CN1176032C - Producing process and technology for electronic grade water by intergrated film process - Google Patents
Producing process and technology for electronic grade water by intergrated film process Download PDFInfo
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Abstract
The present invention relates to a producing technology and a course for an integrated membrane course of electronic grade water. Tap water is used as raw water so as to manufacture electronic grade ultrapure water by four component parts, namely pretreatment, a first stage pure water system, a second stage pure water system and precise treatment of terminal membrane filtration orderly, wherein a pretreatment unit mainly comprises sand filtration, ultrafiltration, activated carbon adsorption and sodium filtration; the first stage pure water system is mainly composed of a reverse osmosis unit, a membrane degassing unit, an electro-deionizing unit, an ion exchange resin unit with boron selectivity, etc.; the second stage pure water system is mainly composed of an ultraviolet lamp oxidizing unit and polishing mixed-bed resin; the terminal membrane filtration adopts a polishing reverse osmosis membrane for the treatment. High-efficiency, clean and reliable non-chemical regeneration type ultrapure water production can be realized by the water manufacturing system without draining environmental hazard wastewater. In addition, boron as an impurity can be effectively removed, and the cost of the water manufacturing system is reduced. The utilization rate of water is increased, and the terminal filtration is safer and more reliable.
Description
Technical field
The present invention relates to a kind of production method of ultrapure water, especially a kind of integrated membrane process production method of electronic-grade ultrapure water.
Background technology
The ultrapure water of indication of the present invention, be meant the various suspended impurities in the water, mineral ion and nonionic impurity, comprise various organism, microorganism such as bacterium, virus, and fine particle etc. is removed to " deionized water " or " high resistivity water " or " the ultra-high purity water " of the ultimate value that can reach.
Standard GB/T 11446.1-1997 definition " electronic grade water " is " making used high purity water in the electronic devices and components technological process ".The highest ranking of electronic grade water is to be used for rinse water ultra-large and that very large scale integration production is used.Electronic industry is to the quality requirements of ultrapure water, is different from other all industrial sector and needs to consider all contaminants in the water.
Pure water is as the part of integrated circuit production environment, and its quality quality directly plays great influence to quality product.In per pass manufacturing procedure almost, conduction or the insulating material layer be added to the surface of silicon chip.Before one deck adds down, need to fall the part on surface with corrosive pharmaceutical chemicals acid etching.Therefore, for guaranteeing rinsing up hill and dale and removing the chemicals of silicon chip surface, need to use pure water that product is cleaned.Yet the trace impurity in this process in the employed pure water may make product be polluted once more again.Therefore, the quality of production and the production cost of the product confrontation unicircuit of pure water have fundamental influence.
When phase later 1950s, semi-conductor industry was just come out, resistivity is unique water-quality guideline that 18M Ω cm (25 ℃) is considered to ultrapure water, and degree of depth deionization technology at that time---ion-exchange is to produce the ultrapure water of resistivity 18M Ω cm sometimes.Gradually find that only weighing the product quality with index of resistivity also is nowhere near thereafter.Middle nineteen seventies has proposed particulate, bacterium, carbonic acid gas, sodium, five new indexs of total organic carbon (TOC), and system water process begins to adopt reverse osmosis and ion-exchange process combined.The eighties, more and more tighter to the control of particulate and bacterium, ultra-filtration technique correspondingly has been introduced in the production of electronic grade water, and has increased the restriction index of dissolved oxygen in addition.Entered the ULSI epoch during the nineties, the ultrapure water manufacturing system that new adaptation mega bit order unicircuit is produced is all constantly being inquired into by each state.Therefore, the unicircuit integrated level to improve constantly the index request that makes to pollutent in the pure water strict day by day, ULSI becomes the extreme value of contemporary ultrapure water water quality to the pure water requirements in water quality.
Table one has provided the Japanese technical indicator of the unicircuit production of 64M DRAM integrated level being used ultrapure water and China's " electronic grade water " standard GB/T 11446.1-1997 EW-I level water.
Table one, electronic grade water water quality standard
| Project | Japan unicircuit pure water water quality standard integrated level 64M, live width 0.35 μ m | GB/T 11446.1-1997 EW-I |
| Resistivity (M Ω cm, 25 ℃) | ＞18.2 | ＞18 (95% times), be not less than 17 |
| Micropartical is (individual/mL)＞1 μ m＞0.05 μ m＞0.03 μ m | ＜1 ＜10 | ＜0.1 |
| Bacterium (individual/mL) | ＜0.001 | ＜0.01 |
| TOC(ppb) | ＜1 | ＜20 |
| SiO 2(ppb) | ＜0.1 | ＜2 |
| Na(ppb) | ＜0.01 | ＜0.5 |
| Ni(ppb) | ＜0.1 | |
| K | ＜0.5 | |
| Fe(ppb) | ＜0.01 | |
| Zn(ppb) | ＜0.01 | ＜0.2 |
| Cu(ppb) | ＜0.01 | ＜0.2 |
| Cl -(ppb) | ＜1 | |
| NO 3 -(ppb) | ＜1 | |
| PO 4 3- | ＜1 | |
| SO 4 2- | ＜1 | |
| Amide (ppb) | ＜0.01 | |
| Dissolved oxygen DO (ppb) | ＜5 |
For the production of electronic grade water, weak Ionized silicon (SiO in its desired inorganic impurity
2Deng), boron, (B), dissolved carbon dioxide (CO
2) removal be a difficult problem in the water technology always, the removal with silicon and boron is more difficult especially.
The silicate ion of silicon, especially solubility except influencing graphic defects, also can cause phosphorus silicon mist and threshold voltage to change.The content of boron is not generally paid close attention to by the people in the ultrapure water, but the progress of analysis science makes people recognize that trace B contained in the ultrapure water is another the important dopant species that influences the semiconductor machining quality in recent years.Boron concentration in the lattice substrate is to having decisive influence based on the transistorized threshold voltage of the hyperchannel that substrate generated, and the boron that therefore cleans higher concentration in the used ultrapure water can make the boron concentration in the substrate be difficult to control, thereby causes product defects.In addition, when with trickle hyperchannel transistor when producing the highly intergrated semiconductor product, so trickle process of producing product just need make in the substrate boron concentration along thickness direction accurately be controlled, and the boron concentration in this product process of will seeking survival conversely in the used ultrapure water has quite low value.
Traditional pure water preparation technology, unless generally contain three unit such as pre-treatment, desalination ionized impurities at least, but generally all have two significant disadvantages.The one, investment cost of equipment and operation and maintenance cost are high; The 2nd, face the processing emission problem of a large amount of environmental hazard waste liquids, this mainly is to need the ion exchange resin of chemical regeneration to cause owing to using.Use ion exchange technique, not only because of the consumption of a large amount of soda acids with regenerating resin cause that production efficiency is low, complicated operation, system can not continuous operation, its main problem is that the more a large amount of spent acid waste lyes that discharge are difficult to processing and serious environment pollution.In recent years, the pure water manufacturing technology that does not contain any chemical regeneration type receives much concern, and traditional ion-exchange is replaced by reverse osmosis (RO), electrodeionization technology such as (EDI).These new pure water preparation technology are technological core with the membrane sepn process generally, form integrated membrane process to adapt to production requirement in conjunction with other pre-process and post-process means.The use of technology such as RO and EDI has solved the inefficiency of water manufacturing system to a great extent, produces problems such as environmental hazard wastewater.
Patent JP 11244853A2 has designed following technical process and has been used for semi-conductor, optical lens and the required rinse water of liquid crystal production process.At first will be after the pH of pretreated tap water value be adjusted to 4-5, remove gases such as dissolved carbon dioxide through first-stage reverse osmosis desalination, degas module again, readjust the pH value again and enter the two-pass reverse osmosis desalination for behind the 7-11, the product water of two-pass reverse osmosis obtains ultrapure water through the electrodeionization deep desalting again.
The design of patent JP 11244854A2 then at first will be adjusted to 8-11 through the pH of pretreated tap water value, then earlier after first-stage reverse osmosis and electrodeionization process and obtain ultrapure water.The condensed water of first-stage reverse osmosis enters another reverse osmosis units, its condensed water discharging, and the condensed water of desalination water and EDI is recycled to the water inlet of first-stage reverse osmosis to improve water use efficiency.
It is the flow scheme design of core that patent JP 11262771A2 has taked equally with " reverse osmosis/electrodeionization ", but preprocessing means is comparatively complicated.At first the pH value of former water is adjusted to 3-5 and outgases, adopt the anionite-exchange resin adsorb organic compound then, the pH value of re-adjustment water enters the downstream to 6-9.5 " reverse osmosis/electrodeionization " system obtains ultrapure water.
Yet existing pure water, ultrapure water technology of preparing still are difficult to take into account simultaneously water quality purity and economy and the high efficiency of making the water process; In addition, the latest developments of analysis science have also brought a new problem and a difficult problem for the electronic-grade PREPARATION OF ULTRA-PURE WATER.This mainly shows the following aspects:
One, can not effectively remove boron
Be used for the former water that ultrapure water is produced, as tap water, well water or river, wherein the concentration of boron is generally dozens of ppb, and existing ultrapure water production technique all is difficult to remove ideally the trace B of this lower concentration.For the ion exchange process of taking chemical regeneration, the bed leakage just will take place from the boron of property in weak solution in the very short time of operation, therefore can only control the boron concentration in the product water by the regeneration frequency that increases the ion exchange resin bed layer.In addition, RO that has been widely used and EDI also can only remove about 40% and 75% boron respectively.For the production technique of using " two steps ro-mixed bed ion exchange " and " reverse osmosis-electrodeionization " deep desalting, its terminal membrane filtration product water afterwards still will contain the boron of 3-10ppb, and that this concentration level is still is too high.
Two, the facility investment of one-level pure water system is too high, and water use efficiency is on the low side
For current ultrapure water production process, in the one-level pure water system, all generally adopt two steps ro to add the design of ion-exchange (or EDI).Though two steps ro can alleviate the burden of follow-up ion exchange column greatly, the cost of investment of system is too high, and the water use efficiency of water manufacturing system is on the low side simultaneously.Total water use efficiency of general two steps ro is no more than 35%.
Three, the terminal precision processing still can not meet the requirements fully
When lithographic line width is reduced to 1 μ m when following, generally adopt ultra-filtration membrane to carry out end-filtration.At present more adopted be the terminal processing method of 0.1 μ mUF-UV (ultraviolet ray)-0.04 μ mUF, but for integrated level surpasses the unicircuit production of 64MDRAM, still can not guarantee indexs such as particulate qualified in the product water.
Therefore, preparation for the most complicated electronic grade water, need to adopt more scientific and reasonable comprehensive integration technology, can remove the various organic and inorganic impurity in the water fully, reliably, the qualified ultrapure water of the quality of production safely, further reduce simultaneously system's investment cost again, and improve the utilization ratio of water resources.
Summary of the invention
The objective of the invention is to shortcoming at existing ultrapure water production technology, a kind of new integrated membrane process that multiple membrane sepn process and other water technologies are combined is provided, effectively remove the various impurity in the water, realize efficient, cleaning, the ultrapure water production of regeneration type non-chemically reliably, its distinguishing feature not only is to exempt the handling problem of environmental hazard wastewater, and system water efficient is higher, system's operation is more reliable, can more effectively remove boron impurities, the water use efficiency of water manufacturing system is improved, the end-filtration safety and reliability.
The objective of the invention is to realize by the following technical solutions:
Design a kind of integrated membrane process that technologies such as ultrafiltration (UF), nanofiltration (NF), reverse osmosis (RO), electrodeionization (EDI), the film degassing, polishing reverse osmosis multiple membrane sepn processes such as (PRO) and sand filtration, charcoal absorption, pH regulator, uviolizing, the exchange of polishing mixed bed ion combine that is integrated with simultaneously, this technological process contains pretreatment unit, one-level pure water system (containing except that the boron unit), secondary pure water system, four integral parts in terminal precision processing unit.With city tap-water is former water, passes through above-mentioned four treatment steps successively, final electron gain level ultrapure water.
(1) pretreatment unit
It is the flow scheme design of core that the pretreatment unit employing is united with " UF-NF ".
UF is to be motivating force with pressure, utilizes the physics sieving action that liquid is carried out isolating membrane sepn process, and its working pressure is generally 0.2-0.3MPa.For the adoptable UF film of the present invention, can be the UF film of organic polymer material or inorganic materials.Organic materials UF film mainly contains polysulfones and polyolefin film, as polysulfones (PS), SPSF (SPS), polyethersulfone (PES), polypropylene (PP), polyacrylonitrile (PAN) etc.; Inorganic materials UF film mainly is an inorganic ceramic film.Employed UF film among the present invention, its molecular weight cut-off control is chosen as 20,000-50,000.
With city tap-water is former water, through the UF membrane sepn, can remove impurity such as colloid in the former water, particulate, larger molecular organics, bacterium, and the pollution index of former water is reduced to below 3.
NF is to be motivating force with pressure equally, utilizes the physics sieving action that liquid is carried out isolating membrane sepn process, and its pore diameter range is the 1-3 nanometer, mean pore size 2 nanometers.The membrane pore size of NF, working pressure, separation performance are between RO and UF.Main spendable NF film kind has cellulose acetate-cellulosetri-acetate (CA-CTA) film, aromatic polyamides composite membrane and sulfonated polyether sulfone film etc.Less than 20%, to calcium, magnesium hardness ion and other divalence and high valence ion, decreasing ratio can reach more than 95% the NF film to the rejection of univalent ion, and ratio of desalinization reaches 50-70% simultaneously.In addition, NF also can reach more than 90% the decreasing ratio of the various organic impurities of molecular weight more than 200.The spendable NF film trade mark has ESNA1-4040, ESNA1 etc., and its working pressure is about 0.5MPa, and for many and large-scale NF film system, by the appropriate design of flow process, its system water rate of recovery can be up to 85%.
Between UF and RO, use the NF film softening, can prevent the RO film fouling in downstream, and alleviate the organic impurity pollution of downstream process.
The charcoal absorption filter is set between UF and NF, and further microorganisms such as organism and bacteriophage are removed in absorption, alleviate the organic contamination burden of NF film.
The security personnel's strainer that uses the honeycomb filter core is set between charcoal absorption filter and NF, enters the NF membrane module in downstream to prevent active carbon powder.The filtering pore size filter of ensuring public security is 1-5 μ m.
If raw water quality deviation, then visual concrete water quality situation was provided with devices such as quartz sand filter, mechanical filter to strengthen pre-treatment before UF, thereby impurity such as the suspended substance in the removal water, big particle also reduces turbidity, prevents that the fenestra of UF film from stopping up, and flux descends.Used sand-bed filter, its filtration medium are the quartz sand of 0.4-1.0.
(2) one-level pure water system
Contain pH regulator, one-level RO, ozone sterilization, the film degassing, deep desalting unit in the one-level pure water system successively and remove the boron unit.
Through the pretreated former water of " UF-NF " associating, owing to most hardness ionses is removed, so can avoid the fouling in the RO membrane module of downstream.Water was taked to add methods such as dilute NaOH solution its pH value is adjusted to the weakly alkaline of 8.0-11.0 before entering one-level RO membrane module, was that 9.0-10.0 is good especially with pH, thereby helped dissolving CO
2, TOC, SiO
2Abundant removal, and the ultrapure water that after RO, obtains high resistivity by the EDI unit.After one-level RO desalination, the product water conductivity reaches 1-5 μ s/cm to NF water through pH regulator, and the RO film also can further be removed remaining organism and bacterium, particulate simultaneously.For the present invention, used RO film, be the low pressure polymeric amide of high desalination rate (greater than 99%) compound (TFC) film, the available commodity RO film trade mark has CPA-ULTRAPURE, CPA-3, CPA-4, ESPA-ULTRAPURE etc., and its standard operation pressure is 1.05-1.55MPa.
The pure water that obtains by one-level RO enters one-level pure water water tank, carries out the inflated with nitrogen protection in water tank, is subjected to the secondary pollution of impurity such as airborne particulate, carbonic acid gas to avoid pure water.In addition, employing on-site ozone producer adds the ozone of concentration 0.1-0.3ppm in the pure water case, to prevent bacterial growth.
One-level RO pure water enters hollow-fibre membrane degassing assembly through pure water pump and removes dissolved oxygen in the water.This assembly adopts the RO film of hydrophobic TEFLON or PE material, can only see through gas or oxygen.Pure water passes through in tubular fibre, and dissolved oxygen then is penetrated into the film outside, through nitrogen purging the remaining dissolved oxygen concentration in the water is dropped to below the 5ppb.The film de-gassing vessel be except that removing the dissolved oxygen, also can remove remaining dissolved carbon dioxide and alleviates the burden of the resin in downstream.
Employed EDI deep desalting device among the present invention, be a kind of new deep desalting means of being promoted the use of rapidly in recent years, its technical characterictic is to fill strong acid and strong base mixed bed ion exchange resin in the freshwater room of the electrodialyzer that thickness increases, electrodialysis and ion-exchange are combined, by electric energy and ion exchange resin and film deep desalting, realize simultaneously the cyclic regeneration of resin again by electric energy, exempted ion exchange resin is used the frequent regeneration of soda acid and produces the ultrapure water of resistivity 16-18M Ω cm directly, continuously.
For the present invention, former water again by the EDI deep desalting, is compared with traditional chemical regeneration type or non-regeneration type mixed bed ion exchange bed after membrane process such as UF, NF, RO are handled, and need not carry out complicated regeneration or frequently change resin resin.In addition, EDI also has the pH regulator of exempting from except that impurity and antibacterial such as dissolved carbon dioxide, silicon-dioxide, boron, germ-resistant ability.The weakly alkaline pH regulator that before RO, carries out, and distinctive water decomposition effect and the H that generates in the EDI process
+And OH
-Ion helps the ionization of these weak solutions from property impurity.This ionization in the EDI process is, the dissociation of water can take place on the surface of the freshwater room intermediate ion exchange membrane of EDI and ion exchange resin, and water molecules is dissociated into H
+And OH
-Ion, part of O H
-Weak Ionized silicon, boron impurity combine in ion and the water, generate silicate and borate ion respectively, move in the condensed water and remove thereby see through resin and film from freshet under the effect of applying direct current electric field.EDI device used in the present invention has been made specific descriptions in patent ZL00200207.8.
Removing the boron unit is by being filled with the ion exchange resin column that possesses the boron selective adsorption function with pure water.The resin that uses in this resin column is different from employed strongly basic anion exchange resin in the general ultrapure water production process, and the activity functional groups of its ion-exchange is a polyhydroxy-alcohol, belongs to weakly basic anion resin.Containing this is the weak-base ion-exchange resin of function of exchange base with the polyhydroxy-alcohol, can very effectively stably remove the trace B in the water, guarantees that the boron content of its water outlet is lower than 0.01-0.1ppb.
In system current journey, the boron selective resin is set at after the EDI deep desalting, to remove the Determination of Trace Boron that participates in the EDI product water fully, protects and increases water quality.Among the present invention, the boron selective ion exchange column is designed to non-regeneration pattern Cl when avoiding chemical regeneration
-, OH
-Etc. anionic pollution.Resin is directly changed in the saturated back of absorption.
(3) secondary pure water system
The secondary pure water system comprises ultrapure water water tank, ultraviolet lamp oxidizer and the exchange of polishing mixed bed ion successively.
In ultrapure water water tank and polishing mixed bed ion exchange column, all protect with high pure nitrogen.The ultraviolet ray oxidizer adopts the ultraviolet lamp of low pressure 185nm, decomposes the minute quantity TOC composition that remains in the one-level pure water system, is particularly useful for decomposing the lower low-molecular-weight organic matter of clearance in the RO film, further reduces below the TOC to 1ppb.Polishing mixes the equal grain ion exchange resin that bed is selected low stripping formula, removes preposition ultraviolet oxidizer and decomposes small organic molecule and the CO that TOC produces
2, thoroughly remove impurity such as measurement ion remaining in anhydrating and silicon simultaneously, make resistivity be stabilized in accessible highest level.Employed resin with uniform particle, its be defined as 95% anion-cation exchange resin particle grain size all median size 10% in.Polishing mixes bed and is designed to non-regeneration and mixes the secondary pollution that bed is produced when avoiding regenerating, regularly direct replacing resin.
(4) terminal membrane filtration
Adopting molecular weight cut-off is that 100 ultralow pressure polishing complex reverse osmosis membrane (PRO) is made end-filtration, replace conventional ultrafiltration, hold back size of particles 0.0001 μ m, thoroughly remove the upstream polishing and mix issuable micro-TOC and impurity such as particulate, bacterium in the bed, guarantee that product water quality meets that lithographic line width has reached 0.13 μ m even than the water requirement of littler unicircuit.
Each integral part collection among the present invention is an one, can produce following effect:
UF-gac-NF associating pre-treatment can be removed impurity such as various colloids in the water, particulate, organism, bacterium, and the salt of calcium, magnesium hardness ion and 50-70%, prevents the RO film fouling in downstream, guarantees its work-ing life; Unit such as the RO in the one-level pure water system, the film degassing, EDI deep desalting and boron selective resin can be removed the microorganisms such as mineral ion, boron, silicon, dissolved oxygen and bacterium in the water efficiently, continuously, and water outlet resistivity reaches 16-18M Ω cm; Ultraviolet lamp oxidizer in the secondary pure water system and polishing mix remaining micro-low-molecular-weight organic matter, bacterium and impurity in ionized state in the thorough removal system of bed; Terminal polishing reverse osmosis membrane filtration is thoroughly removed particulate, TOC and the bacterium of measurement, finally obtains the electronic grade water of ultra-high purity.
Description of drawings
Fig. 1 is the production technique block diagram of electronic-grade ultrapure water provided by the present invention;
Embodiment
In the technical process shown in Figure 1, the salt of suspended substance, particle, pigment, turbidity, organism, colloid, microorganism and calcium, magnesium hardness ion and 50-70% in the former water is removed in sand-bed filter-ultrafiltration-gac-security personnel's filtration-nanofiltration pre-treatment, wherein ultrafiltration employing molecular weight cut-off is 20,000-50,000 poly (ether-sulfone) ultrafiltration membrane, and aromatic polyamides ESNA1 film is adopted in nanofiltration.Ion and nonionic (organism, the particle etc.) impurity in pretreated water is removed in reverse osmosis.Under the necessary situation, carrying out pH regulator between NF and RO, the water inlet pH value of RO is adjusted to weakly alkaline, is 9.5 as pH, is beneficial to remove effectively TOC, CO
2And SiO
2Employed RO film is aromatic polyamides CPA-ULTRAPURE film.
The reverse osmose pure-water water tank is protected with nitrogen, avoids being subjected to the secondary pollution of air.In addition, it is suitable to fill with concentration in water tank, and the on-the-spot ozone of making is to prevent breed bacteria.The film degas module is in order to remove oxygen, nitrogen and carbonic acid gas remaining in the water.The continuous deep desalting of electrodeionization unit is exempted the repeated regeneration of pharmaceutical chemicals to resin, and the exhaust emission wastewater is not used the water resistance rate and reached 16-18M Ω cm.The exchange column that is filled with boron selective ion exchange resin places the downstream of electrodeionization unit, thoroughly removes in the water boron of trace, makes boron concentration in the product water be lower than 0.01ppb and obtains the one-level pure water.Remove resin column and protect with nitrogen equally, the spendable boron selective resin trade mark has Rome ﹠amp; The DIAION CRB02 of the AMBERLITEIRA-743T of Hass company and Mitsubishi Chemical Industries company etc.
The ultrapure water of one-level pure water system production enters the secondary pure water system, increases water quality and terminal polishing reverse-osmosis treated through ultrapure water tank, ultraviolet oxidation, polishing mixed-bed resin successively, obtains product water supply ultrapure water water spot.Employed ultraviolet lamp oxidizer, its ultraviolet wavelength are 185nm, in order to decompose in the one-level pure water system remaining low-molecular-weight organic matter polishing mix bed and then can remove the small organic molecule and the CO of measurement
2, further improve water outlet resistivity.Polishing mixes bed and equally also fills with nitrogen protection.The polishing reverse osmosis is thoroughly removed fine particle, bacterium and remaining TOC then as final water quality protection means.
Thereby the ultrapure water Production Flow Chart that Fig. 1 provided does not then contain the deionization unit of any chemical regeneration type, but the ultrapure water that does not contain boron is produced in the long-time continuous operation, does not produce any environmental hazard waste liquid simultaneously.With respect to the design of using " two steps ro-electrodeionization " or " two steps ro-ion-exchange mixes bed ", not only facility investment reduces, water use efficiency is improved simultaneously, and can stablize, remove efficiently unicircuit is produced disadvantageous trace B.
In the Production Flow Chart that Fig. 1 provided, the pipeline of its preprocessing part adopts clean polyvinyl chloride (C-PVC), polypropylene (PP) or ABS material, stainless steel or polishing stainless steel pipe are partly adopted in reverse osmosis in nanofiltration and the one-level pure water system, all adopt standard poly(vinylidene fluoride) (PVDF) or high-purity PVDF (PVDF-HP) or teflon (PFA) material with the pipeline between the water spot to terminal after reverse osmosis.When production line was used to warm ultrapure water is provided, corresponding pipeline then only adopted PVDF-HP or PFA material.PVDF, PFA are in chemical stability, and aspects such as maximum operating temperature all are much better than PVC, PP and ABS, and additive-free, no leachable, and bacterium can't depend on for existence, so its bacterium, TOC index are all very low, can not cause the decline of product water resistance rate.
Claims (7)
1, a kind of integrated membrane process production method of electronic grade water, with city tap-water is former water, make the electronic-grade ultrapure water through pre-treatment, one-level pure water system, secondary pure water system and four integral parts of terminal membrane filtration precision processing successively, it is characterized in that making the water process and take following integrated membrane process technology:
(1) adopt " sand filtration-ultrafiltration-gac-security personnel's filtration-nanofiltration " integrating process to form pretreatment system;
(2) adopt " pH regulator-reverse osmosis-ozone sterilization-film degassing-electrodeionization-boron selective ion exchange resin " integrating process to form the one-level pure water system, and to fill with the high pure nitrogen in reverse osmosis water tank, boron selective ion exchange resin column and one-level ultrapure water water tank be to protect gas;
(3) adopt " ultraviolet lamp oxidizer-polishing mixed bed ion exchange " to form secondary pure water system, and to fill with the high pure nitrogen in polishing mixed-bed resin post be to protect gas;
(4) adopt " polishing reverse osmosis " as the terminal membrane filtration system.
2, the integrated membrane process production method of electronic grade water according to claim 1 is characterized in that, the filtration medium of employed sand-bed filter is the quartz sand of 0.4-1.0mm in the pre-treatment.
3, the integrated membrane process production method of electronic grade water according to claim 1 is characterized in that, the adjusting of between nanofiltration and reverse osmosis the pH value of water being carried out is to add dilute NaOH solution to make the water inlet pH value of reverse osmosis be 8.0-11.0.
4, the integrated membrane process production method of electronic grade water according to claim 1, it is characterized in that, employed ultra-filtration membrane in the pre-treatment, be that molecular weight cut-off is 20,000-50,000 organic polymer material ultra-filtration membrane or inorganic ceramic ultra-filtration membrane, the material of organic polymer ultra-filtration membrane wherein is a kind of in polysulfones or SPSF, polyethersulfone, polypropylene and the polyacrylonitrile.
5, the integrated membrane process production method of electronic grade water according to claim 1, it is characterized in that, employed nanofiltration membrane in the pre-treatment, its pore diameter range is the 1-3 nanometer, its material is cellulose acetate-cellulosetri-acetate, or a kind of in aromatic polyamides and the sulfonated polyether sulfone.
6, the integrated membrane process production method of electronic grade water according to claim 1, it is characterized in that, employed reverse osmosis membrane in the one-level pure water system is standard operation pressure 1.05-1.55MPa, and ratio of desalinization is greater than 99% low pressure polyamide composite reverse osmosis membrane.
7, the integrated membrane process production method of electronic grade water according to claim 1 is characterized in that, the polishing reverse osmosis membrane that end-filtration is used, and for holding back size of particles 0.0001 μ m, molecular weight cut-off is 100 ultralow pressure complex reverse osmosis membrane.
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