CN116374957A - Method and system for separating hydrofluoric acid or/and nitric acid - Google Patents
Method and system for separating hydrofluoric acid or/and nitric acid Download PDFInfo
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- CN116374957A CN116374957A CN202310338328.3A CN202310338328A CN116374957A CN 116374957 A CN116374957 A CN 116374957A CN 202310338328 A CN202310338328 A CN 202310338328A CN 116374957 A CN116374957 A CN 116374957A
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- rectification
- storage tank
- pretreatment
- conveying
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 title claims abstract description 70
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910017604 nitric acid Inorganic materials 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000047 product Substances 0.000 claims abstract description 12
- 238000010521 absorption reaction Methods 0.000 claims abstract description 8
- 239000008213 purified water Substances 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 4
- 229960002050 hydrofluoric acid Drugs 0.000 claims description 30
- 238000002156 mixing Methods 0.000 claims description 16
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 238000005342 ion exchange Methods 0.000 claims description 6
- 238000012805 post-processing Methods 0.000 claims description 6
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims description 4
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 4
- 235000010333 potassium nitrate Nutrition 0.000 claims description 4
- 239000004323 potassium nitrate Substances 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
- 239000012065 filter cake Substances 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 150000002823 nitrates Chemical class 0.000 claims description 2
- 235000010344 sodium nitrate Nutrition 0.000 claims description 2
- 239000004317 sodium nitrate Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 abstract description 18
- 239000012716 precipitator Substances 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 239000012535 impurity Substances 0.000 description 5
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 239000012855 volatile organic compound Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000003957 anion exchange resin Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- -1 fluoride ions Chemical class 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Images
Classifications
-
- 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
- C01B7/19—Fluorine; Hydrogen fluoride
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/146—Multiple effect distillation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/38—Nitric acid
- C01B21/46—Purification; Separation ; Stabilisation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for separating hydrofluoric acid and/or nitric acid, which comprises the following steps: s1, conveying a solution to be separated in a first storage tank to a pretreatment system, and conveying a precipitant in a second storage tank to the pretreatment system; s2, conveying filtrate in the pretreatment system to a rectification system, conveying noncondensable gas in the rectification system to an absorption system, and conveying rectification products in the rectification system to a post-treatment system; s3, conveying the separated products in the post-treatment system to a third storage tank and a fourth storage tank respectively to obtain separated hydrofluoric acid or/and nitric acid and purified water. The method and the system for separating hydrofluoric acid or/and nitric acid separate out fluosilicic acid through the precipitator, and then rectify to obtain hydrofluoric acid or/and nitric acid, wherein the purity of the hydrofluoric acid or/and nitric acid after separation is electronic grade, and purified water is obtained.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a method and a system for separating hydrofluoric acid and/or nitric acid.
Background
In order to reduce reflection loss on the surface of the solar cell silicon wafer, a layer of antireflection film is deposited on the surface of the cell silicon wafer or a suede is manufactured, and the surface of the polycrystalline silicon is subjected to chemical corrosion by utilizing a mixed acid solution containing hydrofluoric acid due to disordered grain orientation of the polycrystalline silicon, so that a suede structure is obtained. This consumes a lot of mixed acid, and in the processes of texturing and etching, metal ions and impurities such as organic matters are inevitably generated, and in order to control the impurity content, it is necessary to continuously discharge acid and supplement new mixed acid solution, and the discharged acid solution is the solution to be separated.
At present, the treatment method of the solution to be separated adopts alkali neutralization and then calcium chloride is added to precipitate and remove fluoride ions, so that the treatment cost is high, and a large amount of wastewater is generated.
Thus, there is a need for a method and system for separating hydrofluoric acid and/or nitric acid.
Disclosure of Invention
The invention aims at overcoming the defects in the prior art and provides a method and a system for separating hydrofluoric acid or/and nitric acid.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
in a first aspect, the present invention provides a method for separating hydrofluoric acid and/or nitric acid, comprising the steps of:
s1, conveying a solution to be separated in a first storage tank to a pretreatment system, and conveying a precipitant in a second storage tank to the pretreatment system;
s2, conveying filtrate in the pretreatment system to a rectification system, conveying noncondensable gas in the rectification system to an absorption system, and conveying rectification products in the rectification system to a post-treatment system;
s3, conveying the separated products in the post-treatment system to a third storage tank and a fourth storage tank respectively to obtain separated hydrofluoric acid or/and nitric acid and purified water;
wherein the pretreatment system comprises: a precipitation unit and a filtration unit;
the rectification system comprises: at least one stripping-rectifying unit, a reflux unit and a reboiling unit;
the aftertreatment system includes: a collection mixing system and a water collection treatment system, the water collection treatment system comprising: a purification unit and an ion exchange unit.
Preferably, the precipitating agent comprises: and the nitrate is used for precipitating the hydrosilyl fluoric acid in the solution to be separated.
Preferably, the nitrate salt comprises: at least one of potassium nitrate, sodium nitrate, calcium nitrate or barium nitrate.
Preferably, the operating pressure of the rectification unit is lower than 0.1MPa and the operating temperature is 110-150 ℃.
A second aspect of the invention provides a system for separating hydrofluoric acid and/or nitric acid, suitable for use in a method as hereinbefore described, comprising:
a first tank for storing a solution to be separated;
the second storage tank is used for storing the precipitant;
the pretreatment system comprises a pretreatment system, wherein a first storage tank discharge port of a first storage tank is connected with a first feed inlet pipeline of the pretreatment system, and a second storage tank discharge port of a second storage tank is connected with a second feed inlet pipeline of the pretreatment system;
the first pretreatment system discharge port of the pretreatment system is connected with the feed port pipeline of the rectification system;
a post-processing system, the post-processing system comprising:
the first rectification system discharge port of the rectification system is connected with the feed inlet pipeline of the collection mixing system;
the fourth rectifying system discharge port of the rectifying system is connected with the feed port pipeline of the water collecting and treating system;
the collecting and mixing system discharge port of the collecting and mixing system is connected with the feeding port of the third storage tank through a pipeline;
and a fourth storage tank, wherein a water collecting and treating system discharge port of the water collecting and treating system is connected with a feed inlet pipeline of the third storage tank.
Preferably, a second pretreatment system discharge port of the pretreatment system is connected with a filter cake treatment working section pipeline.
Preferably, the method further comprises: and a discharge port of a second rectifying system of the rectifying system is connected with a feed port pipeline of the absorbing system.
Preferably, a third rectification system discharge port of the rectification system is connected with a kettle bottom product treatment working section pipeline.
Compared with the prior art, the invention has the following technical effects:
the method and the system for separating hydrofluoric acid or/and nitric acid separate out fluosilicic acid through the precipitator, and then rectify to obtain hydrofluoric acid or/and nitric acid, wherein the purity of the hydrofluoric acid or/and nitric acid after separation is electronic grade, and purified water is obtained.
Drawings
FIG. 1 is a schematic diagram of a system for separating hydrofluoric acid and/or nitric acid according to the present invention;
wherein, the reference numerals include:
a first tank 1; a first tank discharge port 101; a pretreatment system 2; a first pretreatment system outlet 201; a second pretreatment system outlet 202; a rectification system 3; a first rectification system discharge port 301; a second rectification system discharge port 302; a third rectification system outlet 303; a fourth rectification system discharge port 304; a post-processing system 4; a collection mixing system 41; a post-processing system discharge port 401; a water collection treatment system 42; a water collection treatment system discharge port 402; a third tank 5; a second tank 6; a second tank feed 601; a second tank outlet 602; an absorption system 7; an absorption system discharge port 701; a fourth reservoir 8.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
The invention is further described below with reference to the drawings and specific examples, which are not intended to be limiting.
Example 1
As shown in fig. 1, the present embodiment provides a system for separating hydrofluoric acid and/or nitric acid, including:
a first tank 1 for storing a solution to be separated;
a second tank 6 for storing a precipitant;
a first storage tank discharge port 101 of the first storage tank 1 is connected with a first feed port pipeline of the pretreatment system 2, and a second storage tank discharge port 602 of the second storage tank 6 is connected with a second feed port pipeline of the pretreatment system 2; a second pretreatment system discharge port 202 of the pretreatment system 2 is connected with a filter cake treatment working section pipeline;
the rectification system 3, a first pretreatment system discharge port 201 of the pretreatment system 2 is connected with a feed port pipeline of the rectification system 3; a third rectification system discharge port 303 of the rectification system 3 is connected with a kettle bottom product treatment working section through a pipeline;
an aftertreatment system 4, the aftertreatment system 4 comprising:
the first rectification system discharge port 301 of the rectification system 3 is connected with the feed port pipeline of the collection mixing system 41;
the fourth rectifying system discharge port 304 of the rectifying system 3 is connected with the feed port pipeline of the water collecting and treating system 42;
the second rectification system discharge port 302 of the rectification system 3 is connected with the feed inlet pipeline of the absorption system 7;
a collecting and mixing system discharge port 401 of the collecting and mixing system 41 is connected with a feed port pipeline of the third storage tank 5;
and a fourth storage tank 8, wherein a water collecting and treating system discharge port 402 of the water collecting and treating system 42 is connected with a feed port pipeline of the third storage tank 8.
As a preferred embodiment, the pretreatment system 2 includes: a precipitation unit and a filtration unit.
As a preferred embodiment, the rectification system 3 comprises: at least one rectifying unit, a reflux unit and a reboiling unit.
As a preferred embodiment, the aftertreatment system 4 comprises: a purification unit and an ion exchange unit.
Example 2
This example provides a method for separating hydrofluoric acid and/or nitric acid using the system of example 1, comprising the steps of:
s1, conveying a solution to be separated (200 kg, wherein hydrofluoric acid accounts for about 12% of the total mass, water accounts for about 82% of the total mass, fluosilicic acid accounts for about 5% of the total mass, and the balance is metal ions, COD and other impurities) in a first storage tank 1 to a pretreatment system 2, and conveying a precipitant (potassium nitrate for precipitating the hydrofluoric acid in the solution to be separated) in a second storage tank 6 to the pretreatment system 2;
the solution to be separated containing fluosilicic acid or/and nitric acid and the precipitant react as follows:
H 2 SiF 6 +2KNO 3 →K 2 SiF 6 ↓+2HNO 3
the filtering unit conveys the precipitated potassium fluosilicate to a drying working section; the filtering unit can adopt filtering, centrifugation and other modes for filtering;
s2, delivering filtrate of fluosilicic acid, hydrofluoric acid, nitric acid and excessive potassium nitrate into a rectification system 3;
the rectifying unit obtains hydrofluoric acid at the tower bottom and obtains nitric acid at the tower top; the rectifying unit can adopt batch type or continuous type;
in the batch rectifying device, the aqueous solution obtained from the top of the tower contains volatile organic compounds VOCs, and the VOCs in the water are removed through an activated carbon adsorption unit in a water collecting and treating system 42; along with the increase of the temperature of the bottom of the tower, the water solution obtained by the reflux at the top of the tower contains trace acid, but does not reach the recovered concentration, and the water solution is treated by an alkaline anion exchange resin unit to obtain purified water, and is conveyed into a fourth storage tank 8 through a discharge port 402 of a water collecting and treating system; for convenient operation, the activated carbon adsorption unit and the basic anion exchange resin unit are connected in series; the active carbon unit and the ion exchange unit are regenerated by steam, the active carbon regenerated solution is conveyed to a wastewater treatment system, and the regenerated acid liquor of the ion exchange system is returned to the inlet of the rectification system; as the bottom temperature increases, the acid concentration gradually increases to a recovery level, at which time the reflux liquid is switched to the collection mixing system 41; due to the intermittent operation, the acid concentration is gradually increased, and when the rectification is completed, the collecting and mixing system 41 is conveyed into the third storage tank 5 through the discharging port 401 of the collecting and mixing system; the rectification is finished depending on the liquid level of the tower kettle and is also related to entrainment of metal ions;
in the continuous rectifying device, the reflux liquid at the top of the tower is an aqueous solution containing trace VOCs and trace acid; the product acid needs to be taken as an intermediate product in a rectifying section of a rectifying system; the treatment steps are similar to those of the batch rectifying device, so that the description is omitted;
the theoretical plate number of the rectification unit may be 10 or more, for example, 20 to 30; the reflux ratio of the reflux unit may be 1 or more, for example 3 or more;
delivering non-condensable gas in the rectification system 3 to an absorption system 7, and delivering rectification products (170 kg, the first batch is an aqueous solution containing a trace amount of hydrofluoric acid and about 130kg, and the second batch is a solution containing 37.5% of hydrofluoric acid and about 40 kg) in the rectification system 3 to a post-treatment system 4;
the ion exchange unit can adopt strong alkaline ion exchange resin to adsorb low-concentration acid;
s3, conveying the separated products in the post-treatment system 4 to a third storage tank 5 and a fourth storage tank 8 respectively to obtain separated hydrofluoric acid or/and nitric acid and purified water.
The total carbon value of impurities in hydrofluoric acid or/and nitric acid separated by the method is 10-50 mugC/g; the content of metal ion impurities is 10-100 mug/kg.
In summary, the method and system for separating hydrofluoric acid and/or nitric acid of the invention separate out fluosilicic acid by using a precipitator, and then rectify to obtain hydrofluoric acid and/or nitric acid, wherein the purity of the hydrofluoric acid and/or nitric acid after separation is electronic grade.
The foregoing description is only illustrative of the preferred embodiments of the present invention and is not to be construed as limiting the scope of the invention, and it will be appreciated by those skilled in the art that equivalent substitutions and obvious variations may be made using the description and illustrations of the present invention, and are intended to be included within the scope of the present invention.
Claims (8)
1. A method for separating hydrofluoric acid and/or nitric acid, comprising the steps of:
s1, conveying a solution to be separated in a first storage tank (1) to a pretreatment system (2), and conveying a precipitant in a second storage tank (6) to the pretreatment system (2);
s2, conveying filtrate in the pretreatment system (2) to a rectification system (3), conveying noncondensable gas in the rectification system (3) to an absorption system (7), and conveying rectification products in the rectification system (3) to a post-treatment system (4);
s3, conveying the separated products in the post-treatment system (4) to a third storage tank (5) and a fourth storage tank (8) respectively to obtain separated hydrofluoric acid or/and nitric acid and purified water;
wherein the pretreatment system (2) comprises: a precipitation unit and a filtration unit;
the rectification system (3) comprises: at least one stripping-rectifying unit, a reflux unit and a reboiling unit;
the aftertreatment system (4) comprises: a collection mixing system (41) and a water collection treatment system (42), the water collection treatment system (42) comprising: a purification unit and an ion exchange unit.
2. The method of claim 1, wherein the precipitation agent comprises: and the nitrate is used for precipitating the hydrosilyl fluoric acid in the solution to be separated.
3. The method of claim 2, wherein the nitrate salt comprises: at least one of potassium nitrate, sodium nitrate, calcium nitrate or barium nitrate.
4. The method according to claim 1, wherein the rectification unit operates at a pressure of less than 0.1MPa and at a temperature of 110 ℃ to 150 ℃.
5. A system for separating hydrofluoric acid and/or nitric acid, suitable for use in a method according to any one of claims 1 to 4, comprising:
a first tank (1) for storing a solution to be separated;
a second storage tank (6) for storing a precipitant; the pretreatment system (2), a first storage tank discharge port (101) of the first storage tank (1) is connected with a first feed port pipeline of the pretreatment system (2), and a second storage tank discharge port (602) of the second storage tank (6) is connected with a second feed port pipeline of the pretreatment system (2);
the rectification system (3), a first pretreatment system discharge port (201) of the pretreatment system (2) is connected with a feed port pipeline of the rectification system (3);
-a post-processing system (4), the post-processing system (4) comprising:
the device comprises a collecting and mixing system (41), wherein a first rectifying system discharge port (301) of the rectifying system (3) is connected with a feed port pipeline of the collecting and mixing system (41);
the fourth rectification system discharge port (304) of the rectification system (3) is connected with the feed port pipeline of the water collection and treatment system (42);
the collecting and mixing system discharge port (401) of the collecting and mixing system (41) is connected with the feed inlet pipeline of the third storage tank (5);
and a fourth storage tank (8), wherein a water collecting and treating system discharge port (402) of the water collecting and treating system (42) is connected with a feed port pipeline of the third storage tank (8).
6. A system according to claim 5, characterized in that the second pretreatment system outlet (202) of the pretreatment system (2) is connected to a filter cake treatment section line.
7. The system of claim 5, further comprising:
and the second rectification system discharge port (302) of the rectification system (3) is connected with the feed inlet pipeline of the absorption system (7).
8. The system according to claim 5, wherein a third rectification system outlet (303) of the rectification system (3) is connected to the tank bottom product treatment section by pipeline.
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