A kind of process for producing photoinitiator 1173 and 184 cycle

A photoinitiator and production process technology, applied in chemical instruments and methods, preparation of carbon-based compounds, organic chemistry, etc., can solve the problems of restricting the use of chlorine gas, difficult to handle, large quantities, etc., to save freight costs and achieve good quality stability. , the effect of reducing risk

Active Publication Date: 2021-11-02
TIANJIN JIURI NEW MATERIALS CO LTD
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0004] And the wastewater generated in the whole process is sodium chloride solution. If the traditional double-effect or triple-effect evaporation salt production method is adopted, not only a large amount of investment in equipment and energy is required, but also the prepared by-product industrial salt Restricted by environmental protection laws and regulations, it is also difficult to handle and cannot achieve effective recycling
[0005] Chlorine gas, an important raw material used in the above-mentioned process, is a toxic gas and has certain corrosiveness. During production, strict requirements should be placed on pressure vessels and other equipment to prevent chlorine gas leakage. Therefore, chlorine gas transportation and storage are not safe. , such as the United States, Germany, Japan and other developed countries quite restrict the use of chlorine, especially Germany also prohibits the transportation of chlorine

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  • A kind of process for producing photoinitiator 1173 and 184 cycle
  • A kind of process for producing photoinitiator 1173 and 184 cycle

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The electrolysis of embodiment 1 photoinitiator 1173 waste water

[0036] 1. Pretreatment of sodium chloride solution produced in 1173 alkaline hydrolysis process

[0037] Take 2500.0g of the 1173 alkali hydrolysis sodium chloride solution that has been settled in the production workshop, and detect the sodium chloride content is 23.1%, and add 50.2g of 30% hydrochloric acid dropwise under stirring, and the pH value is 2-3. Add 40g of powdered activated carbon (400 mesh), and stir for 0.5 hours at 40°C. Activated carbon was removed by filtration under reduced pressure to obtain a colorless, clear and transparent solution with a COD value of 499 mg / L.

[0038] 2. Electrolysis of sodium chloride solution

[0039] Install and fix the anode, cathode and cation exchange membrane of the electrolytic cell. Take 2000.0 g of alkali hydrolysis sodium chloride solution after step 1 pretreatment, then preheat to 80-85 ° C, transfer to the anode chamber of the electrolytic cell, ...

Embodiment 2

[0042] The electrolysis of embodiment 2 photoinitiator 184 wastewater solutions

[0043] 1. Pretreatment of sodium chloride solution produced in the 184 alkaline hydrolysis process

[0044] Take 2500.0g of the 184 alkali hydrolysis sodium chloride solution that has been settled in the production workshop, detect the sodium chloride content of 22.5%, add 45.7g of 30% hydrochloric acid dropwise, and the pH value is 3. Add 45g of powdered activated carbon (400 mesh) and stir for 0.5 hours. Activated carbon was removed by filtration under reduced pressure to obtain a colorless, clear and transparent solution with a COD value of 425 mg / L.

[0045] 2. Electrolysis of sodium chloride solution

[0046] Install and fix the anode, cathode and cation exchange membrane of the electrolytic cell. Take 2000.0 g of alkali hydrolysis sodium chloride solution after step 1 pretreatment, then preheat to 80-85 ° C, transfer to the anode chamber of the electrolytic cell, and put 5% sodium hydrox...

Embodiment 3

[0049] The preparation of embodiment 3 photoinitiator 1173

[0050] 1. Chlorination reaction: put 100g of cuminone into a 500mL four-necked bottle, and start stirring. Feed in the chlorine gas that has been dried in step 1 or step 2. Keep the temperature of the material in the bottle at 40-45°C during the process of passing chlorine. After passing chlorine for about 10 hours, the material in the bottle began to turn yellow. Sampling was carried out for gas phase detection, and the remaining 0.12% of cuminyl ketone, the content of the product 2-chloro-2methyl-1-phenylacetone was 99.2%, and the reaction was completed.

[0051]2. Alkaline hydrolysis reaction: Put 100 g of 2-chloro-2-methyl-1-phenylacetone prepared above into a 500 mL four-necked bottle. Start stirring, and then dropwise add 100 g of 27.4% lye produced by electrolysis in the four-necked bottle. During the dropping process, the temperature of the reaction solution was controlled at 70-75°C. After adding the ly...

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Abstract

The invention relates to a technology for recycling process waste water containing sodium chloride of photoinitiator 1173 / 184. On the one hand, the high-salt wastewater generated during the preparation of photoinitiator 1173 / 184 has been effectively treated, which solves the huge environmental pressure, and can turn waste into treasure, transform it into reaction raw materials, and recycle resources; on the other hand, it is relatively The traditional chlor-alkali industry simplifies the post-treatment process of chlorine gas and sodium hydroxide, achieves the purpose of resource recycling, is environmentally friendly and meets the requirements of green chemistry, and at the same time reduces production costs.

Description

technical field [0001] The invention relates to a technology for recycling process waste water containing sodium chloride of photoinitiator 1173 / 184. Background technique [0002] UV curing initiators 1173 and 184 have similar production process conditions. All need to adopt the hydrogen atom that first passes into chlorine gas to replace carbonyl α-position carbon atom, generates chloride. Then the chloride reacts with sodium hydroxide, and finally the hydroxyl group replaces the chlorine atom in the reaction process. Specific process routes such as figure 1 . [0003] From figure 1 The process route shows that during the chlorination step, one chlorine atom in the chlorine molecule replaces the hydrogen atom on the α-position carbon atom, and the other one chlorine atom generates hydrogen chloride molecules. Hydrogen chloride is absorbed by sodium hydroxide solution to finally generate sodium chloride solution. During the alkaline hydrolysis step, sodium hydroxide re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/63C07C49/813C07C49/80C07C45/64C07C49/82C07C49/83C25B1/34
CPCC07C45/63C07C45/64C07C49/80C07C49/813C07C49/82C07C49/83C25B1/34
Inventor 罗想赵建新敖文亮吴吉蒋雷何昶钱林张齐
Owner TIANJIN JIURI NEW MATERIALS CO LTD
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