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Preparation method of UV770

A reactor, tetramethylpiperidol technology, applied in the preparation field of UV770, can solve problems such as unfavorable light stabilizer production efficiency, environmental pollution, etc., and achieve the effect of increasing collision frequency and improving efficiency

Active Publication Date: 2016-08-31
杭州欣阳精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, this process requires the participation of solvent oil, so at the end of the reaction, it is necessary to separate the solvent oil and the reaction product, which is not conducive to improving the production efficiency of the light stabilizer, and excessive use of solvent oil will also pollute the environment

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0021] A preparation method of UV770, comprising step 1: 2,2,6,6-tetramethylpiperidinol and sebacic acid Pass into the reaction tank with a molar ratio of 2.2:1 to 2.4:1 and use magnetic stirring to melt and mix; Step 2: Pass nitrogen into the reactor to protect the reaction, so that the pressure in the reactor is at a standard atmospheric pressure ; Step 3: Add 8% to 12% n-butyl titanate as the substrate into the reactor, and keep it warm for reaction; Step 4: After the reaction is completed, reduce the temperature of the reactant to 100°C to 110°C, and Filtration; step 5: cooling the filtrate to precipitate crystals, washing with water, further refining the crude product to obtain pure UV770 or directly obtaining the product by distilling off water.

[0022] Since the reaction process of 2,2,6,6-tetramethylpiperidinol and sebacic acid is theoretically consumed in a 2:1 manner, the 2,2,6,6-tetramethylpiperidinol and The molar ratio of sebacic acid is set to 2.2:1~2.4:1, m...

Embodiment 1

[0031]Pass 2,2,6,6-tetramethylpiperidinol and sebacic acid into the reaction tank at a molar ratio of 2.35:1 and stir 2,2,6,6-tetramethylpiperidinol and Sebacic acid, and continuously heated to 140 ° C to melt and mix them; at the same time, feed nitrogen into the reactor, empty the reactor, protect the reaction, and keep the pressure in the reactor at a standard atmospheric pressure state; then, in the reactor, add 8% n-butyl titanate as the substrate, and keep it warm for reaction, and release the gas in the reactor every 2 hours, and constantly replenish nitrogen; the reaction duration is 10 Hours, the conversion rate of sebacic acid in the reaction was 95.3%. After the reaction was completed, the temperature of the reactant was reduced to 110°C, and filtered while it was hot; or evaporation, directly obtain bis(2,2,6,6-tetramethyl-4-piperidinyl) sebacate with a purity of 99.1%.

Embodiment 2

[0033] Pass 2,2,6,6-tetramethylpiperidinol and sebacic acid into the reaction tank at a molar ratio of 2.35:1 and stir 2,2,6,6-tetramethylpiperidinol and Sebacic acid, and continuously heated to 220 ° C to melt and mix them; at the same time, feed nitrogen into the reactor, empty the reactor, protect the reaction, and keep the pressure in the reactor at a standard atmospheric pressure state; then, in the reactor, add 12% n-butyl titanate as the substrate, and keep it warm for reaction, and release the gas in the reactor every 2 hours, and constantly replenish nitrogen; the reaction duration is 8 Hours, the conversion rate of sebacic acid in the reaction was 97.4%. After the reaction was completed, the temperature of the reactant was reduced to 100°C, and filtered while it was hot; or evaporation, directly obtain bis(2,2,6,6-tetramethyl-4-piperidinyl) sebacate with a purity of 99.7%.

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Abstract

The invention relates to a preparation method of UV770. The preparation method comprises the following steps: (S1) adding (a) 2,2,6,6-tetramethylpiperidine alcohol with the formula shown in the specification and (b) sebacic acid with the formula shown in the specification into a reaction tank, and carrying out fusion mixing; (S2) introducing nitrogen to protect the reaction; (S3) adding titanium catalysts into the reactor, and carrying out thermal response reaction; (S4) cooling reactants to 100-110 DEG C after the reaction is finished, and immediately filtering; and (S5) cooling filtrate, separating out crystals, washing, and further refining rough products to obtain the purified product UV770, or evaporating water to directly obtain the product. The preparation method has the characteristics of high reaction efficiency and convenience in refining.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a preparation method of UV770. Background technique [0002] Due to its superior performance, hindered amine light stabilizers (HALS) have become the mainstream of the light stabilizer consumption market in synthetic material additives, and occupy a dominant position in the consumption structure of the light stabilizer market in the world. With the continuous deepening of basic research and applied research on light stabilizers, the application range of HALS has been continuously expanded. At present, the application of HALS has covered many fields such as agricultural film, engineering plastics, fibers, polymer coatings, artificial carpets and various outdoor plastic products. [0003] However, the existing preparation methods of hindered amine light stabilizers all use solvent oil to dissolve and mix the reaction raw materials to react. The preparation method of UV770 is to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/46
CPCC07D211/46
Inventor 周兴旺潘行平
Owner 杭州欣阳精细化工有限公司
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