The esterification method is the core mainstream technology for the production of acetyl tributyl citrate (ATBC). In 2023, the domestic production capacity of this process will account for about 65%: anhydrous citric acid and butanol are used as raw materials, and sulfuric acid is used as a catalyst to perform an esterification reaction to produce crude tributyl citrate TBC. The crude tributyl citrate TBC is then acylated with acetic anhydride to become acetyl tributyl citrate (ATBC). Waste treatment is included.
1. Esterification reaction: Butanol is pumped into the esterification kettle through the butanol tank or feeding kettle, and citric acid monohydrate is pumped into the esterification kettle through the feeding kettle. During this process, the feeding kettle will produce waste gas butanol. After the feeding is completed, transfer the material to the esterification kettle, add the catalyst sulfuric acid, use steam to raise the temperature, and control the reaction temperature to 120-160°C until the esterification is completed.
2. Vacuum dealcoholization: It is completed in the alcohol water heater, esterification kettle reflux tower, condenser, and condenser. At the same time, most of the butanol in the generated water is removed by vacuum to the alcohol water evaporation tank. The separated butanol is then flowed out of the esterification kettle and used for the next batch of production. The separated water is reused in the water washing and neutralization process.
3. Acylation and deacidification: During production, the ATBC crude ester is cooled to 60-80°C, acetic anhydride is added to vinegar, and after acylation, acetic acid is removed with a vacuum pump and transferred to the acid tank. The acylation process will produce waste gas. Acetic acid is stored in an acetic acid storage tank and delivered to an acetic acid recycling company. After the acetic acid is removed, the ATBC crude ester is transferred to the treatment tank for washing and neutralization.
4. Post-processing (washing and neutralization, stripping, washing, vacuum dehydration, filtration): ATBC is first washed with distilled water and washing wastewater in the alcohol evaporation tank in the treatment tank. After washing, the material is tested for acid value, and an appropriate amount of 20% liquid alkali is added to neutralize it for 1 hour. After standing for 1 hour, the wastewater is released from the bottom of the tank, and the waste oil is reused until it is washed and neutralized; after neutralization The temperature of the ATBC is raised to 100~140°C, and tap water from the tap water storage tank is added. During the stripping process, exhaust gas butanol and waste water are produced. After stripping, the finished product is washed with tap water storage tanks to produce washing waste water, which is temporarily stored in Wash the water storage tank and reuse it to the washing and neutralization process; after washing, the temperature of the finished product is raised to 100°C, and the water is removed by vacuum. After vacuum dehydration, activated carbon is added to cool it. After passing through the filter and bag filter, the product ATBC is produced.