CN106957060A - The application method and the product by its acquisition of useless silicon mud - Google Patents
The application method and the product by its acquisition of useless silicon mud Download PDFInfo
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- CN106957060A CN106957060A CN201610018093.XA CN201610018093A CN106957060A CN 106957060 A CN106957060 A CN 106957060A CN 201610018093 A CN201610018093 A CN 201610018093A CN 106957060 A CN106957060 A CN 106957060A
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- silicon mud
- medicament
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- useless
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
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- 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
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- 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
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- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Treatment Of Sludge (AREA)
Abstract
The present invention discloses a kind of application method of useless silicon mud, and it is comprised the following steps：(A) the useless silicon mud containing cutting oil and metal is obtained；(B) for the useless silicon mud of the first chemicals treatment with cutting oil reaction；(C) the useless silicon mud is handled for the second medicament with the metal reaction；(D) separation lives through the product of the step (B) and the step (C) to obtain solid portion；And (E) with the 3rd chemicals treatment solid portion to obtain the products such as silicate and hydrogen.
Description
Technical field
The present invention relates to a kind of application method of useless silicon mud, useless silicon mud is particularly recycled into the method to manufacture various products.
Background technology
Useless silicon mud comes from electronics industry largely using caused by silicon.The method that industry has the useless silicon mud of many recyclings.Citing
For, TW96112970 discloses one kind, and using separating at high temperature, (heating the temperature between silicon and carborundum fusing point is about
1420 DEG C to 1500 DEG C), the method to reclaim silicon from useless silicon mud.TW99118261 and TW99118266 individually disclose one
The method that carborundum and silicon are reclaimed from useless silicon mud is planted, useless silicon mud is placed in pyrolysis furnace by its teaching, with more than 250 DEG C temperature
Carry out distillation heating.TW99133041 discloses a kind of recovery method of cutting fluid in useless silicon mud, and useless silicon mud is placed in by its teaching
Until cutting fluid is vaporized in the room of poor oxygen condition.Temperature is at a relatively high needed for the above method, haves the shortcomings that to expend the energy.
TW98115605 discloses one kind and reclaims silicon using so-called " particle phase transfer " from useless silicon mud, and it needs to undergo repeatedly quiet
Put, centrifuge, drying.TW95150091, which is disclosed, cleans silicon mud with acetone and via centrifugal treating and dry acquisition silicon and carbonization
Silicon, adds flotation agent to separate silicon with carborundum.Above two method is relatively time consuming method.Although industry has perhaps
The method of many useless silicon mud of recycling, but still there are various shortcomings unavoidably, it is therefore desirable to the technology more innovated is each to solve as far as possible
The problem of kind.
The content of the invention
It is a kind of comprising the useless silicon for cutting oil and metal ingredient especially with regard to handling the present invention relates to a kind of application method of useless silicon mud
The method of mud.The present invention relates to anticipate useless silicon mud using medicament newly developed so that its cutting oil dissolved in metal ingredient it is water-soluble
In liquid or oil reservoir.Then, useless silicon mud cake is obtained after appropriate separation of solid and liquid.Then using can be with pasc reaction formation silicate cement
The useless silicon mud cake of the chemicals treatment of solution, thus produces silicate and hydrogen.The present invention at least has one in following features.
The oil of the cutting in useless silicon mud, metal and silicon composition can be removed, are substantially free of with reclaiming using the method for the present invention
State the product that the product or mentioned component of composition have largely been removed.The present invention relates to reapply this recovery product in other productions
Industry, such as grinding agent industry, cosmetic industry.Therefore, the useless silicon mud of present invention processing may achieve substantially without solid waste
The environmental protection treatment program of output.
For the useless silicon mud containing carborundum, the present invention effectively can separate carborundum with silicon, can be derived from the carbon of high-purity
SiClx product.
The method of the present invention, its process does not result in obstruction.
The method of the present invention without operation temperature more than 140 DEG C the step of, compared to the prior art, it can more save the energy.This hair
It is bright to comprise at least following various modes.
A kind of application method of useless silicon mud, it is comprised the following steps：
Step (A)：Obtain the useless silicon mud containing cutting oil and metal；Step (B)：For the first medicine with cutting oil reaction
Agent handles the useless silicon mud；Step (C)：The useless silicon mud is handled for the second medicament with the metal reaction；Step (D)：Separation
The product of the step (B) and the step (C) is lived through to obtain solid portion；And step (E)：With the 3rd chemicals treatment solid
Part is to obtain silicate and hydrogen.
The application method of foregoing useless silicon mud, wherein cutting oil be comprising mineral oil and selected from sulfonate, amine salt or
Hydroxyl, containing carboxylic acid group, amino-contained or with the compound or above-mentioned one of in the elements such as nitrogen, sulphur, chlorine, phosphorus
Any combinations, first medicament includes the one or more any combination for the compound for meeting structure formula (I)：
Structure formula (I)：M-X
Wherein M is selected from alkalies and alkaline earth and X is selected from halogen (halogen), sulfate radical (sulfate) and nitrate anion
(nitrate)；Or M is selected from C5-C12 alkyl (alkyl group) and X is selected from hydrogen and hydroxyl (hydroxyl).
The various application methods of foregoing useless silicon mud, wherein, the compound of the structure formula (I) is selected from following compound：Chlorine
Change the various combinations of sodium, potassium chloride, calcium chloride, sodium sulphate, sodium nitrate, ethanol, n-hexane and above-mentioned substance.
The various application methods of foregoing useless silicon mud, wherein, the metal includes iron, and the second medicament is included selected from inorganic
The one or more of which any combination of acid or the compound in organic acid.
The various application methods of foregoing useless silicon mud, wherein, the second medicament is selected from following compound：Oxalic acid, lemon
Acid and acetic acid.
The various application methods of foregoing useless silicon mud, wherein, first medicament is sodium-chloride water solution；And second medicine
Agent is oxalic acid and citric acid.
The various application methods of foregoing useless silicon mud, wherein, the step (C) is also included according to selected first medicament
Species determines the species of the selected second medicament.
The various application methods of foregoing useless silicon mud, wherein, when first medicament comprising wherein M selected from C5-C12 alkane
During the compound of the structure formula (I) of base (alkyl group) and X selected from hydrogen and hydroxyl (hydroxyl), the second medicament is selected from such as
Lower compound：Oxalic acid, citric acid and acetic acid.
A kind of aqueous silicate solution, it is made by foregoing various methods.
A kind of powder of silicon carbide-containing, it is made by foregoing various methods, and wherein the useless silicon mud contains carborundum.
The present invention also includes other each side and various embodiments, is disclosed in detail with solving other problems and merging above-mentioned each side
In implementation below.
Brief description of the drawings
Fig. 1 is the flow chart of the application method of the useless silicon mud according to the present invention.
The photo of Fig. 2 useless silicon mud used in the present invention.
Fig. 3 for useless silicon mud cake manufactured in the present invention photo.
Fig. 4 for sodium silicate aqueous solution manufactured in the present invention photo.
Fig. 5 is the useless silicon mud cake residue for being substantially free of silicon that is reclaimed in the present invention.
Embodiment
Presently preferred embodiments of the present invention is illustrated below with reference to accompanying drawing.Similar component is accorded with using identical component in appended accompanying drawing
Number.It should be noted that not drawn to clearly appear from each component in the present invention, appended accompanying drawing according to the ratio of material object, and to avoid
Fuzzy present disclosure, illustrates also to omit the parts being conventionally known, associated materials below, and its correlation processing technique.
As shown in figure 1, the present invention discloses a kind of application method of useless silicon mud, it is comprised the following steps：(A) obtain containing cutting oil
And the useless silicon mud of metal；(B) for the useless silicon mud of the first chemicals treatment with cutting oil reaction；(C) for the metal
The second medicament of reaction handles the useless silicon mud；(D) separation lives through the product of the step (B) and the step (C) to obtain solid part
Point；And (E) with the 3rd chemicals treatment solid portion to obtain the products such as silicate and hydrogen.Step (B) and the purpose of (C) exist
In anticipating useless silicon mud, to eliminate caking phenomenon of the useless silicon mud in water, its various composition is set to separate and uniformly break up
In the aqueous solution or oil reservoir, and make cutting oil, metal as far as possible other compositions are soluble in water or oil reservoir in.Can be according to being obtained
The composition of useless silicon mud one of determine to perform in step (B) and (C)；Or both be performed both by.In selection step (B) and (C)
In the case of being performed both by, can carry out in any order or simultaneously carry out step (B) and (C), wherein it is preferred that first progress step (B) it
Carry out step (C) again afterwards.The purpose of step (D) is that will carry out separation of solid and liquid through pretreated useless silicon mud.The purpose of step (E)
It is to remove the silicon in solid part.Each step is described below in detail.
Step (A)：Obtain the useless silicon mud comprising cutting oil and metal.
Useless silicon mud of the present invention mostlys come from the residue produced by silicon crystal bar is cut into during silicon.Thus may be used
Know, the composition of the silicon mud of giving up comprising silicon wafer chip, cutting oil, and a small amount of metal from Metal Cutting line for example copper, iron, tungsten,
Zinc, aluminium etc..Metal may not be produced if with diamond nicking line and produces a small amount of diamond (diamond) chip.Useless silicon
Mud can also contain the various compositions as cutting grinding agent such as aluminum oxide, carborundum, diamond, cerium oxide and silica.Cut
The mineral oil of the substantially a variety of hydrocarbon mixing of oil is cut, several classes such as blended wax base, cycloalkyl and aromatic radical are different
Oil product, wherein being used for manufacturing cutting oil relatively conventional with paraffinic base ratio is higher, aromatic radical ratio is less collocation.Cutting oil
Effect be lubricate.Different heats and pressure can be produced during cutting in silicon crystal bar cutting region.Light viscosity oil is leaner, have compared with
Good penetration and wetting power, whole cutting region can be diffused into more quickly, and because thin, its cool down cleansing power compared with
It is good.Heavy oil is denser, with preferably lubricity and larger metal surface isolating power, but mobility and cooling
Not as light viscosity oil.Cutting oil can also add emulsifying agent, rust-inhibiting additive, extreme pressure agent or other auxiliary agents in addition to comprising mineral oil,
Its composition can contain such as sulfonate, amine salt or hydroxyl, containing carboxylic acid group, amino-contained or with nitrogen, sulphur, chlorine, phosphorus
Compound or above-mentioned any combination of cutting oil one of in element.
Step (B)：For the useless silicon mud of the first chemicals treatment with the oily reaction of cutting.
The main purpose of the first medicament in the present invention is：First, eliminating useless caking phenomenon of the silicon mud in water；Second, place
Reason cutting oil component, to dissolve in the aqueous solution or oil reservoir.The first medicament in the present invention includes water and meets structure formula (I)
One or more any combination in compound.
Structure formula (I)：M-X,
Wherein M is selected from alkalies and alkaline earth and X is selected from halogen (halogen), sulfate radical (sulfate) and nitrate anion
(nitrate)；Or M is selected from C5-C12 alkyl (alkyl group) and X is selected from hydrogen and hydroxyl (hydroxyl).M is selected from alkali
First medicament of metal and alkaline-earth metal belongs to inorganic type, and it is preferable over cutting of the processing containing sulfonate, the compound of amine salt
Oil.First medicaments of the M selected from alkyl (alkyl group) belongs to organic forms, and it is preferable over processing such as hydroxyl, containing carboxylic acid
Base, amino-contained or the cutting oil with the compound one of in the elements such as nitrogen, sulphur, chlorine, phosphorus or any of the above described combination,
The cutting oil containing extreme pressure agent can be used in particular for handling.Extreme pressure agent is generally sulfide aliphatic acid ester or alkyl chloride or phosphide or nitrogen
Compound is constituted.
Structure formula (I) for the compound of inorganic type it is water-soluble in, water solubility scope is 25 DEG C of weight hundred at 1 atmosphere pressure
Divide rate concentration at least more than 1%, its preferred example is sodium chloride, potassium chloride, calcium chloride, sodium sulphate, sodium nitrate.Structural formula
(I) for organic forms compound it is water-soluble in (such as alcohols) or it is insoluble form an oil reservoir (such as alkanes), alkyl compound example
Such as n-hexane is applied to the oily situation containing chlorinated paraffin Oil-soluble extreme pressure agent of cutting.The preferred process method of step (B) is as follows in detail
It is described.By the compound of one or more structure formula (I)s be deployed into the aqueous solution of the gross weight percentage concentration range within 10% with
As the first medicament, wherein the compound that appropriate structure formula (I) is organic forms can be contained.Then the first appropriate medicament is taken to add
In container equipped with useless silicon mud.The weight of the relatively useless silicon mud of first medicament is 1 than scope：2 to 10：1.It can be stirred in good time
Or do not stir.The temperature adjustment of useless silicon mud of the first medicament can will be added to higher than room temperature, preferably 50 DEG C, but be not to be exceeded 60
℃.Treatment time regard whether stir and treatment temperature and useless silicon mud characteristic in itself and it is different, normally about need 30 exemplified by 100 kilograms
Minute to a few hours.The criterion for completing this step can be to obtain appropriate sample from the useless silicon mud for adding the first medicament, measure
Its without more than 100 microns of particle, more preferably its without more than 1 micron of particle when can be considered completion.The present invention is not comprising yet
Carry out the example of step (B), it is adaptable to which the cutting oil content in useless silicon mud is low or situation about being practically free of.
Step (C)：The useless silicon mud is handled for the second medicament with the metal reaction.
The main purpose of second medicament in the present invention is：Metal ingredient in the useless silicon mud of processing, to dissolve in the aqueous solution.
One of which of the second medicament comprising water and the compound in inorganic acid or organic acid in the present invention is a variety of any groups
Close.
During the inorganic acid compound or organic acid compound of the present invention are water-soluble, water solubility scope is at 1 atmosphere pressure 25
DEG C weight percent concentration at least more than 1%.Its preferred example be sulfuric acid, nitric acid, oxalic acid, citric acid and acetic acid, its
In more preferably citric acid, acetic acid and oxalic acid.The preferred process method of step (C) is as follows in detail.By one or more inorganic acid chemical combination
Thing or organic acid compound are deployed into the aqueous solution of the gross weight percentage concentration range within 10% second medicament is made.Then
Appropriate second medicament is taken to add in the container equipped with useless silicon mud.The weight of the relatively useless silicon mud of second medicament is 1 than scope：2 to
10：1.It can in good time be stirred or not stirred.The temperature adjustment of useless silicon mud of second medicament can will be added to room temperature is higher than, preferably
For 30 DEG C, but it is not to be exceeded 60 DEG C.Treatment time regard whether stir and treatment temperature and useless silicon mud characteristic in itself and it is different, with
30 minutes are normally about needed exemplified by 100 kilograms to a few hours.The criterion for completing this step can be from the useless silicon mud for adding second medicament
It is middle to obtain appropriate sample, remove after moisture removal to measure its tenor less than or equal to 150ppm.The present invention also include without
The example of step (C), it is adaptable to which the tenor in useless silicon mud is low or situation about being practically free of.Step (B) the first medicament and
In the case that the second medicament of step (C) is added, preferably first carry out carrying out step (C), preferred condition again after step (B)
It is the species that selected second medicament is determined according to the species of the first selected medicament.Perform the benefit of the preferred condition
It is that the first medicament can be avoided with second medicament to conflict to cause to anticipate effect reduction.For example, when using organic
The first medicament (such as n-hexane) of type is handled during useless silicon mud, can avoid the second medicament from inorganic type, it can be real
Now preferably anticipate effect.First medicament of organic forms is frequently used for the useless silicon mud more than processing extreme pressure agent content.It is inorganic
The second medicaments such as acid such as nitric acid and sulfuric acid with the organic component in solution because with higher oxidisability, (such as may make
For the sulfide aliphatic acid ester of extreme pressure agent, ethanolamines) react or produce precipitated impurities with the first medicament reaction of organic forms.
Step (D)：Separation lives through the product of the step (B) and the step (C) to obtain solid portion.
The purpose of step (D) is to carrying out separation of solid and liquid through above-mentioned pretreated useless silicon mud, (can be described as with obtaining solid part
Useless silicon mud cake).This step can be carried out with any of appropriate means, such as any suitable filtering or centrifugation apparatus, including
Utilize known filter press, filter bell or centrifuge etc..
Step (E)：With the 3rd chemicals treatment solid portion to obtain the products such as silicate and hydrogen.
The purpose of step (E) is to utilize the 3rd medicament to remove silicon from useless silicon mud cake.The 3rd medicament in the present invention comprising water and
The compound of silicate can be generated with pasc reaction, the compound can be one or more any combination.Silicic acid is generated with pasc reaction
The compound of salt, which is included in water, can produce the alkaline matter of hydroxide ion, such as alkali metal highly basic LiOH, NaOH, KOH
Or alkaline earth belongs to highly basic Ca (OH)2Deng.The 3rd typical typical example of medicament is sodium hydrate aqueous solution.The preferred process method of step (E)
It is as described below in detail.The compound (such as NaOH) that silicate can be generated with pasc reaction is deployed into gross weight percentage concentration
The aqueous solution of the scope within 50% is used as the 3rd medicament.Then the 3rd appropriate medicament is taken to add in the container equipped with useless silicon mud cake
(this container can be closed container and open container).The part by weight scope of the relatively useless silicon mud cake of 3rd medicament is between 0.4~6.
It can in good time be stirred or not stirred.The temperature adjustment of useless silicon mud cake of the 3rd medicament can will be added to higher than room temperature, preferably 40
DEG C, but it is not to be exceeded 140 DEG C.Container equipped with useless silicon mud cake can be pressurizeed, pressure limit is 1-20kg/cm2.Treatment time is regarded
Whether stir and treatment temperature and useless silicon mud cake characteristic in itself and it is different, normally about need 30 minutes to a few hours.In course of reaction
The hydrogen for reacting obtained can be collected by storage of higher pressures bucket.By isolating and purifying equipment acquisition aqueous silicate solution and reclaiming reality
Not siliceous or silicon wafer useless silicon mud cake residue in matter.The composition of useless silicon mud cake residue is depending on the composition of former useless silicon mud.It is logical
Normal undressed useless silicon mud contains carborundum, and the composition of the useless silicon mud cake residue after being handled via the above method can be high-purity
Silicon carbide powder.
Embodiment 1：The useless silicon mud 10g containing cutting oil and metal is taken to be placed in appropriate container first, as shown in the photo in Fig. 2.
The ratio of each composition is contained by measuring in advance in useless silicon mud：Have in 45.16wt% liquid contents, 54.84wt% solid contents, solid content
Have 36.3wt% carborundum, altogether 57.3wt% iron, silicon and silica, the other impurity of 6.4wt%, its about carborundum,
The content of silicon and silica is detected by X-ray diffraction analyzer (XRD).Contained each composition can use other sides in useless silicon mud
Method is detected, for example, take appropriate grams to detect moisture content with cassette moisture teller, recycles NaOH to be reacted and drawing of arranging in pairs or groups with useless silicon mud
Graceful spectrum analysis, can obtain component ratio is：Moisture content is about 30~33%, and silicone content is about 40~45%, and carborundum is then
22~28%.Prepare the first medicament in addition：Sodium chloride (NaCl) solution, concentration is 0.4wt% (0.2g solutes are added in 50g water).
Above-mentioned sodium chloride solution about 50g is taken to pour into 10g useless silicon mud.Then heating-up temperature is stirred 3 hours to 50 DEG C.
Comparing embodiment 1：Carried out using step same as Example 1, difference is, without using the first medicament, to be changed to add
About 50g water.
Embodiment 2 to 9：Carried out using step same as Example 1, difference is that the first medicament is changed to following component respectively：
Embodiment 2 is concentration identical Klorvess Liquid, and embodiment 3 is concentration identical calcium chloride solution, and embodiment 4 is concentration identical
Metabisulfite solution, embodiment 5 is concentration identical sodium nitrate solution, and embodiment 6 is 10ml ethanol solutions (technical grade alcohol 95 %),
Embodiment 7 is the mixed chlorinated potassium solution of concentration identical sodium chloride (solute ratio respectively accounts for half), and embodiment 8 is that sodium chloride mixes second
Alcoholic solution (sodium-chloride water solution and addition 3ml technical grades alcohol 95 % of 50.2g embodiments 1), embodiment 9 is that sodium chloride is mixed just
Hexane solution (sodium-chloride water solution and addition 3ml n-hexanes of 50.2g embodiments 1).
Compared with comparing embodiment 1, its useless silicon mud under the processing of the first medicament of embodiment 1 to 9 significantly can be stirred out equably
Come.Comparing embodiment 1, which is then stirred, also significantly has non-compliant bulk to stir not open for 3 hours.
Embodiment 10：Prepare second medicament：Oxalic acid solution, concentration is 0.4wt% (0.2g sodium oxalates are added in 50g water).Take
Second medicament about 50g is stated to pour into the useless silicon mud product for having added sodium chloride in embodiment 1.Heating-up temperature is to 50 DEG C, stirring 3
Hour, then products therefrom is centrifuged, upper strata filtrate (sampling and measuring metal concentration) is removed, solid portion such as Fig. 3 is taken out and shines
Useless silicon mud cake shown in piece.Prepare the 3rd medicament：Sodium hydroxide solution, concentration is 4wt%.100g the 3rd medicament is taken to add 10
Gram useless silicon mud cake in.In 10kg/cm2Pressure, react 3 hours at a temperature of 80 DEG C, to produce sodium metasilicate and hydrogen.Pass through separation
Purifier apparatus obtains sodium silicate solution (as shown in photo in Fig. 4) and reclaims substantially not siliceous or silicon wafer useless silicon mud cake residual
Thing, as shown in photo in Fig. 5, it is the powder higher than carborundum content in former useless silicon mud containing carborundum content.
Embodiment 11 to 13：Carried out using step same as in Example 10, difference is that second medicament is changed to same concentrations
Following component：Embodiment 11 is citric acid solution, and embodiment 12 is acetum, and embodiment 13 mixes molten for oxalic acid with citric acid
(proportioning of its mesoxalic acid and citric acid is 1 to liquid：50).
Comparing embodiment 2：This embodiment is without using second medicament.Directly the product that the first medicament has been added in embodiment 1 is carried out
Centrifugation, removes upper strata filtrate (sampling and measuring metal concentration), takes out useless silicon mud cake.Prepare the 3rd medicament：Sodium hydroxide solution,
Concentration is 4wt%.100g the 3rd medicament is taken to add in 10 grams of useless silicon mud cake.In 10kg/cm2Pressure, react at a temperature of 80 DEG C
3 hours, to produce sodium metasilicate and hydrogen.By isolate and purify equipment obtain sodium silicate aqueous solution and reclaim substantially it is not siliceous or
The useless silicon mud cake residue of silicon wafer.
Embodiment 14 and 15：Carried out using step same as in Example 10, difference is that second medicament is changed to same concentrations
Following component：Embodiment 14 is sulfuric acid solution, and embodiment 15 is salpeter solution.
Embodiment 16：Prepare second medicament：Citric acid solution, concentration is 0.8wt% (0.4g citric acids are added in 50g water).Take
Above-mentioned second medicament about 50g, which is poured into, have been added in embodiment 9 in the useless silicon mud product of sodium chloride and n-hexane.Heating-up temperature is to 50
DEG C, stir 3 hours, then centrifuged products therefrom, remove upper strata filtrate (sampling and measuring metal concentration), take out solid
Part.Prepare the 3rd medicament：Sodium hydroxide solution, concentration is 4wt%.Take the useless silicon mud cake of 100g 10 grams of the 3rd medicament addition
In.In 10kg/cm2Pressure, react 3 hours at a temperature of 80 DEG C, to produce sodium metasilicate and hydrogen.Obtained by isolating and purifying equipment
To sodium silicate aqueous solution and recovery substantially not siliceous or silicon wafer useless silicon mud cake residue, wherein being higher than containing carborundum content
The powder of carborundum content in the useless silicon mud of original.
Table one shows the iron content in the mixed liquor that embodiment 10 to 16 and comparing embodiment 2 are crossed through three kinds of chemicals treatments.
Comparing embodiment 2 shows that iron content is up to more than 700ppm in the mixed liquor handled without using second medicament.Can be from relatively in fact
Apply the content that example 2 understands iron in undressed useless silicon mud.The display of embodiment 10 to 15 uses iron content in mixed liquor after second medicament
Below 180ppm can be dropped to.In these embodiments, it is possible to find the removal effect order of quality of iron be followed successively by oxalic acid adding citric acid,
Citric acid, acetic acid, oxalic acid, sulfuric acid, nitric acid.The display of embodiment 16, which is worked as, uses the first medicament containing organic forms (n-hexane)
To handle during useless silicon mud, the second medicament (citric acid) from organic forms carries out subsequent treatment.
It should be noted that only demonstrate preferred embodiment above, the present invention still includes the various embodiments that are stated clearly in present invention and other
Embodiment.And the various embodiments described above are not limited to the present invention to illustrate the invention.It is all other without departing from institute of the present invention
The lower equivalent change or modification completed of spirit is disclosed, is intended to be limited solely by the application the scope of the claims.
Claims (10)
1. a kind of application method of useless silicon mud, it is comprised the following steps：
Step (A)：Obtain the useless silicon mud containing cutting oil and metal；
Step (B)：For cutting the silicon mud that given up described in the first chemicals treatment that oil reacts with described；
Step (C)：For handling the useless silicon mud with the second medicament of the metal reaction；
Step (D)：Separation lives through the product of the step (B) and the step (C) to obtain solid portion；And
Step (E)：With solid portion described in the 3rd chemicals treatment to obtain silicate and hydrogen.
2. the application method for the silicon mud that gives up as claimed in claim 1, wherein, first medicament, which is included, meets structure formula (I)
Compound in one or more any combination：
Structure formula (I)：M-X
Wherein M is selected from alkali and alkaline earth metal ions and X is selected from halogen, sulfate radical and nitrate anion；Or M is selected from
Hydrogen and hydroxyl are selected from C5-C12 alkyl and X.
3. the application method for the silicon mud that gives up as claimed in claim 2, wherein, the step (C) is also included according to selected
The species of first medicament determine the species of the selected second medicament.
4. the application method for the silicon mud that gives up as claimed in claim 1 or 2, wherein, the compound of the structure formula (I) is selected from
In following compound：Sodium chloride, potassium chloride, calcium chloride, sodium sulphate, sodium nitrate, ethanol, n-hexane, and they
Various combinations.
5. the application method for the silicon mud that gives up as claimed in claim 1 or 2, wherein, the second medicament, which is included, is selected from nothing
The one or more of which any combination of the compound of machine acid or organic acid.
6. the application method for the silicon mud that gives up as claimed in claim 5, wherein, the second medicament is selected from following compound：
Oxalic acid, citric acid and acetic acid.
7. the application method for the silicon mud that gives up as claimed in claim 6, wherein, first medicament is sodium-chloride water solution；
And the second medicament is oxalic acid and citric acid.
8. the application method for the silicon mud that gives up as claimed in claim 3, wherein, selected when first medicament includes wherein M
From in C5-C12 alkyl and X selected from hydrogen and hydroxyl structural formula (I compound when, the second medicament is selected from such as
Lower compound：Oxalic acid, citric acid and acetic acid.
9. a kind of aqueous silicate solution, it is made as the method as any one of claim 1-8.
10. a kind of powder of silicon carbide-containing, it is made as the method as any one of claim 1-8, wherein,
The useless silicon mud contains carborundum.
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| CN201610018093.XA CN106957060A (en) | 2016-01-12 | 2016-01-12 | The application method and the product by its acquisition of useless silicon mud |
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| CN201610018093.XA CN106957060A (en) | 2016-01-12 | 2016-01-12 | The application method and the product by its acquisition of useless silicon mud |
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Citations (4)
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| CN101691216A (en) * | 2009-10-05 | 2010-04-07 | 山东科技大学 | Method for recycling silicon carbide and co-producing white carbon black from waste mortar for wire cutting |
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| CN101691216A (en) * | 2009-10-05 | 2010-04-07 | 山东科技大学 | Method for recycling silicon carbide and co-producing white carbon black from waste mortar for wire cutting |
| US20120073952A1 (en) * | 2010-09-29 | 2012-03-29 | Yu-Lung Sun | Method for recycling cutting fluid |
| CN102079520A (en) * | 2011-01-12 | 2011-06-01 | 虹京环保有限公司 | Recycling method of silicon carbide |
| CN102659112A (en) * | 2012-05-23 | 2012-09-12 | 北京科技大学 | Method for recovering silicon powder from monocrystalline and polycrystalline silicon cutting wastes by utilizing potential adjustment centrifugal process |
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