CN1931709A - Prepn process of high purity hydrofluoric acid - Google Patents
Prepn process of high purity hydrofluoric acid Download PDFInfo
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- CN1931709A CN1931709A CN 200610096593 CN200610096593A CN1931709A CN 1931709 A CN1931709 A CN 1931709A CN 200610096593 CN200610096593 CN 200610096593 CN 200610096593 A CN200610096593 A CN 200610096593A CN 1931709 A CN1931709 A CN 1931709A
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- Prior art keywords
- hydrofluoric acid
- high purity
- hydrogen fluoride
- weight
- rectifying
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 238000000034 method Methods 0.000 title claims description 16
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 6
- 239000012498 ultrapure water Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 8
- CQXADFVORZEARL-UHFFFAOYSA-N Rilmenidine Chemical compound C1CC1C(C1CC1)NC1=NCCO1 CQXADFVORZEARL-UHFFFAOYSA-N 0.000 abstract 1
- 230000008030 elimination Effects 0.000 abstract 1
- 238000003379 elimination reaction Methods 0.000 abstract 1
- 239000012286 potassium permanganate Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 12
- JCMGUODNZMETBM-UHFFFAOYSA-N arsenic trifluoride Chemical compound F[As](F)F JCMGUODNZMETBM-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 229910052785 arsenic Inorganic materials 0.000 description 3
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 3
- 230000010354 integration Effects 0.000 description 3
- 239000010970 precious metal Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The preparation process of high purity hydrofluoric acid includes the following steps: 1. rectifying and purifying anhydrous hydrogen fluoride liquid at 19-35 deg.c via adding depurant KMnO4 solution of 1-3 wt% concentration in 1-5 wt% of anhydrous hydrogen fluoride liquid; 2. absorbing the purified hydrogen fluoride gas to obtain semi-finished hydrofluoric acid; and 3. ultraclean filtering the semi-finished hydrofluoric acid to obtain high purity hydrofluoric acid. The present invention has the advantages of effective elimination of arsenic trifluoride impurity, capacity of obtaining high purity hydrofluoric acid product meeting the requirement of SIME-C8 standard, low cost and great output.
Description
One, technical field
The present invention relates to a kind of preparation method of hydrofluoric acid, especially the preparation method of high purity hydrofluoric acid.
Two, technical background
Hydrofluoric acid (hydrofluoric, HF), relative molecular weight 20.1 is colourless transparent liquid, strongly-acid; It has intensive corrodibility to metal, glass, is severe toxicity.Hydrofluoric acid density (25 ℃) is 1.13g/ml (40 weight %).And high purity hydrofluoric acid is that strongly-acid cleans, etching reagent, can use with preparations such as nitric acid, glacial acetic acid, hydrogen peroxide and ammonium hydroxide, is mainly used in the production of super large-scale integration Technology.The high purity hydrofluoric acid main production methods is at present, the water absorption of anhydrous hydrogen fluoride elder generation is deployed into the hydrofluoric acid that concentration is 40 weight %, absorb by rectifying still rectifying and hydrogen fluoride again and make the hydrofluoric acid work in-process, filter by ultra-clean again and make high purity hydrofluoric acid; It is 106 ℃ that this production method is utilized the boiling point of 40 weight % hydrofluoric acid, the impurity that the great majority that it contained exist with the fluorochemical form has very high boiling point, most of impurity are separated goes out so make by rectifying still rectifying, but arsenous fluoride impurity is difficult to separate in the hydrofluoric acid, its easily and hydrofluoric acid together azeotropic come out, and arsenic is critical impurities in the ultra-clean and high pure chemical reagent, so the hydrofluoric acid of this method preparation is difficult to be suitable in super large-scale integration; Because hydrofluoric acid has severe corrosive, and rectifying device need be used platinum, gold and silver precious metal or polytetrafluoroethylmaterial material manufacturing, this equipment price is quite expensive, makes plant capacity not too large simultaneously, and output also suffers restraints thereupon, and production cost is very high; This production technique needs earlier hydrogen fluoride to be dissolved into hydrofluoric acid, and hydrofluoric acid is the loaded down with trivial details technology of two steps of rectifying again, needs the work-yard wider, is unfavorable for very much the management and the operation of these type of emphasis dangerization product of hydrogen fluoride.
Three, technology contents
At above-mentioned shortcoming, the object of the present invention is to provide and a kind ofly can effectively remove the preparation method that arsenous fluoride impurity, rectifying device low price and capacity are big, be suitable for mass-produced high purity hydrofluoric acid.
Technology contents of the present invention is, a kind of preparation method of high purity hydrofluoric acid, and it comprises the steps:
(1), carry out the rectifying purifying, add cleaner KMnO simultaneously with anhydrous hydrogen fluoride liquid
4Solution, its concentration are 1～3 weight %, and add-on is 1～5 weight % of raw material anhydrous hydrogen fluoride liquid; Rectification temperature is 19～35 ℃;
(2), with ultrapure water rectifying is purified into hydrogen fluoride gas and absorbs, make the hydrofluoric acid work in-process;
(3), the hydrofluoric acid work in-process are carried out the ultra-clean filtration and make high purity hydrofluoric acid.
This production method has been cast out anhydrous hydrogen fluoride and has been absorbed into the hydrofluoric acid loaded down with trivial details operation of rectifying again, directly carry out the rectifying purifying with anhydrous hydrogen fluoride liquid, rectifying still is the titanium still, utilized the inert principle of pure hydrogen fluoride liquid, thereby reduced the expensive cost of equipment use precious metal or Teflon the titanium still.And this technology has been strengthened the arsenous fluoride separate impurities, adopts cleaner with tervalent arsenic complete oxidation, makes it to generate difficult evaporable compound, it is enriched in rectifying in the tower still and is removed.
The advantage that the present invention is compared with prior art had is:
1, can effectively remove arsenous fluoride impurity, make the high purity hydrofluoric acid of making meet the SIME-C8 standard, be applicable to the production of super large-scale integration Technology.
2, rectifying still does not need with precious metal or Teflon manufacturing, and manufacturing cost reduces, and the production cost of high purity hydrofluoric acid has been reduced.
3, the manufacturing cost of rectifying still reduces, and makes its volume can obtain increasing, and output is improved a lot
Four, specific embodiment
Example 1,300kg anhydrous hydrogen fluoride liquid is carried out the rectifying purifying, adding concentration simultaneously is the cleaner KMnO of 2 weight %
4Solution, its add-on are 4.5kg; Its rectification temperature is 23 ℃; With ultrapure water rectifying is purified into hydrogen fluoride gas again and absorbs, make the hydrofluoric acid work in-process, its concentration 49 weight %, weight 480kg; The hydrofluoric acid work in-process are carried out the ultra-clean filtration make high purity hydrofluoric acid, weight 460kg.
Example 2,200kg anhydrous hydrogen fluoride liquid is carried out the rectifying purifying, adding concentration simultaneously is the cleaner KMnO of 2 weight %
4Solution, its add-on are 2kg; Its rectification temperature is 25 ℃; With ultrapure water rectifying is purified into hydrogen fluoride gas again and absorbs, make the hydrofluoric acid work in-process, its concentration 50 weight %, weight 300kg; The hydrofluoric acid work in-process are diluted and ultra-clean filters and to make high purity hydrofluoric acid, weight 300kg.
Example 3,350kg anhydrous hydrogen fluoride liquid is carried out the rectifying purifying, adding concentration simultaneously is the cleaner KMnO of 2 weight %
4Solution, its add-on are 5kg; Its rectification temperature is 34 ℃; With ultrapure water rectifying is purified into hydrogen fluoride gas and absorbs, make the hydrofluoric acid work in-process, concentration 49 weight %, weight 560kg; The hydrofluoric acid work in-process are carried out the ultra-clean filtration make high purity hydrofluoric acid, weight 550kg.
Example 4,100kg anhydrous hydrogen fluoride liquid is carried out the rectifying purifying, adding concentration simultaneously is the cleaner KMnO of 2 weight %
4Solution, its add-on are 1.6kg; Its rectification temperature is 26 ℃; With ultrapure water rectifying is purified into hydrogen fluoride gas again and absorbs, make the hydrofluoric acid work in-process, concentration 49 weight %, weight 150kg; The hydrofluoric acid work in-process are carried out the ultra-clean filtration make high purity hydrofluoric acid, weight 130kg.
The physical index data such as the table 1 of example 1～4:
| Physical index | Example 1 | Example 2 | Example 3 | Example 4 |
| Silicofluoric acid (H 2SiF 6)，ppm；max | 50 | 50 | 50 | 50 |
| Ignition residue, max | 2000 | 2000 | 2000 | 2000 |
| Muriate (Cl), max | 2000 | 2000 | 2000 | 2000 |
| Phosphoric acid salt (PO 4)，max | 500 | 500 | 500 | 500 |
| Vitriol (SO 4)，max | 1000 | 1000 | 1000 | 1000 |
| Sulphite (SO 3)，max | 500 | 500 | 500 | 500 |
| Aluminium (Al), max | ≤1 | ≤1 | ≤1 | ≤1 |
| Arsenic (As), max | ≤1 | ≤1 | ≤1 | ≤1 |
| Calcium (Ca), max | ≤1 | ≤1 | ≤1 | ≤1 |
| Chromium (Cr), max | ≤1 | ≤1 | ≤1 | ≤1 |
| Copper (Cu), max | ≤1 | ≤1 | ≤1 | ≤1 |
| Gallium (Ga), max | ≤1 | ≤1 | ≤1 | ≤1 |
| Iron (Fe), max | ≤2 | ≤2 | ≤2 | ≤2 |
| Plumbous (Pb), max | ≤1 | ≤1 | ≤1 | ≤1 |
| Magnesium (Mg), max | ≤1 | ≤1 | ≤1 | ≤1 |
| Manganese (Mn), max | ≤1 | ≤1 | ≤1 | ≤1 |
| Nickel (Ni), max | ≤1 | ≤1 | ≤1 | ≤1 |
| Potassium (K), max | ≤1 | ≤1 | ≤1 | ≤1 |
| Silver (Ag), max | ≤1 | ≤1 | ≤1 | ≤1 |
| Sodium (Na), max | ≤1 | ≤1 | ≤1 | ≤1 |
| Tin (Sn), max | ≤1 | ≤1 | ≤1 | ≤1 |
Table 1
Claims (2)
1, a kind of preparation method of high purity hydrofluoric acid, it comprises the steps:
(1), carry out the rectifying purifying, add cleaner KMnO simultaneously with anhydrous hydrogen fluoride liquid
4Solution, its concentration are 1～3 weight %, and add-on is 1～5 weight % of raw material anhydrous hydrogen fluoride liquid; Rectification temperature is 19～35 ℃;
(2), with ultrapure water rectifying is purified into hydrogen fluoride gas and absorbs, make the hydrofluoric acid work in-process;
(3), the hydrofluoric acid work in-process are carried out the ultra-clean filtration and make high purity hydrofluoric acid.
2, the preparation method of high purity hydrofluoric acid according to claim 1 is characterized by cleaner KMnO
4The concentration of solution is 2 weight %.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100965931A CN100443398C (en) | 2006-10-09 | 2006-10-09 | Prepn process of high purity hydrofluoric acid |
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| CNB2006100965931A CN100443398C (en) | 2006-10-09 | 2006-10-09 | Prepn process of high purity hydrofluoric acid |
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|---|---|
| CN1931709A true CN1931709A (en) | 2007-03-21 |
| CN100443398C CN100443398C (en) | 2008-12-17 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100546903C (en) * | 2007-08-06 | 2009-10-07 | 江阴市润玛电子材料有限公司 | Purifying method of ultrahigh pure hydrofluoric acid |
| CN103086327A (en) * | 2013-02-18 | 2013-05-08 | 苏州晶瑞化学有限公司 | Preparation method of ultra-clean high-purity hydrofluoric acid |
| CN103613075A (en) * | 2013-12-02 | 2014-03-05 | 浙江凯圣氟化学有限公司 | Preparation method of ultrapure electronic-grade hydrofluoric acid |
| CN103864018A (en) * | 2014-03-05 | 2014-06-18 | 福建省邵武市永飞化工有限公司 | Method for removing arsenic from industrial hydrofluoric acid |
| CN103910334A (en) * | 2014-04-21 | 2014-07-09 | 仲晓武 | Preprocessing process and device of ultrahigh pure hydrofluoric acid in mass production |
| US9896334B2 (en) | 2014-12-18 | 2018-02-20 | Mexichem Fluor, Sociedad Anonima de Capical Variable | Process for purification of hydrofluoric acid including obtaining arsenious acid by-product |
| CN111661860A (en) * | 2020-06-19 | 2020-09-15 | 锦洋高新材料股份有限公司 | Production method of anhydrous aluminum fluoride |
| CN113401874A (en) * | 2021-07-14 | 2021-09-17 | 浙江凯圣氟化学有限公司 | Method for removing arsenic in electronic-grade hydrofluoric acid |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE632837A (en) * | 1962-06-04 | 1963-10-21 | ||
| GB1192474A (en) * | 1968-05-21 | 1970-05-20 | Vnii Khim Reaktinov I Osbo Chi | Method and Apparatus for Producing Hydrofluoric Acid of High Purity |
| US3663382A (en) * | 1969-08-19 | 1972-05-16 | Du Pont | Process of recovering hydrogen fluoride free of arsenic by distillation |
| JP2821947B2 (en) * | 1990-11-02 | 1998-11-05 | 森田化学工業株式会社 | Method for producing ultrapure hydrofluoric acid |
-
2006
- 2006-10-09 CN CNB2006100965931A patent/CN100443398C/en active Active
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100546903C (en) * | 2007-08-06 | 2009-10-07 | 江阴市润玛电子材料有限公司 | Purifying method of ultrahigh pure hydrofluoric acid |
| CN103086327A (en) * | 2013-02-18 | 2013-05-08 | 苏州晶瑞化学有限公司 | Preparation method of ultra-clean high-purity hydrofluoric acid |
| CN103086327B (en) * | 2013-02-18 | 2013-11-13 | 苏州晶瑞化学有限公司 | Preparation method of ultra-clean high-purity hydrofluoric acid |
| CN103613075A (en) * | 2013-12-02 | 2014-03-05 | 浙江凯圣氟化学有限公司 | Preparation method of ultrapure electronic-grade hydrofluoric acid |
| CN103864018A (en) * | 2014-03-05 | 2014-06-18 | 福建省邵武市永飞化工有限公司 | Method for removing arsenic from industrial hydrofluoric acid |
| CN103864018B (en) * | 2014-03-05 | 2016-02-10 | 福建省邵武市永飞化工有限公司 | The method of industrial hydrofluoric acid arsenic removal |
| CN103910334A (en) * | 2014-04-21 | 2014-07-09 | 仲晓武 | Preprocessing process and device of ultrahigh pure hydrofluoric acid in mass production |
| CN103910334B (en) * | 2014-04-21 | 2016-06-22 | 仲晓武 | The pretreating process of a kind of volume production ultra-pure hydrofluoric acid and device thereof |
| US9896334B2 (en) | 2014-12-18 | 2018-02-20 | Mexichem Fluor, Sociedad Anonima de Capical Variable | Process for purification of hydrofluoric acid including obtaining arsenious acid by-product |
| CN111661860A (en) * | 2020-06-19 | 2020-09-15 | 锦洋高新材料股份有限公司 | Production method of anhydrous aluminum fluoride |
| CN113401874A (en) * | 2021-07-14 | 2021-09-17 | 浙江凯圣氟化学有限公司 | Method for removing arsenic in electronic-grade hydrofluoric acid |
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Assignee: Jiangyin Jianghua Micro-electric Materials Co., Ltd. Assignor: Yin Fuhua Contract fulfillment period: 2009.3.20 to 2019.3.19 contract change Contract record no.: 2009320000745 Denomination of invention: Prepn process of high purity hydrofluoric acid Granted publication date: 20081217 License type: Exclusive license Record date: 2009.5.5 |
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