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transcritical co 2 Catalytic esterification-separation coupling method and device for preparing rosin ester

A technology of catalyzing esterification and rosin ester, which is applied in the field of rosin deep processing, can solve the problems of rosin ester pollution, high production cost, and low profit, and achieve the effects of avoiding pollution, strengthening stirring and heat and mass transfer, and eliminating feedback inhibition

Active Publication Date: 2017-06-16
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the current technology, in the technology of preparing rosin esters after deep processing of rosin with catalysts, most of the catalysts use metal catalysts to esterify rosin to obtain rosin esters, but the use of metal catalysts for catalysis will cause metal ions to pollute rosin esters. If rosin ester contaminated by metal ions is used for food production, it will have adverse effects on the human body after use
Moreover, the preparation of rosin esters in the present technology is due to the use of metal catalysts, and sometimes even noble metal catalysts are used for catalytic reaction production, resulting in problems such as higher production costs, making the profit not high in the process of producing rosin esters

Method used

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  • transcritical co <sub>2</sub> Catalytic esterification-separation coupling method and device for preparing rosin ester
  • transcritical co <sub>2</sub> Catalytic esterification-separation coupling method and device for preparing rosin ester
  • transcritical co <sub>2</sub> Catalytic esterification-separation coupling method and device for preparing rosin ester

Examples

Experimental program
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Effect test

Embodiment 1

[0037] as attached Figure 1-4 As shown, the device for catalyzing esterification-separation coupling to prepare rosin ester method includes: dissolution kettle 1, esterification reactor 2, expander 3, gas-liquid separator 4, turbine compressor 5, separation tower 6, Return pump7.

[0038] The discharge port of the dissolution kettle 1 is connected with the feed port of the esterification reactor 2, and the dissolution kettle 1 is used for dissolving raw materials required for production. The esterification reactor 2 is cylindrical, and the top of the esterification reactor is provided with a feed inlet 21, a gas outlet 22, and the bottom is provided with a discharge outlet 23, and the esterification reactor 2 includes a heating pipe 24, which is a heating coil. It is arranged inside the esterification reactor; the gas distributor 25 includes an air inlet 251 and a plurality of nozzles 252 for exhaust; the expander 3 is connected to the gas outlet of the esterification reacto...

Embodiment 2

[0044] The reaction device that uses is identical with embodiment 1, and a kind of catalytic esterification-separation coupling prepares rosin ester method:

[0045] Add ethanol and rosin in a molar ratio of 3:1 to melting kettle 1, then add glycerin and dimethyl carbonate of 25% of the weight of rosin, heat and melt to form a mixed material, and pass into CO 2 Press the material into the esterification reactor 2, then raise the temperature to 150°C, and continuously feed CO 2 Until the pressure in the esterification reactor 2 is 0.01Mpa, then open the gas outlet valve of the esterification reactor 2 to make the water vapor, glycerin vapor, dimethyl carbonate vapor, CO 2 The mixed gas phase material flows out continuously, and the outflow is ≤12000m 3 / h, the pressure is ≤10.0MPa, it enters the gas-liquid separator 4 after being throttled and expanded by the expander 3, and the pressure is reduced to ≤0.5MPa through the expansion of the expander 3 or the throttle expansion is...

Embodiment 3

[0047] The reaction device that uses is identical with embodiment 1, and a kind of catalytic esterification-separation coupling prepares rosin ester method:

[0048] Add glycerin (glycerol) and rosin to melting kettle 1 at a molar ratio of 5:1, then add 200# solvent oil of glycerin and 10% of rosin weight, heat and melt to form a mixed material, and pass into CO 2 Press the material into the esterification reactor 2, then raise the temperature to 100°C, and continuously feed CO 2 When the pressure in the esterification reactor 2 is 3.0Mpa, then open the gas outlet valve of the esterification reactor 2 to make the water vapor, glycerin vapor, 200# solvent oil vapor, CO 2 The mixed gas phase material flows out continuously, and the outflow volume is ≤12000m 3 / h, the pressure is ≤10.0MPa, it enters the gas-liquid separator 4 after being throttled and expanded by the expander 3, and the pressure is reduced to ≤0.5MPa through the expansion of the expander 3 or the throttle expans...

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Abstract

The invention relates to a method for preparing rosin ester by coupling catalytic esterification and separation, which comprises the following operation steps: (1) mixing an alcohol compound, a rosin and a solvent, and dissolving; (2) putting the dissolved substance in the step (1) into an esterification reactor, and introducing 0.01-10.0-MPa CO2 to perform esterification reaction at 150-300 DEG C; (3) recovering the gas phase in the esterification reaction process, sending the gas phase into a gas-liquid separator through an expander, and returning the separated CO2 and newly supplemented CO2 into the esterification reactor through a turbine compressor; and (4) after reacting in the esterification reactor for 1.0-8.0 hours, relieving the pressure, and taking the obtained product out of the esterification reactor. The invention aims to provide a preparation method which has the advantages of lower cost and high rosin ester quality.

Description

technical field [0001] The invention belongs to the technical field of rosin deep processing and relates to a transcritical CO 2 A method and device for preparing rosin ester through catalytic esterification-separation coupling. Background technique [0002] Rosin ester is the most important species in rosin deep processing, accounting for more than 60% of rosin deep processing products. Because rosin resin acid has a three-ring phenanthrene skeleton structure, the steric hindrance of the carboxyl group is large, resulting in high activation energy of the esterification reaction, and the viscosity of the rosin reaction system is high, resulting in difficulty in interphase transfer between reactants. The esterification reaction of rosin resin acid can only be carried out under the conditions of acidic metal oxide catalyst and high temperature. However, under high temperature conditions, the rosin resin acid is prone to decarboxylation side reactions, resulting in a reductio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09F1/04B01J19/24
Inventor 陈小鹏王琳琳梁杰珍韦小杰丁胜芳
Owner GUANGXI UNIV
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