Device and method for continuously preparing high-purity AKD without solvent

A kind of method for continuous preparation of high purity AKD without solvent, wherein:

• the mentioned raw materials are tertiary amine and acyl chloride;
• the applied tertiary amine is:
• in the chemical equation (I), R1, R2 and R3 are C1˜C6 alkyl, alkenyl or cycloalkyl;
• the applied acyl chloride is:
• in the chemical equation (II), R is C8˜C22 alkyl or alkenyl;
• the adopted device includes a kind of reactor which could make continuous mixing reaction of raw materials;
• the reactor has the axially setup internal cylinder and external cylinder;
• under the operating state, the internal cylinder is driven by motor to rotate in relation to external cylinder to form an annular column passage between internal cylinder and external cylinder;
• the annular column passage is set with conveying section and mixing section along the axial direction and the conveying section and mixing section are arranged one after another along the axial direction of annular column passage;
• and the conveying section is set with blades to convey and mix the materials and the bottom of blades is fixed to the internal cylinder and the tip of blades is fitted with inner wall of external cylinder;
• the mixing section is set with shearing blades and kneading blades to shear and mix the materials;
• the shearing blade consists of supporting block and shearing rod;
• one end of supporting block is fixed on the internal cylinder and the other end is connected to the shearing rod;
• one side of shearing rod is fitted with inner wall of external cylinder;
• the kneading blade consists of support bar and kneading block;
• one end of support bar is fixed on the external cylinder and the other end is connected to kneading block;
• one side of kneading block is fitted with outer wall of internal cylinder, the above-mentioned reactor is set with one tertiary amine feeding port, 3-10 acyl chloride feeding ports and one outlet connecting the annular column passage;
• one tertiary amine feeding port and first acyl chloride feeding port are located at one end of axial direction of annular column passage in reactor, one outlet is located at the other end of axial direction of annular column passage and the other acyl chloride feeding ports are alternatively arranged along the axial direction of annular column passage from the first acyl chloride feeding port;
• the above-mentioned reactor has two sets of internal and external heat exchange systems, wherein the internal heat exchange system uses the wall of internal cylinder as heat exchange interface and it consists of pipeline, heat exchange medium and inner chamber of internal cylinder;
• the external heat exchange system uses the wall of external cylinder as heat exchange interface and it consists of pipeline, heat exchange medium and water jacket at outskirt of internal cylinder, wherein the preparation process includes;
• Step 1:
• Prepare the raw materials required for continuous feeding into reactor according to the mole ratio of 1.05˜1.2:1 between tertiary amine and acyl chloride within any unit time and feed the acyl chloride required for continuous feeding into reactor through three to ten lines and the feeding amount of acyl chloride in each line shall be 10˜60% of total feeding amount of acyl chloride within any unit time;
• Step 2:
• Use the metering pump to continuously feed the tertiary amine through the mentioned tertiary amine feeding port in reactor according to the requirement of Step 1 and use the metering pump to continuously feed the acyl chloride through the corresponding three to ten acyl chloride feeding ports in three to ten lines according to the requirement of Step 1;
• under the operating state of reactor, the main motor drives the internal cylinder to rotate in relation to external cylinder, forcing the fed materials to be conveyed and stirred by blades in the conveying section of annular column passage and forcing the fed materials to be sheared and mixed by relative movement of shearing blades and kneading blades at mixing section of annular column passage;
• due to multiple feedings of acyl chloride and alternate arrangement of conveying section and mixing section along the axial direction of annular column passage, it causes the sufficient dimerization reaction of fed materials and gradually moves the materials from feeding ports of reactor to outlet along the annular column passage;
• during the dimerization reaction process of materials, it uses two sets of internal and external heat exchange systems to control the temperature of materials inside the reactor between 50° C. and 100° C. and control the material viscosity in range of 1˜70 Pa·s;
• the duration period of materials inside the reactor is 5˜20 minutes until the reaction products are discharged continuously from outlet;
• Step 3:
• The reaction products discharged continuously from outlet of reactor fall to the continuous extractor;
• continuously feed diluted mineral acid solution to continuous extractor for dispersion with reaction products to get the extracted mixing solution, which is finally conveyed to settling basin for separation of oil phase and water phase;
• the oil phase on the top is molten AKD product and discharged from overflow port of settling basin and the water phase at the bottom is tertiary amine mineral acid solution and discharged from the lower port of settling basin.