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Preparation method of hindered amine light stabilizer 770

A technology of hindered amines and light stabilizers, which is applied in the field of preparation of hindered amine light stabilizers 770, which can solve the problems of unqualified light transmittance, unqualified light transmittance, and presence of carboxyl groups, etc., so as to facilitate large-scale production , low equipment requirements and cheap raw materials

Inactive Publication Date: 2014-08-13
新纶电子材料(常州)有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But in prior art, there will be following problems in the technique of direct esterification: the first, usually direct esterification reaction is difficult to esterify completely, and there will be carboxyl in the product; The 2nd, the carboxyl that exists in the product can cause the transparent Light rate failed
The light transmittance is unqualified, and it is unacceptable to the commercially available light stabilizer 770, so there is no literature report in the industry at home and abroad to use the direct esterification route to prepare this product

Method used

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  • Preparation method of hindered amine light stabilizer 770
  • Preparation method of hindered amine light stabilizer 770
  • Preparation method of hindered amine light stabilizer 770

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Embodiment 1

[0030] This embodiment provides a preparation method of hindered amine light stabilizer 770, specifically as follows:

[0031] In a 500ml four-neck flask equipped with a stirrer, a thermometer, and a reflux condenser, add 0.37mol (75.33g) of sebacic acid, 0.76mol (120.15g) of tetramethylpiperidinol, and 3.88g of dioctyltin oxide at room temperature and 213.5g of trimethylbenzene, slowly warming up to the reflux temperature under stirring, and keeping it at 170°C-175°C for 4h under reflux and water separation. During the reaction process, the reaction process is judged by GC analysis of the ratio of mono- and di-esters generated by the reaction, and the reaction is controlled to the end.

[0032] After the reaction, the solution was cooled to 80° C., the catalyst was removed by filtration, and trimethylbenzene was distilled off under reduced pressure. Add equal weight of petroleum ether and 3.5g of activated carbon to the remaining material, heat to 60°C-70°C and stir for 1h, ...

Embodiment 2

[0034] This embodiment provides a preparation method of hindered amine light stabilizer 770, specifically as follows:

[0035] In a 500ml four-neck flask equipped with a stirrer, a thermometer, and a reflux condenser, add 0.37mol (75.33g) of sebacic acid, 0.76mol (120.15g) of tetramethylpiperidinol, and 3.88g of dioctyltin oxide at room temperature and 213.5 g of trimethylbenzene, slowly warming up to the reflux temperature with stirring, and keeping at 175° C. for reflux and water separation reaction for 6 h. During the reaction process, the reaction process is judged by GC analysis of the ratio of mono- and di-esters generated by the reaction, and the reaction is controlled to the end.

[0036] After the reaction, the solution was cooled to 80° C., the catalyst was removed by filtration, and trimethylbenzene was distilled off under reduced pressure. Add equal weight of water and 3.5g of activated carbon to the remaining material, heat to 60°C-70°C and stir for 1h, then filt...

Embodiment 3

[0038] This embodiment provides a preparation method of hindered amine light stabilizer 770, specifically as follows:

[0039] In a 500ml four-neck flask equipped with a stirrer, a thermometer, and a reflux condenser, add 0.37mol (75.33g) of sebacic acid, 0.76mol (120.15g) of tetramethylpiperidinol, and 3.88g of stannous octoate at room temperature and 213.5 g of trimethylbenzene, slowly warming up to the reflux temperature with stirring, and keeping it at 170°C-175°C for 8h under reflux and water separation. During the reaction process, the reaction process is judged by GC analysis of the ratio of mono- and di-esters generated by the reaction, and the reaction is controlled to the end.

[0040] After the reaction, the solution was cooled to 80° C., the catalyst was removed by filtration, and trimethylbenzene was distilled off under reduced pressure. Add equal weight of petroleum ether and 3.5g of activated carbon to the remaining material, heat to 60°C-70°C and stir for 1h, ...

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Abstract

The invention provides a preparation method of a hindered amine light stabilizer 770. According to the method, sebacic acid and tetramethylpiperidinol as reactants and an oxide and / or organic compound of the fourth main group element tin as a catalyst are subjected to a heating refluxing reaction in a solvent to obtain the hindered amine light stabilizer 770. The invention uses sebacic acid as raw material instead of dimethyl sebacate, and the sebacic acid under the effect of an appropriate catalyst performs a direct esterification dehydration reaction with tetramethylpiperidinol; and appropriate technology conditions such as an appropriate proportion of raw materials, reaction temperature adjustment and suitable solvent are employed to solve the technical problems of low esterification rate and poor light transmittance of a final product in a common direct esterification reaction, and to prepare the light stabilizer 770 product in line with the requirements of market quality standards. Compared with the ester exchange method in the prior art, the method has the advanategs of cheap raw materials, higher yield, low requirements for equipment, simple process and easiness for scale production.

Description

technical field [0001] The invention relates to a preparation method of hindered amine light stabilizer 770, which belongs to the technical field of chemical synthesis. Background technique [0002] Hindered amine light stabilizers (HALS) have been a hot topic in the development and research of polymer stabilizers in the past 20 years. Due to the unique and excellent light protection performance of HALS itself, its efficiency is 2-3 times that of general traditional light stabilizers. At the same time, it has a good synergistic effect with UV absorbers, antioxidants and other additives, and does not color the resin. , low toxicity or non-toxic, so it is an additive with broad development prospects. According to statistics in 1996, the annual consumption of HALS in the world has accounted for 54% of the total consumption of light stabilizers in the world, and it is still growing at an annual rate of 8%. [0003] Light stabilizer 770 is a typical low molecular weight product...

Claims

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Application Information

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IPC IPC(8): C07D211/46
CPCC07D211/46
Inventor 刁建高王大保岳威
Owner 新纶电子材料(常州)有限公司
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