Process for preparing high-purity molecular distillation monoacylglycerol

A molecular distillation and monoglyceride technology, which is applied in the direction of fat oil/fat refining, fat production, fatty acid esterification, etc., can solve the problems of equipment loss, poor economic benefits, high energy consumption, etc., to reduce emissions and reduce environmental protection costs , the effect of improving economic efficiency

Inactive Publication Date: 2013-01-16
NANCHANG UNIV
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AI-Extracted Technical Summary

Problems solved by technology

[0007] The main disadvantages of the existing molecular distillation monoglyceride production process are: (1) The transesterification reaction is an equilibrium reaction, and due to the poor solubility of glycerol in hydrogenated oil, the monoglyceride content in the crude product is only 35-40%, which is very low. Difficult to break through 60%
On this basis, using molecular distillation to obtain high-purity (>95%) monoglycerides generally requires 3 tons of 40% monoglyceride raw materials to obtain 1 ton of high-purity monoglycerides. The distillation device requires ultra-high vacuum (1~0.5Pa), consumes a lot of energy (about 200°C...
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Abstract

The invention relates to a process for synthesizing high-purity molecular distillation monoacylglycerol. The process comprises the following steps of: (1) mixing glycerol and a catalyst A, vacuumizing, stirring for heating, adding hydrogenated oil added with a catalyst B into a reaction system in batches to perform ester exchange reaction, after the ester exchange reaction is finished, keeping temperature, adding phosphoric acid for neutralizing, cooling and standing a reactant for demixing, wherein an upper layer is a crude glyceride layer, a lower layer is materials which are not reacted completely and impurities generated in the reaction process; (2) dehydrating and degassing the crude glyceride layer by primary distillation; (3) performing secondary distillation on the product, and removing free fatty acid and excessive glycerol; and (4) performing third-level distillation on the product to obtain a distillment and a distillation remnant, wherein the distillment is the high-purity molecular distillation monoacylglycerol, and the distillation remnant is diglyceride and triglyceride. By the process, the content of total monoester in crude ester can be improved obviously, the abrasion of equipment in subsequent molecular distillation process is reduced, the energy consumption of distillation is reduced, and the economic benefit is improved obviously.

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  • Process for preparing high-purity molecular distillation monoacylglycerol
  • Process for preparing high-purity molecular distillation monoacylglycerol

Examples

  • Experimental program(3)

Example Embodiment

[0020] Example 1
[0021] (1) Synthesis of fatty acyl monoglycerides: Take 1kg of glycerin and 10g of NaOH into the reaction kettle, mix well, reduce pressure to 3000Pa, and heat to 200°C for 30min. Add 1.5kg of hydrogenated oil and 30g of benzyltriethylammonium chloride to the mixing kettle, mix them evenly, heat to 200°C, and add them to the reaction kettle three times with an interval of 30 minutes each time. After all the reaction materials were added to the reactor, the reaction was continued for 30 minutes. After the esterification reaction is over, phosphoric acid is added to neutralize, and the reaction mixture is allowed to stand for 30 minutes. The upper layer is the glyceride layer, and the lower layer is the unreacted materials and impurities generated during the reaction. Release the glyceride layer and the slag layer in sequence. The monoglyceride content of the glyceride layer was determined using the method described in the national standard GB15612-1995. The result showed that the monoglyceride content in the crude ester reached 75.89%.
[0022] (2) Transfer the glyceride layer obtained in step (1) to the distillation device, set the distillation temperature of the first stage distillation to 140°C, the pressure to 500 Pa, and the condenser temperature in the first stage distillation device to 50 ℃; continuous feeding, dehydration and degassing operation. Glycerides, as the heavy phase that has not been steamed out, continue to enter the second stage of molecular distillation.
[0023] (3) Transfer the glyceride layer obtained in step (2) to the second-stage molecular distillation device, set the distillation temperature to 175°C and pressure to 75 Pa, and distill out the free fatty acids and glycerin not in it. Glycerides are used as the heavy phase that has not been distilled off and continue to enter the third stage of molecular distillation.
[0024] (4) The glyceride layer obtained in step (3) is transferred to the third-stage molecular distillation device, and the distillation temperature is set to 201° C. and the pressure is 0.5 Pa. The fatty acyl monoglycerides are distilled out, and the light phase product collected in the inner condenser is 1.7kg. The purity of the monoglycerides is detected by gas chromatography, and the purity reaches 95.07%.

Example Embodiment

[0025] Example 2
[0026] (1) Synthesis of fatty acyl monoglycerides: Take 1kg of glycerin and 10g of NaOH into the reaction kettle, mix well, reduce pressure to 3000Pa, and heat to 200°C for 30min. Add 1.5kg of hydrogenated oil, 20g of benzyltriethylammonium chloride and 18g of polyethylene glycol dialkyl ether to the mixing kettle and mix them evenly, and heat to 200°C. Add them to the reaction kettle three times at intervals 30min. After all the reaction materials were added to the reactor, the reaction was continued for 30 minutes. After the esterification reaction is over, phosphoric acid is added to neutralize, and the reaction mixture is allowed to stand for 30 minutes. The upper layer is the glyceride layer, and the lower layer is the unreacted materials and impurities generated during the reaction. Release the glyceride layer and the slag layer in sequence. The monoglyceride content in the glyceride layer was determined using the method described in the national standard GB15612-1995, and the result showed that the monoglyceride content in the crude ester reached 81.27%.
[0027] (2) Transfer the glyceride layer obtained in step (1) to the distillation device, set the distillation temperature of the first stage distillation to 140°C, the pressure to 500 Pa, and the condenser temperature in the first stage distillation device to 50 ℃; continuous feeding, dehydration and degassing operation. Glycerides, as the heavy phase that has not been steamed out, continue to enter the second stage of molecular distillation.
[0028] (3) Transfer the glyceride layer obtained in step (2) to the second-stage molecular distillation device, set the distillation temperature to 175°C and pressure to 75 Pa, and distill out the free fatty acids and glycerin not in it. Glycerides are used as the heavy phase that has not been distilled off and continue to enter the third stage of molecular distillation.
[0029] (4) The glyceride layer obtained in step (3) is transferred to the third-stage molecular distillation device, and the distillation temperature is set to 201° C. and the pressure is 0.5 Pa. The fatty acyl monoglyceride is distilled out, and 1.83 kg of light phase product is collected in the inner condenser. The purity of the monoglyceride is detected by gas chromatography, and its purity reaches 95.30%.

Example Embodiment

[0030] Example 3
[0031] (1) Synthesis of fatty acyl monoglycerides: Take 1kg of glycerin and 10g of NaOH into the reaction kettle, mix well, reduce pressure to 3000Pa, and heat to 200°C for 30min. Add 1.5 kg of hydrogenated oil and 28 g of cetyl tributyl phosphonium chloride to the mixing kettle, mix them evenly, heat to 200°C, and add them to the reaction kettle three times at 30 min intervals. After all the reaction materials were added to the reactor, the reaction was continued for 30 minutes. After the esterification reaction is over, phosphoric acid is added to neutralize, and the reaction mixture is allowed to stand for 30 minutes. The upper layer is the glyceride layer, and the lower layer is the unreacted materials and impurities generated during the reaction. Release the glyceride layer and the slag layer in sequence. The monoglyceride content of the glyceride layer was determined using the method described in the national standard GB15612-1995. The result showed that the monoglyceride content in the crude ester reached 80.65%.
[0032] (2) Transfer the glyceride layer obtained in step (1) to the distillation device, set the distillation temperature of the first stage distillation to 140°C, the pressure to 500 Pa, and the condenser temperature in the first stage distillation device to 50 ℃; continuous feeding, dehydration and degassing operation. Glycerides, as the heavy phase that has not been steamed out, continue to enter the second stage of molecular distillation.
[0033] (3) Transfer the glyceride layer obtained in step (2) to the second-stage molecular distillation device, set the distillation temperature to 175°C and pressure to 75 Pa, and distill out the free fatty acids and glycerin not in it. Glycerides are used as the heavy phase that has not been distilled off and continue to enter the third stage of molecular distillation.
[0034] (4) The glyceride layer obtained in step (3) is transferred to the third-stage molecular distillation device, and the distillation temperature is set to 201° C. and the pressure is 0.5 Pa. The fatty acyl monoglyceride is distilled out, and 1.81 kg of the light phase product is collected in the inner condenser. The purity of the monoglyceride is detected by gas chromatography, and its purity reaches 95.87%.
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