Technique for recycling triethylamine from hydrochloric acid triethylamine water solution

A technology of triethylamine hydrochloride and triethylamine, which is applied in the direction of amino compound purification/separation, organic chemistry, etc., can solve the problems of difficult disposal of three wastes, high price, low recovery rate, etc., and achieves low price, low cost, and easy processing. Effect

Active Publication Date: 2008-10-29
凯米拉天成万丰化学品(兖州)有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Aiming at the above-mentioned problems such as high price, low recovery rate and difficult disposal of three wastes in the recovery of triethylamine from triethylamine hydrochloride aqueous solution, the present invention discloses a method for regenerating triethylamine by the action of calcium oxide and triethylamine hydrochloride aqueous solution. The method of drying triethylamine with calcium oxide, the calcium oxide after drying triethylamine can be used mechanically to produce triethylamine, which is easy to operate, cheap, high recovery rate and no waste discharge

Method used

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  • Technique for recycling triethylamine from hydrochloric acid triethylamine water solution

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Embodiment 1

[0020] (1) produce triethylamine from triethylamine hydrochloride aqueous solution with calcium oxide

[0021] Add 1200Kg of 48% (w / w) triethylamine hydrochloride aqueous solution into the reaction kettle, add 240Kg of powdered calcium oxide with a purity of 80% under stirring, distill the triethylamine at 50-150°C, and drain the aqueous solution into the storage tank for later use. deal with.

[0022] (2) Remove moisture in triethylamine with calcium oxide

[0023] Add 240Kg of powdered calcium oxide with a purity of 80% to the steamed triethylamine. After heating to remove water, what is collected by distillation is colorless and transparent triethylamine with a water content of less than 0.5%. The recovery rate of triethylamine is 96%. .

[0024] (4) Treatment of calcium chloride aqueous solution

[0025] After the aqueous solution discharged in the storage tank is cooled to room temperature, the solid matter is separated and adjusted to neutrality with 30% hydrochloric ...

Embodiment 2

[0027] (1) produce triethylamine from triethylamine hydrochloride aqueous solution with calcium oxide

[0028] Add 1200Kg of 48% (w / w) triethylamine hydrochloride aqueous solution into the reaction kettle, add 200Kg of powdered calcium oxide with a purity of 90% under stirring, distill the triethylamine at 50-150°C, and drain the aqueous solution into the storage tank for later use. deal with.

[0029] (2) Remove moisture in triethylamine with calcium oxide

[0030] Add 200Kg of powdered calcium oxide with a purity of 90% to the steamed triethylamine. After heating to remove water, what is collected by distillation is colorless and transparent triethylamine with a water content of less than 0.5%. The recovery rate of triethylamine is 98%. .

[0031] (4) Treatment of calcium chloride aqueous solution

[0032] After the aqueous solution discharged in the storage tank is cooled to room temperature, the solid matter is separated and adjusted to neutrality with 30% hydrochloric ...

Embodiment 3

[0034] (1) produce triethylamine from triethylamine hydrochloride aqueous solution with calcium oxide

[0035] Add 1200Kg of 48% (w / w) triethylamine hydrochloride aqueous solution into the reaction kettle, add 160Kg of powdered calcium oxide with a purity of 95% under stirring, distill the triethylamine at 50-150°C, and drain the aqueous solution into the storage tank for later use. deal with.

[0036] (2) Remove moisture in triethylamine with calcium oxide

[0037] Add 160Kg of powdered calcium oxide with a purity of 95% to the steamed triethylamine. After heating to remove water, what is collected by distillation is colorless and transparent triethylamine with a water content of less than 0.5%. The recovery rate of triethylamine is 99%. .

[0038] (4) Treatment of calcium chloride aqueous solution

[0039] After the aqueous solution discharged in the storage tank is cooled to room temperature, the solid matter is separated and adjusted to neutrality with 30% hydrochloric ...

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Abstract

A method for recovering triethylamine from triethylamine hydrochloride aqueous solution comprises allowing calcium oxide and the triethylamine hydrochloride to react, and distilling at 50-150 DEC C to obtain the triethylamine; adding the calcium oxide into the collected triethylamine, refluxing under heating to remove water, and distilling to collect the triethylamine having water content smaller than 0.5%, distilling to obtain the triethylamine, separating solid from a turbid aqueous solution residual in a reaction kettle, adjusting the pH value of the aqueous solution to 7 with hydrochloric acid, and removing water to respectively obtain calcium chloride hexahydrate, calcium chloride dehydrate and anhydrous calcium chloride; and allowing the calcium oxide after drying the triethylamine and the triethylamine hydrochloride to react to obtain the triethylamine. Compared with the prior method for recovering the triethylamine from the triethylamine hydrochloride aqueous solution, the method has the advantages of simple operation, low price, high recovery rate, and no three wastes discharge.

Description

(1) Technical field [0001] The invention relates to a process for recovering triethylamine from triethylamine hydrochloride aqueous solution. (2) Background technology [0002] In many organic synthesis reactions, it is usually necessary to add triethylamine as a catalyst or to absorb by-product hydrogen chloride, and dilute hydrochloric acid is added during post-treatment to dissolve triethylamine or triethylamine hydrochloride in water and separate from organic products, thereby producing hydrochloric acid triethylamine aqueous solution. [0003] Take the production of alkyl ketene dimer (AKD) as an example. The reaction to synthesize AKD is as follows: [0004] [0005] In the above reaction, fatty acid chloride reacts with excess triethylamine to form AKD, and by-product triethylamine hydrochloride. An appropriate amount of dilute hydrochloric acid is added to the reaction mixture, excess triethylamine and triethylamine hydrochloride are dissolved in water and sepa...

Claims

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Application Information

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IPC IPC(8): C07C211/05C07C209/82
Inventor 朱年德
Owner 凯米拉天成万丰化学品(兖州)有限公司
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