Succinic acid
Succinic Acid
disodium succinate
Succinic Acid
Succinic acid
disodium succinate
Phthalocyanine pigment
Succinic Acid
Compound dyes
Compound green
Composite blue
Production of a Succinic Ester Mixture of the Invention in succinic acid(cas:110-15-6)
Release time:2016/8/19 16:48:26

Production of a Succinic Ester Mixture of the Invention in succinic acid. Synthesis of the succinic ester mixtures (succinates) by esterification of succinic acid(cas:110-15-6) with two monohydric alkyl alcohols:

151 g of succinic acid(cas:110-15-6), 230 g of 1-octanol, and 283 g of 1-decanol were used as initial charge in a nitrogen-gas-inertized 1 l multinecked round-bottomed flask with water separator and reflux condenser, internal thermometer, and stirrer. 1-octanol was charged to the water separator. After addition of 0.3 g of tetrabutyl titanate, the mixture was heated to reflux, with stirring, and resultant water of reaction was removed from the system. The course of the reaction was monitored by means of titration [acid number] and water separation. Once an acid number smaller than or equal to 1 had been reached, the reaction was terminated. After modification of the apparatus, the excess of alcohol was removed by distillation in vacuo, starting at 20 mbar; the bottom temperature at the end of the distillation process was 185° C. After cooling, the catalyst was washed with water and aqueous sodium carbonate solution. The volatile constituents were then removed by distillation from the organic phase, starting at 120° C. and 20 mbar, and the performance of the mixture as plasticizer was tested. Yield of the ester mixture was 456 g (about 96%, based on n-octyl n-decyl succinate). Composition by GC area percent was: 22.8% di-n-octyl succinate, 50.4% n-octyl n-decyl succinate, 26.4% di-n-decyl succinate.

The comparative products di-n-octyl succinate and di-n-decyl succinate were produced in the same way.

Determination of Hardness:

Hardness was determined by homogenizing and gelling a plasticizer-containing PVC powder mixture on a two-roll mill; the compounded material was then pressed to give test sheets, and hardness was determined by Zwick Shore-hardness equipment. Hardness (Shore A) was measured on smooth and even test samples measuring 6 mm×40 mm×50 mm. Low Shore A hardness values mean relatively soft products and are a measure of the efficiency of the plasticizers.

A rod was used to mix 100 g of polyvinyl chloride (Vinnolit® S4170, Vinnolit GmbH & Co. KG, Germany) with 60 phr (parts per hundred resin) of plasticizer or plasticizer preparation and 3 phr of PVC stabilizer (Ca/Zn carboxylate) in a porcelain dish in such a way that the liquid constituents were absorbed well by the powder, rather than adhering to the vessel. The resultant powder mixture was charged in portions to the nip (0.7 mm) of a two-roll mill at 165° C. roll temperature, and homogenized and gelled. Once the milled sheet had formed, the nip was widened to 1 mm. The success of the mixing process was improved by frequent turning of the milled sheet. After 10 minutes of mixing time and processing time, the milled sheet was removed. After portioning, test samples measuring 6 mm×40 mm×50 mm were pressed. The temperature of the press was 170° C.; total press time was 10 minutes, including 7 minutes of heating phase with pressure100 bar. After cooling under pressure in a cooling press to at most 30° C., the test samples were demolded. The Shore A hardness of the test samples was determined by Zwick H04.3150 equipment in accordance with DLN 53505 at five different locations after, at the earliest, 24 hours of storage at 23° C., and the average value was recorded.

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