CN102583853B - Combined treatment method for two kinds of waste acid water generated in tetraacetylethylenediamine (TAED) production - Google Patents
Combined treatment method for two kinds of waste acid water generated in tetraacetylethylenediamine (TAED) production Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 239000002253 acid Substances 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000002699 waste material Substances 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- FRPJTGXMTIIFIT-UHFFFAOYSA-N tetraacetylethylenediamine Chemical compound CC(=O)C(N)(C(C)=O)C(N)(C(C)=O)C(C)=O FRPJTGXMTIIFIT-UHFFFAOYSA-N 0.000 title abstract description 23
- 238000011282 treatment Methods 0.000 title abstract description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000007788 liquid Substances 0.000 claims abstract description 33
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 13
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 238000001704 evaporation Methods 0.000 claims abstract description 10
- 239000006227 byproduct Substances 0.000 claims abstract description 9
- 230000008020 evaporation Effects 0.000 claims abstract description 9
- BDKLKNJTMLIAFE-UHFFFAOYSA-N 2-(3-fluorophenyl)-1,3-oxazole-4-carbaldehyde Chemical compound FC1=CC=CC(C=2OC=C(C=O)N=2)=C1 BDKLKNJTMLIAFE-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 229940087562 sodium acetate trihydrate Drugs 0.000 claims abstract description 8
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000004064 recycling Methods 0.000 claims abstract description 4
- 239000003513 alkali Substances 0.000 claims abstract description 3
- 238000002425 crystallisation Methods 0.000 claims description 29
- 230000008025 crystallization Effects 0.000 claims description 24
- 239000012141 concentrate Substances 0.000 claims description 21
- 230000000694 effects Effects 0.000 claims description 18
- 238000011284 combination treatment Methods 0.000 claims description 14
- -1 thiourea peroxide Chemical class 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- UMGDCJDMYOKAJW-UHFFFAOYSA-N aminothiocarboxamide Natural products NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 10
- 238000004061 bleaching Methods 0.000 claims description 7
- 239000003643 water by type Substances 0.000 claims description 7
- 230000018044 dehydration Effects 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 230000032696 parturition Effects 0.000 claims description 4
- BGRWYDHXPHLNKA-UHFFFAOYSA-N Tetraacetylethylenediamine Chemical compound CC(=O)N(C(C)=O)CCN(C(C)=O)C(C)=O BGRWYDHXPHLNKA-UHFFFAOYSA-N 0.000 claims 3
- 239000007787 solid Substances 0.000 abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 238000005406 washing Methods 0.000 abstract description 2
- RYYXDZDBXNUPOG-UHFFFAOYSA-N 4,5,6,7-tetrahydro-1,3-benzothiazole-2,6-diamine;dihydrochloride Chemical compound Cl.Cl.C1C(N)CCC2=C1SC(N)=N2 RYYXDZDBXNUPOG-UHFFFAOYSA-N 0.000 abstract 2
- 230000000274 adsorptive effect Effects 0.000 abstract 1
- 239000013078 crystal Substances 0.000 abstract 1
- 239000002910 solid waste Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 238000009833 condensation Methods 0.000 description 12
- 230000005494 condensation Effects 0.000 description 12
- 239000012452 mother liquor Substances 0.000 description 9
- 239000002351 wastewater Substances 0.000 description 9
- 230000004087 circulation Effects 0.000 description 7
- 238000007789 sealing Methods 0.000 description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000000049 pigment Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 5
- 238000007599 discharging Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000001632 sodium acetate Substances 0.000 description 5
- 229960004249 sodium acetate Drugs 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 4
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 description 4
- WNYIBZHOMJZDKN-UHFFFAOYSA-N n-(2-acetamidoethyl)acetamide Chemical compound CC(=O)NCCNC(C)=O WNYIBZHOMJZDKN-UHFFFAOYSA-N 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002440 industrial waste Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 235000017550 sodium carbonate Nutrition 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- AYRVGWHSXIMRAB-UHFFFAOYSA-M sodium acetate trihydrate Chemical compound O.O.O.[Na+].CC([O-])=O AYRVGWHSXIMRAB-UHFFFAOYSA-M 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 230000010933 acylation Effects 0.000 description 1
- 238000005917 acylation reaction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
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- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a combined treatment method for two kinds of waste acid water generated in tetraacetylethylenediamine (TAED) production. The combined treatment method is characterized by comprising the following steps of: evaporating dark acid water generated after washing TAED crystals by using live steam; carrying out multi-effect concentration on decolored neutralized liquid by using the acid steam generated by evaporation as a heat source; cooling and crystallizing; and separating solid from liquid to obtain sodium acetate trihydrate which is a by-product, wherein the live steam can be generated by burning residues for recycling after the dark acid water is evaporated, The decolored neutralized liquid is generated by the method that after the acid steam is subjected to heat exchange, the acid steam is condensed into colorless acid water; then the colorless acid water is mixed with light acid water generated by high-temperature dewatering after acetic acid and ethanediamine react in the production of the TAED; alkali is added to the mixed liquid for neutralization; and then the mixed liquid is decolored by using thiourea dioxide. According to the combined treatment method, the acid steam of the dark acid water is used as a primary heat source for carrying out the multi-effect concentration on the mixed liquid of the mixed acid, therefore, energy can be greatly saved, and environment friendliness is facilitated; and the thiourea dioxide is used as a decoloring agent, the complication of solid and liquid separation and the generation of solid waste residues, which are brought by decoloring solid adsorptive substances such as activated carbon, are also avoided.
Description
Technical field
The invention belongs to technical field of waste water processing, particularly a kind of method of two kinds of different waste acid waters that produce in the tetraacetyl ethylene diamine production process being carried out combination treatment.
Background technology
Tetraacetyl ethylene diamine (TAED) has outstanding cold bleaching performance as a kind of effective bleach-activating agent, and favorable environment protection is washed the industry widespread use both at home and abroad at present.
General tetraacetyl ethylene diamine is by excessive acetic acid and quadrol diacylization; generate diacetyl ethylenediamine behind the high temperature dehydration; synthetic by aceticanhydride and diacetyl ethylenediamine four acylations again, become finished product after the TAED process crystallization of synthetic back, filtration, washing, oven dry, granulation, the packing.High temperature dehydration produces the light sour water of a kind of acetate concentration about 20% after the diacylization, wherein also contains micro-foreign pigment by product; TAED after crystallization is filtered washes wherein foreign pigment with water, thereby produces the dark sour water of another acetate concentration about 10%, wherein also contains a small amount of diacetyl ethylenediamine, triacetyl quadrol, tetraacetyl ethylene diamine and a large amount of foreign pigment by product.Two kinds of sour water concentration are all lower, and the recovery of Dichlorodiphenyl Acetate can not embody economic worth.Because the high COD of two kinds of sour waters and its contain the singularity of impurity, are not suitable for directly entering the biochemical treatment process, so the processing that two kinds of waste acid waters are had an economic benefit is extremely important.
In the prior art, do not see as yet to unite and utilize tetraacetyl ethylene diamine production process waste water to prepare the report of sodium-acetate both at home and abroad, do not see in the industrial waste acid water treatment yet, use the report of thiourea peroxide decolouring.Introduce the technology of utilizing the multiple-effect concentrating unit to handle industrial waste acid water among Chinese patent CN1865128A and the CN101066817A, handle nonvolatile sulfuric acid in the waste acid water, obtain volatility hydrochloric acid and various soluble sulphate recycling.Chinese patent CN101492362A discloses a kind of technology of utilizing the acetic acid waste acid water to produce Sodium acetate trihydrate, technology relates to air distillation, the neutralization of distillation back condensation sour water, neutralizer decolouring, crystalline product, this process steam energy consumption is higher, uses activated carbon decolorizing, and execute-in-place is numerous and diverse.Introduced among the Chinese patent CN101747173A and contain the acetic acid containing waste water treatment technology, technology relates to rectifying acetic acid, neutralization, concentrates, removal of impurities, crystallization, drying, and this process steam energy consumption is higher.
Summary of the invention
The object of the present invention is to provide the method for two kinds of different waste acid waters that produce in a kind of combination treatment TAED production process, can obtain a kind of byproduct Sodium acetate trihydrate, use steam few, it is easy to decolour, environmental protection and energy saving.
A kind of combination treatment method to two kinds of waste acid waters in the tetraacetyl ethylene diamine production, it is characterized in that comprising step: will wash the dark sour water evaporation that produces after the TAED crystallization with giving birth to steam, the acid vapour that evaporation produces carries out multiple-effect as thermal source to the neutralizer after decolouring and concentrates, crystallisation by cooling, solid-liquid separation gets the byproduct Sodium acetate trihydrate, dark sour water evaporites burns back heat energy and produces living steam recycling; Neutralizer after the described decolouring is: be condensed into colourless sour water after the acid vapour heat exchange, the light sour water that high temperature dehydration produces behind acetic acid and the reacting ethylenediamine in colourless sour water and the TAED production process mixes, add the alkali neutralization, then the liquid that generates with thiourea peroxide decolouring back.
Further, concentrated two effects that are preferably of described multiple-effect concentrate.
Neutralizer can with following current, adverse current and and flow three kinds of modes and enter multiple-effect and concentrate, concentrate outlet neutralizer temperature in order to reduce, be conducive to crystallization, neutralizer of the present invention two imitate concentrate in the flow direction be preferably following current.
Further, concentrate 60 ~ 75 ℃ of back liquid drop temperatures.
Two imitate in the concentration processs, one imitate temperature be preferably 80 ~ 95 ℃, pressure and be preferably-0.03 ~-0.055MPa; Two imitate temperature be preferably 60 ~ 75 ℃, pressure and be preferably-0.07 ~-0.09MPa.
In the neutralizer decolorization, described thiourea peroxide usage quantity is 0.02% ~ 0.1% of neutralizer quality, is preferably 0.05%.
Described bleaching time is 5 minutes to 24 hours, is preferably 15 minutes.
Among the present invention, described " dark sour water " washes wherein foreign pigment with water for the TAED of crystallization after filtering, thereby the dark waste water of a kind of acetate concentration about 10% that produces wherein also contains a small amount of diacetyl ethylenediamine, triacetyl quadrol, tetraacetyl ethylene diamine and a large amount of foreign pigment by product.Described " light sour water " is the light waste water of a kind of acetate concentration about 20% that high temperature dehydration produces after acetic acid and the reaction of quadrol diacyl, wherein also contains micro-foreign pigment by product.
The present invention by dark sour water evaporate, mix sour water neutralization, decolouring, concentrate, crystallization, solid-liquid separation handle waste acid water.The acid vapour that characteristics are to utilize dark sour water the neutralizer that mixes sour water is carried out multiple-effect concentrate, thereby the least possible use steam is handled industrial waste acid water as the one-level thermal source, and save energy is conducive to environmental protection greatly; The present invention selects thiourea peroxide as discoloring agent neutralizer to be decoloured, obtain the byproduct Sodium acetate trihydrate, the generation of the numerous and diverse and solid slag of the solid-liquid separation of having avoided the decolouring of solid absorption materials such as gac to bring.
The inventive method can specifically comprise some steps:
1, dark sour water evaporation
Dark waste acid water is continuously pumped in the reboiler, with 0.4 ~ 0.7MPa(gauge pressure) the evaporation of living steam heating, acid vapour is as the one-level thermal source, connect the multiple-effect concentration systems and concentrate neutralizer, reboiler is connected with the high liquid sealing pipe of 4 ~ 10m, guarantee 105 ~ 130 ℃ of acid vapour temperature, the preferred high liquid sealing pipe of 4m, 110 ℃ of acid vapour temperature.
2, mix the sour water neutralization
Acid vapour is condensed into the colourless sour water of high temperature after concentrating heat exchange through multiple-effect, and the colourless sour water of high temperature can be to entering the dark acid water preheat of reboiler, and then enters light sour water groove and mix with light sour water.Mix sour water in and feel secure in the still, use soda ash or liquid caustic soda to drip neutralization, in and terminal temperature be that 40 ~ 80 ℃, Ph value are 7.5 ~ 10.5, preferably 50 ~ 70 ℃ of terminal temperatures, Ph value 8.0 ~ 9.0.
3, decolouring
Neutralizer is that 40 ~ 80 ℃, Ph value are under 7.5 ~ 10.5 the prerequisite in temperature, adds 0.02 ~ 0.1% thiourea peroxide with respect to the neutralizer quality of waiting to decolour, and bleaching time is more than 5 minutes, and preferred add-on is 0.05%, and bleaching time is 15 minutes.
4, concentrate
Concentrate with acid vapour in the reboiler as thermal source, the multiple-effect concentrating unit be two imitate concentrate more than, preferred two imitate and concentrate, and along with the reduction of sodium-acetate concentration in the neutralizer, can suitably calculate the back and select triple effect or the concentrating unit of multiple-effect more.Concentrating unit is imitated in the present invention two, and each effect is divided into interchanger and evaporator room.Neutralizer is imitated the interchanger absorption from the latent heat of dark sour water acid vapour one, imitates the evaporator room evaporation one, produces one and imitates steam; One imitates steam imitates interchanger and neutralizer heat exchange two, and water of condensation connects a high liquid sealing pipe of 6m, and connects condenser, and neutralizer is imitated the evaporator room evaporation two, produces two and imitates steam; Two imitate steam passes through condenser condenses.
Each imitates the stream material to regulate the neutralizer turnover, and control one is imitated and is concentrated into concentration is 50% ~ 70% acetate trihydrate sodium solution, and two imitate and are concentrated into 90% ~ 100% acetate trihydrate sodium solution.
One imitate the evaporator room service temperature be 80 ~ 95 ℃, pressure be-0.03 ~-the 0.055MPa(gauge pressure); Two imitate the evaporator room service temperatures be 60 ~ 75 ℃, pressure be-0.07 ~-the 0.09MPa(gauge pressure).
5, crystallization
Crystallization is the continuous crystallisation mode.Cooling heat transferring is selected the plug-in interchanger of still formula.A large amount of sodium-acetate slurries are arranged as receiving mother liquor in the crystallization kettle, accept from the sodium acetate soln after concentrating, and be continuously pumped into the sodium-acetate centrifuge mother liquor.
Description of drawings
Fig. 1 is general flow chart of the present invention, and as shown in FIG.: 1 is that the colourless sour water of high temperature is to entering the dark acid water preheater of reboiler; 2 is dark sour water reboiler; 3 is the multiple-effect first-class heat exchanger; 4 is multiple-effect flash trapping stage chamber; 5 is the multiple-effect secondary heat exchanger; 6 is multiple-effect secondary separate chamber; 7 is the multiple-effect condenser; 8 are the wastewater collection jar; 9 is light sour water storage tank; 10 are neutralization decolouring still; 11 is crystallization kettle; 12 are the crystallization interchanger; 13 is whizzer; 14 is an effect forced circulation pump; 15 is an effect concentrated solution discharging pump; 16 is two effect forced circulation pumps; 17 is two effect concentrated solution discharging pumps; 18 is the sewage discharging pump; 19 are the crystallization forced circulation pump; 20 is the centrifuge mother liquor discharging pump; 21 are decolouring back neutralizer discharging pump.
Embodiment
Embodiment 1:
As shown in Figure 1,
1, acetic acid content be 10% dark waste acid water behind interchanger 1, go in the reboiler 2, utilize the living steam of 0.7MPa that dark waste acid water is heated, giving birth to steam flow is 1.1t/h, 130 ℃ of acid vapours.
2, acid vapour is imitated interchanger 3 and is entered a neutralizer heat exchange of imitating one, the acid vapour condensation is by the excess pressure liquid sealing pipe, the condensation sour water advances the dark waste acid water preheating of reboiler on 1 pair on interchanger, and the condensation sour water advances light sour water groove 9 after the heat exchange, mixes with the light sour water of acetic acid content 20%.
3, mix sour water in and in the still 10 with the soda ash neutralization, terminal point Ph value is 7.5, temperature is 40 ℃.
4, adding is stirred decolouring in 5 minutes with respect to the thiourea peroxide of neutralizer 0.1% in neutralizer.
5, the neutralizer after the decolouring is squeezed into one by pump 21 and is imitated concentrating unit.
6, the neutralizer behind the absorption acid vapour latent heat is imitated separate chamber's 4 vapor-liquid separation one, produces one and imitates secondary steam, and one imitates separate chamber's pressure is-the 0.03MPa(gauge pressure), an effect separate chamber concentrates 95 ℃ of back neutralizer temperature.
7, one imitate secondary steam and imitate interchanger 5 and the two neutralizer heat exchange of imitating two, one imitates the secondary steam condensation by the excess pressure liquid sealing pipe, after entering multiple-effect condenser 7 and cooling off, enters wastewater collection jar 8.
8, the neutralizer behind the absorption one effect secondary steam latent heat is imitated separate chambers' 6 vapor-liquid separation two, produces two and imitates secondary steams, and two effect separate chamber pressure are-the 0.07MPa(gauge pressure), it is 75 ℃ that two effect separate chambers concentrate back neutralizer temperature.
9, two effect secondary steams enter vacuum tightness-0.07MPa(gauge pressure) multiple-effect condenser 7, water enters wastewater collection jar 8 after the condensation.
10, two neutralizers of imitating after concentrating are squeezed into crystallization kettle 11 through pump 17, and crystallization forced circulation pump 19 is squeezed into crystallization interchanger 12 with feed liquid, crystallisation by cooling, and Tc is 45 ℃.
11, the crystallization disposed slurry is by whizzer 13 solid-liquid separation, and solid phase prod is packed, and liquid mother liquor is squeezed into crystallization kettle 11 through pump 20 circulations, as receiving the bottoming mother liquor.
The TAED wastewater treatment capacity is 30t/d, and steam consumption is the 1.8t/t Sodium acetate trihydrate.The every index of product is qualified and stable in the production process, and product and mother liquor do not have the color burn phenomenon.
Embodiment 2:
1, acetic acid content be 10% dark waste acid water behind interchanger 1, go in the reboiler 2, utilize the living steam of 0.4MPa that dark waste acid water is heated, giving birth to steam flow is 1.1t/h, 110 ℃ of acid vapours.
2, acid vapour is imitated interchanger 3 and is entered a neutralizer heat exchange of imitating one, the acid vapour condensation is by the excess pressure liquid sealing pipe, the condensation sour water advances the dark waste acid water preheating of reboiler on 1 pair on interchanger, and the condensation sour water advances light sour water groove 9 after the heat exchange, mixes with the light sour water of acetic acid content 20%.
3, mix sour water in and in the still 10 with the soda ash neutralization, terminal point Ph value is 10.5, temperature is 80 ℃.
4, adding is stirred decolouring in 15 minutes with respect to the thiourea peroxide of neutralizer 0.02% in neutralizer.
5, the neutralizer after the decolouring is squeezed into one by pump 21 and is imitated concentrating unit.
6, the neutralizer behind the absorption acid vapour latent heat is imitated separate chamber's 4 vapor-liquid separation one, produces one and imitates secondary steam, and one imitates separate chamber's pressure is-the 0.055MPa(gauge pressure), an effect separate chamber concentrates 80 ℃ of back neutralizer temperature.
7, one imitate secondary steam and imitate interchanger 5 and the two neutralizer heat exchange of imitating two, one imitates the secondary steam condensation by the excess pressure liquid sealing pipe, after entering multiple-effect condenser 7 and cooling off, enters wastewater collection jar 8.
8, the neutralizer behind the absorption one effect secondary steam latent heat is imitated separate chambers' 6 vapor-liquid separation two, produces two and imitates secondary steams, and two effect separate chamber pressure are-the 0.09MPa(gauge pressure), two effect separate chambers concentrate 60 ℃ of back neutralizer temperature
9, two effect secondary steams enter vacuum tightness-0.09MPa(gauge pressure) multiple-effect condenser 7, water enters wastewater collection jar 8 after the condensation.
10, two neutralizers of imitating after concentrating are squeezed into crystallization kettle 11 through pump 17, and crystallization forced circulation pump 19 is squeezed into crystallization interchanger 12 with feed liquid, crystallisation by cooling, and Tc is 45 ℃.
11, the crystallization disposed slurry is by whizzer 13 solid-liquid separation, and solid phase prod is packed, and liquid mother liquor is squeezed into crystallization kettle 11 through pump 20 circulations, as receiving the bottoming mother liquor.
The TAED wastewater treatment capacity is 30t/d, and steam consumption is the 1.6t/t Sodium acetate trihydrate.The every index of product is qualified and stable in the production process, and product and mother liquor do not have the color burn phenomenon.
The above only is preferred embodiment of the present invention, be not that the present invention is done any pro forma restriction, any for breaking away from invention technical scheme content, according to technical spirit of the present invention above embodiment is made any simple modification, equivalent variations and modification, all belong in the scope of technical solution of the present invention.
Claims (10)
- One kind tetraacetyl ethylene diamine produced in the combination treatment method of two kinds of waste acid waters, it is characterized in that comprising step: will wash the dark sour water evaporation that produces after the TAED crystallization with giving birth to steam, the acid vapour that evaporation produces carries out multiple-effect as thermal source to the neutralizer after decolouring and concentrates, crystallisation by cooling, solid-liquid separation gets the byproduct Sodium acetate trihydrate, dark sour water evaporites burns back heat energy and produces living steam recycling; Neutralizer after the described decolouring is: be condensed into colourless sour water after the acid vapour heat exchange, the light sour water that high temperature dehydration produces behind acetic acid and the reacting ethylenediamine in colourless sour water and the TAED production process mixes, add the alkali neutralization, then the liquid that generates with thiourea peroxide decolouring back.
- 2. combination treatment method as claimed in claim 1 is characterized in that, described multiple-effect simmer down to two is imitated and concentrated.
- 3. combination treatment method as claimed in claim 2 is characterized in that, described neutralizer flows in two effects concentrate and is following current.
- 4. combination treatment method as claimed in claim 3 is characterized in that, concentrates 60 ~ 75 ℃ of back liquid drop temperatures.
- 5. combination treatment method as claimed in claim 4 is characterized in that, one imitate temperature be 80 ~ 95 ℃, pressure be-0.03 ~-0.055MPa; Two imitate temperature be 60 ~ 75 ℃, pressure be-0.07 ~-0.09MPa.
- 6. combination treatment method as claimed in claim 5 is characterized in that, described thiourea peroxide usage quantity is 0.02% ~ 0.1% of neutralizer quality.
- 7. combination treatment method as claimed in claim 5 is characterized in that, described thiourea peroxide usage quantity is 0.05% of neutralizer quality.
- 8. combination treatment method as claimed in claim 5 is characterized in that, described bleaching temperature is 40 ~ 80 ℃.
- 9. combination treatment method as claimed in claim 5 is characterized in that, described bleaching time is 5 minutes to 24 hours.
- 10. combination treatment method as claimed in claim 8 is characterized in that, described bleaching time is 15 minutes.
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| CN103193670B (en) * | 2013-04-02 | 2015-01-07 | 浙江金科日化原料有限公司 | System for recovering heat generated in production of tetraacetylethylenediamine |
| CN109354211A (en) * | 2018-10-29 | 2019-02-19 | 侨昌现代农业有限公司 | The method for preparing efficient carbon source sewage-treating agent needed for denitrifying microorganism with by-product sodium acetate |
| CN113101682B (en) * | 2021-05-28 | 2023-03-24 | 新疆心连心能源化工有限公司 | Device for reducing evaporation of condensation compound and stabilizing urea production and treatment method |
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| CN101492362A (en) * | 2008-01-25 | 2009-07-29 | 山东方兴科技开发有限公司 | Production process for large-particle sodium acetate |
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