-products; in addition, because salicylonitrile is solid at room temperature, the temperature of the pipeline needs to be controlled at 150°C, which increases the Complexity of equipment; the highest yield of final salicylonitrile is only 88.2%, low yield, and increases the difficulty of separation and purification process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The metal-doped supported boron phosphate catalyst comprises the following steps:

[0033] Add 20g of boric acid, 37.3g of phosphoric acid, 0.54g of telluric acid dihydrate, 1.2g of stearic acid and 140mL of water into the reactor in sequence, heat and stir evenly. Then 77.8 g of acidic silica sol with a silica content of 25% was added to the system. Heating and evaporating to dryness under stirring conditions until gelatinous, shaped after drying, and then calcined at 400° C. for 5 hours to obtain catalyst 1. The loading of boron phosphate is 67.3%, the content of tellurium is 0.5%, and the addition of stearic acid is 2%, to obtain the target catalyst.

[0034] Adopt above-mentioned catalyzer, prepare the method for salicylonitrile with salicylamide continuous method, operation steps are as follows:

[0035] Fill 10mL of Catalyst 1 in the fixed bed reactor, pass N 2 Preheat to 370°C. Preheat the benzonitrile solution of salicylamide with a concentration of 0.1g / mL ...

Embodiment 2

[0037] The metal-doped supported boron phosphate catalyst comprises the following steps:

[0038] Add 5g of boric acid, 9.3g of phosphoric acid, 0.18g of telluric acid dihydrate, 1.0g of hydroxymethylcellulose and 50mL of water into the reactor in sequence, heat and stir evenly. Then add 442.9g of ammonia type alkaline silica sol with silica content of 40% to the system. Heating and evaporating to dryness under stirring conditions until it was gelatinous, dried and shaped, and then calcined at 400° C. for 4 hours to obtain catalyst 2. The loading of boron phosphate is 5%, the content of tellurium is 0.1%, and the addition of stearic acid is 0.5%.

[0039] Adopt above-mentioned catalyzer, prepare the method for salicylonitrile with salicylamide continuous method, operation steps are as follows:

[0040] Fill 10mL catalyst 2 in the fixed-bed reactor, pass N 2 Preheat to 480°C. Preheat the benzonitrile solution of salicylamide with a concentration of 0.1g / mL and ammonia gas t...

Embodiment 3

[0042] The metal-doped supported boron phosphate catalyst comprises the following steps:

[0043] 20g of boric acid, 37.3g of phosphoric acid, 17.0g of aluminum nitrate nonahydrate, 1.3g of stearic acid and 140mL of water were successively added into the reactor, heated and stirred evenly. Then add 9.7g 3A molecular sieves to the system. Heating and evaporating to dryness under stirring conditions until gelatinous, shaped after drying, and then calcined at 300°C for 4 hours to obtain catalyst 3. The boron phosphate loading was 80%, the aluminum content was 5%, and the carboxymethyl cellulose addition was 5%.

[0044] Adopt above-mentioned catalyzer, prepare the method for salicylonitrile with salicylamide continuous method, operation steps are as follows:

[0045] Fill 10mL catalyst 3 in the fixed-bed reactor, pass through N 2 Preheat to 340°C. Preheat the p-xylene solution of salicylamide with a concentration of 1.1g / mL and ammonia gas to 150°C, and then pass it into the ...

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Abstract

The invention relates to a preparation method of nitrile compounds, in particular to a method for preparing salicylonitrile by a salicylamide continuous method. The technical key points are as follows: the method comprises the following operation steps: dissolving salicylamide in an organic solvent to form a solution, preheating the salicylamide solution, introducing the preheated salicylamide solution into a fixed bed reactor filled with a catalyst, reacting under a heating condition, cooling effluent steam, and collecting to obtain a solution of a salicylonitrile product. The salicylamide solution is prepared by dissolving salicylamide in the organic solvent, the defect that a salicylonitrile reaction system is prepared by adopting a melting mode in the prior art is overcome, the reaction energy consumption is effectively reduced, the selectivity and yield of a final product are improved by matching with the improvement of other preparation processes, and the method has industrial value.

Description

technical field [0001] The invention relates to a preparation method of nitrile compounds, in particular to a method for preparing salicylonitrile by a continuous salicylamide method. Background technique [0002] Salicylonitrile is an important chemical intermediate widely used in the synthesis and production of medicines, pesticides, spices and liquid crystal materials. Therefore, it is of great significance to provide a preparation method with higher selectivity and yield of salicylonitrile. [0003] In the prior art: patent FR2332261 describes a method using boron phosphate as a catalyst, but the raw material methyl salicylate will be converted into phenol, resulting in a decrease in the yield of salicylonitrile and increasing the difficulty of product purification. Patent CN102174002A discloses a method for synthesizing salicylonitrile from ammonium salicylate. The catalyst preparation process is complicated, there are many types of solvents, and the reaction time is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/20C07C255/53B01J27/18
CPCC07C253/20B01J27/1802B01J27/1808B01J37/036B01J37/082C07C255/53
Inventor 陈群何明阳周维友陈关虎孔臻极孙中华钱俊峰
Owner CHANGZHOU UNIV
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