CN108178127A - The minimizing technology of arsenic in hydrofluoric acid - Google Patents
The minimizing technology of arsenic in hydrofluoric acid Download PDFInfo
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- CN108178127A CN108178127A CN201810163785.2A CN201810163785A CN108178127A CN 108178127 A CN108178127 A CN 108178127A CN 201810163785 A CN201810163785 A CN 201810163785A CN 108178127 A CN108178127 A CN 108178127A
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- arsenic
- hydrofluoric acid
- minimizing technology
- graphene
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- 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
- C01B7/191—Hydrogen fluoride
- C01B7/195—Separation; Purification
- C01B7/197—Separation; Purification by adsorption
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Abstract
The invention belongs to technical field of chemistry, and in particular to the minimizing technology of arsenic in a kind of hydrofluoric acid；By expanded graphite is carried out it is acidified modified and plus after irony additive carries out secondary modification, the surface of graphene oxide of acquisition carries iron content functional group, arsenic in hydrofluoric acid aqueous solution can effectively be adsorbed, graphene is separated to the removal that arsenic in hydrofluoric acid can be realized later.Method provided by the invention is simple and safe, easily operated, easy to utilize.
Description
Technical field
The invention belongs to technical field of chemistry, and in particular to the minimizing technology of arsenic in a kind of hydrofluoric acid.
Background technology
Hydrofluoric acid is a kind of important industrial acids, and corrosivity is extremely strong, can engraved glass, thus in photovoltaic industry and collection
It is used as the reducer of glass or the etching solution of chip into circuit industry.At present, hydrofluoric acid is typically by the concentrated sulfuric acid and firefly
Stone is reacted and is obtained.Due to the trivalent arsenic element (As contained in fluorite ore3+) can be reacted with hydrofluoric acid generation azeotropic, it is difficult to it is detached
Out, because prepared by hydrofluoric acid in often contain arsenic impurities, the too high application effect that can limit hydrofluoric acid of arsenic concentration.
In the prior art, there are two types of common arsenic removal process, one is by potassium permanganate by the trivalent arsenic in hydrofluoric acid
Pentavalent arsenic is oxidized to, the second is the trivalent arsenic aoxidized by fluorine gas in hydrofluoric acid aoxidizes.However, potassium permanganate is explosive chemistry
Product, fluorine gas are toxic chemical, and two all there are some potential safety problemss in use.
Invention content
The purpose of the present invention is to provide a kind of minimizing technologies of arsenic in hydrofluoric acid, and the method is simple and safe, should convenient for promoting
With.
To achieve the above object, the technical solution adopted by the present invention is：The minimizing technology of arsenic in a kind of hydrofluoric acid, including such as
Lower step：
(1) graphene nanometer sheet is added in into sulfonitric mixed liquor, dispersion, stirring, heating 6~12 hours, then mistake
It filters and uses deionized water rinse product, obtain stannic oxide/graphene nano piece；
(2) polyvinylpyrrolidone and ferrous sulfate are sequentially added into ethanol solution, is stirred respectively to being completely dissolved, obtained
To mixed solution；
(3) stannic oxide/graphene nano piece is added in into mixed solution, ultrasonic disperse 2~6 hours, filtering later and with anhydrous
Ethyl alcohol washs, and is then dried in vacuo at 50~60 DEG C, obtains modified graphene oxide；
(4) modified graphene oxide is added in the hydrofluoric acid containing arsenic, sealed and stirred 1~24 hour, then filtered
.
The advantageous effect generated using above-mentioned technical proposal is：The acidified modification of graphene nanometer sheet and plus irony addition
After agent carries out secondary modification, the stannic oxide/graphene nano piece surface of acquisition, can be in hydrofluoric acid aqueous solution with iron content functional group
Arsenic carry out You effect Xi Fu And co-sedimentations, graphene is separated to the removal that arsenic in hydrofluoric acid can be realized later.The present invention
The method of offer is simple and safe, easily operated, easy to utilize.
Specific embodiment
1-3 is further described technical solution disclosed by the invention with reference to embodiments.
Embodiment 1：The removal of arsenic in hydrofluoric acid
(1) 98% sulfuric acid and 65% nitric acid are 50 according to volume ratio:50 are mixed to get sulfonitric mixed liquor, according to body
Product mass ratio is 100ml：1g adds in graphite nano plate, ultrasonic disperse, while stirring at 80 DEG C into sulfonitric mixed liquor
Heating water bath 8 hours, then filtering and with deionized water rinse product, obtains stannic oxide/graphene nano piece；
(2) it is 90 according to mass ratio is added：0.1：5 sequentially add polyvinylpyrrolidine into the ethanol solution of 20vt%
Ketone and ferrous sulfate stir respectively to being completely dissolved, obtain mixed solution；
(3) stannic oxide/graphene nano piece is added in into mixed solution, ultrasonic disperse 3 hours, filtering later and with anhydrous second
Alcohol washs, and is then dried in vacuo at 55 DEG C, obtains modified graphene oxide；
(4) according to 5g:Modified graphene oxide nanometer sheet is added to a concentration of 49% hydrogen by the mass volume ratio of 95ml
It in fluoric acid, seals and stirs 16 hours, after being separated by filtration, the arsenic concentration in hydrofluoric acid filtrate is measured, as a result such as 1 institute of table
Show.
Embodiment 2：The removal of arsenic in hydrofluoric acid
(1) 98% sulfuric acid and 65% nitric acid are 60 according to volume ratio：40 are mixed to get sulfonitric mixed liquor, according to body
Product mass ratio is 100ml：5g adds in graphene nanometer sheet, ultrasonic disperse, while stirring at 85 DEG C into sulfonitric mixed liquor
Lower heating water bath 10 hours, then filtering and with deionized water rinse product, obtains stannic oxide/graphene nano piece；
(2) it is 85 according to mass ratio is added：0.5：10 sequentially add carboxymethyl cellulose into the ethanol solution of 40vt%
Element and ferrous sulfate, stir respectively to being completely dissolved, obtain mixed solution；
(3) stannic oxide/graphene nano piece is added in into mixed solution, ultrasonic disperse 4 hours, filtering later and with anhydrous second
Alcohol washs, and is then dried in vacuo at 60 DEG C, obtains modified graphene oxide；
(4) according to 10g:Modified graphene oxide nanometer sheet is added to a concentration of 49% hydrogen by the mass volume ratio of 90ml
It in fluoric acid, seals and stirs 12 hours, after being separated by filtration, the arsenic concentration in hydrofluoric acid filtrate is measured, as a result such as 1 institute of table
Show.
Embodiment 3：The removal of arsenic in hydrofluoric acid
(1) 98vt% sulfuric acid and 65vt% nitric acid are 70 according to volume ratio：30 are mixed to get sulfonitric mixed liquor, press
It is 100ml according to volume mass ratio：10g adds in graphene nanometer sheet into sulfonitric mixed liquor, ultrasonic disperse, while stirring
Heating water bath 12 hours at 90 DEG C, then filtering and with deionized water rinse product, obtain stannic oxide/graphene nano piece；
(2) it is 80 according to mass ratio is added：1：15 sequentially add polyethylene glycol and sulphur into the ethanol solution of 60vt%
It is sour ferrous, it is stirred respectively to being completely dissolved, obtains mixed solution；
(3) stannic oxide/graphene nano piece is added in into mixed solution, ultrasonic disperse 2 hours, filtering later and with anhydrous second
Alcohol washs, and is then dried in vacuo at 60 DEG C, obtains modified graphene oxide nanometer sheet；
(4) according to 20g:Modified graphene oxide nanometer sheet is added to a concentration of 49% hydrogen by the mass volume ratio of 80ml
Fluoric acid is sealed and is stirred 20 hours, after being separated by filtration, the arsenic concentration in hydrofluoric acid filtrate is measured, as a result such as 1 institute of table
Show.
Comparative example 1：Untreated a concentration of 49% hydrofluoric acid is taken, the arsenic concentration in solution is measured,
The results are shown in Table 1.
Table 1：ICP-OES test data tables
As shown in Table 1, method using the present invention can effectively remove the arsenic in hydrofluoric acid solution, and removal rate is up to 25%
More than.
Claims (7)
1. the minimizing technology of arsenic in a kind of hydrofluoric acid, which is characterized in that include the following steps：
(1) graphene nanometer sheet is added in into sulfonitric mixed liquor, dispersion, is heated 6~12 hours at stirring, is then filtered simultaneously
With deionized water rinse product, stannic oxide/graphene nano piece is obtained；
(2) dispersant and ferrous sulfate are sequentially added into ethanol solution, is stirred respectively to being completely dissolved, obtains mixed solution；
(3) stannic oxide/graphene nano piece is added in into mixed solution, ultrasonic disperse 2~6 hours filters and uses absolute ethyl alcohol later
Washing, is then dried in vacuo at 50~60 DEG C, obtains modified graphene oxide；
(4) modified graphene oxide nanometer sheet is added in the hydrofluoric acid containing arsenic, seals and stirs 1~24 hour, then mistake
Filter.
2. the minimizing technology of arsenic in hydrofluoric acid according to claim 1, which is characterized in that sulfuric acid in the step (1)-
It according to volume ratio is 40~70 that nitric acid mixed liquor, which is 98% sulfuric acid and 65% nitric acid,：30~60 mix.
3. the minimizing technology of arsenic in hydrofluoric acid according to claim 1, which is characterized in that sulfuric acid in the step (1)-
The content of nitric acid mixed liquor and graphene nanometer sheet is 1~20%.
4. the minimizing technology of arsenic in hydrofluoric acid according to claim 1, which is characterized in that the dispersion in the step (1)
Method is ultrasonic disperse, and heating means are heating water bath, and bath temperature is 80~90 DEG C.
5. the minimizing technology of arsenic in hydrofluoric acid according to claim 1, which is characterized in that ethyl alcohol is molten in the step (2)
A concentration of 20~60vt% of liquid.
6. the minimizing technology of arsenic in hydrofluoric acid according to claim 1, which is characterized in that step (2) ethanol solution,
The mass ratio that adds of dispersant and ferrous sulfate is 80~95：0.1~3：5~20.
7. the minimizing technology of arsenic in hydrofluoric acid according to claim 1, which is characterized in that the dispersant is selected from polyethylene
One in pyrrolidones, ethylene oxide, polyethylene glycol, carboxymethyl cellulose, neopelex, lauryl sodium sulfate
Kind.
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| CN201810163785.2A CN108178127A (en) | 2018-02-27 | 2018-02-27 | The minimizing technology of arsenic in hydrofluoric acid |
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| CN201810163785.2A CN108178127A (en) | 2018-02-27 | 2018-02-27 | The minimizing technology of arsenic in hydrofluoric acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109678114A (en) * | 2019-02-19 | 2019-04-26 | 苏州晶瑞化学股份有限公司 | The minimizing technology of arsenic impurities in a kind of electronic grade hydrochloric acid |
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Cited By (2)
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| CN109678114A (en) * | 2019-02-19 | 2019-04-26 | 苏州晶瑞化学股份有限公司 | The minimizing technology of arsenic impurities in a kind of electronic grade hydrochloric acid |
| CN109678114B (en) * | 2019-02-19 | 2021-04-02 | 苏州晶瑞化学股份有限公司 | Method for removing arsenic impurity in electronic grade hydrochloric acid |
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