Method for producing glyceryl triacetate by atomizing raw materials

A technology of glycerol triacetate and raw materials, which is applied in chemical instruments and methods, chemical methods for reacting liquids with liquids, preparation of carboxylic acid esters, etc., can solve the problems of many side reactions, large energy loss, high reaction temperature, etc. Achieve the effect of shortening the esterification reaction time, complete the esterification reaction and improving the conversion rate

Active Publication Date: 2009-12-30
云南玉溪环腾科工贸有限公司
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AI Technical Summary

Problems solved by technology

[0005] There are the following problems in the production of glycerol triacetate by the above method: 1. the esterification reaction in the esterification kettle is a full liquid phase reaction, and the reaction raw materials and products exist in the reaction kettle at the same time, the raw material contact is insufficient, and the esterification reaction time is long , not only the color of triacetin produced becomes darker, but also has many side reactions, the content of triacetin in the finished product is only 98-99%, and the yield is only 95%; Shut down to take out the reactants, and the triacetin produced earlier stays in the high-temperature reactor for a long time and becomes darker in color, resulting in high product chroma, and the semi-finished product chroma / (Hazen(Pt-Co) without post-treatment decolorization process is 30 , after the decolorization treatment, the color of the finished product / (Hazen(Pt-Co) is 15; ③The reaction temperature is high, and the production needs to be stopped after the reaction is completed, and the product is taken out from the esterification kettle, and the energy consumption during shutdown and startup Large loss; ④The esterification reaction time will increase with the increase of reactants, such as: the laboratory uses a 500ml three-necked bottle for reaction, and the average reaction time is 6 hours, and uses a 5000ml three-necked bottle for reaction, and the average reaction time is 9 hours ; 2m is used in industrial production 3 Reactor, the average reaction time is 20 hours, using 5m 3 Reactor, the average reaction time is 25 hours

Method used

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  • Method for producing glyceryl triacetate by atomizing raw materials
  • Method for producing glyceryl triacetate by atomizing raw materials
  • Method for producing glyceryl triacetate by atomizing raw materials

Examples

Experimental program
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Effect test

Embodiment 1

[0024] In this example, ionic liquid [HSO3-pmim][HSO4] is used to catalyze the synthesis of glycerol triacetate, and the implementation method is as follows:

[0025] A, glycerin, acetic acid, liquid catalyst and water-carrying agent are matched in proportion, wherein by molar ratio, n (glycerol): n (acetic acid)=1: 8, and liquid catalyst accounts for 2.5% of reactant gross weight, and water-carrying The agent accounts for 4% of the total weight of the reactants, and the mixture is stirred and preheated to 90°C;

[0026] B. atomize the mixture obtained in step A, make it undergo esterification reaction at a temperature of 120°C for 2 hours, and obtain a liquid mixture with a triacetin content of 98%;

[0027] C, adding 1.5% acetic anhydride to the liquid mixture obtained in step B to carry out a deep esterification reaction, the reaction temperature is 110 ° C, and the reaction time is 20 minutes to obtain a liquid mixture with a triacetin content of 99.7%;

[0028] D. The se...

Embodiment 2

[0031] In this example, ionic liquid [HSO3-pmim][HSO4] is used to catalyze the synthesis of glycerol triacetate, and the implementation method is as follows:

[0032] A, glycerin, acetic acid, liquid catalyst and water-carrying agent are matched in proportion, wherein in molar ratio, n (glycerin): n (acetic acid)=1: 8, and liquid catalyst accounts for 4% of reactant gross weight, and water-carrying The agent accounts for 5% of the total weight of the reactants, and the mixture is stirred and preheated to 100°C;

[0033] B. atomize the mixture obtained in step A, and make it undergo esterification reaction at a temperature of 110°C for 1.5 hours to obtain a liquid mixture with a triacetin content of 98.5%;

[0034] C, the mixture obtained in step B is cooled to 30° C., and the liquid catalyst is layered and recovered;

[0035] D, adding 1.3% acetic anhydride to the liquid mixture obtained in step C to carry out a deep esterification reaction, the reaction temperature is 100° C...

Embodiment 3

[0039] In this example, ionic liquid [HSO3-pmim][HSO4] is used to catalyze the synthesis of glycerol triacetate, and the implementation method is as follows:

[0040] A, glycerin, acetic acid, liquid catalyst and water-carrying agent are matched in proportion, wherein in molar ratio, n (glycerin): n (acetic acid)=1: 8, and liquid catalyst accounts for 5% of reactant gross weight, and water-carrying The agent accounts for 6% of the total weight of the reactants, and the mixture is stirred and preheated to 95°C;

[0041] B. The mixture obtained in step A was atomized to allow esterification reaction to occur at a temperature of 105°C for 1.5 hours to obtain a liquid mixture with a triacetin content of 98.7%;

[0042] C, further reacting the liquid mixture obtained in step B for 1 hour at a temperature of 85° C. to obtain a liquid semi-finished product with a triacetin content of 98.8%;

[0043]D, adding 1% acetic anhydride to the liquid mixture obtained in step C to carry out a...

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Abstract

The invention discloses a method for producing glyceryl triacetate by atomizing raw materials. The production method can help shorten esterification reaction time and improve product yield, quality and chroma. The objective is achieved in virtue of the following technical scheme: mixing glycerol and acetic acid at a mol ratio of 1:6-9; adding a proper amount of a liquid catalyst and an entrainer,stirring and preheating to 80-100 DEG C; atomizing the mixture to allow the mixture to be subject to esterification reaction at 100-120 DEG C for 1-2h to obtain a liquid mixture containing 98-99% of glyceryl triacetate; adding 1-1.5% of acetic anhydride to the obtained liquid mixture for deep esterification reaction at the temperature of 90-110 DEG C for 10-20min to obtain a semi-finished product; removing the entrainer and the acetic acid, neutralizing, decoloring and filtering to obtain the glyceryl triacetate finished product.

Description

technical field [0001] The invention relates to the field of cigarette tip forming, and more specifically relates to a production method of a cigarette tip curing molding agent. Background technique [0002] Glyceryl triacetate (GTA) is a fine chemical product with a wide range of uses. It is mainly used as a plasticizer for cigarette filters, and can also be used as a plasticizer for some plastic products and a spice fixative. The market demand is very large. In industrial production, acidic ionic liquids such as [HSO3-pmim][HSO4], [HSO3-pmim]Cl, [HSO3-pmim][BF4], [HSO3-pmim][H2PO4] are often used as catalysts to prepare glycerol triacetate. Its reaction equation is as follows: [0003] [0004] The technique of producing glyceryl triacetate in the prior art is as figure 1 Shown: Glycerol, acetic acid, water-carrying agent and acidic ionic liquid are matched well according to regulations, wherein by molar ratio, n (glycerol): n (acetic acid) = 1: 6~9, liquid catalyst a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/18C07C67/08B01J14/00A24D3/14C08K5/103
Inventor 蒋海明
Owner 云南玉溪环腾科工贸有限公司
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