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CN1883790A - Process for reclaiming catalyst for use in synthesis of acesulfame potassium - Google Patents

Process for reclaiming catalyst for use in synthesis of acesulfame potassium Download PDF

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Publication number
CN1883790A
CN1883790A CN 200610085795 CN200610085795A CN1883790A CN 1883790 A CN1883790 A CN 1883790A CN 200610085795 CN200610085795 CN 200610085795 CN 200610085795 A CN200610085795 A CN 200610085795A CN 1883790 A CN1883790 A CN 1883790A
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CN
China
Prior art keywords
triethylamine
acesulfame potassium
alkali
recovering
synthesizing
Prior art date
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Pending
Application number
CN 200610085795
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Chinese (zh)
Inventor
陈小萍
陈颖
沈建惠
包忠祥
刘纪才
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ZHANGJIAGANG HAOBO CHEMICAL PRODUCT CO Ltd
Original Assignee
ZHANGJIAGANG HAOBO CHEMICAL PRODUCT CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Priority to CN 200610085795 priority Critical patent/CN1883790A/en
Publication of CN1883790A publication Critical patent/CN1883790A/en
Pending legal-status Critical Current

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a process for recovering catalyst in synthesizing potassium acetylsulfanilate, which includes steps of: (1) neutralizing mixture containing triethylamine sulphate with base or basic salt, rising the temperature to 70-120 DEG C for distilling triethylamine. (2) removing water of triethylamine received in step (1) to obtain high purity triethylamine. In addition, acid could be added to the mixture of removing triethylamine in step (1) to neutralizing excess base, and gypsum is obtained by filtrating reactive liquid. The excellence of this method is that the process is simple, processing time is short, damage to the device is slight, having no contamination to environment, the retrieving triethylamine have high purity and can be used for synthesizing potassium acetylsulfanilate after removing water, and the byproduct such as gypsum also has some economic benefit

Description

Process for recovering catalyst used in process of synthesizing acesulfame potassium
Technical Field
The invention relates to a process for recovering triethylamine from a mixture generated in the process of synthesizing acesulfame potassium by taking triethylamine as a catalyst.
Background
Acesulfame potassium is a sweetener widely used in food and beverage industries. The compound has the advantages of good water solubility, high sweetness, stable physicochemical property, strong synergistic effect, non-metabolic property and the like.
The method for synthesizing the acesulfame potassium is various. The synthesis method of acesulfame potassium related by the invention is the US patent with the patent number US4,695,629 which is expired in 3 months in 2005, and the synthesis method is as follows: reacting sulfamic acid with diketene under the catalysis of triethylamine to generate acetoacetamidosulfonic acid triethylamine salt, then carrying out ring closure by using sulfur trioxide to prepare acesulfame, and then reacting with potassium hydroxide to prepare acesulfame potassium. In the introduction, triethylamine is used as a catalyst to synthesize the acesulfame potassium, and other related data are as follows: as in US patent nos. US4,695,629 and US5,011,982 and US5,103,046, no relevant process for recovering triethylamine as a catalyst has been found. According to research, an acidic mixture is generated in the process of synthesizing the acesulfame potassium by using triethylamine as a catalyst, the acidic mixture contains sulfuric acid and triethylamine sulfate, and the triethylamine recovered from the acidic mixture has certain economic value.
Disclosure of Invention
Aiming at the problems, the invention provides a process for recovering triethylamine from a mixture generated in the process of synthesizing potassium acetylsulfanilate by taking triethylamine as a catalyst.
In order to realize the purpose, the invention adopts the following specific process steps: firstly, neutralizing a mixture containing triethylamine sulfate by using alkali or basic salt, and heating to 70-120 ℃ to distill triethylamine. In this process, the amount of the base or basic salt to be added can be controlled with the aim of substantially distilling off triethylamine. And (II) removing water from the triethylamine obtained in the step (I) to obtain high-purity triethylamine.
The alkali or alkali salt used in the step (one) is selected from one of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, calcium carbonate and alkali prepared from oxide or a mixture of several of the alkali prepared from oxide and non-reactive with each other. The base prepared from the oxides described above may be: calcium hydroxide is prepared by reacting calcium oxide with water.
The further technical scheme of the invention is as follows: and (2) adding acid into the mixture obtained in the step (I) after the triethylamine is distilled off to neutralize excessive alkali, and filtering the reaction solution after the reaction is finished to obtain gypsum. And, the acid used may be sulfuric acid.
The invention has the advantages that: the process is simple, convenient and feasible to operate, short in treatment time, less in damage to equipment and free of pollution to the environment. The recovered triethylamine has high purity, and can be used for synthesizing potassium acetylsulfanilate after water is removed. In addition, the quality of the byproduct gypsum reaches the national standard, and the gypsum can be used for firing baking-free bricks and the like, and can bring certain economic benefit.
Detailed Description
The invention is further described below by means of specific examples; the invention should not be limited to this embodiment.
Examples
Firstly, 40.0g of calcium oxide and 70.0g of water are added into a 500ml three-necked reaction bottle with a stirring and temperature measuring device and a distilling device, 330.0g of triethylamine sulfate-containing mixture (containing 5 percent of triethylamine and 27.85 percent of sulfuric acid) is dropwise added while stirring, the temperature of a reaction system is raised to 70-120 ℃, and distillation is carried out for 150 minutes. 16.5g of triethylamine are obtained, containing 65.33% o of water. The reaction equation is as follows:
(II) adding 22g of concentrated sulfuric acid dropwise to the mixture obtained in the step (I) except for the triethylamine while stirring, and after completion of the reaction, filtering the reaction mixture to obtain 233.0g of gypsum (containing 10% of water). The reaction equation is as follows:
and thirdly, adding the triethylamine obtained in the step one and 3.5g of calcium oxide into a three-neck flask provided with a reflux condenser and a thermometer. The upper opening of the condensing pipe is provided with an anhydrous calcium chloride drying pipe communicated with the atmosphere. Heated to reflux for 1 hour. The reflux condenser tube was removed and directly distilled to yield 14.9g triethylamine containing 0.5% o water. The content was 99.84% by gas chromatography (FID). The yield was about 90.3%.

Claims (5)

1. A process for recovering a catalyst used in the process of synthesizing acesulfame potassium is characterized in that: the method comprises the following steps:
firstly, neutralizing a mixture containing triethylamine sulfate by using alkali or basic salt, and heating to 70-120 ℃ to distill triethylamine.
And (II) removing water from the triethylamine obtained in the step (I) to obtain high-purity triethylamine.
2. The process for recovering the catalyst used in the process of synthesizing acesulfame potassium according to claim 1, wherein: the alkali or basic salt used in the step (one) is selected from one of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, calcium carbonate and alkali prepared from oxide or a mixture of several of the alkali prepared from oxide and non-reactive with each other.
3. The process for recovering the catalyst used in the synthesis of acesulfame potassium according to claim 2, wherein: the alkali prepared from the oxides is as follows: calcium hydroxide is prepared by reacting calcium oxide with water.
4. The process for recovering the catalyst used in the processof synthesizing acesulfame potassium according to claim 1, wherein: and (2) adding acid into the mixture obtained in the step (I) after the triethylamine is distilled off to neutralize excessive alkali, and filtering the reaction solution after the reaction is finished to obtain gypsum.
5. The process for recovering the catalyst used in the synthesis of acesulfame potassium according to claim 4, wherein: the acid used is sulfuric acid.
CN 200610085795 2006-06-30 2006-06-30 Process for reclaiming catalyst for use in synthesis of acesulfame potassium Pending CN1883790A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 200610085795 CN1883790A (en) 2006-06-30 2006-06-30 Process for reclaiming catalyst for use in synthesis of acesulfame potassium

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 200610085795 CN1883790A (en) 2006-06-30 2006-06-30 Process for reclaiming catalyst for use in synthesis of acesulfame potassium

Publications (1)

Publication Number Publication Date
CN1883790A true CN1883790A (en) 2006-12-27

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Family Applications (1)

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Cited By (16)

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CN102040522A (en) * 2010-12-14 2011-05-04 青岛瀚生生物科技股份有限公司 Method for recycling triethylamine from production of propargite
CN102079712A (en) * 2010-12-31 2011-06-01 大连联化化学有限公司 Method for recycling anhydrous organic amine from organic amine salt
EP2380870A1 (en) 2010-04-19 2011-10-26 Celanese International Corporation Method to recover organic tertiary amines from waste sulfuric acid employing a plug flow reactor
EP2380869A1 (en) 2010-04-19 2011-10-26 Celanese International Corporation Method to recover organic tertiary amines from waste sulfuric acid
WO2011133467A1 (en) 2010-04-19 2011-10-27 Celanese International Corporation Process for producing ammonium salts
CN102834352A (en) * 2010-04-19 2012-12-19 国际人造丝公司 Method for the manufacture of ammonium sulfate composition
WO2013096152A1 (en) 2011-12-21 2013-06-27 Celanese International Corporation Process for producing ammonium salts
CN104193625A (en) * 2014-09-27 2014-12-10 安徽金禾实业股份有限公司 Recovery method of catalyst triethylamine in acesulfame potassium production
US9024016B2 (en) 2012-06-08 2015-05-05 Nutrinova Nutrition Specialists & Food Ingredients GmbH Process for producing acesulfame potassium
CN105111088A (en) * 2015-09-02 2015-12-02 江苏瑞克医药科技有限公司 Method for recycling triethylamine from wastewater containing triethylamine hydrochloride
US10023546B2 (en) 2016-09-21 2018-07-17 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
US10030000B2 (en) 2016-09-21 2018-07-24 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
US10029999B2 (en) 2016-09-21 2018-07-24 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
US10029998B2 (en) 2016-09-21 2018-07-24 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
CN112142602A (en) * 2019-06-27 2020-12-29 南通醋酸化工股份有限公司 Continuous treatment method for acesulfame potassium waste acid
CN113454074A (en) * 2021-05-28 2021-09-28 安徽金禾实业股份有限公司 Preparation method of acesulfame potassium

Cited By (48)

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WO2011133467A1 (en) 2010-04-19 2011-10-27 Celanese International Corporation Process for producing ammonium salts
CN102834352A (en) * 2010-04-19 2012-12-19 国际人造丝公司 Method for the manufacture of ammonium sulfate composition
EP2380870A1 (en) 2010-04-19 2011-10-26 Celanese International Corporation Method to recover organic tertiary amines from waste sulfuric acid employing a plug flow reactor
EP2380869A1 (en) 2010-04-19 2011-10-26 Celanese International Corporation Method to recover organic tertiary amines from waste sulfuric acid
WO2011131531A1 (en) 2010-04-19 2011-10-27 Celanese International Corporation Method to recover organic tertiary amines from waste sulfuric acid employing a plug flow reactor
WO2011131530A1 (en) 2010-04-19 2011-10-27 Celanese International Corporation Method to recover organic tertiary amines from waste sulfuric acid
US8658830B2 (en) 2010-04-19 2014-02-25 Nutrinova Nutrition Specialties & Food Ingredients Gmbh Method to recover organic tertiary amines from waste sulfuric acid
US8303921B2 (en) 2010-04-19 2012-11-06 Celanese International Corporation Process for producing ammonium salts
US8496905B2 (en) 2010-04-19 2013-07-30 Nutrinova Nutrition Specialties & Food Ingredients Gmbh Method for the manufacture of an ammonium sulfate composition
US8309048B2 (en) 2010-04-19 2012-11-13 Celanese International Corporation Process for producing ammonium salts
WO2011133468A1 (en) 2010-04-19 2011-10-27 Celanese International Corporation Process for producing ammonium salts
CN102040522A (en) * 2010-12-14 2011-05-04 青岛瀚生生物科技股份有限公司 Method for recycling triethylamine from production of propargite
CN102079712A (en) * 2010-12-31 2011-06-01 大连联化化学有限公司 Method for recycling anhydrous organic amine from organic amine salt
WO2013096152A1 (en) 2011-12-21 2013-06-27 Celanese International Corporation Process for producing ammonium salts
US8663595B2 (en) 2011-12-21 2014-03-04 Celanese International Corporation Process for producing ammonium salts
USRE48464E1 (en) 2012-06-08 2021-03-16 Celanese Sales Germany Gmbh Process for producing acesulfame potassium
US9024016B2 (en) 2012-06-08 2015-05-05 Nutrinova Nutrition Specialists & Food Ingredients GmbH Process for producing acesulfame potassium
CN104193625B (en) * 2014-09-27 2015-12-09 安徽金禾实业股份有限公司 The recovery method of catalyst of triethylamine in acesulfame potassium production
CN104193625A (en) * 2014-09-27 2014-12-10 安徽金禾实业股份有限公司 Recovery method of catalyst triethylamine in acesulfame potassium production
CN105111088A (en) * 2015-09-02 2015-12-02 江苏瑞克医药科技有限公司 Method for recycling triethylamine from wastewater containing triethylamine hydrochloride
US10759771B2 (en) 2016-09-21 2020-09-01 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
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US10208004B2 (en) 2016-09-21 2019-02-19 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
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US10590097B2 (en) 2016-09-21 2020-03-17 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
US10590096B2 (en) 2016-09-21 2020-03-17 Celenese International Corporation Acesulfame potassium compositions and processes for producing same
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US10759770B2 (en) 2016-09-21 2020-09-01 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
US10030000B2 (en) 2016-09-21 2018-07-24 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
US10029999B2 (en) 2016-09-21 2018-07-24 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
US10781191B2 (en) 2016-09-21 2020-09-22 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
US11731948B2 (en) 2016-09-21 2023-08-22 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
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US10954203B2 (en) 2016-09-21 2021-03-23 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
US10954204B2 (en) 2016-09-21 2021-03-23 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
US10961207B2 (en) 2016-09-21 2021-03-30 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
US10975047B2 (en) 2016-09-21 2021-04-13 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
US11724994B2 (en) 2016-09-21 2023-08-15 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
US11724993B2 (en) 2016-09-21 2023-08-15 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
US11718594B2 (en) 2016-09-21 2023-08-08 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
CN112142602B (en) * 2019-06-27 2023-02-03 南通醋酸化工股份有限公司 Continuous treatment method for acesulfame potassium waste acid
CN112142602A (en) * 2019-06-27 2020-12-29 南通醋酸化工股份有限公司 Continuous treatment method for acesulfame potassium waste acid
CN113454074B (en) * 2021-05-28 2022-11-25 安徽金禾实业股份有限公司 Preparation method of acesulfame potassium
CN113454074A (en) * 2021-05-28 2021-09-28 安徽金禾实业股份有限公司 Preparation method of acesulfame potassium

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