CN100567182C - Sulphuric anhydride cyclisation legal system is equipped with spent acid treatment process and the treatment system in the acesulfame potassium technology - Google Patents
Sulphuric anhydride cyclisation legal system is equipped with spent acid treatment process and the treatment system in the acesulfame potassium technology Download PDFInfo
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- CN100567182C CN100567182C CNB2007101211620A CN200710121162A CN100567182C CN 100567182 C CN100567182 C CN 100567182C CN B2007101211620 A CNB2007101211620 A CN B2007101211620A CN 200710121162 A CN200710121162 A CN 200710121162A CN 100567182 C CN100567182 C CN 100567182C
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Abstract
The invention provides a kind of sulphuric anhydride cyclisation legal system and be equipped with spent acid treatment process in the acesulfame potassium technology, wherein adopt Mg (OH)
2Perhaps MgO and water are by weight 1: 1-1: 6 proportional range preparating mixture, add in the neutralization reaction still, and drip spent acid then, in MgO, spent acid is in 100%, the usage quantity of spent acid and Mg (OH)
2Or the weight ratio proportional range of MgO is 3: 2-3: between 4, dripping spent acid reacts, the heat that reaction is emitted makes the gas that flashes to that produces triethylamine in the reaction process gradually, be cooled to triethylamine liquid and be collected in the triethylamine receiving tank by water cooler, and the material that neutralization reaction is finished in the post neutralization reactor put into pH value equalizing tank, with the pH value of material in 98% the sulfuric acid and in the equalizing tank is between the 5-7, filters then and filtered liquid is sent to MgSO
4In the cooling still, decrease temperature crystalline is separated out MgSO
4NH
2O, n are the natural number of 1-7.Method of the present invention makes MgSO
4Productive rate reach more than 95%, stopped high salt sewage emissions basically.Make N (C
2H
5)
3The rate of recovery reach more than 95%, thereby efficiently solve environmental issue in the acesulfame potassium production process.
Description
Technical field
The present invention relates to spent acid and handle, be specifically related to a kind of sulphuric anhydride (SO
3) the cyclisation legal system is equipped with spent acid treatment process and the treatment system in the acesulfame potassium technology.
Background technology
With sulphuric anhydride (SO
3) the cyclisation method produces in the process of acesulfame potassium, produces the sulfuric acid that a certain amount of concentration is 30%-80%, sulfuric acid contains the sulfuric acid triethylamine salt in mutually.Usually sulfuric acid and sulfuric acid triethylamine salt need be neutralized under alkaline condition, triethylamine maximum ground be reclaimed to generate salt.Existing treatment process, the mixing solutions that is sulfur waste is sour and sulfuric acid triethylamine salt is at Ca (OH)
2With neutralize in the mixing solutions of water, reaction generates CaSO then
42H2O.
Wherein reaction formula is:
H
2SO
4+Ca(OH)
2→CaSO
4+H
2O
H
2SO
4·N(C
2H
5)
3+Ca(OH)
2→CaSO
4+H
2O+N(C
2H
5)
3↑
With reference to existing spent acid system shown in Fig. 1 and the spent acid treatment system of Fig. 2, its concrete treating processes is: earlier with Ca (OH)
2In adding in proportion with water and in the still 2, drip the H that is stored in the spent acid storage tank 1 lentamente
2SO
4And H
2SO
4N (C
2H
5)
3Mixed solution will guarantee Ca (OH) in this reactions steps
2Slightly be in excess in H
2SO
4And H
2SO
4N (C
2H
5)
3Molar weight, control reacting balance simultaneously, heat release is even, to guarantee N (C
2H
5)
3A large amount of recovery.After spent acid dropwises, in opening and still 2 and heating steams, with in and remaining N (C in the still 2
2H
5)
3Be evaporated, after water cooler 3 cooling, be received in the triethylamine receiving tank 4, after finishing will in and the reaction mass in the still 2 put into reception tank 5, and isolate CaSO with whizzer 7
42H
2O is subsequently with CaSO
42H
2Thermal dehydration generates anhydrous CaSO in the O adding stoving oven 6
4But, because Ca (OH)
2Purity be not very high, usually between 70-80%, so the CaSO that generates
42H
2The purity of O is corresponding can be very not high yet, and centrifuge dripping CaSO
42H
2The energy consumption of O is bigger, simultaneously, and the centrifugal CaSO that comes out
42H
2O will could generate anhydrous CaSO through high-temperature roasting
4, increased most energy consumption so again, at last the CaSO of Sheng Chenging
4Purity neither be very high, sell relatively difficulty as material of construction and industrial chemicals.If directly the neutralization back is discharged and can be caused environmental pollution again, therefore be necessary to seek a kind of new to sulphuric anhydride (SO
3) the cyclisation legal system is equipped with the method that the spent acid in the acesulfame potassium technology is handled, thereby can solve the environmental issue that spent acid is handled effectively.
Summary of the invention
The object of the present invention is to provide a kind of sulphuric anhydride (SO
3) the cyclisation legal system is equipped with the spent acid treatment process in the acesulfame potassium technology, utilizes this method can reclaim triethylamine N (C to greatest extent
2H
5)
3
Another object of the present invention is to provide a kind of sulphuric anhydride (SO
3) the cyclisation legal system is equipped with the spent acid treatment system in the acesulfame potassium technology.
Purpose of the present invention can be finished by following technical scheme:
A kind of sulphuric anhydride cyclisation legal system is equipped with the spent acid treatment process in the acesulfame potassium technology, wherein adopts Mg (OH)
2Perhaps MgO and water are by weight 1: 1-1: 6, preferred 1: 1-1: 3 proportional range preparating mixture, add in the neutralization reaction still, and drip spent acid then, in MgO, spent acid is in 100%, the usage quantity of spent acid and Mg (OH)
2Or the weight ratio proportional range of MgO is 3: 2-3: between 4, be preferably 1: 1 ratio, dripping spent acid then reacts, the heat that reaction is emitted makes the gas that flashes to that produces triethylamine in the reaction process gradually, be cooled to triethylamine liquid and be collected in the triethylamine receiving tank by water cooler, and the material that neutralization reaction is finished in the post neutralization reactor put into the pH value equalizing tank, be that the pH value of material is between the 5-7 in 50%, preferred 98% the sulfuric acid and in the equalizing tank with percentage concentration, filter regulator solution then, and the clear liquid after will filtering is sent to MgSO
4In the cooling still, decrease temperature crystalline is separated out MgSO
4NH
2O, n are the natural number of 1-7.
In the aforesaid method, be included in the step of passing through the whizzer fractional crystallization after crystallization is finished.
In the aforesaid method, also comprise and separate the back by the dry isolating crystallization of roasting.
In the aforesaid method, the Mg of use (OH)
2Or the purity of MgO is more than 80%, and is preferred more than 90%.
A kind of enforcement system for carrying out said process, comprise the spent acid storage tank, in and still, water cooler, triethylamine receiving tank, pH value equalizing tank, strainer, cooling still, whizzer, during wherein the spent acid storage tank feeds by valve and in the still, in and the still upper end be connected with water cooler, connect on the water cooler the other end and receive through water cooler refrigerative triethylamine receiving tank, in and still bottom be connected in the PH equalizing tank that holds reacting rear material by valve, the PH equalizing tank is connected in the cooling still by strainer, and the bottom is connected with whizzer.
The present invention selects Mg (OH) especially for use
2Or MgO replaced C a (OH)
2Method handle (SO
3) the cyclisation legal system is equipped with the spent acid in the acesulfame potassium technology, can reach the cycling and reutilization of waste to greatest extent.And MgSO
4The water of separating after the crystallization also can reuse to neutralization reaction, and repeating utilization factor is 100%, simultaneously MgSO
4Productive rate reach more than 95%, stopped high salt sewage emissions basically.Make N (C
2H
5)
3The rate of recovery reach more than 95%, thereby efficiently solve environmental issue in the acesulfame potassium production process.
Description of drawings
Fig. 1 is available technology adopting Ca (OH)
2Handle the synoptic diagram of the system of spent acid.
Wherein, 1, spent acid storage tank; 2, in and still; 3, water cooler; 4, triethylamine receiving tank; 5, accept the pond; 6, stoving oven; 7, whizzer.
Fig. 2 is available technology adopting Ca (OH)
2Handle the step block diagram of spent acid.
Fig. 3 is employing Mg of the present invention (OH)
2Or MgO handles the synoptic diagram of the system of spent acid.
Wherein, 11, spent acid storage tank; 12, in and still; 13, water cooler; 14, triethylamine receiving tank; 15, pH value equalizing tank; 16, strainer; 17, cooling still; 18, whizzer.
Fig. 4 is the step block diagram of processing spent acid of the present invention.
Embodiment
Below in conjunction with accompanying drawing the present invention is elaborated:
With reference to accompanying drawing 2 and accompanying drawing 3, Fig. 2 has illustrated employing Mg (OH) 2 of the present invention or MgO to handle the synoptic diagram of the system of spent acid.This system comprise spent acid storage tank 11, in and still 12, water cooler 13, triethylamine receiving tank 14, pH value equalizing tank 15, strainer 16, cooling still 17, whizzer 18, during wherein spent acid storage tank 1 feeds by valve and in the still 12, in and still 12 upper end be connected with water cooler 13, connect on water cooler 13 the other ends and receive through water cooler refrigerative triethylamine receiving tank 14, in and still 12 bottoms be connected in the PH equalizing tank 15 that holds reacting rear material by valve, PH equalizing tank 15 is connected in the cooling still 17 by strainer 16, and the bottom is connected with whizzer 18.
Fig. 3 has illustrated the step block diagram of processing spent acid of the present invention.Wherein the spent acid that is equipped with in the acesulfame potassium technology of sulphuric anhydride cyclisation legal system is stored in the spent acid storage tank 11, then with Mg (OH)
2Or MgO and water are according to weight ratio 1: 1-1: 6 proportional range preparating mixture, in joining and in the still 12, during spent acid is added dropwise to through valve and carry out following reaction in the still 12:
H
2SO
4+ Mg (OH)
2(or MgO) → MgSO
4+ H
2O;
H
2SO
4N (C
2H
5)
3+ Mg (OH)
2(or MgO) → MgSO
4+ H
2O+N (C
2H
5)
3↑
The reaction heat of emitting makes triethylamine flash to steam, then triethylamine steam liquid and being collected in the triethylamine receiving tank 14 after supercooler 13 coolings.Will in and in the still 12 reacted material import in the pH value equalizing tank 15, the pH value of regulating material with sulfuric acid (percentage concentration more than 50%, preferred 98%) is between the 5-7, filter through filter 16, and the clear liquid after will filtering is sent to MgSO again
4Cooling still 17 in, decrease temperature crystalline is separated out MgSO then
4NH
2O, n are the natural number of 1-7, will separate out Crystallization Separation by whizzer 18 subsequently and come.
Although above the specific embodiment of the present invention has been given to describe in detail and explanation; but should indicatedly be; we can carry out various equivalences to above-mentioned embodiment according to conception of the present invention and change and modification; when the function that it produced does not exceed spiritual that specification sheets and accompanying drawing contain yet, all should be within protection scope of the present invention.
Claims (9)
1, a kind of sulphuric anhydride cyclisation legal system is equipped with the spent acid treatment process in the acesulfame potassium technology, wherein adopts Mg (OH)
2Perhaps MgO and water are by weight 1: 1-1: 6 proportional range preparating mixture, add in the neutralization reaction still, and drip spent acid then, in MgO, spent acid is in 100%, the usage quantity of spent acid and Mg (OH)
2Perhaps the weight ratio proportional range of MgO is 3: 2-3: between 4, dripping spent acid reacts, the heat that reaction is emitted makes the triethylamine that produces gradually in the reaction process flash to gas, be cooled to triethylamine liquid and be collected in the triethylamine receiving tank by water cooler, and the material that neutralization reaction is finished in the post neutralization reactor put into pH value equalizing tank, with the pH value of material in the sulfuric acid of percentage concentration more than 50% and in the equalizing tank is between the 5-7, filter regulator solution then, and the clear liquid after will filtering is sent to MgSO
4In the cooling still, decrease temperature crystalline is separated out MgSO
4NH
2O, n are the natural number of 1-7.
2, the method for claim 1, wherein further be included in the step of passing through the whizzer fractional crystallization after crystallization is finished.
3, method as claimed in claim 1 or 2 wherein, further comprises and separates the back by the dry isolating crystallization of roasting.
4, method as claimed in claim 1 or 2, wherein, described Mg (OH)
2Or the purity of MgO is more than 80%.
5, method as claimed in claim 1 or 2, wherein, Mg (OH)
2Perhaps the weight ratio of MgO and water is 1: 1-1: 3.
6, method as claimed in claim 1 or 2, wherein, described Mg (OH)
2Or the purity of MgO is more than 90%.
7, method as claimed in claim 1 or 2, wherein, the usage quantity of spent acid and Mg (OH)
2Perhaps the weight ratio ratio of MgO is 1: 1.
8, method as claimed in claim 1 or 2, wherein, in and in the equalizing tank vitriolic percentage concentration of material pH value be 98%.
9, a kind of system that implements each described method of claim 1-8, comprise the spent acid storage tank, the neutralization reaction still, water cooler, the triethylamine receiving tank, pH value equalizing tank, strainer, the cooling still, whizzer, wherein the spent acid storage tank feeds in the neutralization reaction still by valve, neutralization reaction still upper end connects water cooler, connect the triethylamine receiving tank that is used to receive through water cooler refrigerative triethylamine on the water cooler the other end, neutralization reaction still bottom is connected in the pH regulator pond that holds reacting rear material by valve, the pH regulator pond is connected in the cooling still by strainer, and the bottom of cooling still connects whizzer.
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|---|---|---|---|
| CNB2007101211620A CN100567182C (en) | 2007-08-30 | 2007-08-30 | Sulphuric anhydride cyclisation legal system is equipped with spent acid treatment process and the treatment system in the acesulfame potassium technology |
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|---|---|---|---|
| CNB2007101211620A CN100567182C (en) | 2007-08-30 | 2007-08-30 | Sulphuric anhydride cyclisation legal system is equipped with spent acid treatment process and the treatment system in the acesulfame potassium technology |
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| CN101148300A CN101148300A (en) | 2008-03-26 |
| CN100567182C true CN100567182C (en) | 2009-12-09 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11718594B2 (en) | 2016-09-21 | 2023-08-08 | 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 |
| US11731948B2 (en) | 2016-09-21 | 2023-08-22 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
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|---|---|---|---|---|
| US9024016B2 (en) | 2012-06-08 | 2015-05-05 | Nutrinova Nutrition Specialists & Food Ingredients GmbH | Process for producing acesulfame potassium |
| CN105152446B (en) * | 2015-09-25 | 2017-10-17 | 浙江奇彩环境科技股份有限公司 | A kind of acesulfame potassium produces the handling process of waste water |
| CN105523573B (en) * | 2016-01-21 | 2017-06-30 | 青海盐湖工业股份有限公司 | A kind of epsom salt and preparation method thereof |
| CN105565347A (en) * | 2016-03-17 | 2016-05-11 | 吴迪 | Method for preparing magnesium sulfate heptahydrate from desalinated seawater |
| CN109942438A (en) * | 2019-04-15 | 2019-06-28 | 东营市科维生物技术有限公司 | The method and apparatus for recycling organic amine |
| 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 |
| CN110386710A (en) * | 2019-07-19 | 2019-10-29 | 北京朗新明环保科技有限公司南京分公司 | A method of epsom salt is produced using heat-engine plant desulfurized waste water |
| CN113474325B (en) * | 2021-05-28 | 2023-10-20 | 安徽金禾实业股份有限公司 | Method for treating acesulfame potassium waste liquid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11718594B2 (en) | 2016-09-21 | 2023-08-08 | 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 |
| US11731948B2 (en) | 2016-09-21 | 2023-08-22 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
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| CN101148300A (en) | 2008-03-26 |
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