Preparation method for sodium saccharin
A technology of sodium saccharin and heating conditions, applied in the direction of organic chemistry, etc., can solve the problems of high production cost and environmental protection cost of saccharin sodium, affect production efficiency, and excessive three wastes, etc., achieve good economic value, low production cost and environmental protection cost, and three wastes little effect
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Embodiment 1
[0021] A kind of preparation method of sodium saccharin, concrete steps are as follows:
[0022] 1. Ammonification:
[0023] (1) Add 3800 g of toluene solution of o-methoxycarbonylbenzenesulfonyl chloride to a 5000 mL four-neck flask with mechanical stirring, thermometer and reflux condenser, and heat to 60 degrees;
[0024] (2) feed ammonia in the system, TLC monitors the progress of the reaction, until most of the o-methoxycarbonylbenzenesulfonyl chloride reacts completely, stop feeding ammonia, down to room temperature;
[0025] (3) suction filtration, the filtrate contains a small amount of o-methoxycarbonylbenzenesulfonyl chloride, and the filtrate can be used for the extraction of o-methoxycarbonylbenzenesulfinic acid chloride to prepare o-methoxycarbonylbenzenesulfinic acid chloride process. The filter cake was washed with water (1000 mL*2), suction filtered, and dried to obtain 1220 g of o-methoxycarbonylbenzenesulfonamide.
[0026] 2. Preparation of sodium saccharin...
Embodiment 2
[0033] A kind of preparation method of sodium saccharin, concrete steps are as follows:
[0034] 1, ammoniation: (same as embodiment 1).
[0035] 2. Preparation of sodium saccharin by ring closure:
[0036] (1) In a 1000mL there-necked flask with mechanical stirring, thermometer, and reflux condenser, add the filtrate (392g) that Example 1 has reacted;
[0037] (2) heating to 60 degrees, then adding sodium carbonate and o-methoxycarbonylbenzenesulfonamide in batches in the system;
[0038] (3) Sodium carbonate (8g) and o-methoxycarbonylbenzenesulfonamide (32g) are added to the system each time, and the next batch is added until the system is saturated after the system is clarified, and an appropriate amount of water is added to clarify the system;
[0039] (4) O-methoxycarbonylbenzenesulfonamide (320 g, 1.49 mol) and sodium carbonate (80 g, 0.75 mol) were added in total, and 24 g of water was added.
[0040] (5) Cool down to room temperature, suction filter, and the filtrat...
Embodiment 3
[0042] A kind of preparation method of sodium saccharin, concrete steps are as follows:
[0043] 1, ammoniation: (same as embodiment 1).
[0044] 2. Preparation of sodium saccharin by ring closure:
[0045] (1) add the filtrate (481g) that embodiment two has reacted in the 1000mL there-necked flask that has mechanical stirring, thermometer, reflux condenser one by one;
[0046] (2) heating to 60 degrees, then adding sodium carbonate and o-methoxycarbonylbenzenesulfonamide in batches in the system;
[0047] (3) Add sodium carbonate (8g) and o-methoxycarbonylbenzenesulfonamide (32g) to the system each time. After the system is clarified, add the next batch of reactants until the system is saturated. Add an appropriate amount of water to clarify the system ;
[0048] (4) O-methoxycarbonylbenzenesulfonamide (256 g, 1.2 mol) and sodium carbonate (64 g, 0.6 mol) were added in total, and 40 g of water was added.
[0049] (5) Cool down to room temperature, suction filter, and the ...
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