CN101817531A - Treatment method for establishing anticorrosion system in silica sol - Google Patents
Treatment method for establishing anticorrosion system in silica sol Download PDFInfo
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- CN101817531A CN101817531A CN 201010166476 CN201010166476A CN101817531A CN 101817531 A CN101817531 A CN 101817531A CN 201010166476 CN201010166476 CN 201010166476 CN 201010166476 A CN201010166476 A CN 201010166476A CN 101817531 A CN101817531 A CN 101817531A
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- silicon sol
- anticorrosion
- bactericidal agent
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Abstract
The invention provides a treatment method for establishing an anticorrosion system in silica sol, which comprises the following steps of: treating raw materials, production equipment and a pipeline before the silica sol is produced; ensuring the purity of required materials; performing heating treatment on the silica sol after the silica sol is produced and then adding various anticorrosive bactericides into the silica sol according to different additive amounts and treatment steps; and then performing certain subsequent treatment and packaging on the silica sol body treated by the anticorrosive bactericides so as to establish a complete set of anticorrosion system for the production of the silica sol. The method has the advantages of effectively ensuring the consistency of the physical properties of the silica sol before and after the treatment, not causing conditions, such as smell, mildew and the like, in the shelf life of the silica sol body, and simultaneously ensuring the stability of polishing solution of various types prepared by the silica sol, and is applied to large-scale production.
Description
Technical field
The present invention relates to the production method of silicon sol, relate in particular to precision polishing technique through silicon sol materials such as silicon materials surface, gallium arsenide, silicon carbide, sapphire surface and quartz in microelectronic industry of rotproofing.
Background technology
Silicon sol has many advantageous properties and characteristics, as a kind of fine chemical product, is the good mineral binder bond that is widely used in fields such as electronics, chemical industry, precision casting, weaving, papermaking, coating, food.
Silicon sol comprises acid and alkaline two kinds, in its quality guaranteed period, owing to be subjected to the limitations affect of various compositions in many environmental factorss and the silicon sol, acidic silicasol is in metastable condition, in put procedure, can produce pectisation and rotten situation, be generally stationary phase 3-6 month.And alkaline silica sol is in metastable state equally, deposits the rotten situation that may produce equally in the process in various degree.Its concrete rotten situation is: 1) colloid itself sends the smell of similar rotten egg; 2) colloid surface has the yellow or red floating matter of a small amount of sheet; 3) variable color (becoming grey or black) by white.Analyze above-mentioned rotten situation produce concrete reason may for: 1) cause smelly reason: mix impurity in the raw material, produce impurely or do not reach the requirement that needs usefulness with deionized water, production is subjected to microbial contamination etc. with pure water; 2) cause exist floating matter former because: have a large amount of microorganisms in the whole rotten silicon sol system, its rapidly the refuse macro manifestations after the breeding be different colours; 3) cause the variable color reason: microorganism breeds in a large number in the rotten silicon sol of long-term storage, and its secular movement has caused that the colloid color gradually changes.
Follow contingent spoilage problems two conditions in the application of all trades and professions with it based on silicon sol, in silicon sol, set up protective system and be very important.Anti-corrosion method and knowledge use are in many product treatment at present, patent 95119538.7 discloses in protective system and the patent 03124269 and discloses a kind of the preservation of timber against decay treatment process etc., but very few for silicon sol rot-resistant pertinent literature patent, therefore need set up a whole set of protective system to guarantee its better stability to the production of silicon sol.
In order to guarantee the stability of silicon sol, prolong stationary phase, and avoid rotten this problem, the character that keeps colloid itself is played an important role.Under this big market environment of silicon sol, set up silicon sol and produce protective system and solve the rotten problem of silicon sol, will advance the whole market and play crucial effects.Therefore, setting up protective system in silicon sol, reduce the factor that influences the silicon sol characteristic, is the problem that needs solution at present.
Summary of the invention
Main purpose of the present invention is to prevent that existing silicon sol product from producing spoilage problems, provide a kind of before silicon sol production in after set up the treatment process of protective system.
The objective of the invention is to realize by following technical scheme:
Silicon sol is produced preceding processing to raw material: comprise that raw material is carried out ultraviolet-sterilization to be handled, need be made into the required low concentration solution of reaction process for high concentration liquid raw material and solid material, adopt ultraviolet lamp direct contact type irradiation low concentration solution, irradiation duration is 3-5 minute;
Silicon sol is produced preceding germicidal treatment to production unit and pipeline: comprise that the preparation massfraction is the non-oxide sterilant aqueous solution of 0.03-0.2% earlier, scrub after production unit, intermediate product container and the pipeline with the described non-oxide sterilant aqueous solution, soak 1-2h again, scrub again once, then the non-oxide sterilant aqueous solution is drained, rinse well with tap water at last;
During silicon sol was produced: the specific conductivity of used pure water was controlled at 1-3us/cm, and used intermediate product of reaction process and pure water were all used the ultraviolet lamp direct irradiation 1-3 minute, and sealing is preserved then;
Silicon sol is produced post-heating and handled: temperature is controlled at 50-90 ℃, adopts anticorrosion and bactericidal agent to handle then;
Subsequent disposal and packing: the pail pack spirituous solution of silicon sol product is scrubbed, used the pure water rinse again, dry, then silicon sol is filtered 2 times with double-layer filter cloth, be divided in the pail pack.
The present invention utilizes scientific and reasonable anti-corrosion method method and is equipped with suitable non-oxidizable sterilant and handles producing the back silicon sol, effectively suppressing the silicon sol product may produce smelly and the iso-metamorphism situation of going mouldy, parameters such as the pH value of assurance silicon sol, proportion, viscosity do not influence the stability by its polishing fluid of preparing simultaneously.
The present invention can effectively change the perishable characteristic of silicon sol itself, suppress the situation that colloid itself is smelly and go mouldy, prolong its quality guaranteed period, can guarantee simultaneously the consistence of parameters before and after rotproofing such as pH value, proportion, viscosity of silicon sol, not change the stability that silicon sol after this system is handled is mixed with various model polishing fluids; In addition, this treatment process cost is lower, simple, is applicable in the scale production.
The silicon sol of handling through protective system of the present invention is divided into industrial and two types of electron types.The former is mainly used in the manufacturing and the coating preparation of support of the catalyst and sorbent material in precision casting industry, petroleum industry, pharmaceutical industry, the organic synthesis industry, also can be used for industries such as paper-making industry, refractory materials, cold-reduced silicon sheet, printing, store battery.The latter is mainly used in the glossing of materials such as silicon materials surface, gallium arsenide, silicon carbide, sapphire surface and quartz in the microelectronic industry, also can be used for the polishing of diffusion sheet.Wherein contain SiO
220%, the acidic silicasol of pH=2.5-4.5 when making the manipulation of regeneration of fluorescent material, has the dispersiveness of height.If can obtain high-purity potassium silicate with high-purity silicasol and the reaction of High Purity Hydrogen potassium oxide, it is the excellent dispersants and the binding agent of fluorescent material in the black and white kinescope.
Anticorrosion and bactericidal agent of the present invention be chlorophenols or thiazoles or season phosphonium salt class or heterocyclic compound or organic aldehydes or contain cyanides or heavy metal organic compound or amides anticorrosion and bactericidal agent.
The anticorrosion and bactericidal agent that adopts after the silicon sol production of the present invention carries out rotproofing after with water-soluble reagent sterilant being diluted earlier again.
When the present invention adopts anticorrosion and bactericidal agent to handle after silicon sol production, join in the silicon sol a kind of sterilant is disposable, fully stirred 3-10 minute; The anticorrosion and bactericidal agent consumption is the 0.01%-0.5% of silicon sol gross weight.
When adopting anticorrosion and bactericidal agent to handle after the silicon sol production, be divided into 2-3 processing, each identical anticorrosion and bactericidal agent, add at every turn stir behind the anticorrosion and bactericidal agent after, leave standstill after 3 minutes to 24 hours and add next time again, each anticorrosion and bactericidal agent consumption is the 0.01-0.3% of silicon sol gross weight.
Embodiment
The present invention sets up the treatment process of protective system in silicon sol, comprise that silicon sol is produced before, the processing of raw material, production unit and pipeline; In the production, guarantee the purity of required material; After the production, after the silicon sol heat treated, more different types of anticorrosion and bactericidal agent is added in the silicon sol by different additions and treatment step; Colloid after anticorrosion and bactericidal agent is handled is again through certain subsequent disposal and packing then, thereby set up the protective system that a whole set of silicon sol is produced.Its improvements are, described a whole set of protective system comprise silicon sol produced before, produce after neutralization produces, adopt different treatment processs to set up different protective systems; The consistence of the rerum natura that can effectively guarantee silicon sol before and after handling, and can not produce smelly in the quality guaranteed period and situation such as go mouldy at colloidal; Guarantee to be made into the stability of various model polishing fluids simultaneously by this silicon sol; Be applicable in the scale production.
Operating features:
1, the processing to raw material comprises that all raw materials that the production silicon sol is used carry out ultraviolet-sterilization and handle before the silicon sol production, need be made into the required low concentration solution of reaction process for high concentration liquid raw material and solid material, utilize ultraviolet lamp direct irradiation low concentration solution, require UV-light directly to contact with solution, irradiation duration is 3-5 minute, should avoid operator on the scene during this, in order to avoid be subjected to unnecessary damages.After disposing, in can putting into production.Germicidal treatment to production unit and pipeline before the silicon sol production comprises that the preparation massfraction is the non-oxide sterilant aqueous solution of 0.03-0.2% earlier, scrub after production unit, production process intermediate product container and the pipeline with it, soak 1-2h, scrub again once, then microbicide solution is drained, with the tap water flushing, promptly dispose at last.
2, in silicon sol, set up the treatment process of protective system, during producing, silicon sol guarantees the purity of required material, the specific conductivity that is used pure water is controlled at 1-3us/cm, and used intermediate product of reaction process and pure water were all used the ultraviolet lamp direct irradiation 1-3 minute, and sealing is preserved then.
3, after silicon sol production it is set up the heat treated that protective system comprises silicon sol: temperature is controlled at 50-90 ℃, and preferred temperature is 60-80 ℃; Adopt the treatment process that carries out single step or multistep processing with different types of anticorrosion and bactericidal agent then.The addition means of sanitas: different types of sterilant is the ampoule 0.01%-0.5% that single step is handled, multistep is handled ampoule 0.01-0.3%, in one treatment time 3-10 minute step, in case of necessity can water-soluble reagent in the treating processes carry out rotproofing again after with the sterilant dilution process.
Anticorrosion and bactericidal agent can be a chlorophenols: as bis-chlorophenols, and pentachlorophenol; Thiazoles: as isothiazolinone; Season the phosphonium salt class: heterocyclic compound: organosulfur compound, organic amine compound; Organic aldehydes: as glutaraldehyde; Contain cyanides; Heavy metal organic compound: as organotin; Other organism: as dibromo nitrilo propionic acid amide (amides).
The single step treatment process is about to that a kind of sterilant is disposable to join in the system, gets final product after stirring.
The multistep treatment process is generally the processing of two to three steps, and the adding mode of anticorrosion and bactericidal agent is divided into continous way and intermittent type.
To add be to add anticorrosion and bactericidal agent of the same race once to continous way in the multistep treatment process, after fully stirring minute, left standstill 3-5 minute, adds for the second time again, and after the identical time of abundant stirring, this process that circulates repeatedly promptly disposes again.
It is to add anticorrosion and bactericidal agent of the same race once that multistep treatment process discontinuous formula adds, and fully stirs, and 24h or above time add for the second time at interval, and fully stirs aftertreatment and finish.
4, the colloid after anticorrosion and bactericidal agent is handled is again through certain subsequent disposal and packing: the pail pack of silicon sol product is scrubbed once with certain density alcohol, used the pure water rinse more once, dry.Silicon sol after will handling then filters 2 times with double-layer filter cloth, is divided in the finished product packing bucket.
Shows that through many group tests the polishing average removal rate that is mixed with polishing fluid through the silicon sol of germicidal treatment is not 0.68 μ m/min, and be 0.64 to 0.67 μ m/min through the polishing average removal rate that the silicon sol that the present invention handles is mixed with polishing fluid.It is suitable substantially to remove speed, illustrates after setting up protective system before and after the silicon sol production, with the not variation of its polishing performance of polishing fluid of this silicon sol preparation.
Claims (5)
1. in silicon sol, set up the treatment process of protective system, it is characterized in that comprising:
Silicon sol is produced preceding processing to raw material: comprise that raw material is carried out ultraviolet-sterilization to be handled, need be made into the required low concentration solution of reaction process for high concentration liquid raw material and solid material, adopt ultraviolet lamp direct contact type irradiation low concentration solution, irradiation duration is 3-5 minute;
Silicon sol is produced preceding germicidal treatment to production unit and pipeline: comprise that the preparation massfraction is the non-oxide sterilant aqueous solution of 0.03-0.2% earlier, scrub after production unit, intermediate product container and the pipeline with the described non-oxide sterilant aqueous solution, soak 1-2h again, scrub again once, then the non-oxide sterilant aqueous solution is drained, rinse well with tap water at last;
During silicon sol was produced: the specific conductivity of used pure water was controlled at 1-3us/cm, and used intermediate product of reaction process and pure water were all used the ultraviolet lamp direct irradiation 1-3 minute, and sealing is preserved then;
Silicon sol is produced post-heating and handled: temperature is controlled at 50-90 ℃, adopts anticorrosion and bactericidal agent to handle then;
Subsequent disposal and packing: the pail pack spirituous solution of silicon sol product is scrubbed, used the pure water rinse again, dry, then silicon sol is filtered 2 times with double-layer filter cloth, be divided in the pail pack.
2. according to the described treatment process of in silicon sol, setting up protective system of claim 1, it is characterized in that described anticorrosion and bactericidal agent be chlorophenols or thiazoles or season phosphonium salt class or heterocyclic compound or organic aldehydes or contain cyanides or heavy metal organic compound or amides anticorrosion and bactericidal agent.
3. according to the described treatment process of in silicon sol, setting up protective system of claim 1, it is characterized in that carrying out rotproofing again after the anticorrosion and bactericidal agent that adopts after the described silicon sol production dilutes sterilant with water-soluble reagent earlier.
4. according to claim 1 or the 2 or 3 described treatment processs of in silicon sol, setting up protective system, when it is characterized in that adopting anticorrosion and bactericidal agent to handle after the silicon sol production, join in the silicon sol a kind of sterilant is disposable, fully stirred 3-10 minute; The anticorrosion and bactericidal agent consumption is the 0.01%-0.5% of silicon sol gross weight.
5. according to claim 1 or the 2 or 3 described treatment processs of in silicon sol, setting up protective system, when it is characterized in that adopting after the silicon sol production anticorrosion and bactericidal agent to handle, be divided into 2-3 processing, each identical anticorrosion and bactericidal agent, add at every turn stir behind the anticorrosion and bactericidal agent after, leave standstill after 3 minutes to 24 hours and add next time again, each anticorrosion and bactericidal agent consumption is the 0.01-0.3% of silicon sol gross weight.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010166476 CN101817531A (en) | 2010-04-26 | 2010-04-26 | Treatment method for establishing anticorrosion system in silica sol |
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| CN 201010166476 CN101817531A (en) | 2010-04-26 | 2010-04-26 | Treatment method for establishing anticorrosion system in silica sol |
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| CN101817531A true CN101817531A (en) | 2010-09-01 |
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| CN 201010166476 Pending CN101817531A (en) | 2010-04-26 | 2010-04-26 | Treatment method for establishing anticorrosion system in silica sol |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104119802A (en) * | 2014-08-06 | 2014-10-29 | 江苏天恒纳米科技股份有限公司 | Special nano-slurry for surface ultra-precision machining of sapphire material |
| CN105819456A (en) * | 2016-03-17 | 2016-08-03 | 江苏天恒纳米科技股份有限公司 | Processing method for establishing anticorrosion system in acidic silica sol |
| US10400109B2 (en) | 2013-10-04 | 2019-09-03 | 3M Innovative Properties Company | Coatable composition, antistatic composition, antistatic articles, and methods of making the same |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3148110A (en) * | 1962-11-07 | 1964-09-08 | Du Pont | Method of disinfecting with formaldehyde-colloidal silica aquasols |
| US3816330A (en) * | 1970-10-05 | 1974-06-11 | Du Pont | Method of protecting colloidal silica aquasols from bacterial degradation |
| US4352744A (en) * | 1980-09-05 | 1982-10-05 | E. I. Du Pont De Nemours And Company | Protecting colloidal silica aquasols from bacterial degradation |
-
2010
- 2010-04-26 CN CN 201010166476 patent/CN101817531A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3148110A (en) * | 1962-11-07 | 1964-09-08 | Du Pont | Method of disinfecting with formaldehyde-colloidal silica aquasols |
| US3816330A (en) * | 1970-10-05 | 1974-06-11 | Du Pont | Method of protecting colloidal silica aquasols from bacterial degradation |
| US4352744A (en) * | 1980-09-05 | 1982-10-05 | E. I. Du Pont De Nemours And Company | Protecting colloidal silica aquasols from bacterial degradation |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10400109B2 (en) | 2013-10-04 | 2019-09-03 | 3M Innovative Properties Company | Coatable composition, antistatic composition, antistatic articles, and methods of making the same |
| CN104119802A (en) * | 2014-08-06 | 2014-10-29 | 江苏天恒纳米科技股份有限公司 | Special nano-slurry for surface ultra-precision machining of sapphire material |
| CN104119802B (en) * | 2014-08-06 | 2015-09-02 | 江苏天恒纳米科技股份有限公司 | A kind of sapphire material surface Ultra-precision Turning special-purpose nanometer slurry |
| CN105819456A (en) * | 2016-03-17 | 2016-08-03 | 江苏天恒纳米科技股份有限公司 | Processing method for establishing anticorrosion system in acidic silica sol |
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Open date: 20100901 |