CN109232233A - A kind of system and method handling the mixed acid containing phosphoric acid, nitric acid and acetic acid - Google Patents
A kind of system and method handling the mixed acid containing phosphoric acid, nitric acid and acetic acid Download PDFInfo
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- CN109232233A CN109232233A CN201811277704.8A CN201811277704A CN109232233A CN 109232233 A CN109232233 A CN 109232233A CN 201811277704 A CN201811277704 A CN 201811277704A CN 109232233 A CN109232233 A CN 109232233A
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- acid
- reaction tank
- neutralization reaction
- sodium nitrate
- phosphoric acid
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title claims abstract description 135
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 239000002253 acid Substances 0.000 title claims abstract description 62
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 49
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910017604 nitric acid Inorganic materials 0.000 title claims abstract description 27
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 123
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 78
- 239000004317 sodium nitrate Substances 0.000 claims abstract description 62
- 235000010344 sodium nitrate Nutrition 0.000 claims abstract description 62
- 238000001035 drying Methods 0.000 claims abstract description 51
- 238000004821 distillation Methods 0.000 claims abstract description 40
- 239000007787 solid Substances 0.000 claims abstract description 36
- 238000001704 evaporation Methods 0.000 claims abstract description 31
- 230000008020 evaporation Effects 0.000 claims abstract description 31
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 27
- 239000000203 mixture Substances 0.000 claims abstract description 25
- 238000006396 nitration reaction Methods 0.000 claims abstract description 25
- 238000002425 crystallisation Methods 0.000 claims abstract description 23
- 230000008025 crystallization Effects 0.000 claims abstract description 23
- 239000001632 sodium acetate Substances 0.000 claims abstract description 20
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- 239000012530 fluid Substances 0.000 claims description 25
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 16
- 239000010865 sewage Substances 0.000 claims description 16
- 238000009833 condensation Methods 0.000 claims description 15
- 230000005494 condensation Effects 0.000 claims description 15
- 239000000706 filtrate Substances 0.000 claims description 14
- 239000002893 slag Substances 0.000 claims description 11
- 239000000047 product Substances 0.000 claims description 8
- 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 description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 7
- 239000011574 phosphorus Substances 0.000 claims description 7
- 229910052698 phosphorus Inorganic materials 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 229940087562 sodium acetate trihydrate Drugs 0.000 claims description 7
- 239000011973 solid acid Substances 0.000 claims description 6
- 230000018044 dehydration Effects 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 3
- VNFVKWMKVDOSKT-LREBCSMRSA-N (2r,3r)-2,3-dihydroxybutanedioic acid;piperazine Chemical compound C1CNCCN1.OC(=O)[C@H](O)[C@@H](O)C(O)=O VNFVKWMKVDOSKT-LREBCSMRSA-N 0.000 claims description 2
- BTYPWVDULNVBHU-UHFFFAOYSA-N disodium;dinitrate Chemical compound [Na+].[Na+].[O-][N+]([O-])=O.[O-][N+]([O-])=O BTYPWVDULNVBHU-UHFFFAOYSA-N 0.000 claims 1
- 239000002699 waste material Substances 0.000 abstract description 6
- 238000009835 boiling Methods 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 4
- 235000011121 sodium hydroxide Nutrition 0.000 description 4
- 238000003912 environmental pollution Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- BDKZHNJTLHOSDW-UHFFFAOYSA-N [Na].CC(O)=O Chemical compound [Na].CC(O)=O BDKZHNJTLHOSDW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- -1 filter Chemical compound 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
- C01B25/234—Purification; Stabilisation; Concentration
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D9/00—Nitrates of sodium, potassium or alkali metals in general
- C01D9/04—Preparation with liquid nitric acid
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Materials Engineering (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The present invention discloses a kind of system and method for handling the mixed acid containing phosphoric acid, nitric acid and acetic acid, belong to field of waste liquid treatment, the processing system includes filter (1), distillation equipment (2), bleacher (3), condenser I (4), neutralization reaction tank I (5), sodium nitrate evaporation drying device (6), neutralization reaction tank II (7), neutralization reaction tank III (8), sodium acetate evaporative crystallization drying device (9) and condenser II (10).The system of mixed acid of the processing containing phosphoric acid, nitric acid and acetic acid of the present invention, the high boiling phosphoric acid in nitration mixture can be separated in distillation equipment, the purity of resulting sodium nitrate solid and sodium acetate solid is recycled 99% or more, not only avoid the pollution to environment, and recovery article can also further be sold, and economic benefit is improved.
Description
Technical field
The invention belongs to field of waste liquid treatment, and in particular to a kind of mixed acid of the processing containing phosphoric acid, nitric acid and acetic acid
System and method.
Background technique
In recent years the liquid crystal manufacturing industry and semiconductor manufacturing industry developed rapidly, flows out a variety of waste water in its manufacturing process,
But it is discharged after the processing adapted to according to implementations such as the type of each waste water, properties.For example, from liquid crystal manufacturing process or semiconductor system
The mixed acid waste liquor that outflow acetic acid, nitric acid, phosphoric acid are mixed to form during making, if can for example separate and recover phosphorus in these mixed acid waste liquors
Acid as fertilizer it is expected that efficiently use, but be technically also difficult to separate and recover phosphorus from such nitration mixture degree liquid at present
Acid, so being drained after generally implementing neutralisation treatment to this mixed acid waste liquor.But directly after neutralisation treatment draining exist with
Lower defect:
(1) the reason of forming the salt such as acetate, nitrate and phosphate after neutralizing, unavoidably becoming Heavy environmental pollution；
(2) discharge method of neutralisation treatment is not recycle spent acid completely and discard ground method, causes the waste of resource.
Summary of the invention
In order to solve the defect of above-mentioned environmental pollution existing in the prior art and the wasting of resources, the invention proposes one
The system and method for mixed acid of the kind processing containing phosphoric acid, nitric acid and acetic acid.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of system handling the mixed acid containing phosphoric acid, nitric acid and acetic acid, including filter, distillation equipment, bleacher, condensation
Device I, neutralization reaction tank I, sodium nitrate evaporation drying device, neutralization reaction tank II, neutralization reaction tank III, sodium acetate evaporative crystallization are dry
Dry device and condenser II, the filter are connected with distillation equipment by fluid pipeline, distillation equipment by fluid pipeline with
Bleacher is connected, and distillation equipment is connected by gas pipeline with condenser I, and condenser I passes through fluid pipeline and neutralization reaction tank I
It is connected, neutralization reaction tank I is connected by fluid pipeline with sodium nitrate evaporation drying device, and sodium nitrate evaporation drying device passes through gas
Body pipeline is connected with condenser II, and neutralization reaction tank II is connected by fluid pipeline with sodium nitrate evaporation drying device, condenser
II is connected by fluid pipeline with neutralization reaction tank III, and neutralization reaction tank III is dry by fluid pipeline and sodium acetate evaporative crystallization
Device is connected.
In this system, the trend of material are as follows: the nitration mixture wait dispose is introduced into filter after being separated by solid-liquid separation, solid slag removing,
Filtrate enters distillation equipment, obtains phosphoric acid solution and nitration mixture steam；Phosphoric acid solution enters bleacher decoloration, and nitration mixture steam enters cold
Condenser I obtains the acid gas of mixed acid solution and non-total condensation；Mixed acid solution enters neutralization reaction tank I, in neutralization reaction tank I
Soda bath reaction after, obtained solution enters sodium nitrate evaporation drying device, obtain sodium nitrate solid and acetic acid steam, this
Solid enters neutralization reaction tank II after water-soluble and neutralization reaction occurs, and the sodium nitrate solution after neutralization enters sodium nitrate evaporation drying
Device, acetic acid steam enter condenser II, obtain acetic acid liquid, and acetic acid liquid enters neutralization reaction tank III and reacts with soda bath
Afterwards, into sodium acetate evaporative crystallization drying device, Sodium acetate trihydrate solid is obtained.
It further, further include with water pot, described to be arranged between distillation equipment and bleacher with water pot, distillation equipment is logical
It crosses fluid pipeline to be connected with water pot, be connected by fluid pipeline with bleacher with water pot.
It further, further include sewage-treatment plant, sewage-treatment plant passes through process condensate delivery pipe and sodium nitrate
Evaporation drying device is connected, and sewage-treatment plant passes through process condensate delivery pipe and sodium acetate evaporative crystallization drying device phase
Even.
It further, further include exhaust gas processing device, the exhaust gas processing device passes through gas pipeline and I phase of condenser
Even, the exhaust gas processing device is connected by gas pipeline with condenser II.
Soda bath is housed in the neutralization reaction tank I, neutralization reaction tank II and neutralization reaction tank III.
The method of mixed acid based on the processing of above system containing phosphoric acid, nitric acid and acetic acid, comprising the following steps:
S1: nitration mixture to be disposed being added in filter and is separated by solid-liquid separation, filtrate and solid slag are obtained, solid slag is removed, will be described
Filtrate, which adds in distillation equipment, is distilled, and high concentration phosphorus acid solution and nitration mixture steam are obtained, and the high concentration phosphorus acid solution is added
It decolourizes to bleacher；
S2: by the nitration mixture steam through condenser condense mixed acid solution and non-total condensation acid gas, by the mixed acid solution
Neutralization reaction tank I is added to, after reacting with the soda bath in neutralization reaction tank I, acquired solution is added into sodium nitrate evaporation drying
Sodium nitrate solid and acetic acid steam are evaporated to obtain in device；
S3: the sodium nitrate solid is added in neutralization reaction tank II after water dissolves, molten with the caustic soda in neutralization reaction tank II
Liquid is neutralized, its pH value 7.5-10.5 is controlled；Sodium nitrate solution after neutralization is added to again in sodium nitrate evaporation drying device
After being evaporated dehydration, sodium nitrate crystallization and drying, high-purity sodium nitrate solid and process condensate I are obtained；
S4: by the acetic acid steam after condensing, adding in neutralization reaction tank III and react with soda bath, controls its pH value and exists
7.5-10.5, then acquired solution is added in sodium acetate evaporative crystallization drying device and is evaporated crystallizing and drying, obtain high-purity
Sodium acetate trihydrate solid and process condensate II.
Further, the high concentration phosphorus acid solution is added to before bleacher decolourized, is first added to in water pot
The phosphoric acid product of concentration needed for obtaining is mixed with desalted water.
Further, it is sent after the process condensate I and process condensate II being converged to sewage-treatment plant and is disposed.
Further, the acid gas of the non-total condensation is sent to exhaust gas processing device processing.
Further, the filtrate is added to when being distilled in distillation equipment, temperature is 100-200 DEG C, and pressure is
Under 0.1-0.8barA, distillation time 0.5-5h.
Compared with prior art, the beneficial effects of the present invention are:
The system of mixed acid of the processing containing phosphoric acid, nitric acid and acetic acid of the present invention, can will be in nitration mixture in distillation equipment
High boiling phosphoric acid separate, recycle the purity of resulting sodium nitrate solid and sodium acetate solid 99% or more, can be into
Row further sale, improves economic benefit, avoids environmental pollution.
Detailed description of the invention
Fig. 1 is the schematic diagram of embodiment one,
Fig. 2 is the schematic diagram of embodiment two；
In figure: 1- filter, 2- distillation equipment, 3- bleacher, 4- condenser I, 5- neutralization reaction tank I, the evaporation of 6- sodium nitrate are dry
Dry device, 7- neutralization reaction tank II, 8- neutralization reaction tank III, 9- sodium acetate evaporative crystallization drying device, 10- condenser II, 11-
With water pot, 12- sewage-treatment plant, 13- exhaust gas processing device.
Specific embodiment
For a clearer understanding of the technical characteristics, objects and effects of the present invention, this hair of Detailed description of the invention is now compareed
Bright specific embodiment, but protection scope of the present invention be not limited to it is as described below.
Embodiment one
A kind of system handling the mixed acid containing phosphoric acid, nitric acid and acetic acid, as shown in Figure 1, including filter 1, distillation equipment
2, bleacher 3, condenser I 4, neutralization reaction tank I 5, sodium nitrate evaporation drying device 6, neutralization reaction tank II 7, neutralization reaction tank
III 8, sodium acetate evaporative crystallization drying device 9, condenser II 10, the filter 1 pass through fluid pipeline phase with distillation equipment 2
Even, distillation equipment 2 is connected by fluid pipeline with bleacher 3, and distillation equipment 2 is connected by gas pipeline with condenser I 4, cold
Condenser I 4 is connected by fluid pipeline with neutralization reaction tank I 5, and neutralization reaction tank I 5 passes through fluid pipeline and sodium nitrate evaporation drying
Device 6 is connected, and sodium nitrate evaporation drying device 6 is connected by gas pipeline with condenser II 10, and neutralization reaction tank II 7 passes through liquid
Body pipeline is connected with sodium nitrate evaporation drying device 6, and condenser II 10 is connected by fluid pipeline with neutralization reaction tank III 8, in
It is connected by fluid pipeline with sodium acetate evaporative crystallization drying device 9 with reactor tank III 8.
In the present embodiment system, the trend of material are as follows: the nitration mixture wait dispose first is pumped into filter 1 after being separated by solid-liquid separation, Gu
Slag removing, filtrate are pumped into distillation equipment 2, obtain phosphoric acid solution and nitration mixture steam；Phosphoric acid solution is pumped into the decoloration of bleacher 3, nitration mixture
Steam enters condenser I 4, obtains the acid gas of mixed acid solution and non-total condensation；Mixed acid solution is pumped into neutralization reaction tank I 5, in
After the soda bath reaction in reactor tank I 5, obtained solution is pumped into sodium nitrate evaporation drying device 6, obtains sodium nitrate solid
With acetic acid steam, this solid enters neutralization reaction tank II 7 after water-soluble and neutralization reaction occurs, and the sodium nitrate solution after neutralization is pumped into
Sodium nitrate evaporation drying device 6, obtains high-purity sodium nitrate solid and process condensate water, and acetic acid steam enters condenser II 10, obtains
The exhaust gas of acetic acid liquid and non-total condensation, acetic acid liquid are pumped into after neutralization reaction tank III 8 reacts with soda bath, are pumped into acetic acid
Sodium evaporative crystallization drying device 9, obtains Sodium acetate trihydrate solid and process condensate water.
Embodiment two
The present embodiment advanced optimizes on the basis of example 1, further includes with water pot 11, sewage-treatment plant 12 and tail gas
Processing unit 13；Described to be arranged between distillation equipment 2 and bleacher 3 with water pot 11, distillation equipment 2 passes through fluid pipeline and matches
Water pot 11 is connected, and is connected by fluid pipeline with bleacher 3 with water pot 11；The sewage-treatment plant 12 passes through process condensate
Delivery pipe is connected with sodium nitrate evaporation drying device 6, and sewage-treatment plant 12 is steamed by process condensate delivery pipe and sodium acetate
Crystallizing and drying device 9 is sent out to be connected；The exhaust gas processing device 13 is connected by gas pipeline with condenser I 4, the vent gas treatment
Device 13 is connected by gas pipeline with condenser II 10.
In the present embodiment, the phosphoric acid solution obtained at distillation equipment 2 enters with water pot 11 and with the desalted water in water pot 11
Mixing, after being configured to the phosphoric acid for needing concentration, enters back into bleacher 3 and decolourizes；At condenser I 4 and at condenser II 10 not
The exhaust gas of total condensation is sent to the processing of exhaust gas processing device 13；At sodium nitrate evaporation drying device 6 and sodium acetate evaporative crystallization is dry
The process condensate obtained at dry device 9 enters sewage-treatment plant 12.
The invention also includes a kind of method for handling the mixed acid containing phosphoric acid, nitric acid and acetic acid, this method is based on upper
The method for stating the system of mixed acid of the processing containing phosphoric acid, nitric acid and acetic acid.
Embodiment one
A method of mixed acid of the processing containing phosphoric acid, nitric acid and acetic acid, comprising the following steps:
S1: nitration mixture to be disposed being added in filter 1 and is separated by solid-liquid separation, filtrate and solid slag are obtained, solid slag is removed, will be described
Filtrate, which adds in distillation equipment 2, is distilled, and distillation condition is 200 DEG C of temperature, and pressure is under 0.1barA, and distillation time is
0.5h；70-90% phosphoric acid solution and nitration mixture steam, the phosphoric acid solution of 70-90% is added to mixing in water pot 11 with desalted water
The phosphoric acid product for preparing required concentration is closed, then obtained certain density phosphoric acid product is added into bleacher 3 and is decolourized；
S2: by the nitration mixture steam through condenser 4 condense mixed acid solution and non-total condensation acid gas, by the mixed acid solution
Neutralization reaction tank I 5 is added to, after reacting with the soda bath in neutralization reaction tank I 5, it is dry that acquired solution is added into sodium nitrate evaporation
It is evaporated to obtain sodium nitrate solid and acetic acid steam in dry device 6, the acid gas of the non-total condensation is sent to vent gas treatment and is filled
Set 13 processing；
S3: the sodium nitrate solid is added in neutralization reaction tank II 7 after water dissolves, with the caustic soda in neutralization reaction tank II 7
Solution is neutralized, its pH value 7.5-10.5 is controlled；Sodium nitrate solution after neutralization is added into sodium nitrate evaporation drying device 6 again
In be evaporated dehydration, sodium nitrate crystallization and it is dry after, obtain the sodium nitrate solid and process condensate of 99.3 % of purity
Ⅰ；
S4: by the acetic acid steam after condensing, adding in neutralization reaction tank III 8 and react with soda bath, controls its pH value and exists
7.5-10.5, then acquired solution is added in sodium acetate evaporative crystallization drying device 9 and is evaporated crystallizing and drying, obtain purity
99.5% Sodium acetate trihydrate solid and process condensate II；Sent after the process condensate I and process condensate II are converged to
Sewage-treatment plant 12 is disposed.
Embodiment two
A method of mixed acid of the processing containing phosphoric acid, nitric acid and acetic acid, comprising the following steps:
S1: nitration mixture to be disposed being added in filter 1 and is separated by solid-liquid separation, filtrate and solid slag are obtained, solid slag is removed, will be described
Filtrate, which adds in distillation equipment 2, is distilled, and distillation condition is 100 DEG C of temperature, and pressure is distillation time 5h under 0.8barA；
70-90% phosphoric acid solution and nitration mixture steam, the phosphoric acid solution of 70-90% is added to being mixed in water pot 11 with desalted water
The phosphoric acid product of concentration needed for obtaining, then obtained certain density phosphoric acid product is added into bleacher 3 and is decolourized；
S2: by the nitration mixture steam through condenser 4 condense mixed acid solution and non-total condensation acid gas, by the mixed acid solution
Neutralization reaction tank I 5 is added to, after reacting with the soda bath in neutralization reaction tank I 5, it is dry that acquired solution is added into sodium nitrate evaporation
It is evaporated to obtain sodium nitrate solid and acetic acid steam in dry device 6, the acid gas of the non-total condensation is sent to vent gas treatment and is filled
Set 13 processing；
S3: the sodium nitrate solid is added in neutralization reaction tank II 7 after water dissolves, with the caustic soda in neutralization reaction tank II 7
Solution is neutralized, its pH value 7.5-10.5 is controlled；Sodium nitrate solution after neutralization is added into sodium nitrate evaporation drying device 6 again
In be evaporated dehydration, sodium nitrate crystallization and it is dry after, obtain the sodium nitrate solid and process condensate of 99.4 % of purity
Ⅰ；
S4: by the acetic acid steam after condensing, adding in neutralization reaction tank III 8 and react with soda bath, controls its pH value and exists
7.5-10.5, then acquired solution is added in sodium acetate evaporative crystallization drying device 9 and is evaporated crystallizing and drying, obtain purity
99.7% Sodium acetate trihydrate solid and process condensate II；Sent after the process condensate I and process condensate II are converged to
Sewage-treatment plant 12 is disposed.
Embodiment three
A method of mixed acid of the processing containing phosphoric acid, nitric acid and acetic acid, comprising the following steps:
S1: nitration mixture to be disposed being added in filter 1 and is separated by solid-liquid separation, filtrate and solid slag are obtained, solid slag is removed, will be described
Filtrate, which adds in distillation equipment 2, is distilled, and distillation condition is 150 DEG C of temperature, and pressure is distillation time 3h under 0.4barA；
70-90% phosphoric acid solution and nitration mixture steam, the phosphoric acid solution of 70-90% is added to being mixed in water pot 11 with desalted water
The phosphoric acid product of concentration needed for obtaining, then obtained certain density phosphoric acid product is added into bleacher 3 and is decolourized；
S2: by the nitration mixture steam through condenser 4 condense mixed acid solution and non-total condensation acid gas, by the mixed acid solution
Neutralization reaction tank I 5 is added to, after reacting with the soda bath in neutralization reaction tank I 5, it is dry that acquired solution is added into sodium nitrate evaporation
It is evaporated to obtain sodium nitrate solid and acetic acid steam in dry device 6, the acid gas of the non-total condensation is sent to vent gas treatment and is filled
Set 13 processing；
S3: the sodium nitrate solid is added in neutralization reaction tank II 7 after water dissolves, with the caustic soda in neutralization reaction tank II 7
Solution is neutralized, its pH value 7.5-10.5 is controlled；Sodium nitrate solution after neutralization is added into sodium nitrate evaporation drying device 6 again
In be evaporated dehydration, sodium nitrate crystallization and it is dry after, obtain the sodium nitrate solid and process condensate of 99.4 % of purity
Ⅰ；
S4: by the acetic acid steam after condensing, adding in neutralization reaction tank III 8 and react with soda bath, controls its pH value and exists
7.5-10.5, then acquired solution is added in sodium acetate evaporative crystallization drying device 9 and is evaporated crystallizing and drying, obtain purity
99.6% Sodium acetate trihydrate solid and process condensate II；Sent after the process condensate I and process condensate II are converged to
Sewage-treatment plant 12 is disposed.
Disclosed above is only presently preferred embodiments of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, therefore makees ground equivalent variations according to the claims in the present invention, be still within the scope of the present invention.
Claims (10)
1. a kind of system for handling the mixed acid containing phosphoric acid, nitric acid and acetic acid, it is characterised in that: including filter (1), distillation
Equipment (2), bleacher (3), condenser I (4), neutralization reaction tank I (5), sodium nitrate evaporation drying device (6), neutralization reaction tank
II (7), neutralization reaction tank III (8), sodium acetate evaporative crystallization drying device (9) and condenser II (10)；The filter (1) with
Distillation equipment (2) is connected by fluid pipeline, and distillation equipment (2) is connected by fluid pipeline with bleacher (3), distillation equipment
(2) it is connected by gas pipeline with condenser I (4), condenser I (4) is connected by fluid pipeline with neutralization reaction tank I (5), in
It is connected by fluid pipeline with sodium nitrate evaporation drying device (6) with reactor tank I (5), sodium nitrate evaporation drying device (6) passes through
Gas pipeline is connected with condenser II (10), and neutralization reaction tank II (7) passes through fluid pipeline and sodium nitrate evaporation drying device (6)
It is connected, condenser II (10) is connected by fluid pipeline with neutralization reaction tank III (8), and neutralization reaction tank III (8) passes through liquid line
Road is connected with sodium acetate evaporative crystallization drying device (9).
2. a kind of system for handling the mixed acid containing phosphoric acid, nitric acid and acetic acid according to claim 1, feature exist
In: it further include with water pot (11), described to be arranged between distillation equipment (2) and bleacher (3) with water pot (11), distillation equipment
(2) it is connected by fluid pipeline with water pot (11), is connected by fluid pipeline with bleacher (3) with water pot (11).
3. a kind of system for handling the mixed acid containing phosphoric acid, nitric acid and acetic acid according to claim 1 or 2, feature
It is: further includes sewage-treatment plant (12), sewage-treatment plant (12) is evaporated by process condensate delivery pipe and sodium nitrate
Drying device (6) is connected, and sewage-treatment plant (12) passes through process condensate delivery pipe and sodium acetate evaporative crystallization drying device
(9) it is connected.
4. a kind of system for handling the mixed acid containing phosphoric acid, nitric acid and acetic acid according to claim 3, feature exist
In: it further include exhaust gas processing device (13), the exhaust gas processing device (13) is connected by gas pipeline with condenser I (4), institute
Exhaust gas processing device (13) are stated to be connected by gas pipeline with condenser II (10).
5. a kind of system for handling the mixed acid containing phosphoric acid, nitric acid and acetic acid according to claim 1, feature exist
In: soda bath is housed in the neutralization reaction tank I (5), neutralization reaction tank II (7) and neutralization reaction tank III (8).
6. the processing of the system based on any one of the claim 1-5 mixed acid of the processing containing phosphoric acid, nitric acid and acetic acid contains
There is the method for the mixed acid of phosphoric acid, nitric acid and acetic acid, which comprises the following steps:
S1: nitration mixture to be disposed being added in filter (1) and is separated by solid-liquid separation, filtrate and solid slag is obtained, solid slag is removed, by institute
It states filtrate and adds in distillation equipment (2) and distilled, obtain high concentration phosphorus acid solution and nitration mixture steam, the high-concentration phosphoric acid is molten
Liquid adds to bleacher (3) and decolourizes；
S2: by the nitration mixture steam through condenser (4) condense mixed acid solution and non-total condensation acid gas, the nitration mixture is molten
Liquid adds to neutralization reaction tank I (5), and after the soda bath reaction in neutralization reaction tank I (5), acquired solution is added to sodium nitrate
Sodium nitrate solid and acetic acid steam are evaporated to obtain in evaporation drying device (6)；
S3: the sodium nitrate solid is added in neutralization reaction tank II (7) after water dissolves, in neutralization reaction tank II (7)
Soda bath is neutralized, its pH value 7.5-10.5 is controlled；Sodium nitrate solution after neutralization is added into sodium nitrate evaporation drying again
After being evaporated dehydration, sodium nitrate crystallization and drying in device (6), high-purity sodium nitrate solid and process condensate are obtained
Ⅰ；
S4: it by the acetic acid steam after condensing, adds in neutralization reaction tank III (8) and is reacted with soda bath, control its pH value
In 7.5-10.5, then acquired solution is added in sodium acetate evaporative crystallization drying device (9) and is evaporated crystallizing and drying, obtains height
Purity Sodium acetate trihydrate solid and process condensate II.
7. the method for mixed acid of the processing containing phosphoric acid, nitric acid and acetic acid according to claim 6, it is characterised in that: will
The high concentration phosphorus acid solution adds to before bleacher decolourized, and is first added to being mixed in water pot (11) with desalted water
The phosphoric acid product of concentration needed for obtaining.
8. the method for mixed acid of the processing containing phosphoric acid, nitric acid and acetic acid according to claim 6 or 7, it is characterised in that:
It is sent after the process condensate I and process condensate II are converged to sewage-treatment plant (12) and is disposed.
9. the method for mixed acid of the processing containing phosphoric acid, nitric acid and acetic acid according to claim 6 or 7, it is characterised in that:
The acid gas of the non-total condensation is sent to exhaust gas processing device (13) and is handled.
10. the method for mixed acid of the processing containing phosphoric acid, nitric acid and acetic acid according to claim 6 or 7, feature exist
In: the filtrate is added in distillation equipment (2) distilled when, temperature be 100-200 DEG C, pressure be 0.1-0.8barA under,
Distillation time is 0.5-5h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811277704.8A CN109232233A (en) | 2018-10-30 | 2018-10-30 | A kind of system and method handling the mixed acid containing phosphoric acid, nitric acid and acetic acid |
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| CN201811277704.8A CN109232233A (en) | 2018-10-30 | 2018-10-30 | A kind of system and method handling the mixed acid containing phosphoric acid, nitric acid and acetic acid |
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| CN110590036A (en) * | 2019-09-03 | 2019-12-20 | 四川蓝魔方环境科技有限公司 | Waste acid resource recycling process |
| CN111020614A (en) * | 2019-12-31 | 2020-04-17 | 湖北永绍科技股份有限公司 | Method for recycling phosphoric acid by electrolyzing mixed acid solution |
| CN115028526A (en) * | 2022-06-18 | 2022-09-09 | 黄冈Tcl环境科技有限公司 | Method for treating secondary waste acid generated after evaporation of waste etching solution |
| CN115974020A (en) * | 2023-01-04 | 2023-04-18 | 瀚蓝工业服务(嘉兴)有限公司 | Process for resource production of ammonium dihydrogen phosphate and byproducts from waste phosphoric acid in chip industry |
| CN116040596A (en) * | 2022-01-09 | 2023-05-02 | 四川大学 | Comprehensive utilization method of phosphoric acid by wet method with nitric acid method |
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