CN100420625C - Process for preparation of ultrapure hydrogen peroxide - Google Patents
Process for preparation of ultrapure hydrogen peroxide Download PDFInfo
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- CN100420625C CN100420625C CNB200610030212XA CN200610030212A CN100420625C CN 100420625 C CN100420625 C CN 100420625C CN B200610030212X A CNB200610030212X A CN B200610030212XA CN 200610030212 A CN200610030212 A CN 200610030212A CN 100420625 C CN100420625 C CN 100420625C
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Abstract
The invention discloses a making method of ultrapure hydrogen peroxide, which comprises the following steps: adopting industrial hydrogen peroxide as raw material; predisposing through ionic exchanging method or distilling method to reach agent grade standard; adopting large-hole adsorbing resin to remove organic carbon; removing impurity ion through two-segment of ionic exchanging column; gathering the dust particle from film filter to obtain the object.
Description
Technical field
The present invention relates to a kind of preparation method of ultrapure hydrogen peroxide, refer to a kind of semi-conductor, super large-scale integration of being used for more specifically, meet the preparation method of the ultrapure hydrogen peroxide of SEMI C12 standard.
Background technology
The ultra-clean high-purity hydrogen peroxide is as a kind of important microelectronics chemistry product, be widely used in aspects such as cleaning in the assembling of semi-conductor, super large-scale integration and the course of processing, corrosion, fast development along with electronic industry, requirement to hydrogen peroxide purity is also more and more higher, develop into ultrapure hydrogen peroxide (single cations is the ppb level) by high-purity hydrogen peroxide (single cations is the ppm level), every index request reaches 12 grades-SEMI of the chemical material part C12 standard (hereinafter to be referred as SEMI C12 standard) of semiconductor equipment and material structure formulation.
Hydrogen peroxide is the explosion hazard product, in the ultrapure hydrogen peroxide preparation process, be subjected to the influence of the sequential scheduling various factors of temperature, flow velocity, pressure, ion exchange resin: can produce heat in the ion exchange process, if the service temperature height easily makes hydrogen peroxide decomposition, along with temperature rises, the decomposition reaction aggravation, have an accident, finally cause blast, temperature must be controlled in the safe scope; According to another mensuration, the hydrogen peroxide flow velocity is in 3.8-6.4 rice/time in the ultrapure hydrogen peroxide preparation process, and temperature control is more stable, has operability; Working pressure should be reasonable, and pressure is crossed the change that conference causes the hydrogen peroxide flow velocity, and the resistance that produces in the ion exchange column makes hydrogen peroxide leave standstill decomposition in post, causes the generation of accident.
In the prior art, the technical grade hydrogen peroxide adopts cost low mostly, the anthraquinone production of technology maturation, contain in the product a large amount of organic, inorganic impurity.For eliminating these impurity, distillation under vacuum is generally used in the purification of industrial hydrogen peroxide, or uses reverse osmosis method, ion exchange method etc., since its inferior separating effect, the production cost height, the quality instability, product purity does not reach service requirements.
Chinese patent CN1699144A discloses a kind of purification continuous production process for high-purity hydrogen peroxide, with the hydrogen peroxide is raw material, utilize macroporous adsorptive resins absorption organic carbon (TOC), carry out ion-exchange through the single ion exchange column of yin, yang, again through the ion-exchange of zwitterion mixing column, remove the yin, yang ionic impurity,, remove dust granules by polyvinylidene difluoride (PVDF) (PVDF) millipore filter.Can obtain meeting the high-purity hydrogen peroxide product of semiconductor equipment and material structure SEMI C8 standard according to this disclosed report.
The sequential combination of ion exchange resin is very important.Owing to contain in the industrial hydrogen peroxide product a large amount of organicly, inorganic impurity adds the method for zwitterion mixing column ion-exchange with the single ion exchange column of yin, yang, can not make the content of foreign ion reach the requirement of SEMI C12 standard.
The present domestic report of not seeing the suitability for industrialized production ultrapure hydrogen peroxide product that meets SEMI C12 standard.
Summary of the invention
The technical problem that the present invention solves provides a kind of preparation method of ultrapure hydrogen peroxide, and the high-purity hydrogen peroxide product index is lower than the SEMIC12 standard in the prior art to overcome, and quality can not satisfy the deficiency of service requirements.
Technical scheme of the present invention is such:
With industrial hydrogen peroxide is raw material, earlier through ion exchange method or distillation method pre-treatment, reach the SILVER REAGENT standard, adopt absorption with macroporous adsorbent resin to remove organic carbon again, carry out ion-exchange through the ion exchange resin column two-stage tandem and remove foreign ion, film filter filters the integrated approach of removing dust granules, obtains target product of the present invention.
Method of the present invention is carried out ion-exchange with the hydrogen peroxide feed liquid of SILVER REAGENT through the ion exchange resin two-stage tandem, obtains ultrapure hydrogen peroxide of the present invention, comprises the steps:
Under temperature 1-15 ℃, the condition of pressure 0.1-0.15MPa, 30-35% industry hydrogen peroxide is reached the feed liquid of SILVER REAGENT through pre-treatment, with 3.8-6.4 rice/hour superficial velocity by behind the macroporous adsorbent resin, pass through cation exchange resin column successively, anion-exchange resin column carries out first step ion-exchange; Successively by cation exchange resin column, anion-exchange resin column mixes the zwitterion exchange column, carries out second stage ion-exchange again, and the pressure with 0.01-0.08MPa enters the film filter filtration then, collects the target product ultrapure hydrogen peroxide.
The said cation exchange resin column of the present invention, anion-exchange resin column, the column length that mixes the zwitterion exchange column is 0.8-1.5 rice, and length-to-diameter ratio is 8-15 rice/rice.
In the said mixing zwitterion of the present invention exchange column, the volume ratio of zwitterion is 1: 1-1: 2, and ion exchange resin is selected H for use
+The type resin cation (R.C.), OH
-The type resin anion(R.A).
Film filter of the present invention adopts the fluorine material membrane strainer of 0.1 μ m specification; Material is a kind of in tetrafluoroethylene, the fluorinated ethylene propylene, preferably polytetrafluoroethylene, and the present invention filters with two placed in-line modes of film filter.
The ultrapure hydrogen peroxide main content that obtains with preparation method of the present invention is greater than 30%, organic carbon content is lower than 20ppm, and single cations is lower than 0.1ppb, and single anion-content is lower than 30ppb, dust granules greater than 0.5 μ m is lower than 25/milliliter, meets SEMI C12 standard.
Industrial hydrogen peroxide raw material main content used in the present invention is more than 30%, and positively charged ion is more than 10ppm, and negatively charged ion is at 3000-5000ppm.
The technological process of the inventive method makes up on prior art, the ion exchange column of use, and anionite-exchange resin, Zeo-karb and equipment can obtain by the hydrogen peroxide equipment purchase except that indicating, and the present invention repeats no more.
The present invention adopts the ion exchange resin two-stage tandem to carry out the ultrapure hydrogen peroxide that ion-exchange obtains, and has avoided the influence of foreign ion to quality product, and product meets SEMI C12 standard.
With the ultrapure hydrogen peroxide that preparation method of the present invention obtains, security is good, and steady quality is suitable for large-scale industrialization production.
Embodiment
The invention will be further described below by embodiment, but embodiment does not limit protection scope of the present invention.
Embodiment 1
1) temperature is 1～4 ℃, under the condition of pressure 0.10MPa, 35% industrial hydrogen peroxide feed liquid of 2～3 ℃ of feed temperatures after pretreatment quality reaches SILVER REAGENT, by macroporous adsorbent resin (float special company: MNm-220]), is analyzed organic carbon content with 3.8 meters/hour superficial velocitys;
2) temperature is 1～4 ℃, under the condition of pressure 0.10MPa, the feed liquid that the temperature that step 1 is obtained is 2～3 ℃, with 3.8 meters/hour superficial velocitys, enter cation exchange resin column and (float the special SGC-650 of company, post is high 1 meter) leave and enter anion-exchange resin column behind the cation exchange resin column and (float the special SGA-550 of company, post is high 1 meter), the feed liquid that obtains first step ion-exchange enters cation exchange resin column successively, anion-exchange resin column mixes anion-cation exchange resin post (volume ratio of mixing zwitterion in the zwitterion exchange column is 1: 1, and post is high 1 meter), obtain the hydrogen peroxide feed liquid of second stage ion-exchange, enter medial launder;
4) keep 10-15 ℃ of medial launder feed temperature, second stage ion-exchange liquid that will be after middle control analysis is qualified is pressed into two placed in-line tetrafluoroethylene film filter (Mi Keli companies with the perfluor magnetic drive pump with the pressure of 0.03MPa, 0.1 μ m specification) filter, hydrogen peroxide after the filtration enters the product groove, with 2 tons be one batch of analysis of testing, confirm to pack after quality meets SEMI C12 index;
5) check analysis result: hydrogen peroxide main content 30.88%, organic carbon content 5.429ppm, single cations is lower than 0.1ppb, and single anion-content is lower than 30ppb, greater than 6/milliliter of the dust granules (seeing Table 1) of 0.5 μ m.
Embodiment 2
1～5 ℃ of temperature, under the condition of pressure 0.10～0.14MPa, after 35% industrial hydrogen peroxide feed liquid pretreatment quality of 2～3 ℃ of feed temperatures reached SILVER REAGENT, superficial velocity with 6.4 meters/hour passes through macroporous adsorbent resin, remove organic carbon, identical with embodiment 1 method, obtain the ultrapure hydrogen peroxide product, the volume ratio of wherein mixing zwitterion in the zwitterion exchange column is 1: 1.2, and post is high 1 meter, the check analysis result: hydrogen peroxide main content 31.09%, organic carbon content 8.736ppm, single cations is lower than 0.1ppb, and single anion-content is lower than 30ppb, greater than 8/milliliter of the dust granules (seeing Table 1) of 0.5 μ m.
Table 1 hydrogen peroxide standard and analytical results
| Analysis project | SEMI C8 | SEMI C12 | Embodiment 1 | Embodiment 2 | Analytical instrument |
| Content (H 2O 2) | 30.0-32.0％ | 30.0-32.0％ | 30.88 | 31.09％ | Divide |
| Outward appearance (APHA) | 10max | - | / | ＜5 | Divide |
| Residue on evaporation | - | - | / | / | |
| Muriate (Cl) | 200ppbmax | 30ppb max | 26ppb | 29ppb | IC |
| Nitrate (NO3) | 400ppbmax | 30ppb max | / | 29ppb | IC |
| Phosphoric acid salt (PO4) | 200ppbmax | 30ppb max | / | 17ppb | IC |
| Vitriol (SO4) | 200ppbmax | 30ppb max | / | 30ppb | IC |
| Total nitrogen (TOC) | - | - | / | / | / |
| Total organic carbon (TOC) | 20pp max | - | 5.429ppm | 8.736ppm | TOC-V CPH |
| Total carbon (TOC) | - | 10ppm max | / | / | / |
| Free acid | 0.6μeq/gmax | - | / | / | / |
| Aluminium (Al) | 1ppb max | 100ppt max | 20ppt | Less than detection limit | ICP-MS |
| Ammonium (NH 4) | - | - | / | / | / |
| Antimony (Sb) | 1ppb max | 100ppt max | / do not detect | / do not detect | ICP-MS |
| Arsenic (As) | 1ppb max | 100ppt max | / do not detect | / do not detect | ICP-MS |
| Arsenic and antimony (in arsenic) | - | - | / | / | / |
| Barium (Ba) | - | 100ppt max | / do not detect | / do not detect | ICP-MS |
| Beryllium (Be) | - | - | / | / | / |
| Bismuth (bi) | - | - | / | / | / |
| Boron (B) | 1ppb max | 100ppt max | / do not detect | / do not detect | ICP-MS |
| Cadmium (Cd) | 1ppb max | - | / do not detect | / do not detect | ICP-MS |
| Calcium (Ca) | 1ppb max | 100ppt max | 80ppt | 10ppt | ICP-MS |
| Chromium (Cr) | 1ppb max | 100ppt max | 10ppt | Less than detection limit | ICP-MS |
| Cobalt (Co) | 1ppb max | - | 10ppt | Less than detection limit | IC-MS |
| Copper (Cu) | 1ppb max | 100ppt max | 10ppt | Less than detection limit | ICP-MS |
| Sow (Ga) | - | - | / | / | / |
| Germanium (Ge) | - | - | / | / | / |
| Gold (Au) | 10ppb max | - | Less than detection limit | Less than detection limit | ICP-MS |
| Indium (In) | - | - | / | / | / |
| Iron (Fe) | 1ppb max | 100ppt max | 30ppt | Less than detection limit | ICP-MS |
| Plumbous (Pb) | 1ppb max | 100ppt max | / do not detect | / do not detect | ICP-MS |
| Lithium (Li) | 1ppb max | 100pptmax | / do not detect | / do not detect | ICP-MS |
| Magnesium (Mg) | 1ppb max | 100ppt max | Less than detection limit | Less than detection limit | ICP-MS |
| Manganese (Mn) | 1ppb max | 100ppt max | Less than detection limit | Less than detection limit | ICP-MS |
| Molybdenum (Mo) | 1ppb max | - | / do not detect | / do not detect | ICP-MS/ |
| Nickel (Ni) | 1ppb max | 100pp max | 10ppt | Less than detection limit | ICP-MS |
| Niobium (Nb) | - | - | / | / | / |
| Platinum (Pt) | - | - | / | / | / |
| Potassium (K) | 1ppb max | 100ppt max | 70ppt | 10ppt | ICP-MS |
| Silver (Ag) | 1ppb max | - | / do not detect | / do not detect | ICP-MS |
| Sodium (Na) | 1ppb max | 100ppt max | 80ppt | 10ppt | ICP-MS |
| Strontium (Sr) | 1ppb max | - | / do not detect | / do not detect | ICP-MS/ |
| Tantalum (Ta) | - | - | / | / | / |
| Thallium (Tl) | - | - | / | / | / |
| Tin (Sn) | 1ppb max | 100ppt max | / do not detect | / do not detect | /ICP-MS |
| Titanium (Ti) | 1ppb max | 100ppt max | 30ppt | Less than detection limit | ICP-MS |
| Vanadium (V) | 1ppb max | 100ppt max | / do not detect | / do not detect | /ICP-MS |
| Zinc (Zn) | 1ppb max | 100ppt max | 60ppt | Less than detection limit | ICP-MS |
| Zirconium (Zr) | - | - | / | / | / |
| Dust granules/ml | ≥0.5μm， 25max | / | 6pcs | 8pcs |
The ultrapure hydrogen peroxide content analysis adopts and divides method, and organic carbon adopts the analysis of TOC analyser, and positively charged ion adopts ICP-MS to analyze, and negatively charged ion adopts ion chromatography, and dust granules adopts the laser particle calculating instrument to measure (seeing Table 2).
The title model of table 2 testing tool
| Title | Technical requirements | Model |
| Inductance lotus root and plasma spectrum-mass spectrograph (ICP-MS) | Test limit＜1ppt | The HP-7500S of Hewlett-Packard |
| Atomic Absorption Spectroscopy AAS (AA) | Test limit＜0.1ppb | PE5100ZL |
| Total carbon analyzer (TOC) | C＜1ppb | Island Tianjin-TOC-Vwph |
| Ion chromatograph (IC) | Negatively charged ion＜0.1ppb | Dionex 600 |
| Laser light scattering particle determinator (PMC) | Test＜0.2 μ particle | Pacific Scientific HIACROYCO-8000S |
| Purifying air particle test instrument | The same |
Claims (8)
1. the preparation method of a ultrapure hydrogen peroxide is characterized in that the hydrogen peroxide feed liquid of SILVER REAGENT is carried out ion-exchange through the ion exchange resin two-stage tandem, comprises the steps:
Under temperature 1-15 ℃, the condition of pressure 0.1-0.15MPa, 30-35% industry hydrogen peroxide is reached the feed liquid of SILVER REAGENT through pre-treatment, with 3.8-6.4 rice/hour superficial velocity by behind the macroporous adsorbent resin, by cation exchange resin column, anion-exchange resin column, carry out first step ion-exchange successively; Successively by cation exchange resin column, anion-exchange resin column, mixing zwitterion exchange column, carry out second stage ion-exchange again, the pressure with 0.01-0.08MPa enters the film filter filtration then, collects the target product ultrapure hydrogen peroxide.
2. method according to claim 1 is characterized in that the column length of said cation exchange resin column, anion-exchange resin column, mixing zwitterion exchange column is 0.8-1.5 rice, and length-to-diameter ratio is 8-15 rice/rice.
3. method according to claim 1 and 2 is characterized in that the volume ratio of zwitterion in the said mixing zwitterion exchange column is 1: 1-1: 2.
4. method according to claim 1 is characterized in that said ion exchange resin selects H for use
+Type resin cation (R.C.), OH
-The type resin anion(R.A).
5. method according to claim 1 is characterized in that said film filter is the fluorine material membrane strainer of 0.1 μ m specification.
6. method according to claim 5 is characterized in that said fluorine material membrane strainer is two cascade filtrations.
7. method according to claim 5 is characterized in that, the material of said fluorine material membrane strainer is a kind of in tetrafluoroethylene, the fluorinated ethylene propylene.
8. method according to claim 7 is characterized in that, the material of said fluorine material membrane strainer is a tetrafluoroethylene.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8715613B2 (en) | 2010-12-02 | 2014-05-06 | Shanghai Chemical Reagent Research Institute | Method for producing of ultra-clean and high-purity aqueous hydrogen peroxide solution |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101804969A (en) * | 2010-04-02 | 2010-08-18 | 赫格雷(大连)制药有限公司 | Low-carbon environment friendly production method for extra high-purity H2O2 |
| CN102701158B (en) * | 2012-06-21 | 2014-01-08 | 苏州晶瑞化学有限公司 | Continuous preparation method for high-purity hydrogen peroxide |
| CN103466557B (en) * | 2013-09-11 | 2015-07-22 | 杭州精欣化工有限公司 | Preparation method of ultra-pure hydrogen peroxide aqueous solution |
| CN109941967A (en) * | 2019-04-24 | 2019-06-28 | 广州市天夫美新材料科技有限公司 | The production technology of One-step production super-clean high-purity microelectronics grade hydrogen peroxide |
| CN113526470A (en) * | 2021-08-09 | 2021-10-22 | 晶瑞电子材料股份有限公司 | Continuous preparation method of ultra-clean high-purity hydrogen peroxide |
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| CN1189451A (en) * | 1996-12-05 | 1998-08-05 | 斯塔泰克文切斯公司 | On-site manufacture of ultra-high-purity hydrogen peroxide |
| CN1285311A (en) * | 2000-09-21 | 2001-02-28 | 上海哈勃化工有限公司 | Process and equipment for preparation of ultrapure hydrogen peroxide |
| CN1330035A (en) * | 2000-06-21 | 2002-01-09 | 三德化学工业株式会社 | Method for producing purified aqueous hydrogen peroxide solution |
| CN1439600A (en) * | 2003-04-10 | 2003-09-03 | 天津科技大学 | High-purity hydrogen peroxide preparation |
| CN1699144A (en) * | 2005-05-17 | 2005-11-23 | 李祥庆 | Purification continuous production process for high-purity hydrogen peroxide |
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2006
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1189451A (en) * | 1996-12-05 | 1998-08-05 | 斯塔泰克文切斯公司 | On-site manufacture of ultra-high-purity hydrogen peroxide |
| CN1330035A (en) * | 2000-06-21 | 2002-01-09 | 三德化学工业株式会社 | Method for producing purified aqueous hydrogen peroxide solution |
| CN1285311A (en) * | 2000-09-21 | 2001-02-28 | 上海哈勃化工有限公司 | Process and equipment for preparation of ultrapure hydrogen peroxide |
| CN1439600A (en) * | 2003-04-10 | 2003-09-03 | 天津科技大学 | High-purity hydrogen peroxide preparation |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8715613B2 (en) | 2010-12-02 | 2014-05-06 | Shanghai Chemical Reagent Research Institute | Method for producing of ultra-clean and high-purity aqueous hydrogen peroxide solution |
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