前苏联专利SU795451A3 Method of preparing neopentylglycol

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公开号:SU795451A3
申请号:SU792777153
申请日:1979-06-20
公开日:1981-01-07
发明作者:Цур Хаузен Манфред；Кауфхольд Манфред；Ланге Эрхард
申请人:Хемише Верке Хюльс Аг (Фирма)；
IPC主号:

专利说明:

(5) METHOD FOR PRODUCING NEOPENTYLE GLYCOL
one
The invention relates to an improved method for the preparation of neopentyl glycol, which is used in the manufacture of plasticizers and other products of organic synthesis.
A known method of producing neopentyl glycol by reacting isobutyraldehyde with formaldehyde in the presence of a basic catalyst, separating the aqueous phase from the resulting reaction mixture, adding alcohol to the resulting reaction mixture with subsequent gas-phase hydrogenation in the presence of cobalt, copper or nickel catalyst and isolating the desired product ij. You get a 97.8-99% conversion of oxypivaline aldehyde, the selectivity of the process, about.
The disadvantage of this method is the high energy costs caused by the need to evaporate the reaction mixture and solvent to be hydrogenated.
The closest to the essentially proposed method is that none of neopentyl glycol will be obtained, concluded that the isobutyraldehyde, taken in excess, is reacted
with formaldehyde in a water-soluble alcohol and in the presence of a basic catalyst, followed by separation of the aqueous phase, then the alcohol and
unreacted isobutyraldehyde is distilled from the resulting reaction mixture, and the resulting hydroxybenyl aldehyde is extracted from the distillation residue, which is subjected to
liquid-phase hydrogenation at a temperature of 175-220 ° C and under pressure, in the presence of a catalyst activated by barium containing copper and chromium catalyst and the selection of the target
pj product
The disadvantage of this method is low: yield, reaching a maximum of 84% (based on the formaldehyde used).
The aim of the invention is to increase the yield of the target product.
The goal is achieved by the method of obtaining neopentyl glycol,
wherein the liquid-phase hydrogenation is carried out in two stages, and in the first stage the process is carried out at a temperature of 120-160 ° C and the second at a temperature of 170-200 ° C with a load on both stages 0.05-1.0 l
product to be hydrogenated / l. catcher. hour.
It is advisable to carry out each stage of heating for 1-20 hours. This provides an increase in the yield of the target product and its purity up to 99%. The hydrogenation process is expediently carried out in the presence of 3-8% water (this amount is established by saturating the organic phase with water).
Example. The reaction of isobutyraldehyde with formaldehyde is carried out in a reactor having an effective volume of 10 liters. 16 l of isobutyryldehyde and 8 l of formalin (29% aqueous solution) are used every hour. The pH is adjusted to 10.0 and automatically adjusted by the addition of 25% sodium hydroxide. Reaction temperature The iodine phase is separated from the resulting reaction mixture.
19.7 kg of reaction mixture containing 7.9 kg of crude oxypivalnaldehyde are obtained per hour. The product has the following composition (calculated without content of isobutyraldehyde, formaldehyde and water),%:
Oxypivalnaldehyde 65,6 Neopentyl glycol (NPG) 8.3 Acetal from isobutyraldehyde and NPG1,4 Monoisobutyric acid ester NPG6.5 NPG-ester monohydroxypivalic acid 7.2,2,4-Trimethylpentadiol-1, 3 (-MPH) 2, 8 TMP monoisobutyrate 0.2 Other compounds 8.0 Additionally, the water content is 4.85%. The mixture of isobutyraldehyde and oxypivaline aldehyde is subjected to hydrogenation in a high pressure reactor (length 5 m; diameter 90 mm). Which is filled with 24 liters of a copper-chromite catalyst activated by barium, of the following composition,%: 33 CuO, 38, 10 BaO, the rest S t 0 ( .IIO .T company HAfiSHAW), At 1 h served 7. l containing iEobutyraldehyde reaction mixture, i.e. load is 0.292 L of product to be hydrogenated / L of catalyst, h.
The hydrogenation process is carried out at 280 atm of hydrogen pressure at the first stage and 170 ° C and 280 atm of hydrogen pressure at the second stage, and the duration of the process at each stage is approximately 60 minutes, 200 cm / h of circulating gas and 5 fresh gas
7 L / h of the hydrogenation product is obtained, which is dispersed under vacuum, and distilled off. In this case, 3.31 kg (99.9%, based on the formaldehyde used) of neopentyl glycol are obtained, because
146-148C / 124 mm Hg, so pl. 130®С that corresponds to degree of purity over 99%.
EXAMPLE 2 Example 1 is repeated, but the hydrogenation process is carried out on the 5th and second stages at a temperature of 180, 190 and the load on both stages is 0.05 l of the product to be hydrogenated / liter of catalyst. The output is neopentylglycol with so pl. d is 99.8; 97.5 and 93.2% (based on the formaldehyde used).
EXAMPLE 3 Example 1 is repeated, but the hydrogenation process in both f steps is carried out with a load of 1.0 liter of product to be hydrogenated / liter of catalyst. The yield is neopentyl glycol with mp. 129 ° C is 98.5%, based on the formaldehyde used.
PRI me R 4. Similarly applicable. 0 py 1, but the hydrogenation process in the first stage is carried out at a temperature of 120 s. The output neopentylglycol with so pl. 130-s is 94.5%, based on the formaldehyde used.
Example 5. Example 1 is repeated, but the first stage hydrogenation process is carried out at a temperature
Q .180 ° C and the second - at a temperature. The output neopentylglycol with so pl. 129c is 94.6%, based on the formaldehyde used;
Example 5, Example 1 is repeated, but the hydrogenation process in the first stage is carried out at a temperature and at a load of 0.04 L of product to be hydrogenated / L of catalyst-h in both steps. The yield neo0 pentylglycol with so pl. 12 bs (degree of frequency of approximately 98%) is 88.4% (based on the formaldehyde used),
Example 7. Similarly, the reactor and the hydrogenation process are carried out at the first stage at a temperature and at the second stage at a temperature of 210 C. At the same time, the output of neopentyl glycol with mp. (degree of purity
0% (98%) is 84.6% based on the formaldehyde used.
EXAMPLE 8 Example 1 is repeated, but the hydrogenation process in both stages is carried out under a load of 1.2 l -f hydrogenated product / l catalyst .4. At the same time, the output of neopentyl glyco-l with so pl. (purity approximately 98%) is 87.4%, based on formaldehyde.

权利要求:
Claims (2)
[1]
1.Is laid out for Germany
No. 2054601, Cl, il2o5 / 03, 1972,
[2]
2. Published in Germany
No. 1804984 Cl. 12/5/03, 1969 roto type I i

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法律状态:

优先权:

申请号 | 申请日 | 专利标题

DE19782827795|DE2827795A1|1978-06-24|1978-06-24|METHOD FOR PRODUCING PURE NEOPENTYL GLYCOL|

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