The method of obtaining 2,6-directrories stabilizer

 

(57) Abstract:

The inventive Product-2,6-ditertbutyl stabilizer BF C73HIO8O12Sopl.114 - 115oWith the transmission in 425/500 nm (%) - 96,4/99,0 other Reagent 1: -(3,5-ditretbutyl-4 oksifenil)-propionic acid. Reagent 2: a mixture of polyoxypropyleneglycol ethers n-butyl alcohol mol. m 4300 - 4400. Reaction conditions: after crystallization, the product is treated with 20 - 30 wt.h. b -(3,5-ditretbutyl-4 oksifenil)-propionic acid and 0.2 - 0.3 wt.h. the mixture polypropyleneglycol ethers n-butyl alcohol. table 1.

The invention relates to organic chemistry, specifically to a method for producing 2,6-directrories stabilizer (pentaerithrityl-[-(3,5-ditretbutyl-4 oksifenil)] -propionate), which can find application in the polymer industry and agriculture.

A method of obtaining 2,6-directrories stabilizer polymer pentaerithrityl-[-(3,5-ditretbutyl-4 oksifenil)]-propionate by transesterification of methyl--(3,5-ditretbutyl-4 oksifenil)-propionate with pentaerythritol, after which the reaction mass is treated with cyclohexane, filtered and vikrita the relocation of 100-200 mm RT.article Get the target product with so pl. 110-125aboutC, pH of water extract 6-8,5, the transmittance of 85-90% at wavelengths of 425-500 nm, respectively.

The disadvantages of this method are the low yield of the target product; the low quality of the target product; the duration of the process.

The purpose of the invention increase the yield and quality of the target product, the intensification of the process.

This is achieved by a method of obtaining 2,6-directrories stabilizer polymer pentaerithrityl [ -(3,5-ditretbutyl-4 oksifenil)]-propionate lies in the transesterification of methyl -(3,5-ditretbutyl-4 oksifenil)-propionate with pentaerythritol, after which the resulting reaction mass is treated with cyclohexane or isopropyl alcohol, filtered and vykristallizovyvalas upon cooling the resulting adduct, which is subjected to recrystallization from petrol or 87,4 wt. isopropyl alcohol, after which the product is further treated 20-30 wt.h. -(3,5-ditretbutyl-4 oksifenil)-propionic acid and 0.2-0.3 wt.h. the mixture polyoxypropylene ethers N-butyl alcohol mol.m. 4300-4400, with subsequent recrystallization conduct of gasoline or 87,4 wt. isopropyl alcohol, and drying the product to an increase in the 110-130 min, then up to 60-80aboutWith over 110-130 min and up to 80-100aboutWith over 110-130 minutes

Distinctive features is that after recrystallization from petrol or 87,4 wt. isopropyl alcohol product is further treated 20-30 wt. h -(3,5-ditretbutyl-4 oksifenil)-propionic acid and 0.2-0.3 wt.h. the mixture polyoxypropylene ethers N-butyl alcohol mol.m. 4300-4400, with subsequent recrystallization conduct of gasoline or 87,4 wt. isopropyl alcohol, and drying of the product is carried out at a residual pressure of 100-300 mm RT. Art. and speed rise temperature first 40-60aboutWith over 110-130 min, then up to 60-80aboutWith over 110-130 min, and up to 80-100aboutWith over 110-130 minutes

If treating the reaction mixture with a mixture polyoxypropyleneglycol ether N-butyl alcohol mol.m. 4300-4400, taken in an amount less than the lower limits, it increases the number of dropouts increases dusting and drying, and if you handle the reaction mass is taken more than the upper boundary value, decreases the rate of light transmission.

If you handle the reaction mass -(3,5-ditretbutyl-4 oksifenil)-propio new acid taken the duration, and if you handle the reaction mass is taken more than the upper boundary value, increases the melting temperature of the target product 4aboutWith against the standard.

Carrying out drying at a temperature less than the upper boundary value leads to an increase in the duration of the drying process that reduces the transmittance of the target product, and carrying out drying at a temperature greater than the upper limits to the reduction of light transmission and the melting temperature of the finished product due to partial resinification.

When conducting drying at Pleaveless than the lower boundary value of the quality improvement is not observed, and during the drying at the Pleavemore upper boundary value increases drying time, reduces the optical density and melting point.

If the duration of drying is less than the lower limits, it reduces the melting temperature and the rate of light transmission due to the increased moisture content of the product, and if the duration is more than the upper boundary value, then decreases the melting temperature decreases the transmittance increases the number of dropouts.

aboutTo stir for 10 h in the presence of an alkaline catalyst with removal of the reaction of methanol with the help of vacuum or by purging with an inert gas. From the reaction mixture after pre-dissolved in cyclohexane and the Department of purifying catalyst by filtration and crystallization extract the target product in the form of cyclohexane adduct, which is subjected to recrystallization from 250 cm3gasoline, filtered then added 0.25.h. the mixture polyoxypropyleneglycol ethers N-butyl alcohol mol.m. 4300-4400 and 25 wt.h. -(3,5-ditretbutyl-4-hydroxyphenyl)-Pro - pianoboy acid and dried with stirring, a stepwise increase of temperature and Pleave200 mm RT.article first at the 50aboutC for 2 h, then at 70aboutC for 2 h and at 90aboutC for 2 hours, after reaching the volatile content of 0.3% drying cease. Get the target product with so pl. 114,2aboutWith the transmission in 425/500 nm respectively equal 95,1/98,0, aqueous extract pH of 7.0, sifting in the sieve 1C is missing, the dusting is 1.5% Output 125.0 g, which in terms of the pentaerythritol is 81,22%

P R I m m e R 2. 168,9 wt.h. methyl -(3,5-ditretbutyl-4-hydroxyphenyl)-propionate and 17.8 wt.h. pentaerythritol is heated to T 120-155aboutWith, stir what RODEWAY inert gas. From the reaction mixture after pre-dissolved in 250 cm387,4 wt. isopropanol and separation of catalyst cleaning filtering extracts the target product by crystallization and filtration, which was recrystallized from 250 cm387,4 wt. isopropanol, filtered and added to 0.25 wt.h. the mixture polyoxypropyleneglycol ethers N-butyl alcohol (mol. m 4300-4400 and 25 wt.h. -(3,5-ditretbutyl-4-hydroxyphenyl)-propionic acid and dried with stirring, a stepwise increase of temperature and Pleave200 mm RT.article first at the 50aboutC for 2 h, then at 70aboutC for 2 h and at 90aboutC for 2 hours, after reaching the volatile content of 0.3% drying cease. Get the target product with so pl. 114aboutWith the transmission in 425/500 nm respectively equal to 95.5/98,1, aqueous extract pH of 7.0, sifting sieve 1K is missing, the dusting is 1.5% Output 125,9 g, which in terms of pentaerythritol will be 81,80%

P R I m e R s 3 through 115 was carried out similarly to examples 1,2. The number of downloaded reagents and the results are shown in the table.

The proposed method can improve the yield of the target product by 24.8% (according to the proposed method 81,22% prototype is 56.4%); improving the quality of the target about the Chania at 425/500 nm, respectively 10-8% for the proposed method when 425/500 nm 95,0/98,0 respectively, and the prototype when 425/500 nm 85,0/90,0 respectively); the dusting of the target product is reduced by 10 times compared with the prototype; decreases the duration of the technological process 1.2 times.

The METHOD of OBTAINING 2,6-DIRECTRORIES STABILIZER polymer by transesterification of methyl - (3,5-ditretbutyl-4 oksifenil)-propionate with pentaerythritol, after which the resulting reaction mass is treated with cyclohexane or isopropyl alcohol, filtered and vykristallizovyvalas upon cooling the resulting adduct, which is subjected to recrystallization from petrol or isopropyl alcohol and dried, characterized in that, to improve yield and quality of the target product and process intensification, after recrystallization from petrol or 87,4 wt.% isopropyl alcohol product is further treated 20 to 30 wt.h. - (3,5-ditretbutyl-4 oksifenil)-propionic acid and 0.2 - 0.3 wt.h. the mixture polyoxypropylene ethers n-butyl alcohol mol.m. 4300 - 4400, with subsequent recrystallization conduct of gasoline or 87,4 wt.% isopropyl alcohol, and drying of the product is carried out at a residual pressure of 100 - 300 mm RT.article and step the temperature rises initially to 40 - 60oWith over 110 - 130 min, then to 60 - 80<

 

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