CN104193625A - Recovery method of catalyst triethylamine in acesulfame potassium production - Google Patents
Recovery method of catalyst triethylamine in acesulfame potassium production Download PDFInfo
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- CN104193625A CN104193625A CN201410501486.7A CN201410501486A CN104193625A CN 104193625 A CN104193625 A CN 104193625A CN 201410501486 A CN201410501486 A CN 201410501486A CN 104193625 A CN104193625 A CN 104193625A
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Abstract
The invention belongs to the technical field of acesulfame potassium production and relates to a recovery method of catalyst triethylamine in the acesulfame potassium production. A one-step one-kettle reaction is changed into a two-kettle three-step reaction, and the purpose of recovering triethylamine is achieved by the following steps: (1) preheating, and recovering methylene dichloride; (2) carrying out neutralization reaction; (3) reacting in an alkali separation kettle and dropwise adding sulfuric acid; (4) carrying out heat preservation and water distribution. Compared with a traditional method, the recovery method has the advantages that the recovery rate is greatly improved, the labor intensity of workers is reduced at the same time, and produced wastes also reach the environmental treatment standards.
Description
Technical field
The invention belongs to acesulfame potassium production technical field, relate to the recovery method of catalyst of triethylamine in a kind of acesulfame potassium production.
Background technology
Acesulfame potassium is the sweeting agent generally using on current market, is widely used in food beverage industry, and market outlook are wide.Triethylamine is as the main catalyzer of producing acesulfame potassium, and market potential is huge.The today of dominating enterprise's destiny in safety, environmental protection, benefit, optimizes and combines resource, energy-saving and cost-reducing, and technical renovation transformation is the flourish needs of enterprise.From market development in recent years, the Application Areas of acesulfame potassium is constantly being widened, and the market requirement increases, and foreign trade export trade also becomes ascendant trend.The method falling behind, the serious left and right of the recovery yield of low numerical value the production cost of product, and then affect share of market and the competitive power of product.
Original triethylamine recovery method is that spent acid is splashed in the mixture of lime and water as shown in Figure 1, during this method can cause and in still reaction too violent, and acid amount is wayward, once it is excessive to occur, in still, material will cancel completely, cause workman's working strength high, and the rate of recovery is low; And waste water is because reclaiming not thoroughly residual very large amine taste, and to workman's physical and mental health, periphery productive life environment brings very large impact, and produced simultaneously waste water is also failed up to standard, brings obstacle to discharge.
Summary of the invention
Object of the present invention is exactly that will to solve the rate of recovery that existing acesulfame potassium exists in the recovery of catalyst of triethylamine in producing low, problem of environmental pollution, provide a kind of acesulfame potassium produce in the recovery method of catalyst of triethylamine.
In acesulfame potassium production, a recovery method for catalyst of triethylamine, is primarily characterized in that and comprises the following steps
:
A. the cold spent acid producing in producing is passed through to pump, under meter, spent acid well heater, spent acid is preheated to 65-75 DEG C, carry out gas-liquid separation, steam is methylene dichloride, utilizes the mode of brine refrigeration to reclaim, as acesulfame potassium raw materials for production; Hot acid liquid is sent in hot acid conservation tank stand-by;
B. mother liquid coming and stone flour (calcium carbonate) are mixed into proportioning machine stirring by 2.8-3.2:2.4-2.8, in pumping into after mixing and in still; In then the hot acid in hot acid conservation tank being pumped into and still, hot acid and mother liquid coming and stone flour mixture carry out neutralization reaction in the ratio of 5.4-5.8:6.6-6.8, be warming up to 94-100 DEG C and add thermal distillation, PH is controlled between 3-6, distill out after low-boiling-point organic compound impurity, remaining liq is sent into alkali out reaction still;
C. by the material of becoming reconciled put into alkali and analyse still, water lime mixes with mother liquid coming after mixing with the ratio of water 0.8-1:2.2-2.8 in lime again to be sent into alkali and analyses still, until PH is controlled between 10-12, distillation is to more than 100 DEG C, after 40-60min, basic steaming only after triethylamine in still; Stop steaming and be cooled to below 80 DEG C, drip 98% sulfuric acid, until PH is between 4-6 in still, leftover materials are calcium carbonate, after whizzer centrifuge dehydration, come into the market.
On technique scheme basis, there is following further improvement project:
The crude product triethylamine that c step is steamed is through circulation insulation point water, and temperature is controlled between 65-75 DEG C, and moisture, lower than 3.5 ‰ o'clock, is put into cyclic drying tower and utilized the strong absorptive of sheet alkali to be dried.Moisture enters rectifying tower low-temperature distillation lower than 1.5 ‰ o'clock pumps, obtains fine work triethylamine after molecular sieve absorbs water again, and moisture is below 1 ‰.The alkali lye of dry gained is sent to production plant.
The invention has the advantages that recovery method of the present invention avoided the reaction in traditional method violent, excessive acid problem, can not cause loss of material, can make the triethylamine rate of recovery reach more than 95% simultaneously; The solid residue of method is utilized effectively, and byproduct calcium sulfate is widely used in building material field as commodity, and supply falls short of demand in market; Ammonia content in waste water also greatly reduces, and wastewater treatment difficulty declines.
Brief description of the drawings
Fig. 1 is traditional recovery method schema of catalyst of triethylamine during acesulfame potassium is produced.
Fig. 2 is the recovery method schema of catalyst of triethylamine during acesulfame potassium of the present invention is produced.
Embodiment
Embodiment 1
In acesulfame potassium production, a recovery method for catalyst of triethylamine, is primarily characterized in that and comprises the following steps
:
A. the cold spent acid producing in producing is passed through to pump, under meter, spent acid well heater, spent acid is carried out to preheating (65-75 DEG C), carry out gas-liquid separation, steam is methylene dichloride, utilizes the mode of brine refrigeration to reclaim, as acesulfame potassium raw materials for production; Hot acid liquid is sent in hot acid conservation tank stand-by;
B. mother liquid coming and stone flour (calcium carbonate) are mixed into proportioning machine stirring by 3:2.6, in pumping into after mixing and in still; In then approximately 6800 liters of the hot acids in hot acid conservation tank being pumped into by the speed of 20m3/t and still, hot acid and mother liquid coming and stone flour mixture carry out neutralization reaction in the ratio of 5.6:6.8, be warming up to 94 DEG C and add above thermal distillation, PH is controlled between 4.5-5.5, distill out after low-boiling-point organic compound impurity, remaining liq is sent into alkali out reaction still;
C. by the material of becoming reconciled put into alkali and analyse still, water lime mixes with mother liquid coming after mixing with the ratio of water (1:2.5) in lime again to be sent into alkali and analyses still, until PH is controlled between 10.5-11, distillation is to more than 100 DEG C, after 45 min, in still after triethylamine basic steam clean; Stop steaming and be cooled to below 80 DEG C, instead adjust 98% sulfuric acid, until PH is between 4.5-5 in still, leftover materials obtain product after whizzer centrifuge dehydration.
D. crude product triethylamine previous step being steamed is through circulation insulation point water, and temperature is controlled between 65-75 DEG C, and moisture, lower than 3.2 ‰ o'clock, is put into cyclic drying tower and utilized the strong absorptive of sheet alkali to be dried.1.4 ‰ o'clock pumps of moisture enter rectifying tower low-temperature distillation, obtain fine work triethylamine after molecular sieve absorbs water again, and moisture is below 0.8 ‰.The alkali lye of dry gained is sent to production plant.
Claims (3)
1. the recovery method of catalyst of triethylamine in acesulfame potassium production, is characterized in that comprising the following steps
:
A. the cold spent acid producing in producing is passed through to pump, under meter, spent acid well heater, spent acid is preheated to 65-75 DEG C, carry out gas-liquid separation, utilize the mode of brine refrigeration to reclaim methylene dichloride; Hot acid liquid is sent in hot acid conservation tank stand-by;
B. mother liquid coming and stone flour are mixed into proportioning machine stirring in the parts by weight ratio of 2.8-3.2:2.4-2.8, in pumping into after mixing and in still; In then the hot acid in hot acid conservation tank being pumped into, carry out neutralization reaction with still, be warming up to 94-100 DEG C and add thermal distillation, PH is controlled between 3-6, distills out after low-boiling-point organic compound impurity, and remaining liq is sent into alkali out reaction still;
C. by the remaining liq of becoming reconciled put into alkali and analyse still, water lime mixes with mother liquid coming after mixing with the parts by weight ratio of water 0.8-1:2.2-2.8 in lime again to be sent into alkali and analyses still, until PH is controlled between 10-12, distillation is to more than 100 DEG C, time 40-60min, in still, crude product triethylamine steams continuously; Stop steaming and be cooled to below 80 DEG C, drip 98% sulfuric acid, until leftover materials PH, between 4-6, obtains calcium sulfate after whizzer centrifuge dehydration in still.
2. the recovery method of catalyst of triethylamine in a kind of acesulfame potassium production according to claim 1, is characterized in that, the methylene dichloride of recovery can be produced used for acesulfame potassium.
3. the recovery method of catalyst of triethylamine in a kind of acesulfame potassium production according to claim 1, it is characterized in that, alkali is analysed to crude product triethylamine that still distills out through a circulation insulation point water, temperature is controlled between 65-75 DEG C, moisture, lower than 3.5 ‰ o'clock, is put into cyclic drying tower and is utilized the strong absorptive of sheet alkali to be dried; Moisture enters rectifying tower low-temperature distillation lower than 1.5 ‰ o'clock pumps, obtains fine work triethylamine after molecular sieve absorbs water again, and moisture is below 1 ‰; The alkali lye of dry gained is sent to production plant.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10023546B2 (en) | 2016-09-21 | 2018-07-17 | 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 |
| US10029999B2 (en) | 2016-09-21 | 2018-07-24 | 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 |
| CN112110823A (en) * | 2020-09-30 | 2020-12-22 | 安徽金禾实业股份有限公司 | Method for reducing lime consumption in triethylamine recovery section |
| CN112125808A (en) * | 2020-09-26 | 2020-12-25 | 安徽金禾实业股份有限公司 | Triethylamine drying and purifying method |
| 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 |
| USRE48464E1 (en) | 2012-06-08 | 2021-03-16 | Celanese Sales Germany Gmbh | Process for producing acesulfame potassium |
| CN113474327A (en) * | 2021-05-28 | 2021-10-01 | 安徽金禾实业股份有限公司 | Treatment method of acesulfame potassium waste liquid |
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| CN1883790A (en) * | 2006-06-30 | 2006-12-27 | 张家港浩波化学品有限公司 | Process for reclaiming catalyst for use in synthesis of acesulfame potassium |
| CN101157666A (en) * | 2007-09-12 | 2008-04-09 | 安徽金禾实业股份有限公司 | Triethylamine recovery processing method and device for production of acesulfame potassium |
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2014
- 2014-09-27 CN CN201410501486.7A patent/CN104193625B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1883790A (en) * | 2006-06-30 | 2006-12-27 | 张家港浩波化学品有限公司 | Process for reclaiming catalyst for use in synthesis of acesulfame potassium |
| CN101157666A (en) * | 2007-09-12 | 2008-04-09 | 安徽金禾实业股份有限公司 | Triethylamine recovery processing method and device for production of acesulfame potassium |
Cited By (31)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| USRE48464E1 (en) | 2012-06-08 | 2021-03-16 | Celanese Sales Germany Gmbh | Process for producing acesulfame potassium |
| US10781190B2 (en) | 2016-09-21 | 2020-09-22 | 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 |
| US10781191B2 (en) | 2016-09-21 | 2020-09-22 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10208004B2 (en) | 2016-09-21 | 2019-02-19 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10227316B2 (en) | 2016-09-21 | 2019-03-12 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10233164B2 (en) | 2016-09-21 | 2019-03-19 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10233163B2 (en) | 2016-09-21 | 2019-03-19 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10590095B2 (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 |
| US10590097B2 (en) | 2016-09-21 | 2020-03-17 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10590098B2 (en) | 2016-09-21 | 2020-03-17 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10759770B2 (en) | 2016-09-21 | 2020-09-01 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10759771B2 (en) | 2016-09-21 | 2020-09-01 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10023546B2 (en) | 2016-09-21 | 2018-07-17 | 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 |
| US10029999B2 (en) | 2016-09-21 | 2018-07-24 | 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 |
| US11724994B2 (en) | 2016-09-21 | 2023-08-15 | 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 |
| US10954204B2 (en) | 2016-09-21 | 2021-03-23 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10954203B2 (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 |
| 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 |
| CN112125808A (en) * | 2020-09-26 | 2020-12-25 | 安徽金禾实业股份有限公司 | Triethylamine drying and purifying method |
| CN112110823A (en) * | 2020-09-30 | 2020-12-22 | 安徽金禾实业股份有限公司 | Method for reducing lime consumption in triethylamine recovery section |
| CN113474327A (en) * | 2021-05-28 | 2021-10-01 | 安徽金禾实业股份有限公司 | Treatment method of acesulfame potassium waste liquid |
| CN113474327B (en) * | 2021-05-28 | 2023-09-26 | 安徽金禾实业股份有限公司 | Method for treating acesulfame potassium waste liquid |
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Denomination of invention: Recovery of catalyst triethylamine in the production of potassium acetylsulfonate Effective date of registration: 20210115 Granted publication date: 20151209 Pledgee: Bank of China Limited Chuzhou Branch Pledgor: ANHUI JINGHE INDUSTRIAL Co.,Ltd. Registration number: Y2021980000385 |
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Date of cancellation: 20220422 Granted publication date: 20151209 Pledgee: Bank of China Limited Chuzhou Branch Pledgor: Anhui Jinhe Industrial Co.,Ltd. Registration number: Y2021980000385 |
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