CN108147446A - The nitration mixture treatment process and its special equipment of a kind of hydrochloric acid and hydrofluoric acid - Google Patents
The nitration mixture treatment process and its special equipment of a kind of hydrochloric acid and hydrofluoric acid Download PDFInfo
- Publication number
- CN108147446A CN108147446A CN201710875045.7A CN201710875045A CN108147446A CN 108147446 A CN108147446 A CN 108147446A CN 201710875045 A CN201710875045 A CN 201710875045A CN 108147446 A CN108147446 A CN 108147446A
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- CN
- China
- Prior art keywords
- filter
- nitration mixture
- retort
- hydrochloric acid
- calcium chloride
- 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.)
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 47
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000000203 mixture Substances 0.000 title claims abstract description 32
- 238000006396 nitration reaction Methods 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 18
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 26
- 239000001110 calcium chloride Substances 0.000 claims abstract description 18
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000292 calcium oxide Substances 0.000 claims abstract description 9
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 8
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 4
- 239000002002 slurry Substances 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 8
- 238000005276 aerator Methods 0.000 claims description 6
- 239000002893 slag Substances 0.000 claims description 6
- 239000002699 waste material Substances 0.000 abstract description 7
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 230000001376 precipitating effect Effects 0.000 abstract description 2
- 229910001634 calcium fluoride Inorganic materials 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 241000370738 Chlorion Species 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- QGHDLJAZIIFENW-UHFFFAOYSA-N 4-[1,1,1,3,3,3-hexafluoro-2-(4-hydroxy-3-prop-2-enylphenyl)propan-2-yl]-2-prop-2-enylphenol Chemical group C1=C(CC=C)C(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C(CC=C)=C1 QGHDLJAZIIFENW-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 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
- 239000000047 product Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- -1 that is Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/22—Fluorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/03—Preparation from chlorides
- C01B7/035—Preparation of hydrogen chloride from chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention discloses the nitration mixture treatment process and its special equipment of a kind of hydrochloric acid and hydrofluoric acid, and its step are as follows：(1) nitration mixture and weight percent concentration are placed in hybrid reaction in the first retort for 2% 65% calcium chloride solution；(2) fully after reaction, reaction product is filtered by filter；Its filter residue and weight percent concentration are placed in hybrid reaction in the second retort for 20% 65% calcium oxide solution；Its filtrate is collected him and is used；(3) fully after reaction, reaction product is passed through into pressure filter press filtration；The calcium chloride solution that its filtrate is recycled to step (1) for calcium chloride solution is for use；Its filter residue is calcirm-fluoride, as hydrogen fluoride production raw material.The present invention uses CaCl2It, can be with the treatment of wastes with processes of wastes against one another as the precipitating reagent of HF.
Description
Technical field
The present invention relates to a kind of nitration mixture treatment process, specially the nitration mixture treatment process of hydrochloric acid and hydrofluoric acid and its special set
It is standby, belong to environmental technology field.
Background technology
Lithium hexafluoro phosphate is the core material of lithium battery electrolytes, can be generated containing hydrochloric acid, hydrofluoric acid in production process
By-product, that is, waste mixed acid (hereinafter referred to as spent acid).Spent acid is generally containing HCl 30%, HF 7.0%~10%, because containing rotten in spent acid
Corrosion is strong, toxic is big, the HF of difficult separation causes a large amount of hydrochloric acid in spent acid to be difficult to directly utilize, therefore increases the pressure of environmental protection
Power, the present invention are the processing units of a systematization, and the HF in spent acid is made to be converted into raw materials for production, reduce containing for HF in hydrochloric acid
Amount, enables hydrochloric acid to utilize, reduces the pollution to environment, achieve the purpose that waste acid resource.
Invention content
The purpose of the invention is to provide the nitration mixture treatment process and its special equipment of a kind of hydrochloric acid and hydrofluoric acid, with solution
The certainly above problem of the prior art.
The purpose of the present invention is be achieved through the following technical solutions.
The nitration mixture treatment process of a kind of hydrochloric acid and hydrofluoric acid, its step are as follows：
(1) nitration mixture is placed in the calcium chloride solution that weight percent concentration is 2%-65% in the first retort and mixed instead
It should；
(2) fully after reaction, reaction product is filtered by filter；Its filter residue is 20%- with weight percent concentration
65% calcium oxide solution is placed in hybrid reaction in the second retort；Its filtrate is collected him and is used；
(3) fully after reaction, reaction product is passed through into pressure filter press filtration；Its filtrate is recycled to step for calcium chloride solution
(1) calcium chloride solution is for use；Its filter residue is calcirm-fluoride, as hydrogen fluoride production raw material.
In step (1), nitration mixture and CaCl2The mixed temperature of solution is 30 DEG C~60 DEG C.
The special equipment of the nitration mixture treatment process of hydrochloric acid and hydrofluoric acid, nitration mixture storage tank and calcium chloride including storing nitration mixture are matched
Slurry pipe, the nitration mixture storage tank and calcium chloride slurry commanding tank connect respectively from bottom with the top of the first retort；First retort
Bottom be provided with aerator；First retort is connected by pipeline with first filter inlet, and first filter goes out
Liquid mouth is connected with hydrochloric acid tank, and the slag notch of first filter is connected with the top of the second retort；Second retort also with oxygen
Change the connection of calcium slurry commanding tank；The bottom of second retort is provided with aerator；The liquid outlet of second reactor and the second filtering
The inlet connection of device；The liquid outlet of second filter is connected with calcium chloride slurry commanding tank, the slag notch of the second filter and fluorination
Calcium storage tank connects.
Second filter is dry filter.
The temperature of second filter：40 DEG C~95 DEG C；Vacuum degree during filtering is：- 90kP~-20kP.
The invention has the advantages that：
1st, using CaCl2As the precipitating reagent of HF, CaCl2It is the waste product of soda industry, it can be with the treatment of wastes with processes of wastes against one another；
2nd, the suitable temperature of control makes CaF2Generate the particle easily filtered out；
3rd, the solution normal filtration after reaction can be enable using special filter type；
4th, using lime to CaF2Refine and can ensure CaF2Recycling to the greatest extent；
5th, CaF can be made using dry filter mode2Meet the requirement as raw material.
Description of the drawings
Fig. 1 is the processing technological flow figure of the present invention；
Fig. 2 is special equipment scheme of installation of the present invention；
In figure, 1, nitration mixture storage tank 2, calcium chloride slurry commanding tank 3, the first retort 4, first filter 5, hydrochloric acid tank
6th, calcium oxide slurry commanding tank 7, the second retort 8, the second filter 9, calcirm-fluoride storage tank 10, aerator.
Specific embodiment
Below in conjunction with the accompanying drawings with the specific embodiment technical solution that the present invention is further explained.
Hydrochloric acid as shown in Figure 2 and the special equipment of the nitration mixture treatment process of hydrofluoric acid, the nitration mixture storage including storing nitration mixture
Tank and calcium chloride pipe with slurry, the nitration mixture storage tank and calcium chloride slurry commanding tank connect respectively from the top of bottom and the first retort
It is logical；The bottom of first retort is provided with aerator；First retort is connected by pipeline with first filter inlet, the
The liquid outlet of one filter is connected with hydrochloric acid tank, and the slag notch of first filter is connected with the top of the second retort；Second
Retort is also connected with a calcium oxide slurry commanding tank；The bottom of second retort is provided with aerator；Second reactor goes out
Liquid mouth is connected with the inlet of the second filter；The liquid outlet of second filter is connected with calcium chloride slurry commanding tank, the second filter
Slag notch connected with calcirm-fluoride storage tank.
Second filter is dry filter.
The temperature of second filter：40 DEG C~95 DEG C；Vacuum degree during filtering is：- 90kP~-20kP.
A kind of hydrochloric acid as shown in Figure 1 and the nitration mixture treatment process of hydrofluoric acid, its step are as follows：
(1) nitration mixture is placed in the calcium chloride solution that weight percent concentration is 2%-65% in the first retort and mixed instead
It should；
(2) fully after reaction, reaction product is filtered by filter；Its filter residue is 20%- with weight percent concentration
65% calcium oxide solution is placed in hybrid reaction in the second retort；Its filtrate is collected him and is used；
(3) fully after reaction, reaction product is passed through into pressure filter press filtration；Its filtrate is recycled to step for calcium chloride solution
(1) calcium chloride solution is for use；Its filter residue is calcirm-fluoride, as hydrogen fluoride production raw material.
In step (1), nitration mixture and CaCl2The mixed temperature of solution is 30 DEG C~60 DEG C.
Embodiment explanation：
Other conditions are constant；The concentration of calcium chloride and the concentration of calcium oxide are adjusted：
In step (1), the concentration of calcium chloride is respectively：2%th, 10%, 20%, 35%, 50%, 65%.
In step (2), the concentration of calcium oxide is respectively：20%th, 30%, 40%, 50 DEG C, 60%, 65%.
Other conditions are constant, and the temperature of the second filter is adjusted：Respectively 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80
℃、95℃.
In above-described embodiment reaction process, in the waste water of discharge, chlorion and fluorine ion are not found, illustrate the place of the present invention
Science and engineering skill is 100% to the rate of recovery of chlorion and fluorine ion.
Claims (5)
1. a kind of nitration mixture treatment process of hydrochloric acid and hydrofluoric acid, it is characterised in that：Its step are as follows：
(1) nitration mixture and weight percent concentration are placed in hybrid reaction in the first retort for the calcium chloride solution of 2%-65%；
(2) fully after reaction, reaction product is filtered by filter；Its filter residue is 20%-65% with weight percent concentration
Calcium oxide solution be placed in hybrid reaction in the second retort；Its filtrate is collected him and is used；
(3) fully after reaction, reaction product is passed through into pressure filter press filtration；Its filtrate is recycled to step (1) for calcium chloride solution
Calcium chloride solution is for use；Its filter residue is calcirm-fluoride, as hydrogen fluoride production raw material.
2. the nitration mixture treatment process of a kind of hydrochloric acid according to claim 1 and hydrofluoric acid, it is characterised in that：In step (1),
Nitration mixture and CaCl2The mixed temperature of solution is 30 DEG C~60 DEG C.
3. the special equipment of the nitration mixture treatment process of hydrochloric acid described in claims 1 or 2 and hydrofluoric acid, it is characterised in that：Hydrochloric acid and
The special equipment of the nitration mixture treatment process of hydrofluoric acid, including the storage nitration mixture storage tank of nitration mixture and calcium chloride pipe with slurry, described is mixed
Acid storage tank and calcium chloride slurry commanding tank connect respectively from bottom with the top of the first retort；The bottom of first retort is provided with exposure
Device of air；First retort is connected by pipeline with first filter inlet, the liquid outlet and hydrochloric acid tank of first filter
Connection, the slag notch of first filter are connected with the top of the second retort；Second retort is also connected with calcium oxide slurry commanding tank；
The bottom of second retort is provided with aerator；The liquid outlet of second reactor is connected with the inlet of the second filter；
The liquid outlet of second filter is connected with calcium chloride slurry commanding tank, and the slag notch of the second filter is connected with calcirm-fluoride storage tank.
4. the special equipment of the nitration mixture treatment process of hydrochloric acid and hydrofluoric acid according to claim 3, it is characterised in that：Described
Second filter is dry filter.
5. the special equipment of the nitration mixture treatment process of hydrochloric acid and hydrofluoric acid according to claim 3, it is characterised in that：Described
The temperature of second filter：40 DEG C~95 DEG C；Vacuum degree during filtering is：- 90kP~-20kP.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710875045.7A CN108147446A (en) | 2017-09-25 | 2017-09-25 | The nitration mixture treatment process and its special equipment of a kind of hydrochloric acid and hydrofluoric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710875045.7A CN108147446A (en) | 2017-09-25 | 2017-09-25 | The nitration mixture treatment process and its special equipment of a kind of hydrochloric acid and hydrofluoric acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108147446A true CN108147446A (en) | 2018-06-12 |
Family
ID=62468726
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710875045.7A Pending CN108147446A (en) | 2017-09-25 | 2017-09-25 | The nitration mixture treatment process and its special equipment of a kind of hydrochloric acid and hydrofluoric acid |
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| CN (1) | CN108147446A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113415785A (en) * | 2021-07-22 | 2021-09-21 | 盛隆资源再生（无锡）有限公司 | Method for separating and recovering hydrofluoric acid from fluorine-containing mixed acid |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11130427A (en) * | 1997-08-21 | 1999-05-18 | Tadano Ltd | Production of calcium fluoride |
| JP2006159042A (en) * | 2004-12-03 | 2006-06-22 | Nishi Nippon Filter Kk | Method and apparatus for treating fluorine ion-containing waste solution |
| CN1906129A (en) * | 2004-01-21 | 2007-01-31 | 森田化学工业株式会社 | Method for producing calcium fluoride, reusing method and recycling method thereof |
| CN106277017A (en) * | 2016-09-29 | 2017-01-04 | 海南国环清华环境服务有限公司 | A kind of system utilizing solar battery chip to produce the waste water high-purity calcium fluoride of production |
| CN207294203U (en) * | 2017-09-25 | 2018-05-01 | 上海缘脉实业有限公司 | A kind of nitration mixture processing system of hydrochloric acid and hydrofluoric acid |
-
2017
- 2017-09-25 CN CN201710875045.7A patent/CN108147446A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11130427A (en) * | 1997-08-21 | 1999-05-18 | Tadano Ltd | Production of calcium fluoride |
| CN1906129A (en) * | 2004-01-21 | 2007-01-31 | 森田化学工业株式会社 | Method for producing calcium fluoride, reusing method and recycling method thereof |
| JP2006159042A (en) * | 2004-12-03 | 2006-06-22 | Nishi Nippon Filter Kk | Method and apparatus for treating fluorine ion-containing waste solution |
| CN106277017A (en) * | 2016-09-29 | 2017-01-04 | 海南国环清华环境服务有限公司 | A kind of system utilizing solar battery chip to produce the waste water high-purity calcium fluoride of production |
| CN207294203U (en) * | 2017-09-25 | 2018-05-01 | 上海缘脉实业有限公司 | A kind of nitration mixture processing system of hydrochloric acid and hydrofluoric acid |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113415785A (en) * | 2021-07-22 | 2021-09-21 | 盛隆资源再生（无锡）有限公司 | Method for separating and recovering hydrofluoric acid from fluorine-containing mixed acid |
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Application publication date: 20180612 |
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