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Crystallization process for producing photoinitiator and product thereof

A photo-initiator and process technology, applied in the field of photo-initiator production, can solve the problems of less temperature control in the cooling process, lack of control of the cooling process, poor storage performance, etc., to solve the problems of low hardness, high hardness and improved storage performance Effect

Pending Publication Date: 2022-04-08
TIANJIN JIURI NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing photoinitiator dissolution and crystallization process generally adopts heating and dissolving of the photoinitiator, and then directly cools and crystallizes at a low temperature to obtain a photoinitiator magma, that is, directly cooling and crystallizing through low-temperature frozen water or cold brine; its effect on the temperature of the cooling process Less control, the obtained crystals have the problems of low hardness, easy breakage, and poor storage performance;
[0004] CN104817443A discloses a synthesis process of benzoin dimethyl ether, comprising sending the filtrate into a crystallization kettle for cooling and crystallization for 3 hours to obtain a wet fine product, which is dried by filtering, washing and drying three-in-one equipment to obtain a finished product; CN211226974U a light Initiator purification equipment, which uses salt water to cool the photoinitiator solution, can cool down to below zero, and quickly cool and crystallize the solution; the above-mentioned processes all use direct cooling and crystallization, lack of control over the cooling process, and the resulting crystals all exist Corresponding defects above

Method used

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  • Crystallization process for producing photoinitiator and product thereof
  • Crystallization process for producing photoinitiator and product thereof
  • Crystallization process for producing photoinitiator and product thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0070] The present embodiment provides a kind of crystallization process that is used for photoinitiator production, specifically comprises:

[0071] (a) Prepare the solution: dissolve the photoinitiator 184 in petroleum ether to obtain a photoinitiator solution with an initial temperature of 50° C. and a concentration of 43.5 wt %;

[0072] (b) Pre-cooling: Transfer the photoinitiator solution in step (a) to the cooling crystallization kettle, control the cooling rate of 7°C / h to cool down to 28°C, and the difference between the preset temperature value and the crystallization temperature is 1°C;

[0073] (c) Adding seed crystals: adding a particle diameter of 60 mesh to 70 mesh seed crystals to the precooled solution in step (b), the added quality of the seed crystals is the same as that of the photoinitiator in the photoinitiator solution. The mass ratio is 1.6%;

[0074] (d) crystallization by cooling at a uniform rate: in the control step (c), the solution is cooled to ...

Embodiment 2

[0078] The only difference between the crystallization process in this example and Example 1 is that the seed crystal addition temperature is replaced by 29° C., and other parameters and conditions are exactly the same as in Example 1.

Embodiment 3

[0080] The only difference between the crystallization process in this example and Example 1 is that the seed crystal addition temperature is replaced by 30° C., and other parameters and conditions are exactly the same as in Example 1.

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Abstract

The invention relates to a crystallization process for photoinitiator production and a product thereof, and the crystallization process comprises the following steps: pre-cooling a photoinitiator solution to a preset temperature value, controlling the difference value between the preset temperature value and the graining temperature to be 0-5 DEG C, adding a seed crystal at the preset temperature, and then cooling and crystallizing at a constant speed to obtain a photoinitiator crystal, the obtained photoinitiator crystals are blocky in morphology, high in hardness, not prone to breakage, concentrated in crystal particle size distribution and large in particle size, and the mass ratio of the obtained crystals with the particle size distribution within the range of 10-30 meshes can reach 80% or above.

Description

technical field [0001] The invention belongs to the field of photoinitiator production, and relates to a crystallization process for photoinitiator production and products thereof. Background technique [0002] A photoinitiator is a class of compounds that can absorb energy of a certain wavelength in the ultraviolet or visible region to generate free radicals, cations, etc., thereby initiating monomer polymerization, crosslinking and curing; the preparation process of photoinitiators generally includes photoinitiator molecules Synthesis, solvent evaporation, and dissolution crystallization process; among them, the dissolution crystallization process is a key step in the production of photoinitiators, which has an important impact on the crystal structure and performance of photoinitiator products; [0003] The existing photoinitiator dissolution and crystallization process generally adopts heating and dissolving of the photoinitiator, and then directly cools and crystallizes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/81C07C49/83
Inventor 赵国锋张齐毛桂红程兵兵武锦鹏
Owner TIANJIN JIURI NEW MATERIALS CO LTD
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