Novel high pressure alkali fusion production process for H acid

Abstract

The present invention relates to a novel technology of producing high pressure alkali fusion of H acid, and belongs to the technical field of production of high pressure alkali fusion of H acid. In the technology, liquid alkali with a concentration of 75 percent and T acid solution of 20 percent are mixed in a caustic fusion pot according to a mass ratio from 1 to 4 to 1 to 5; dehydration is performed at the temperature between 80 DEG C and 120 DEG C and lasts for 3 to 5 hours; solvent with a mass ratio from 1 to 0.1 to 1 to 0.3 with the T acid is added into the caustic fusion pot at a uniform velocity; the temperature in the caustic fusion pot is raised to be between 150 DEG C and 180 DEG C; the pressure in the pot is raised to be between 2.0 MPa and 3.0 MPa, the temperature and the pressure are maintained for 1 hour, H acid suspended substance can be generated in the reaction, and the finished product H acid can be acquired after filtration and drying processed. The present invention has the advantages that the content of alkali fused substance HPLC is improved from original 74 percent to 86 percent, the finished product quality is greatly improved, the value of amino group is more than or equal to 86 percent, the content of the HPLC is more than or equal to 97 percent, the content of T acid is less than or equal to o.5 percent, the content of chromotropic acid is less than or equal to 1.5 percent, and the reaction in the technology is stable.

Description

Technical field: [0001] The invention relates to a new high-pressure alkali fusion production process of H acid, which belongs to the field of high-pressure alkali fusion production process of H acid. Background technique: [0002] H acid is a special intermediate for the manufacture of dyes, widely used in printing and dyeing, textile, chemical and other industries. In the usual H acid-alkali fusion production process in the reactor, the viscosity of T acid and NaOH after dehydration is extremely high. When the reaction is closed under this condition, the reaction pressure is 0.5-1.0Mpa, because the reaction is required at low pressure. The temperature must be above 210°C. Excessively high reaction temperature will cause some by-products to be produced. At the same time, due to the extremely viscous material, the reaction will be partially unbalanced. Therefore the yield that adopts this method to produce is below 75%, and the content of by-product is higher simultaneously...

AI Technical Summary

Problems solved by technology

In the usual H acid-alkali fusion production process in the reactor, the viscosity of T acid and NaOH after dehydration is extremely high. When the reaction is closed under this condition, the reaction pressure is 0.5-1.0Mpa, because the reaction is required at low pressure. The temperature must be above 210°C. Excessively high reaction temperature will cause some by-products to be produced. At the same time, due to the extremely viscous material, the reaction will be partially unbalanced.

Therefore the yield that adopts this method to produce is below 75%, in addition the content of by-product is higher simultaneously, especially the chromatographic content of chromotropic acid is up to more than 10%, and these by-products can have a strong impact on the quality and the yield of final product H acid product