CN107098783A - The technique that fused silica crucible prepares siliceous fertilizer raw material after a kind of utilization polycrystalline silicon ingot casting - Google Patents
The technique that fused silica crucible prepares siliceous fertilizer raw material after a kind of utilization polycrystalline silicon ingot casting Download PDFInfo
- Publication number
- CN107098783A CN107098783A CN201710395343.6A CN201710395343A CN107098783A CN 107098783 A CN107098783 A CN 107098783A CN 201710395343 A CN201710395343 A CN 201710395343A CN 107098783 A CN107098783 A CN 107098783A
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- China
- Prior art keywords
- fused silica
- raw material
- siliceous fertilizer
- silica crucible
- ingot casting
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Classifications
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D9/00—Other inorganic fertilisers
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/80—Soil conditioners
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Soil Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses the technique that fused silica crucible after a kind of utilization polycrystalline silicon ingot casting prepares siliceous fertilizer raw material, comprise the following steps successively：1）Fused silica crucible is first slightly broken, the crucible fragment that particle diameter is 15 ~ 30cm is obtained；2）Secondary thin broken is carried out using jaw crusher, the particle diameter of fragment is contracted to 2 ~ 5cm；3）Ball milling is carried out using ball mill, the quartz powder that particle diameter is 800 ~ 1000 mesh is finally given；4）Quartz powder is added in potassium hydroxide/sodium hydroxide solution of saturation, pH value is maintained at 13；5）Humic acid is added into above-mentioned solution, adjusts between its pH to 7 ~ 9, that is, obtains siliceous fertilizer raw material.The present invention efficiently utilizes discarded fused silica crucible, has not only saved the economic input of business processes waste quartz crucible, also using waste quartz crucible as raw material, prepare agricultural siliceous fertilizer, resource regeneration is realized, meets the feature of recycling economy, with larger economic value and social effect.
Description
Technical field
Vitreous silica after polycrystalline silicon ingot casting is utilized the present invention relates to a kind of production technology of siliceous fertilizer raw material, more particularly to one kind
The technique that crucible prepares siliceous fertilizer raw material.
Background technology
Silicon, as the important element of content on the earth second, is the fourth-largest battalion necessary to plant in addition to nitrogen, phosphorus, potassium
Element is supported, for happiness silicon plant especially this kind of to paddy rice, supplement element silicon can form siliceous in time in its growth course
Cell, hence it is evident that disease resistance, lodging tolerance of enhancing crop etc.；In addition, the presence of silicon can also promote plant to other nutrition
The absorption of composition, strengthens photosynthesis of plant, reaches the effect for further improving crop yield, at present, the siliceous fertilizer master of in the market
If " solubility in citric acid " siliceous fertilizer by raw material of blast-furnace cinder, its Determination of Soluble Silicon is extremely low, fertilizer efficiency is very poor, therefore, how to improve
The validity of siliceous fertilizer is always the bottleneck for restricting siliceous fertilizer development.
Chinese invention patent discloses a granted patent " a kind of liquid silicon fertilizer and its production technology ", Patent No.
" ZL200810238522.X " is that other auxiliary materials are made with raw material of industry potassium silicate or sodium metasilicate, and addition is passed through in production
The auxiliary materials such as biochemical fulvic acid, chelating agent, trace element, urea are mixed to prepare liquid silicon fertilizer, and its main function composition is " soluble
Silicon " and other auxiliary materials are direct purchase gained, from cost, do not possess competitiveness.
On the other hand, with the development of society, the photovoltaic industry using polysilicon solar cell as representative has been obtained rapidly
Development, and polycrystalline silicon ingot casting is to prepare one of important step of polysilicon solar cell, used in this course
Silica crucible is then disposable product, and consumption is especially big, and after ingot casting completion, the silica crucible of melting is converted into cristobalite
Material, and as trade waste, past processing mode is usually to be used as building filler after simple crushing, at present
Having developed into needs pay the freight ability someone to be ready to pull away, from now on, with the constantly improve of environmental protection policy, will also be used as Industrial Solid
It is useless to be handled and pay huge disposal costs, the great wasting of resources is so not only caused, while it is more to also add preparation
The cost of crystal silicon battery；Therefore, how effectively photovoltaic industry urgent problem to be solved is turned into using useless silica crucible, if energy
Useless crucible is transformed into high value added product by certain processing, can not only save and be spent in the past on the useless crucible of processing
Expense and solve the environmental problem that industrial residue is brought, can also bring certain income.
The granted patent " fused silica crucible renovation process after polycrystalline silicon ingot casting " that Chinese invention patent specification is announced, specially
Profit number is " ZL201410155232.4 " and " cristobalite matter electroceramics prepared by a kind of utilization waste quartz crucible ", Patent No.
The methods that " ZL201210532204.0 " describes two kinds of disposal fused silica crucibles respectively, but both approaches are required for pair
Silica crucible carries out high-temperature calcination, and production cost is high, and its value-added content of product is relatively low, and economic feasibility is poor.
The content of the invention
The technical problems to be solved by the invention are to solve the handling problems of fused silica crucible, overcome prior art
Shortcoming is there is provided the technique that fused silica crucible after a kind of utilization polycrystalline silicon ingot casting prepares siliceous fertilizer raw material, and the technique makes discarded crucible
It is fully utilized, needs the Industrial Solid Waste of payment process to be converted into the agricultural silicon with compared with high added value script
Fertilizer, realizes the purpose of resource regeneration, the problem of not only solving Industrial Solid Waste, and has accomplished recycling for resource, simultaneously
Create certain benefit.
In order to solve the above technical problems, the present invention provides one kind prepares silicon using fused silica crucible after polycrystalline silicon ingot casting
The technique of fertile raw material, the siliceous fertilizer raw material includes following components by mass percentage：Soluble silicon：30 ~ 40%, humate：20
~ 25%, surplus is water, wherein：
Soluble silicon is sodium metasilicate or potassium silicate, and humate is potassium humate or sodium humate；
The technique for preparing siliceous fertilizer raw material using fused silica crucible after polycrystalline silicon ingot casting specifically includes following steps：
（1）Fused silica crucible after ingot casting is first carried out to physics slightly to break, the crucible fragment that size is 15 ~ 30cm is obtained；
（2）Using jaw crusher to step（1）In crucible fragment carry out secondary thin broken, allow fragment to be changed into 2 ~ 5cm of particle diameter
Fragment；
（3）Using ball mill by step（2）In crucible fragment carry out ball milling, obtain particle diameter be 800 ~ 1000 mesh silica flour
End；
（4）In the reactor that above-mentioned quartz powder is added to potassium hydroxide/sodium hydroxide solution equipped with saturation, and pass through alkali
Supplement regulation pH, while make reactor temperature maintain in the range of 90 ~ 100 DEG C using heating mantle, react 2 ~ 3 hours, treat
Reaction is complete, and quartz powder is exhausted, and waits reaction solution cooled and filtered, and filtrate is standby；
（5）Humic acid is added into above-mentioned filtrate, its pH to 7 ~ 9 is adjusted, obtained product is concentrated, that is, obtains siliceous fertilizer former
Material.
The technical scheme that further limits of the present invention is：
Further, fused silica crucible prepares the technique of siliceous fertilizer raw material, step after foregoing utilization polycrystalline silicon ingot casting（1）In right
Fused silica crucible slightly broken using technical grade impact drill electric hammer when physics is slightly broken.
Fused silica crucible prepares the technique of siliceous fertilizer raw material, step after foregoing utilization polycrystalline silicon ingot casting（4）In in silica flour
It is that regulation pH value is maintained at 13 that end carries out course of reaction with alkali, and reaction condition is 90 ~ 100 DEG C.
Fused silica crucible prepares the technique of siliceous fertilizer raw material after foregoing utilization polycrystalline silicon ingot casting, is carrying out step（1）Thing
Reason is thick broken preceding first to the fused silica crucible progress cleaning sorting after ingot casting, is specially：It is using ultrasonic wave and molten using weak acid
Liquid is cleaned, and weak acid solution is the mixture of hydrochloric acid, acetic acid and water, wherein hydrochloric acid by volume：Acetic acid：Water=2:1:100
Ratio is mixed, and the temperature that weak acid solution is controlled during cleaning is 40-50 DEG C, cleans 2-3h.
Fused silica crucible prepares the technique of siliceous fertilizer raw material, step after foregoing utilization polycrystalline silicon ingot casting（5）In it is dense to product
Carry out drying processing after contracting, be specially：It it is 60 DEG C in temperature, humidity dries 2-3h for 40% Indoor Natural.
The beneficial effects of the invention are as follows：
Using polycrystalline silicon ingot casting fused silica crucible as " silicon " source of siliceous fertilizer raw material, both obtained that purity is high, reserves foot exempt from
Take " silicon " source, a silica crucible for being Industrial Solid Waste can be allowed to turn waste into wealth again, resource regeneration.
Step（3）Using ball mill by step（2）In crucible fragment carry out ball milling, using ultra-fine powder technology, will have
There is the fused silica crucible powdered of reactionlessness, improve its reaction rate.
Reacted mixed solution is neutralized using humic acid, to neutralize excessive alkali, the neutrality of pH value is realized, both
PH value can be reduced to normal range (NR), can make to introduce humic acid in siliceous fertilizer raw material again, further improve its fertilizer efficiency.
The siliceous fertilizer raw material and production technology of the present invention, for fused silica crucible disposal difficulties after existing polycrystalline silicon ingot casting and
The problem of absorptivity of existing agricultural siliceous fertilizer is low, using resource regeneration, the thinking of comprehensive utilization, simply to chemically react,
Silica crucible is converted into the siliceous fertilizer raw material rich in " soluble silicon ", opened up to develop the trade waste in photovoltaic industry
New direction.
Brief description of the drawings
Fig. 1 is the process chart of embodiments of the invention.
Embodiment
Embodiment 1
Fused silica crucible prepares the technique of siliceous fertilizer raw material after a kind of utilization polycrystalline silicon ingot casting that the present embodiment is provided, and the siliceous fertilizer is former
Material includes fused silica crucible, potassium hydroxide, humic acid, by chemical reaction, is formed with " potassium silicate " as main component, humic
Sour potassium is the siliceous fertilizer raw material of auxiliary element；
As shown in figure 1, preparing the technique of siliceous fertilizer raw material using fused silica crucible after polycrystalline silicon ingot casting, following step is specifically included
Suddenly：
（1）Fused silica crucible large stretch of after ingot casting is first carried out into physics using technical grade impact drill electric hammer slightly to break, size is obtained
For 15 ~ 30cm crucible fragment；
（2）Using jaw crusher to step（1）In crucible fragment carry out secondary thin broken, allow fragment to be changed into 2 ~ 5cm of particle diameter
Fragment；
（3）Using ultra-fine powder technology, using ball mill by step（2）In crucible fragment carry out ball milling, obtain particle diameter for 800
The CRISTOBALITE POWDER of ~ 1000 mesh, the powdery pulp injection raw material stock tank of gained is standby；
（4）200 kilograms of cristobalite powdery pulp (30wt%), 140 kilograms of potassium hydroxide and 50 kilograms are added in a kettle.
Water, and pH value is maintained at 13 by the supplement of alkali, while making reactor temperature maintain 90 ~ 100 DEG C of models using heating mantle
In enclosing, 2 ~ 3 hours are reacted, after completion of the reaction cold filtration, filtrate is standby；
（5）Nitro humus acid 120 kg is added in filtrate, pH value is adjusted to 8, then obtained product is concentrated,
Obtain silicic acid potassium content 30%, potassium humate 26%, remaining is the product of water, is 500 kilograms of siliceous fertilizer raw materials of the present invention.
In the present embodiment, step is being carried out（1）Physics it is slightly broken before first the fused silica crucible after ingot casting is carried out it is clear
Sorting is washed, is specially：Cleaned using ultrasonic wave and using weak acid solution, weak acid solution is the mixed of hydrochloric acid, acetic acid and water
Compound, wherein hydrochloric acid by volume：Acetic acid：Water=2:1:100 ratio mixing, the temperature that weak acid solution is controlled during cleaning is 40
DEG C, clean 3h；Step（5）In to product concentrate after carry out dry processing, specially：It it is 60 DEG C in temperature, humidity is 40% room
It is interior to dry 2h naturally.
Embodiment 2
The present embodiment provides the technique that fused silica crucible after a kind of utilization polycrystalline silicon ingot casting prepares siliceous fertilizer raw material, specifically include with
Lower step：
（1）Fused silica crucible large stretch of after ingot casting is first carried out into physics using technical grade impact drill electric hammer slightly to break, size is obtained
For 15 ~ 30cm crucible fragment；
（2）Using jaw crusher to step（1）In crucible fragment carry out secondary thin broken, allow fragment to be changed into 2 ~ 5cm of particle diameter
Fragment；
（3）Using ultra-fine powder technology, using ball mill by step（2）In crucible fragment carry out ball milling, obtain particle diameter for 800
The CRISTOBALITE POWDER of ~ 1000 mesh, the powdery pulp injection raw material stock tank of gained is standby；
（4）200 kilograms of cristobalite powdery pulp (30wt%), the sodium hydroxide of 120 kg are added in a kettle. is dissolved in 50 public affairs
Jin water, and pH value is maintained at 13 by the supplement of alkali, while making reactor temperature maintain 90 ~ 100 DEG C using heating mantle
In the range of, react 2 ~ 3 hours, cold filtration after completion of the reaction, filtrate is standby；
（5）Nitro humus acid 120 kg is added in filtrate, pH value is adjusted to 8, then obtained product is concentrated,
Obtain silicic acid potassium content 31%, potassium humate 26.5%, remaining is the product of water, is 450 kilograms of siliceous fertilizer raw materials of the present invention.
In the present embodiment, step is being carried out（1）Physics it is slightly broken before first the fused silica crucible after ingot casting is carried out it is clear
Sorting is washed, is specially：Cleaned using ultrasonic wave and using weak acid solution, weak acid solution is the mixed of hydrochloric acid, acetic acid and water
Compound, wherein hydrochloric acid by volume：Acetic acid：Water=2:1:100 ratio mixing, the temperature that weak acid solution is controlled during cleaning is 50
DEG C, clean 2h；Step（5）In to product concentrate after carry out dry processing, specially：It it is 60 DEG C in temperature, humidity is 40% room
It is interior to dry 3h naturally.
The present invention develops a kind of siliceous fertilizer raw material that can be absorbed by plant efficient and its production technology, and script is needed to pay
The Industrial Solid Waste of expense processing is converted into the agricultural siliceous fertilizer with compared with high added value, realizes the purpose of resource regeneration；Vitreous silica
Crucible belongs to Industrial Solid Waste after the completion of ingot casting, current processing mode be only it is broken after build the road and use, serious waste money
Source, and also need to pay related freight charges.The technology that we are provided makes discarded crucible be fully utilized, and not only solves work
The problem of industry solid waste, and accomplished recycling for resource, while certain benefit is created, with highly important economy
Value and social effect.
In addition to the implementation, the present invention can also have other embodiment.All use equivalent substitution or equivalent transformation shape
Into technical scheme, all fall within the protection domain of application claims.
Claims (5)
1. the technique that fused silica crucible prepares siliceous fertilizer raw material after a kind of utilization polycrystalline silicon ingot casting, it is characterised in that：The siliceous fertilizer is former
Material includes following components by mass percentage：Soluble silicon：30 ~ 40%, humate：20 ~ 25%, surplus is water, wherein：
The soluble silicon is sodium metasilicate or potassium silicate, and the humate is potassium humate or sodium humate；
The technique for preparing siliceous fertilizer raw material using fused silica crucible after polycrystalline silicon ingot casting specifically includes following steps：
（1）Fused silica crucible after ingot casting is first carried out to physics slightly to break, the crucible fragment that size is 15 ~ 30cm is obtained；
（2）Using jaw crusher to step（1）In crucible fragment carry out secondary thin broken, allow fragment to be changed into 2 ~ 5cm of particle diameter
Fragment；
（3）Using ball mill by step（2）In crucible fragment carry out ball milling, obtain particle diameter be 800 ~ 1000 mesh silica flour
End；
（4）In the reactor that above-mentioned quartz powder is added to potassium hydroxide/sodium hydroxide solution equipped with saturation, and pass through alkali
Supplement regulation pH, while make reactor temperature maintain in the range of 90 ~ 100 DEG C using heating mantle, react 2 ~ 3 hours, treat
Reaction is complete, and quartz powder is exhausted, and waits reaction solution cooled and filtered, and filtrate is standby；
（5）Humic acid is added into above-mentioned filtrate, its pH to 7 ~ 9 is adjusted, obtained product is concentrated, that is, obtains siliceous fertilizer former
Material.
2. fused silica crucible prepares the technique of siliceous fertilizer raw material after utilization polycrystalline silicon ingot casting according to claim 1, it is special
Levy and be：Step（1）In to fused silica crucible carry out physics slightly break when slightly broken using technical grade impact drill electric hammer.
3. fused silica crucible prepares the technique of siliceous fertilizer raw material after utilization polycrystalline silicon ingot casting according to claim 1, it is special
Levy and be：Step（4）In to carry out course of reaction in quartz powder and alkali be that regulation pH value is maintained at 13, reaction condition is 90 ~ 100
℃。
4. fused silica crucible prepares the technique of siliceous fertilizer raw material after utilization polycrystalline silicon ingot casting according to claim 1, it is special
Levy and be：Carrying out step（1）Physics it is slightly broken before cleaning sorting first is carried out to the fused silica crucible after ingot casting, be specially：
Cleaned using ultrasonic wave and using weak acid solution, the weak acid solution is the mixture of hydrochloric acid, acetic acid and water, wherein pressing
Volume ratio hydrochloric acid：Acetic acid：Water=2:1:100 ratio mixing, the temperature that weak acid solution is controlled during cleaning is 40-50 DEG C, cleans 2-
3h。
5. fused silica crucible prepares the technique of siliceous fertilizer raw material after utilization polycrystalline silicon ingot casting according to claim 1, it is special
Levy and be：Step（5）In to product concentrate after carry out dry processing, specially：It it is 60 DEG C in temperature, humidity is 40% interior
Naturally 2-3h is dried.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417432A (en) * | 2017-09-21 | 2017-12-01 | 界首市众建家庭农场 | A kind of high-activity humic acid fertilizer synergist |
| WO2019222813A1 (en) * | 2018-05-25 | 2019-11-28 | Agripower Australia Limited | Method for extracting soluble si from an amorphous sio2 bearing material |
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| CN102241401A (en) * | 2011-06-29 | 2011-11-16 | 山西晶都太阳能电力有限公司 | Separation method of quartz and silicon material in single crystal silicon crucible backing material |
| CN102757052A (en) * | 2012-07-31 | 2012-10-31 | 合肥工业大学 | Method for separating and extracting silica micro powders from discarded quartz tailings |
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| CN104276574A (en) * | 2013-07-05 | 2015-01-14 | 河南省超贝工程设备有限公司 | Method for extraction of high-purity silicon from crystal silicon cutting waste liquid |
| CN105254428A (en) * | 2015-10-28 | 2016-01-20 | 昌邑市龙港无机硅有限公司 | Water-soluble solid silicon fertilizer and production method and preparation device thereof |
| CN105858602A (en) * | 2016-04-08 | 2016-08-17 | 北京科技大学 | Polycrystalline silicon cutting waste material treatment method |
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| CN101440001A (en) * | 2008-12-16 | 2009-05-27 | 于春开 | Liquid silicon fertilizer and technique for producing the same |
| CN102241401A (en) * | 2011-06-29 | 2011-11-16 | 山西晶都太阳能电力有限公司 | Separation method of quartz and silicon material in single crystal silicon crucible backing material |
| CN102757052A (en) * | 2012-07-31 | 2012-10-31 | 合肥工业大学 | Method for separating and extracting silica micro powders from discarded quartz tailings |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417432A (en) * | 2017-09-21 | 2017-12-01 | 界首市众建家庭农场 | A kind of high-activity humic acid fertilizer synergist |
| CN107417432B (en) * | 2017-09-21 | 2018-08-24 | 界首市众建家庭农场 | A kind of high-activity humic acid fertilizer synergist |
| WO2019222813A1 (en) * | 2018-05-25 | 2019-11-28 | Agripower Australia Limited | Method for extracting soluble si from an amorphous sio2 bearing material |
| US11667534B2 (en) | 2018-05-25 | 2023-06-06 | Agripower Australia Limited | Method for extracting soluble Si from an amorphous SiO2 bearing material |
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