CN104193625B - The recovery method of catalyst of triethylamine in acesulfame potassium production - Google Patents
The recovery method of catalyst of triethylamine in acesulfame potassium production Download PDFInfo
- Publication number
- CN104193625B CN104193625B CN201410501486.7A CN201410501486A CN104193625B CN 104193625 B CN104193625 B CN 104193625B CN 201410501486 A CN201410501486 A CN 201410501486A CN 104193625 B CN104193625 B CN 104193625B
- Authority
- CN
- China
- Prior art keywords
- still
- triethylamine
- acesulfame potassium
- alkali
- catalyst
- Prior art date
- Legal status (The legal status 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 status listed.)
- Active
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to acesulfame potassium production technical field, relate to the recovery method of catalyst of triethylamine in the production of a kind of acesulfame potassium. change a still single step reaction into two still three-step reactions, through (1) preheating, reclaim methylene dichloride; (2) neutralization reaction; (3) alkali analyses still reaction, drips sulfuric acid; (4) insulation point water, reaches the object reclaiming triethylamine.The present invention comparatively traditional method greatly increases the rate of recovery, reduces the labour intensity of workman simultaneously, and the waste produced also reaches the standard of environmental treatment.
Description
Technical field
The invention belongs to acesulfame potassium production technical field, relate to the recovery method of catalyst of triethylamine in the production of a kind of acesulfame potassium.
Background technology
Acesulfame potassium is the sweeting agent that current market generally uses, and is widely used in food beverage industry, wide market.Triethylamine is as the dominant catalyst producing acesulfame potassium, and market potential is huge.Dominate today of enterprise destiny in safety, environmental protection, benefit, optimize and combine resource, energy-saving and cost-reducing, 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 fallen 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 be in mixture spent acid being instilled lime and water as shown in Figure 1, react too violent during this method can cause and in still, and acid amount is wayward, once occur excessive, in still, material will cancel completely, and cause workman's working strength high, the rate of recovery is low; And waste water is because reclaiming thoroughly residual very not large amine taste, physically and mentally healthy to workman, periphery productive life environment brings very large impact, and the waste water simultaneously produced also is failed up to standard, brings obstacle to discharge.
Summary of the invention
Object of the present invention be exactly to solve existing acesulfame potassium produce in catalyst of triethylamine recovery in the rate of recovery that exists low, problem of environmental pollution, the recovery method of catalyst of triethylamine in providing a kind of acesulfame potassium to produce.
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 produced in production is passed through pump, under meter, spent acid well heater, be preheated to 65-75 DEG C to spent acid, 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 then sent in hot acid conservation tank stand-by;
B. mother liquid coming and stone flour (calcium carbonate) are mixed into proportioning machine by 2.8-3.2:2.4-2.8 to stir, 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 controls between 3 and 6, after distilling out low-boiling-point organic compound impurity, remaining liq sends 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 controls between 10-12, distills to more than 100 DEG C, after 40-60min, in still, after triethylamine, basic steaming is clean; Stop steaming and be cooled to less than 80 DEG C, drip 98% sulfuric acid, until PH is between 4-6 in still, leftover materials are calcium carbonate, come into the market after centrifuge dehydration.
On technique scheme basis, there is following further improvement project:
Crude product triethylamine step c steamed is through a circulation insulation point water, and temperature controls between 65-75 DEG C, moisture lower than 3.5 ‰ time, put into cyclic drying tower and utilize the strong absorptive of sheet alkali to carry out drying.Moisture lower than 1.5 ‰ time pump enter rectifying tower low-temperature distillation, after molecular sieve absorbs water again, obtain fine work triethylamine, moisture is below 1 ‰.The alkali lye of dry gained sends to production plant.
The invention has the advantages that the reaction that recovery method of the present invention avoids in traditional method is violent, excessive acid problem, can not cause loss of material, the triethylamine rate of recovery can be made to 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.
Accompanying drawing explanation
Fig. 1 is the conventional 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 produced in production is passed through pump, under meter, spent acid well heater, carry out preheating (65-75 DEG C) to spent acid, 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 then sent in hot acid conservation tank stand-by;
B. mother liquid coming and stone flour (calcium carbonate) are mixed into proportioning machine by 3:2.6 to stir, in pumping into after mixing and in still; In then the hot acid in hot acid conservation tank about 6800 liters 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 more than 94 DEG C and add thermal distillation, PH controls between 4.5-5.5, after distilling out low-boiling-point organic compound impurity, remaining liq sends 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 controls between 10.5-11, distills to more than 100 DEG C, after 45min, in still after triethylamine basic steam clean; Stop steaming and be cooled to less than 80 DEG C, anti-tune 98% sulfuric acid, until PH is between 4.5-5 in still, leftover materials obtain product after centrifuge dehydration.
D. crude product triethylamine previous step steamed is through a circulation insulation point water, and temperature controls between 65-75 DEG C, moisture lower than 3.2 ‰ time, put into cyclic drying tower and utilize the strong absorptive of sheet alkali to carry out drying.When moisture 1.4 ‰, pump enters rectifying tower low-temperature distillation, and after molecular sieve absorbs water again, obtain fine work triethylamine, moisture is below 0.8 ‰.The alkali lye of dry gained sends to production plant.
Claims (3)
1. acesulfame potassium produce in the recovery method of catalyst of triethylamine, it is characterized in that comprising the following steps:
A. the cold spent acid produced in production is passed through pump, under meter, spent acid well heater, 65-75 DEG C is preheated to spent acid, carries out gas-liquid separation, utilize the mode of brine refrigeration to reclaim methylene dichloride; Hot acid liquid is then sent in hot acid conservation tank stand-by;
B. mother liquid coming and stone flour are mixed into proportioning machine in the parts by weight ratio of 2.8-3.2:2.4-2.8 to stir, in pumping into after mixing and in still; Carry out neutralization reaction with still in then being pumped into by the hot acid in hot acid conservation tank, be warming up to 94-100 DEG C and add thermal distillation, pH controls between 3-6, and after distilling out low-boiling-point organic compound impurity, remaining liq sends 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 controls between 10-12, distills to more than 100 DEG C, time 40-60min, in still, crude product triethylamine steams continuously; Stop steaming and be cooled to less than 80 DEG C, drip 98% sulfuric acid, until leftover materials pH, between 4-6, obtains calcium sulfate after centrifuge dehydration in still.
2. a kind of acesulfame potassium according to claim 1 produce in the recovery method of catalyst of triethylamine, it is characterized in that, the methylene dichloride of recovery is that acesulfame potassium is produced used.
3. a kind of acesulfame potassium according to claim 1 produce in the recovery method of catalyst of triethylamine, it is characterized in that, alkali is analysed crude product triethylamine that still distills out through a circulation insulation point water, temperature controls between 65-75 DEG C, moisture lower than 3.5 ‰ time, put into cyclic drying tower and utilize the strong absorptive of sheet alkali to carry out drying; Moisture lower than 1.5 ‰ time pump enter rectifying tower low-temperature distillation, after molecular sieve absorbs water again, obtain fine work triethylamine, moisture is below 1 ‰; The alkali lye of dry gained sends to production plant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410501486.7A CN104193625B (en) | 2014-09-27 | 2014-09-27 | The recovery method of catalyst of triethylamine in acesulfame potassium production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410501486.7A CN104193625B (en) | 2014-09-27 | 2014-09-27 | The recovery method of catalyst of triethylamine in acesulfame potassium production |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104193625A CN104193625A (en) | 2014-12-10 |
| CN104193625B true CN104193625B (en) | 2015-12-09 |
Family
ID=52079037
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410501486.7A Active CN104193625B (en) | 2014-09-27 | 2014-09-27 | The recovery method of catalyst of triethylamine in acesulfame potassium production |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104193625B (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9024016B2 (en) | 2012-06-08 | 2015-05-05 | Nutrinova Nutrition Specialists & Food Ingredients GmbH | Process for producing acesulfame potassium |
| LT3319948T (en) | 2016-09-21 | 2021-10-11 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| RS61004B1 (en) | 2016-09-21 | 2020-11-30 | Celanese Int Corp | Acesulfame potassium compositions and processes for producing same |
| EP3753930A1 (en) | 2016-09-21 | 2020-12-23 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| ES2763930T3 (en) | 2016-09-21 | 2020-06-01 | Celanese Int Corp | Potassium acesulfame compositions and processes to produce them |
| 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 |
| 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 |
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2014
- 2014-09-27 CN CN201410501486.7A patent/CN104193625B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104193625A (en) | 2014-12-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104193625B (en) | The recovery method of catalyst of triethylamine in acesulfame potassium production | |
| CN103588728B (en) | With direct crystallization production technology in acesulfame potassium | |
| CN105417509B (en) | The separation method of sulfuric acid and phosphoric acid in a kind of preparation of nitrosylsulfuric acid and industrial waste acid | |
| CN105129830A (en) | Method for preparation of potassium alum from activated clay production mother liquor | |
| CN105951102A (en) | Method for reclamation of waste acid in hydrofluoric acid etching process | |
| CN109052354A (en) | Wet process concentrated phosphoric acid defluorinate production technology | |
| CN102351692A (en) | Preparation method for dimethyl sebacate | |
| CN102260174A (en) | Application of solid acid catalyst to preparation of 2,5-dichloronitrobenzene | |
| CN104760976A (en) | Comprehensive utilization method of potassium-containing shale by microwave treatment | |
| CN104058539B (en) | A kind of half fine treatment process based on wastewater from viscose fiber producing | |
| CN104276543A (en) | New process for extracting bromine from concentrated seawater | |
| CN104910031A (en) | Method for co-producing glycine and hydantoin, and apparatus thereof | |
| CN105884238A (en) | Naphthalene-based powder water reducing agent and preparation method thereof | |
| CN103073031A (en) | Method for preparing lithium fluoride from phosphate fertilizer by-product sodium fluoride | |
| CN106810412B (en) | Method for improving sulfonation reaction efficiency and production method of dispersing agent MF | |
| CN102732727A (en) | Method for extracting vanadium from high vanadium-sodium-aluminum-silicon slag | |
| CN102320978A (en) | Preparation method of anhydrous system o-nitroanisole | |
| CN104310441A (en) | Reaction heat comprehensive utilization system and reaction heat comprehensive utilization method in coproduction of potassium nitrate and ammonium chloride | |
| CN106117481B (en) | A kind of solvent method concentrates the production method of sulfonation separate mealing type condensation production naphthalene water reducer | |
| CN104628605A (en) | Continuous catalytic sulfonation method of naphthalene and device thereof | |
| CN101417821B (en) | Method for preparing iron oxide red and cogenerating trisodium phosphate by ferro-phosphorus | |
| CN103708524A (en) | Method for preparing chemical materials by decomposing potassium-bearing rock by fluorosilicic acid cycling method | |
| CN103468293A (en) | Tar distillation technology | |
| CN104788304B (en) | The method that mineral acid acidified formates prepare high-pure anhydrous formic acid | |
| CN105271306A (en) | Method for purifying cyan chloride crude product |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
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 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20220422 Granted publication date: 20151209 Pledgee: Bank of China Limited Chuzhou Branch Pledgor: Anhui Jinhe Industrial Co.,Ltd. Registration number: Y2021980000385 |