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Method of inhibiting acid regurgitation caused by plasticizer

A plasticizer and acid-returning technology, applied in the field of phthalate plasticizers, can solve problems such as product quality impact and restrict product quality, reduce raw material and energy consumption, improve wastewater conditions, and simple operation process Effect

Inactive Publication Date: 2007-08-22
山东宏信化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, this problem restricts the further improvement of product quality and has a great impact on subsequent processes and product quality. Therefore, it needs to be improved in industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] On the DBP device with an annual output of 30,000 tons, the reaction kettle is first evacuated, replaced with N2 twice, and then 9400kg of n-butanol, 6000kg of phthalic anhydride, 40kg of 98% concentrated sulfuric acid are added to the kettle, stirred, and slowly heated to reflux reaction, the temperature is 140°C, take a sample to measure the acid value after 6 hours of reaction, the acid value is 2.1mgKOH / g, cool the feed liquid to 80°C, and add 100kgNa 2 CO 3 Dissolve in 1000kg of water, heat up to 75°C, add to the ester solution, stir for 15 minutes, and let stand for 45 minutes. Take a sample to measure the acid value of 0.05mgKOH / g, and remove the bottom water layer. Then wash once with 1200kg of water to obtain 15 tons of crude ester. Add 1kg of sodium carbonate powder (0.5% of the crude ester weight) to the ester solution after washing and stir evenly, then dealcoholize and filter to obtain the finished product DBP, with a weight of 11010kg, a yield of 97.7%, ...

Embodiment 2

[0021] Except that the sodium carbonate powder amount that adds is 0.75kg, other operation and formula are completely identical with embodiment 1, and result DBP yield is 97.5%, and acidity is 0.003%, and waste water amount is 3249kg.

Embodiment 3

[0023] In the 30,000-ton DIBP plant, the reactor is first evacuated, and the N 2 Replaced twice, then added 9400kg of n-butanol, 5529kg of phthalic anhydride, 39kg of 98% concentrated sulfuric acid to the kettle, stirred and slowly heated to reflux at a temperature of 130°C, and took a sample to measure the acid value after 8 hours of reaction. The acid value was 2.3mgKOH / g, the feed liquid is cooled to 70°C, and 90kgNa 2 CO 3 Dissolve in 1000kg of water, heat up to 70°C, add to the ester solution, stir for 15 minutes, and let stand for 45 minutes. Take a sample to measure the acid value of 0.05mgKOH / g, and remove the bottom water layer. Then wash once with 1200kg of water to obtain 14 tons of crude ester. After washing with water, add 1.4 kg of sodium carbonate powder (1% of the weight of the crude ester) to the ester solution and stir evenly, then dealcoholize and filter to obtain the finished DIBP.

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Abstract

The present invention is method of inhibiting acid regurgitation caused by plasticizer, and belongs to the field of phthalic ester plasticizer technology. The phthalic ester plasticizer is prepared with phthalic anhydride and alcohol through reaction under the catalysis of sulfuric acid, and features that before decompressing dealcoholization, alkali powder of sodium carbonate, sodium bicarbonate, calcium bicarbonate or calcium carbonate in 50-100 ppm of coarse ester is added. The present invention can control acid regurgitation caused by plasticizer effectively.

Description

technical field [0001] The invention belongs to the technical field of phthalate plasticizers, in particular to a method for inhibiting acid reversion when dibutyl phthalate or diisobutyl phthalate is prepared. technical background [0002] Phthalate plasticizers are the most important varieties of industrial plasticizers, and their annual sales account for more than 80% of the total sales of plasticizers. They are the central variety series in the large-scale production of plasticizer industry. Most of the phthalate plasticizers have the advantages of wide applicability, good chemical stability, simple production process, cheap raw materials, low cost, and good compatibility with PVC. They are generally used as the main plasticizer use. [0003] Dibutyl phthalate (DBP) and isobutyl phthalate (DIBP) are a class of plasticizers that are widely used in the plastics industry and a large amount of consumption, and the preparation method of the prior art mainly exists in the pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/12C07C67/48C07C69/80
Inventor 王恺卢瑞荣赵增娣魏海燕任国勇毕小明
Owner 山东宏信化工股份有限公司
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