SU899548A1 - Process for producing triacetoneamine - Google Patents

Description

(54) METHOD FOR OBTAINING TRIACETONAMINE

I

The invention relates to a process for the preparation of triacetonamine, which can be used in the chemical industry, as a starting material in the synthesis of antioxidants, polymerization inhibitors, light stabilizers and stable iminoxyl radicals.

Known methods for the preparation of triacene tonamine are known, according to which the starting product of the reaction is an acetone condensation product, for example with ammonia, for example diacetone alcohol, frron, acetonin HP.

The disadvantage is the need for preliminary synthesis of the starting products.

The closest to the proposed method is the method of obtaining triacetonamine, namely, that acetone is condensed with ammonia in the presence of an acidic catalyst, for example, a salt of protic inorganic acid with ammonia, with

2

the ratio of acetone - ammonia, equal to or greater than 1.6: 1, for example, in the presence of solvents, for example alcohols, at. Removal of the target product per unit volume of the reactor does not exceed 0.05 kg / l h G23.

The disadvantage of this method is the low removal of the target product per unit volume of the reactor. In addition, the use of an acidic catalyst, including ammonium chloride, is associated with the use of corrosion-resistant equipment.

The purpose of the invention is to intensify the process, a method for producing triacetonamine, which consists in the fact that acetone is subjected to condensation with ammonia in the presence of a catalyst soy. H., I (OH),

where a is the number of boron atoms 1 or 2;

b is the number of nitrogen atoms 1 or 2;

C is the number of fluorine atoms 2-4;

d is the number of hydrogen atoms 2-8;

38995484

n 2-6; 2.4 g of mesityl oxide. The yield of triacem is 5-9; ammonia tonami is 97.5%. K is a coefficient equal to 0.35-3.5. Example 3. The process is carried out

In addition, the process is usually conducted analogously to example 1, the number

when the molar ratio of acetone - am-gammonia 2.6 g (molar ratio

Miak 10- (12: 1) at 70-100С. acetone - ammonia 10.9: 1) Receive

The process time is usually 24.2 g of triacetonamine (mp, 35 takes about 1 hour) and 2.5 g of mesityl oxide. Output

The side product of the reaction is ammonia triacetonamine 98.5%. mesityl oxide, representing 0- Example 4. The process is carried out

the valuable intermediate of organic syn is analogous to example 1, the amount of amteza ammonia is 2.0 g (the molar ratio of acetonum used in the process of catalysis – ammonia is 14.7: 1). Get 16.0 g

the torus is practically neutral triacetonamine (m.p. 35-36-C) and

and has a pH of 6.9-7.2. This property is 52, O g of mesityl oxide. The yield of triacetopatalyst makes possible the use of amine for ammonia of 83%. call for instrumentation Example 5. The process is carried out

The process is conventional carbon steel. Similarly to Example 1, the amount of amCatalyst is prepared by mixing 6 g of ammonia (the molar ratio of acetone components at 150-160 ° C under conditions of Qammonia 4.9: 1). Obtain 21.9 g of tri-incinerated ablation of ammonia from the system. Acetonamine (mp. 35-36 ° C) and 2.0 g

A.B heated reactionary co-oxide of mesityl. The output of triacetonamine court, equipped with a stirrer, refrigeration-ammonia 40%.

NIKOM to condense water vapor and you- Example 6. The process is carried out

its water and thermometer are loaded 25 as in example 1, the amount of am28, 5 g MNDG-I1F, 31 g of boric acid 8 g (molar ratio of acetone 46 g of glycerol (molar ratio ammonia 3.7: 1). Get 18 g triace1: 1:) , The reaction mixture is heated to a tamine (t. 35-36 0) and 1.8 g of oxide by stirring and withstand primesitil. The output of triacetonamine

150-160С within 0.5 H.jgammiak 24.8%.

B. The catalyst is prepared similarly to Example 7. The process is carried out.

out of 57 g of No. 1 dR HF, 31 g of boric acid is similar to Example 1, but is loaded

and 46 g of glycerin (molar ratio of 3.53 g of catalyst (B). Get

2: 1: 1) .26.1 g of triacetonamine (mp. 35-36 s)

B. Catalyst is prepared in a similar manner to 2.55 g of mesityl oxide. The output of triis 28.5 I4F F) 2 g of boric acid acetonamine ammonia 98.5%.

and 46 g of glycerol (molar ratio of Example 8. The process is carried out

1: 2: 1). Similarly to Example 1, but loading

The prepared catalyst has 3.35 g of catalyst (B). A pH of 6.9-7.2 is obtained. , d25,8 g of triacetonamine t. pl. 35 Example 1. A reactor is loaded with 36 ° C) and 2.45 g of mesityl oxide. Output

100 g of acetone; 2.9 g of ammonia (molleriacetonamine ammonia 97.6%. The ratio of acetone - ammonia 10:) and Example 9. The process is carried out

3.53 g of catalyst (A). similar to example 1, but load

The process is carried out for 1 h3.0 g of catalyst (molar ratio. From the reaction mixture, the distillation of MndR-HF — HjBO — ethylene gline unreacted acetone, col). Obtain 26.0 g of trisatum in a vacuum distills the mesontonamine oxide (mp 35-36 ° C) and 2.52 g

Tyla and triacetonamine. The remaining ka oxide mesityl. Triacetonamine yield

The catalyst mass is used for ammonia 98.5%. re-run. 26.0 g of triacetonamine are obtained (m.p., 35- Example 10. The process is carried out

36 ° C) and 2.63 g of mesityl oxide. Logical to the example, but load

ammonium triacetonamine 98.5% 2.52 g of catalyst (molar ratio Example 2. Process Conduct MHTPHR - HjBO ,, - glycerin as in Example 1, but loading 5 1: 1: 0.35). 25.9 g of triacetone2, 5 g of ammonia (molar ratio of amine (mp 35-36 ° C) and 2.61 g of oxide are obtained

acetone - ammonia 12: 1) Get 22,3 gmesitil. The output of triacetonamine

triacetonamine (t, pl. 35-36 s; iammoniak 98.0%.

Claims (3)

Claim 1. The method of producing triacetonamine 20 by condensation of acetone and ammonia in the presence of a catalyst containing a boron and fluorine compound, which, in order to intensify the process, is carried out in the presence of a catalyst of the composition B ^ N ^ FJl (OH) rw where a - number atoms boron 1 or 2; b - number atoms nitrogen 1 or 2; from - number atoms fluorine 2-4; d - number atoms hydrogen 2-8; η = 2-6; m = 3-9; TO - coefficient, equal to 0.35-3.5 2. Way according to claim 1, about t l and h a- Yu SC I th with i so that * lead the process at 70-100 ° C. Order 12052/30 and 2, about t · l that the process of weighting acetone pp. 1 topics 3. A method for extinguishing with a molar ammonia of 10-12: 1.