Method for producing acrylate and method for recovering acrylic acid
A technology of acrylic ester and production method, applied in the field of production and use of acrylic ester, can solve problems such as being difficult to be perfected, and achieve the effects of easy recovery and excellent recovery efficiency
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Embodiment 1
[0167] 3000g of acrylic acid, 1470g of dipentaerythritol (hereinafter referred to as "DPET"), 70g of 78% sulfuric acid, 10g of hydroquinone (hereinafter referred to as "HQ") and 2450g of toluene were placed in a 10L reactor , under a pressure of 53 kPa, heated in an oil bath set at 100° C., and reacted for 10 hours while removing condensation water as azeotropic water with toluene. The weight of the reaction solution at this time was 6250 g.
[0168] After completion of the reaction, 3500 g of toluene was added. Next, after adding 325 g of pure water and stirring, it left still and separated into the upper layer (organic phase) and the lower layer (water phase). The lower layer (aqueous phase) was extracted from the reactor, and the upper layer (organic phase) was recovered.
[0169] After adding 1700 g of 20% sodium hydroxide aqueous solution to this upper layer (organic phase), it left still after stirring, and obtained the upper layer (organic phase) of 9000g and the lowe...
Embodiment 2
[0179] 78% sulfuric acid was slowly added to 300 g of the neutralized waste water obtained in Example 1 until the pH became 3. In addition, the temperature of the liquid at the time of sulfuric acid addition was maintained at 25 to 30°C. In addition, the added 78% sulfuric acid was 59.0 g.
[0180] Next, the liquid temperature was kept at 30 to 35°C and left to stand to separate into an upper layer (aqueous acrylic acid layer) and a lower layer (aqueous sodium sulfate layer).
[0181] The solution separated into two phases was transferred to a separatory funnel, and the lower layer (sodium sulfate aqueous solution layer) was extracted.
[0182] The obtained upper layer of the acrylic acid aqueous solution layer was 151.8 g, and the acrylic acid concentration was 37.4%, and 76.7% of acrylic acid could be recovered with respect to the acrylic acid contained in the neutralized waste water.
Embodiment 3
[0184] 98% sulfuric acid was slowly added to 300 g of the neutralized wastewater obtained in Example 1 until the pH became 2. In addition, the temperature of the liquid at the time of sulfuric acid addition was maintained at 25 to 30°C. In addition, the added 98% sulfuric acid was 52.1 g.
[0185] Next, the liquid temperature was kept at 30 to 35°C and left to stand to separate into an upper layer (aqueous acrylic acid layer) and a lower layer (aqueous sodium sulfate layer).
[0186] The solution separated into two phases was transferred to a separatory funnel, and the lower layer (sodium sulfate aqueous solution layer) was extracted.
[0187] The obtained upper layer of the acrylic acid aqueous solution layer was 128.4 g, and the acrylic acid concentration was 44.6%, and 77.4% of acrylic acid could be recovered with respect to the acrylic acid contained in the neutralized wastewater.
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