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Crystallizing method of solid antioxidant

An antioxidant and crystallization technology, applied in the field of crystallization of solid antioxidants, can solve the problems of low concentration of antioxidants, difficult polymer particles, and uniform mixing, so as to improve product purity, control the number of crystal nuclei, and achieve uniform crystallization. Effect

Active Publication Date: 2014-07-30
SHANDONG LINYI SUNNY WEALTH CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the transportation process, if the transport truck is exposed to the scorching sun in summer, the temperature inside the cargo box is usually as high as 40-50 ° C. If the crystallization is finer and the number of stacked layers is large, it is easy to cause the product to be heated and compressed during transportation.
After agglomeration, the original crystal form is usually destroyed. Sometimes a bag forms a whole piece, which is difficult to crush evenly. The agglomerated product has the following disadvantages during use: First, the use process is troublesome. After agglomeration, usually A whole bag of product forms a large block, which is difficult to pour out from the packaging bag and cannot be used directly. It usually needs to be physically crushed or returned to the factory for processing, which increases product loss and processing costs; the second is the agglomerated antioxidant product Even if it is broken by physical force and external force, it is usually not uniform, and there are some blocks of different sizes, while polymer products are usually relatively uniform powder or uniform particles with a diameter of less than 5mm. After crushing, these antioxidant products are uneven in shape. , and the shape of the polymer product is too different, which makes it difficult to mix with the polymer particles evenly in the process of adding to the polymer product, and the concentration of antioxidants in some areas is too high, causing autoxidation, and the concentration of antioxidants in some areas is too high Low, can not achieve the desired antioxidant effect, thus resulting in the overall antioxidant effect being affected
[0006] At present, there is no literature report on the method of improving the crystal particle size of antioxidant products

Method used

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  • Crystallizing method of solid antioxidant
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a 500ml three-necked flask equipped with electric stirring, thermometer, vacuum control device, condenser, and cold trap, 60g (0.205mol) of 3,5-di-tert-butyl-4-hydroxyphenylpropionic acid methyl ester (3 , 5-methyl ester), 55 g (0.203 mol) octadecyl alcohol, 0.1 g of dibutyl tin oxide, adjust the vacuum to 50-100mmHg, heat up to 100-120°C, keep stirring, and keep the methanol generated during the reaction Aspirate and collect in a cold trap, keep the reaction under these conditions for about 2 hours, and then raise the temperature to 125-135°C, continuously extract the methanol generated during the reaction, and collect in the cold trap, and keep the reaction under these conditions for about 1 hour , Evacuate until the vacuum degree is less than 2mmHg to complete the reaction. Cool down to 60-70℃, add 300ml (239.28g) of methanol into the reaction flask, keep stirring, heat to boiling, dissolve for about 10 minutes to obtain a colorless and transparent mixed liquid, ke...

Embodiment 2

[0025] In a 500ml three-necked flask equipped with electric stirring, thermometer, vacuum control device, condenser, and cold trap, 60g (0.205mol) of 3,5-di-tert-butyl-4-hydroxyphenylpropionic acid methyl ester (3 , 5-methyl ester), 55 g (0.203 mol) octadecyl alcohol, 0.1 g of dibutyl tin oxide, adjust the vacuum to 50-100mmHg, heat up to 100-120°C, keep stirring, and keep the methanol generated during the reaction Aspirate and collect in a cold trap, keep the reaction under these conditions for about 2 hours, and then raise the temperature to 125-135°C, continuously extract the methanol generated during the reaction, and collect in the cold trap, and keep the reaction under these conditions for about 1 hour , To the vacuum degree less than 2mmHg or less to end the reaction. Cool down to 60-70°C, add 400ml (322.48g) of ethanol to the reaction flask, keep stirring, heat to boiling, dissolve for about 5 minutes to obtain a colorless and transparent mixed liquid, keep stirring, th...

Embodiment 3

[0027] In a 500ml three-necked flask equipped with electric stirring, thermometer, vacuum control device, condenser, and cold trap, 60g (0.205mol) of 3,5-di-tert-butyl-4-hydroxyphenylpropionic acid methyl ester (3 , 5-methyl ester), 55 g (0.203 mol) octadecyl alcohol, 0.1 g of dibutyl tin oxide, adjust the vacuum to 50-100mmHg, heat up to 100-120°C, keep stirring, and keep the methanol generated during the reaction Aspirate and collect in a cold trap, keep the reaction under these conditions for about 2 hours, and then raise the temperature to 125-135°C, continuously extract the methanol generated during the reaction, and collect in the cold trap, and keep the reaction under these conditions for about 1 hour , To the vacuum degree less than 2mmHg or less to end the reaction. Cool down to 60-70°C, add 150ml (117.77g) of isopropanol to the reaction flask, keep stirring, heat to boiling, dissolve for about 20 minutes to obtain a colorless and transparent mixed liquid, keep stirrin...

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Abstract

The invention provides a crystallizing method of a solid antioxidant. Abundant ultrafine crystal grains crystallized in the primary crystallization process are quickly dissolved by a twice quick slight heating method, and large crystal grains are reserved to continue growth in the secondary crystallization process, so that the product crystals can grow bigger and more uniform. The anticaking capacity of the product is greatly enhanced; and meanwhile, since the crystals are more uniform and do not contain abundant fine powder, the subsequent spin-drying can be ensured, and other impurities can be washed out more easily in the washing process, thereby obtaining the product with higher purity.

Description

Technical field [0001] The invention relates to a crystallization method in the production process of solid organic chemical substances, in particular to a crystallization method of a solid antioxidant. [0002] More specifically, the present invention relates to a method for crystallization of the antioxidant β-(3,5-di-tert-butyl-4-hydroxyphenyl) n-stearyl propionate. Background technique [0003] Antioxidant is an indispensable additive in polymer production and processing. If there is no antioxidant, the polymer will be oxidatively degraded during processing and will age quickly during use. Antioxidants can not only help polymers overcome the above problems, but also enable polymer products to obtain excellent physical and mechanical properties. The antioxidant β-(3,5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate is a very important hindered phenolic primary antioxidant with a three-dimensional structure. Hindered phenolic antioxidant. Tests show that the antioxidant β...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/732C07C67/52
Inventor 冯上体付建英郭德宝
Owner SHANDONG LINYI SUNNY WEALTH CHEM CO LTD
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