CN103566606B - Multifunctional purification device and method for purifying ammonium bifluoride by using same - Google Patents
Multifunctional purification device and method for purifying ammonium bifluoride by using same Download PDFInfo
- Publication number
- CN103566606B CN103566606B CN201310539599.1A CN201310539599A CN103566606B CN 103566606 B CN103566606 B CN 103566606B CN 201310539599 A CN201310539599 A CN 201310539599A CN 103566606 B CN103566606 B CN 103566606B
- Authority
- CN
- China
- Prior art keywords
- condenser
- purification
- chamber
- purifier
- purifying
- 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.)
- Active
Links
Landscapes
- Removal Of Specific Substances (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
The invention provides a multifunctional purification device, at least comprising a base plate, and a purification cover arranged on the base plate, wherein an airtight purification chamber is formed between the purification cover and the base plate; a feeding valve, a purifier, a condenser, a condenser pipe and a collecting bottle are arranged inside the purification chamber; a head cover for feeding is arranged at the top of the purification cover; the feeding valve is arranged at the top of the purification chamber and arranged below the head cover; the condenser is arranged below the feeding valve and connected with the feeding valve; the purifier and the collecting bottle are arranged at the lower part inside the purification chamber; the tops of the purifier and the collecting bottle are connected with the bottom of the condenser. By adopting the device, the defects of the prior art are overcome; the device is simple in structure, safe and environment-friendly, high-efficiency and intelligent, convenient to operate, low in cost, small in floor area, and free of rigorous demands on the work environment. The device can be used for purifying ammonium bifluoride and other reagents. The invention also provides a method for purifying the ammonium bifluoride.
Description
Technical field
The invention provides a kind of purifying plant, particularly relate to a kind of device of purifying hydrogen fluoride ammonium, present invention also offers the method for purifying hydrogen fluoride ammonium simultaneously, belong to chemical analysis technology field.
Background technology
Ammonium acid fluoride is white or the crystallization of water white transparency orthorhombic system, in the form of sheets, and slightly tart flavour.Fusing point 125.6 DEG C.Boiling point 240 DEG C.Easy deliquescence in atmosphere.Be slightly soluble in alcohol, be very easily dissolved in cold water, decompose in the hot water.The aqueous solution is highly acid.Poisonous have severe corrosive.Reagent and high-precision end electron trade and pharmaceuticals industry surface conditioning agent, etchant, disinfectant, anticorrisive agent etc. can be cleared up as sample.High-purity ammonium acid fluoride due to its superpower ability of clearing up, extremely short digestion time, extremely low flow process background, do not produce the characteristic of fluoride precipitation and be better than the powerful advantages such as processing safety of hydrofluoric acid, become a kind of brand-new Specimen eliminating reagent, the Specimen eliminating time can greatly be shortened, improve sample pre-treatments efficiency.
And be difficult at present buy as the ultrapure ammonium acid fluoride mainly clearing up reagent.Industrial goods ammonium acid fluoride NH
4hF
2purity 98%, analyzes alcohol ammonium acid fluoride NH
4hF
2purity 99.8%, the content of its impurity metal ion as Li, Be, Cr, Co, Ni, Cu, Zn, Rb, Zr, Ba, As, Pb etc. relatively trace and ultra trace sample analysis higher, can not the requirement of the elementary analysis such as quality sample trace element, isotopic ratio and high-precision end electron trade and pharmaceuticals industry contentedly, ammonium acid fluoride NH4HF2 must be purified.
The method of usual purifying hydrogen fluoride ammonium NH4HF2 has: synthesize after feedstock purification ammonium acid fluoride NH4HF2, industrial goods ammonium acid fluoride NH4HF2 distillation and industrial goods ammonium acid fluoride NH4HF2 be recrystallized.In recrystallization process, mother liquor will concentrate, and crystallization will be dewatered, and causes environmental pollution; By NH
3with the method for HF Reactive Synthesis NH4HF2 with 18.25M Ω cm ultra-pure water for solvent, operating environment requirements is high, need synthesize under 1000 grades of cleanliness factors, operates more complicated.
Summary of the invention
The invention provides a kind of multi-functional purifying plant, solve the deficiency in above-mentioned background technology, this apparatus structure is simple, safety and environmental protection, high efficiency smart, easy to operate, cost is lower, floor space is little and to the requirement of working environment without harshness.This device not only can be used for purifying hydrogen fluoride ammonium, can also various acid and reagent, such as nitric acid, hydrochloric acid, hydrofluoric acid etc. in purifying routine laboratory analysis.
Realizing the technical scheme that above-mentioned purpose of the present invention adopts is:
A kind of multi-functional purifying plant, the purification cover at least comprising chassis and be arranged on chassis, an airtight purification chamber is formed between described purification cover and chassis, inlet valve is provided with in described purification chamber, purifier, condenser, condenser pipe and receiving flask, wherein the top of purification cover is provided with the top cover for feeding intake, inlet valve is positioned at the top and the below being positioned at top cover that purify chamber, condenser is positioned at the below of inlet valve and is connected with inlet valve, purifier and receiving flask are all positioned at the bottom of purification chamber, and both tops are all connected with the bottom of condenser, described purifier and the inside of condenser are the chamber of hollow form, be respectively purifying chamber and condensation chamber, and purifying chamber is connected with condensation chamber, the silica gel heating layer for heating chamber interior is equipped with in the sidewall of purifier and condenser, the bottom of described condenser is provided with the circle boss towards projection, the refluence groove that between boss and the sidewall of condenser, common formation one is annular, liquid outlet is provided with in refluence groove, condenser pipe is arranged on liquid outlet, and liquid outlet is communicated with receiving flask by condenser pipe, the outside of purification cover is also provided with controller, and controller is connected with power supply and silica gel heating layer by wire.
Also be provided with waste liquid processor in described purification chamber, waste liquid processor is positioned at the below of purifier and is provided with tapping valve between the two, and waste liquid processor is communicated with purifier by tapping valve.
Described purification cover is translucent cover, and purification cover is provided with sampling window, and described sampling window is corresponding with the position of receiving flask.
Present invention also offers a kind of method adopting above-mentioned purifying plant purifying hydrogen fluoride ammonium, the method is simple to operate, can obtain highly purified ammonium acid fluoride, and its method of purification is as follows:
(1), open top cover and inlet valve, be added in inlet valve by ammonium acid fluoride powder to be purified, hydrogen ammonium powder to be fluorinated all enters in purifier, closes top cover and inlet valve; (2) power supply, in opening controller, and regulate the silica gel heating layer temperature of purifier to 180-200 DEG C, regulate the silica gel heating layer temperature of condenser to 120-130 DEG C, boil under state and distill in ammonium acid fluoride Asia in purifying chamber, then in condensation chamber, be condensed into droplet and be attached on the inwall of condenser, then flowing in refluence groove; (3), liquid hydrogen fluoride ammonium flows to condenser pipe by liquid outlet, becomes the solid-state ammonium acid fluoride of White crystal particulate, be then collected in receiving flask at condenser pipe intercrystalline; (4), powered-down, take out receiving flask, can obtain purify after ammonium acid fluoride.
After purification, open tapping valve, waste liquid is entered in waste liquid processor by tapping valve.
In the present invention, utilize sub-boiling distillation to balance each other principle purifying hydrogen fluoride ammonium, under state is boiled in Asia, carry out controlling speed distillation then reach from crystallisation by cooling and remove wherein impurity and obtain ultrapure ammonium acid fluoride.Multi-functional purifying plant provided by the invention is primarily of major part compositions such as condenser, purifier, receiving flask, waste liquid processor, controller and purification covers.Purifying plant is vertical full-enclosed structure, and critical piece material is PFA and PTFE.Whole purification process completes in almost completely airtight system, not ingress of air, and not by environmental pollution, do not need cooling water, heater is built-in, existing outward without metal parts.Adjustable temperature and time parameter controls speed and the time of purification, and waste liquid one key operation processes simply and effectively, safety and environmental protection.
Accompanying drawing explanation
Fig. 1 is the overall structure schematic diagram of multi-functional purifying plant provided by the invention;
Fig. 2 is the cut-away view of multi-functional purifying plant;
In figure: 1-top cover, 2-purification cover, 3-chassis, 4-sampling window, 5-controller, 6-inlet valve, 7-condenser, 8-purifier, 9-tapping valve, 10-waste liquid processor, 11-condenser pipe, 12-receiving flask, 13-refluence groove.
Detailed description of the invention
Detailed specific description is done below in conjunction with accompanying drawing and to the present invention.
The structure of the multi-functional purifying plant provided in the present invention as depicted in figs. 1 and 2, at least comprises chassis 3 and is arranged on the purification cover 2 on chassis 3, and described purification cover 2 is translucent cover, forms an airtight purification chamber between purification cover 2 and chassis 3.
Inlet valve 6, purifier 8, condenser 7, condenser pipe 11 and receiving flask 12 is provided with in described purification chamber, wherein the top of purification cover 2 is provided with the top cover 1 for feeding intake, inlet valve 6 is positioned at the top and the below being positioned at top cover 1 that purify chamber, condenser 7 is positioned at the below of inlet valve 6 and is connected with inlet valve 6, purifier 8 and receiving flask 12 are all positioned at the bottom of purification chamber, and both tops are all connected with the bottom of condenser 7; Purification cover 2 is provided with sampling window 4, and described sampling window 4 is corresponding with the position of receiving flask 12.
Also be provided with waste liquid processor 10 in purification chamber, waste liquid processor 10 is positioned at the below of purifier 8 and is provided with tapping valve 9 between the two, and waste liquid processor 10 is communicated with purifier 8 by tapping valve 9.
Described purifier 8 and the inside of condenser 7 are the chamber of hollow form, be respectively purifying chamber and condensation chamber, and purifying chamber is connected with condensation chamber, the silica gel heating layer for heating chamber interior is equipped with in the sidewall of purifier 8 and condenser 7, the bottom of described condenser 7 is provided with the circle boss towards projection, an annular refluence groove 13 is jointly formed between the sidewall of boss and condenser 7, liquid outlet is provided with in refluence groove 13, condenser pipe 11 is arranged on liquid outlet, and liquid outlet is communicated with receiving flask 12 by condenser pipe 11;
The outside of purification cover 2 is also provided with controller 5, and controller 5 is connected with power supply and silica gel heating layer by wire.
Be described below in conjunction with the method for purification of specific embodiment to said apparatus.
Embodiment 1
Above-mentioned multi-functional purifying plant is adopted to purify to ammonium acid fluoride in the present embodiment.
Open top cover and inlet valve, be added in inlet valve by ammonium acid fluoride powder 1000g to be purified, hydrogen ammonium powder to be fluorinated all enters in purifier, closes top cover and inlet valve; (2) power supply, in opening controller, and regulate the silica gel heating layer temperature to 180 DEG C of purifier, regulate the silica gel heating layer temperature to 121 DEG C of condenser, boil under state and distill in ammonium acid fluoride Asia in purifying chamber, then in condensation chamber, be condensed into droplet and be attached on the inwall of condenser, then flowing in refluence groove; (3), liquid hydrogen fluoride ammonium flows to condenser pipe by liquid outlet, becomes the solid-state ammonium acid fluoride of White crystal particulate, be then collected in receiving flask at condenser pipe intercrystalline; (4), powered-down, take out receiving flask, open tapping valve, waste liquid is entered in waste liquid processor by tapping valve.Can obtain the ammonium acid fluoride after purifying, ammonium acid fluoride obtained in the present embodiment detects through ICP-MS, and the content of impurity metal ion is if Li, Be, Cr, Co, Ni, Cu, Zn, Rb, Zr, Ag, Ba, Hf, Pb etc. are all at 0.001 to 0.042 μ g g
-1in scope.
Embodiment 2
Above-mentioned multi-functional purifying plant is adopted to purify to ammonium acid fluoride in the present embodiment.
Open top cover and inlet valve, be added in inlet valve by ammonium acid fluoride powder 1000g to be purified, hydrogen ammonium powder to be fluorinated all enters in purifier, closes top cover and inlet valve; (2) power supply, in opening controller, and regulate the silica gel heating layer temperature to 200 DEG C of purifier, regulate the silica gel heating layer temperature to 129 DEG C of condenser, boil under state and distill in ammonium acid fluoride Asia in purifying chamber, then in condensation chamber, be condensed into droplet and be attached on the inwall of condenser, then flowing in refluence groove; (3), liquid hydrogen fluoride ammonium flows to condenser pipe by liquid outlet, becomes the solid-state ammonium acid fluoride of White crystal particulate, be then collected in receiving flask at condenser pipe intercrystalline; (4), powered-down, take out receiving flask, open tapping valve, waste liquid is entered in waste liquid processor by tapping valve.Can obtain the ammonium acid fluoride after purifying, ammonium acid fluoride obtained in the present embodiment detects through ICP-MS, and the content of impurity metal ion is if Li, Be, Cr, Co, Ni, Cu, Zn, Rb, Zr, Ag, Ba, Hf, Pb etc. are all at 0.001 to 0.042 μ g g
-1in scope.
Embodiment 3
The multi-functional purifying plant provided in the present invention can not only be purified to ammonium acid fluoride, and can purify to reagent such as nitric acid, hydrochloric acid, hydrofluoric acid, pure water, purifies in the present embodiment to hydrofluoric acid HF.
Open top cover and inlet valve, traditional Chinese medicines top grade alcohol hydrofluoric acid HF1000ml to be purified is added in inlet valve, treats that hydrofluoric acid all enters in purifier, close top cover and inlet valve; (2) power supply, in opening controller, and regulate the silica gel heating layer temperature of purifier to 80-90 DEG C, the silica gel heating layer normal temperature of condenser, boil under state and distill in hydrofluoric acid Asia in purifying chamber, then in condensation chamber, be condensed into droplet and be attached on the inwall of condenser, then flowing in refluence groove; (3), hydrofluoric acid flows to condenser pipe by liquid outlet, is then collected in receiving flask; (4), powered-down, take out receiving flask, open tapping valve, waste liquid is entered in waste liquid processor by tapping valve.Can obtain the hydrofluoric acid after purifying, hydrofluoric acid obtained in the present embodiment detects through ICP-MS, and the content of impurity metal ion is if Li, Be, Cr, Co, Ni, Cu, Zn, Rb, Zr, Ag, Ba, Hf, Pb etc. are all at 0.001 to 0.027 μ g g
-1in scope.
Claims (5)
1. a purifying plant, it is characterized in that: at least comprise chassis and be arranged on the purification cover on chassis, an airtight purification chamber is formed between described purification cover and chassis, inlet valve is provided with in described purification chamber, purifier, condenser, condenser pipe and receiving flask, wherein the top of purification cover is provided with the top cover for feeding intake, inlet valve is positioned at the top and the below being positioned at top cover that purify chamber, condenser is positioned at the below of inlet valve and is connected with inlet valve, purifier and receiving flask are all positioned at the bottom of purification chamber, and both tops are all connected with the bottom of condenser, described purifier and the inside of condenser are the chamber of hollow form, be respectively purifying chamber and condensation chamber, and purifying chamber is connected with condensation chamber, the silica gel heating layer for heating chamber interior is equipped with in the sidewall of purifier and condenser, the bottom of described condenser is provided with the circle boss towards projection, the refluence groove that between boss and the sidewall of condenser, common formation one is annular, liquid outlet is provided with in refluence groove, condenser pipe is arranged on liquid outlet, and liquid outlet is communicated with receiving flask by condenser pipe, the outside of purification cover is also provided with controller, and controller is connected with power supply and silica gel heating layer by wire.
2. purifying plant according to claim 1, is characterized in that: be also provided with waste liquid processor in described purification chamber, waste liquid processor is positioned at the below of purifier and is provided with tapping valve between the two, and waste liquid processor is communicated with purifier by tapping valve.
3. purifying plant according to claim 1, is characterized in that: described purification cover is translucent cover, and purification cover is provided with sampling window, and described sampling window is corresponding with the position of receiving flask.
4. one kind adopts the method for device purifying hydrogen fluoride ammonium described in claim 1 or 2 or 3, it is characterized in that comprising the following steps: (1), open top cover and inlet valve, ammonium acid fluoride powder to be purified is added in inlet valve, hydrogen ammonium powder to be fluorinated all enters in purifier, closes top cover and inlet valve; (2) power supply, in opening controller, and regulate the silica gel heating layer temperature of purifier to 180-200 DEG C, regulate the silica gel heating layer temperature of condenser to 121-129 DEG C, boil under state and distill in ammonium acid fluoride Asia in purifying chamber, then in condensation chamber, be condensed into droplet and be attached on the inwall of condenser, then flowing in refluence groove; (3), liquid hydrogen fluoride ammonium flows to condenser pipe by liquid outlet, becomes the solid-state ammonium acid fluoride of White crystal particulate, be then collected in receiving flask at condenser pipe intercrystalline; (4), powered-down, take out receiving flask, can obtain purify after ammonium acid fluoride.
5. the method for purifying hydrogen fluoride ammonium according to claim 4, is characterized in that: after purification, and open tapping valve, waste liquid is entered in waste liquid processor by tapping valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310539599.1A CN103566606B (en) | 2013-11-04 | 2013-11-04 | Multifunctional purification device and method for purifying ammonium bifluoride by using same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310539599.1A CN103566606B (en) | 2013-11-04 | 2013-11-04 | Multifunctional purification device and method for purifying ammonium bifluoride by using same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103566606A CN103566606A (en) | 2014-02-12 |
| CN103566606B true CN103566606B (en) | 2015-03-04 |
Family
ID=50039850
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310539599.1A Active CN103566606B (en) | 2013-11-04 | 2013-11-04 | Multifunctional purification device and method for purifying ammonium bifluoride by using same |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103566606B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107515148A (en) * | 2017-08-07 | 2017-12-26 | 袁洪林 | A kind of sub-boiling distillation device equipment |
| CN113358436B (en) * | 2021-06-11 | 2022-12-30 | 中国科学技术大学 | Device and method for purifying ammonium bifluoride |
| CN114350502B (en) * | 2021-12-24 | 2024-05-17 | 湖南吉大检验检测有限公司 | Public health medicine collection fungus detection device |
| CN117303402B (en) * | 2023-11-30 | 2024-01-30 | 山东飞源东泰高分子材料有限公司 | Ammonium bifluoride refining purification device |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08150301A (en) * | 1994-11-29 | 1996-06-11 | Mitsubishi Kasei Eng Co | Distillation apparatus and operation thereof |
| CN101062776B (en) * | 2006-04-29 | 2011-01-12 | 大连会越科技有限公司 | Preparation method of high-purity ammonium hydrogen fluoride |
| US20080044572A1 (en) * | 2006-08-15 | 2008-02-21 | Loeffler Stephen D | Right-sized vacuum precursor (rsvp) distillation system |
| JP2012183457A (en) * | 2011-03-03 | 2012-09-27 | Seiko Epson Corp | Separation method and separation device |
| JP2012193074A (en) * | 2011-03-16 | 2012-10-11 | Seiko Epson Corp | Separation method and separation apparatus |
| CN102580336B (en) * | 2012-01-12 | 2014-04-16 | 天津大学 | Device and method for purifying volatile inorganic acid reagent |
-
2013
- 2013-11-04 CN CN201310539599.1A patent/CN103566606B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN103566606A (en) | 2014-02-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103566606B (en) | Multifunctional purification device and method for purifying ammonium bifluoride by using same | |
| CN104925759B (en) | Continuous production method of sulfuric acid with ultrahigh purity | |
| JP2012062300A (en) | Method for producing ultra-high purity electronic grade chemical reagent | |
| CN100497161C (en) | Method and equipment for preparing super clean, high purified hydrofluoric acid | |
| JP6371015B2 (en) | Purification system and method for divanadium pentoxide | |
| CN104192803B (en) | A kind of sub-boiling distillation method of high purity hydrochloric acid | |
| JP6347001B2 (en) | Manufacturing system and manufacturing method of divanadium tetroxide powder | |
| CN105174290A (en) | Separation process of potassium salt and sodium salt in concentrated brine | |
| CN104129762A (en) | Preparation method and preparation system of high-purity sulfuric acid solution | |
| CN111186820A (en) | Production process and production system of high-purity sulfuric acid | |
| WO2021129404A1 (en) | Device and method for recycling waste acid liquid for polycrystalline silicon texturing | |
| CN107082407B (en) | A kind of method of purification of anhydrous hydrofluoric acid | |
| CN204588694U (en) | A kind of production system of used in electronic industry hydrofluoric acid | |
| CN100335405C (en) | Analytical pure sulfuric acid production process | |
| CN106422680B (en) | Smelting flue gas purification treatment device and method with byproduct sulfuric acid of more than 40% | |
| CN211871381U (en) | High-purity sulfuric acid production system | |
| CN109052352A (en) | A kind of method of industrial yellow phosphorus production electron-level phosphoric acid | |
| CN102502530A (en) | Method for producing electronic-grade sulfuric acid by static fusion crystallization | |
| CN104445225B (en) | A kind of method of preparing aerosil that is dried taking stalk as raw material low-temperature atmosphere-pressure | |
| CN201214627Y (en) | Super-clean and high-purity electronic grade hydrogen peroxide purification equipment | |
| CN102424369A (en) | Production process for reagent grade high-purity sulfuric acid | |
| RU2517524C2 (en) | Method and apparatus for processing hydrogen in purification unit of terephthalic acid purification device | |
| CN104291281B (en) | A kind of method preparing super-clean high-purity nitric acid | |
| CN209872365U (en) | Environment-friendly energy-saving type ultra-clean high-purity sulfuric acid production equipment | |
| CN103523761A (en) | Continuous nitric acid discoloring device and method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |