CN101982536A - Method for recovering silicon carbide and polyethylene glycol cutting fluid from waste silicon wafer cutting fluid - Google Patents
Method for recovering silicon carbide and polyethylene glycol cutting fluid from waste silicon wafer cutting fluid Download PDFInfo
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- CN101982536A CN101982536A CN201010528143.1A CN201010528143A CN101982536A CN 101982536 A CN101982536 A CN 101982536A CN 201010528143 A CN201010528143 A CN 201010528143A CN 101982536 A CN101982536 A CN 101982536A
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- silicon carbide
- cutting fluid
- liquid
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- polyoxyethylene glycol
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 151
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 150
- 239000002173 cutting fluid Substances 0.000 title claims abstract description 83
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 56
- 239000010703 silicon Substances 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 50
- 239000002699 waste material Substances 0.000 title claims abstract description 34
- 239000002202 Polyethylene glycol Substances 0.000 title abstract 3
- 229920001223 polyethylene glycol Polymers 0.000 title abstract 3
- 239000007788 liquid Substances 0.000 claims abstract description 90
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 86
- 238000005520 cutting process Methods 0.000 claims abstract description 45
- 238000000926 separation method Methods 0.000 claims abstract description 36
- 239000007787 solid Substances 0.000 claims abstract description 33
- 238000005342 ion exchange Methods 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 238000001704 evaporation Methods 0.000 claims abstract description 7
- 230000008020 evaporation Effects 0.000 claims abstract description 7
- 239000003513 alkali Substances 0.000 claims abstract description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 142
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 71
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 71
- -1 polyoxyethylene Polymers 0.000 claims description 71
- 239000000706 filtrate Substances 0.000 claims description 35
- 239000012530 fluid Substances 0.000 claims description 28
- 239000012065 filter cake Substances 0.000 claims description 23
- 239000000047 product Substances 0.000 claims description 21
- 239000003795 chemical substances by application Substances 0.000 claims description 20
- 230000003311 flocculating effect Effects 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 239000012535 impurity Substances 0.000 claims description 12
- 239000011347 resin Substances 0.000 claims description 12
- 229920005989 resin Polymers 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- 239000002585 base Substances 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 150000001450 anions Chemical class 0.000 claims description 6
- 150000001768 cations Chemical class 0.000 claims description 6
- 238000004042 decolorization Methods 0.000 claims description 6
- 239000013618 particulate matter Substances 0.000 claims description 6
- 235000019353 potassium silicate Nutrition 0.000 claims description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 6
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 4
- 239000000920 calcium hydroxide Substances 0.000 claims description 4
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 4
- 239000011707 mineral Substances 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 230000001186 cumulative effect Effects 0.000 claims description 2
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 20
- 239000004744 fabric Substances 0.000 description 20
- 230000008569 process Effects 0.000 description 13
- 229910052742 iron Inorganic materials 0.000 description 10
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- 239000002994 raw material Substances 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 3
- 229920000604 Polyethylene Glycol 200 Polymers 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000000571 coke Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
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- 238000005265 energy consumption Methods 0.000 description 2
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- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 2
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- 150000003839 salts Chemical class 0.000 description 2
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- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a method for recovering silicon carbide and polyethylene glycol cutting fluid from waste silicon wafer cutting fluid. The method is characterized by comprising the following steps: stirring the waste cutting fluid at normal temperature and separating to obtain solid and liquid; adding pure water to the solid, stirring, smashing, adding alkali liquor for reacting, and transferring the obtained reaction product into a centrifugal separator to obtain silicon carbide liquid flow; adding acid liquor for reacting, and then transferring the obtained reaction product into the centrifugal separator to obtain clear silicon carbide liquid flow; cleaning and then transferring the clear silicon carbide liquid flow into a dryer for drying, screening by air classification and packaging; adding a decolorizer and a filter aid to the liquid part after solid-liquid separation, performing mechanical separation, adding the decolorizer and the filter aid again to the separated liquid, performing mechanical separation, filtering and desalinizing with an ion exchange system, and dewatering with a four-effect evaporation system to obtain the polyethylene glycol cutting fluid. The method of the invention can prevent environmental pollution caused by direct emission of the waste silicon wafer cutting fluid and effectively reduce the production cost for cutting silicon wafers.
Description
Technical field
The present invention relates to recovery technology, specifically, relate to silicon carbide and polyoxyethylene glycol Fluid Re-cycling method.
Background technology
Silicon chip is a semi-conductor, sun power, the base mateiral of industries such as liquid-crystal display is divided into monocrystalline silicon piece and polysilicon chip, and its raw material is monomer silicon single crystal or polysilicon, pull into silicon ingot through ingot furnace, be cut into silicon rod again, the use wire cutting machine is processed into the silicon chip of each specification, in cutting process, the suspension of silicon carbide and polyoxyethylene glycol cutting fluid and steel wire one react on silicon rod, play cutting action; From the used cutting liquid after the cutting, extract high-quality silicon carbide again and the polyoxyethylene glycol cutting fluid can directly recycle in the silicon chip cutting process.
Silicon carbide (SiC) claim moissanite again.In non-oxidized substance hi-tech refractory raw materials such as contemporary C, N, B, silicon carbide is most widely used general, most economical a kind of, can be called powder emery or fire sand.Silicon carbide is to form through pyrotic smelting in resistance furnace with raw materials such as quartz sands, refinery coke (or coal tar), wood chip (when producing green silicon carbide need with salt).At present China to be used to cut the silicon carbide of silicon chip generally all be green silicon carbide, it is a hexagonal, proportion is 3.20～3.25, microhardness is 2840～3320kg/mm
2, be to be main raw material with refinery coke and high-quality silica, add salt as additive, form by the resistance furnace pyrotic smelting, its hardness is between corundum and diamond, and physical strength is higher than corundum, contains SiC more than 97%.
The main component of cutting fluid is polyoxyethylene glycol (PEG), molecular formula HO (CH
2CH
2O)
nH is formed by ethylene oxide polymerization, can be divided into several series such as pharmaceutical grade, cosmetics-stage, food grade and technical grade.Low-molecular-weight polyoxyethylene glycol is a thermal barrier, viscosity modifier, wetting agent, the important raw and processed materials of solvent etc.The polyoxyethylene glycol that applies to the silicon chip cutting mainly is PEG100, PEG200, and PEG300 is characterized in liquid, nontoxic, non-stimulated, and good thermostability is arranged.
After silicon carbide and polyoxyethylene glycol cutting fluid are mixed stirring by a certain percentage, in wire cutting machine, cut silicon chip, in this process with steel wire, cutting fluid is as the carrier of silicon carbide, make silicon carbide can be evenly distributed to the silicon rod surface, after cutting through the mill of steel wire, form silicon chip; Simultaneously, the thermostability of cutting fluid has effectively been disperseed a large amount of heat energy of producing in the cutting process, makes broken string, surperficial stria, and fine fisssure collapses silicon chip cutting problem such as limit and seldom takes place.
The silica flour that produces when the cutting silicon rod being arranged through solid in the cutting fluid after the cutting, broken silicon-carbide particle, bigger silicon-carbide particle, iron micro mist and the partial oxidation iron of steel wire through producing after the grinding; Liquid portion mainly is the moisture of polyoxyethylene glycol cutting fluid and trace.
Extraction silicon carbide and polyoxyethylene glycol cutting fluid have very big environmental benefit from the silicon chip cutting mortar, and the social benefit and the performance of enterprises are if the cutting fluid after directly waste silicon chip is cut can produce huge and irreversible pollution to environment so; Though there is complete off-line to reclaim silicon carbide at present in the international coverage, the system of polyoxyethylene glycol, energy consumption height, pollution are greatly.
Present known silicon chip cutting waste fluid recovery technology is mainly based on the simple chemical treatment method, especially to reclaim silicon carbide for very, exemplify the publicity patent: application number: 200710117665.0, publication number: CN 10327622A, the drawback of the technical scheme that this patent application patent is taked:, add soda acid and react, on the one hand in excavation pond, ground, soda acid water can progressively infiltrate through in the soil, destroys environment; On the other hand, the water in the pond can't reuse, produces a large amount of waste water, increases the weight of environmental pressure; And recycling silicon carbide, the rate of recovery is low, and silicon carbide purity is also low.
Summary of the invention
The objective of the invention is to,, provide a kind of method that from silicon chip cutting waste fluid, reclaims silicon carbide and polyoxyethylene glycol cutting fluid at the above-mentioned defective that prior art exists, through solid-liquid separation, add alkali, add acid, filter washing, oven dry, decolouring, desalination, step process such as dehydration, not only can obtain high-quality silicon carbide and polyoxyethylene glycol cutting fluid, the method for employing physical bond chemistry has not only been improved the deficiency of conventional art, and energy consumption is low, pollute little, environmentally friendly, rate of recovery height simultaneously.
A kind of method that reclaims silicon carbide and polyoxyethylene glycol cutting fluid from silicon chip cutting waste fluid provided by the invention may further comprise the steps:
1), silicon chip cutting waste fluid is stirred, control its temperature at 25-60 ℃, add entry in waste liquid, the ratio that water adds is the 1-60% of cutting waste fluid cumulative volume, then carries out solid-liquid separation under 0.5-6bar pressure, obtains solid and liquid;
2), in the solid that step 1) obtains, adding quality is the 1-5 10-60 ℃ of water doubly of solid masses, after the stirring, remove by filter moisture, it is 0.5-30% alkali lye that the solid that obtains adds concentration at normal temperatures, reacts after 0.5-4 hour, separate, obtain water glass and the silicon carbide that contains impurity;
3), with step 2) silicon carbide that contains impurity that obtains, under 10-60 ℃ temperature, adding concentration is the mineral acid of 0.5-30%, react after 0.5-4 hour, separates, the silicon carbide that obtains water ratio 10-80% flows;
4) the silicon carbide flow vacuum of the water ratio 10-80% that step 3) is obtained utilizes 10-60 ℃ water washing silicon carbide after filtering, and the cake moisture after the washing is at 5-30%; So repeat 3 times, the cake moisture after the washing that obtains is at 5-30%;
5) the silicon carbide filter cake that step 4) is obtained dewaters under 80-110 ℃ of condition, dewaters after 3-10 hour, obtains the silicon carbide water ratio and is lower than 0.1% powder; Silicon carbide powder is sieved, screen out the silicon carbide micro-powder that gets product behind the large particulate matter;
6), with the liquid that step 1) obtains, be controlled under temperature 25-60 ℃ the condition, in liquid, add discoloring agent and flocculating aids, carry out solid-liquid separation, obtain solid and liquid; Equal conditions, the liquid that separation is obtained is once more behind the decolorization filtering, carry out solid-liquid separation, separate the liquid that obtains and pass through strainer, filtrate is passed through ion exchange system under 20-35 ℃, carry out the absorption and the exchange of zwitterion, the polyoxyethylene glycol cutting fluid water content that obtains is at 60-80%, and specific conductivity is at 0.1-30us;
7), with step 6) through the polyoxyethylene glycol cutting fluid of ion-exchange, in 70-135 ℃, evaporate under the 0.01-0.09MPa vacuum tightness, the water-content in the polyoxyethylene glycol cutting fluid after the evaporation is at 5-35%; Then, evaporate under the 0.01-0.09MPa vacuum degree condition in 70-135 ℃, in order to removing moisture and other low-boiling-point substances in the cutting fluid, in moisture content during at 0.1-0.9%, the can polyoxyethylene glycol cutting fluid that gets product.
The provided by the invention first preferred method that reclaims silicon carbide and polyoxyethylene glycol cutting fluid from silicon chip cutting waste fluid, described step 2) alkali lye is to be selected from a kind of in sodium hydroxide, calcium hydroxide and the potassium hydroxide in.
The provided by the invention second preferred method that reclaims silicon carbide and polyoxyethylene glycol cutting fluid from silicon chip cutting waste fluid, mineral acid is to be selected from a kind of in sulfuric acid, hydrochloric acid and the nitric acid in the described step 3).
The provided by the invention the 3rd preferred method that from silicon chip cutting waste fluid, reclaims silicon carbide and polyoxyethylene glycol cutting fluid, discoloring agent is for being selected from gac in the described step 6); Described flocculating aids is to be selected from a kind of in diatomite and the perlite.
The provided by the invention the 4th preferred method that reclaims silicon carbide and polyoxyethylene glycol cutting fluid from silicon chip cutting waste fluid, described step 6) strainer are that to be selected from precision be the placed in-line deep bed filter of one or several precision, in the filter stick formula strainer one or both among 0.5um, 1um, 5um, the 10um.
The provided by the invention the 5th preferred method that reclaims silicon carbide and polyoxyethylene glycol cutting fluid from silicon chip cutting waste fluid, described step 6) intermediate ion exchange system comprise big sun bed, big cloudy bed; Described big sun bed adopts the 200CNA strong acid cation resin; Described big cloudy bed adopts the 900CL strong base anion resins.
The provided by the invention the 6th preferred method that reclaims silicon carbide and polyoxyethylene glycol cutting fluid from silicon chip cutting waste fluid, the part by weight of described big sun bed, big cloudy bed is 1: 2.
The provided by the invention the 7th preferred method that from silicon chip cutting waste fluid, reclaims silicon carbide and polyoxyethylene glycol cutting fluid, described finished product silicon carbide, carborundum content is at 90-99%; Described finished product polyoxyethylene glycol cutting fluid, the content of its polyoxyethylene glycol is at 98-100%.
Compared with prior art, a kind of method that reclaims silicon carbide and polyoxyethylene glycol cutting fluid from silicon chip cutting waste fluid provided by the invention has the following advantages:
1, whole comprehensive treating process and to utilize the process of silicon chip cutting mortar be the process of physical bond chemistry is an environmentally friendly technology system, cleaning, and safety is polluted little;
2, the recovery silicon carbide that obtains by the present invention, polyoxyethylene glycol cutting fluid have and product innovation equal quality and equal result of use;
3, can avoid the generation of this type of pollution, accomplish close friendization fully environment;
4, silicon carbide, cutting fluid all can consume a large amount of electric power when producing, resources such as water, by the recovery technology of this invention, uses that move in circles can energy efficient, and the raising service efficiency obtains bigger social benefit;
5, bring considerable economic return for a large amount of silicon chip cutting enterprise;
6, this recovery method is simple, and is convenient, lower to technician's operational requirement.
Description of drawings
Fig. 1 is: a kind of process flow sheet that reclaims the method for silicon carbide and polyoxyethylene glycol cutting fluid from silicon chip cutting waste fluid provided by the invention;
Embodiment
Below by the drawings and the specific embodiments a kind of method that reclaims silicon carbide and polyoxyethylene glycol cutting fluid from silicon chip cutting waste fluid provided by the invention is further explained in more detail.
Correlation test
1200# silicon carbide is example
According to comparative result as can be seen, the silicon carbide size distribution that the present invention reclaims is more concentrated, and purity is higher, and moisture and volatile matter content content still less can play the raising cutting efficiency, reduces effects such as outage.
PEG200 is an example
According to comparative result as can be seen, the polyoxyethylene glycol cutting fluid that the present invention reclaims is as clear as crystal, and specific conductivity is low, can well carry silicon carbide and cut silicon chip and reduce working temperature simultaneously.
Embodiment 1
The silicon chip cutting waste fluid 1000g that weighs uses agitator to stir, and controls its temperature at 25 ℃, adds 10g normal temperature tap water, and the ratio that water adds is squeezed into the cutting waste fluid that is mixed with water in the pressure filter 1%, and pressure-controlling is at 0.5bar; Pressure filter is under this pressure, carry out solid-liquid separation, solids such as the silicon carbide of the overwhelming majority, silicon, iron are stayed and are formed filter cake in the filter cloth, and the polyoxyethylene glycol cutting fluid of the overwhelming majority and water see through filter cloth formation filtrate, obtain the 450g solid, 850g liquid: comprised most silicon carbide in the solid (filter cake), silicon and small amounts of iron; All polyoxyethylene glycol have been comprised in the liquid (filtrate), moisture and micro-silicon carbide, silicon;
The solid that the process solid-liquid separation obtains, additional proportion is 10 ℃ of pure water of 1 times, stirs the back and forms uniform suspension, utilizes band filter elimination moisture, it is 0.5% sodium hydroxide that its solid that obtains adds concentration at normal temperatures, reacted 0.5 hour, and squeezed in the horizontal centrifuge and separate, during owing to separation, the difference of proportion, light filter residue is a water glass, and heavy filter residue is the silicon carbide that contains impurity, respectively from difference outlet discharging;
The silicon carbide that contains impurity that obtains after separating adds concentration under 10 ℃ temperature be 0.5% sulfuric acid, reacted 0.5 hour, squeeze in the inclined plate settler and separate, because when separating, the difference of proportion, heavy filter residue silicon carbide fails to be convened for lack of a quorum and leaches from discharge port, obtains the silicon carbide stream of water ratio 10%;
The cleaning of silicon carbide, the silicon carbide stream of water ratio 10% is squeezed into vacuum adhesive tape type filter, utilize 10 ℃ pure water or tap water washing silicon carbide, filtrate enters filtrate through the filter cloth of vacuum adhesive tape type filter and collects jar, and filter cake then is a water content at 5% pie silicon carbide;
The pure water that in pie silicon carbide, adds 10 ℃ once more, make its water content reach 10%, squeeze into vacuum adhesive tape type filter once more, utilize 10 ℃ pure water washing silicon carbide, filtrate enters filtrate collection jar through the filter cloth of vacuum adhesive tape type filter, filter cake then is a water content at 5% pie silicon carbide, the pure water that in pie silicon carbide, adds 10 ℃ once more, make its water content reach 10%, squeeze into vacuum adhesive tape type filter once more, utilize 10 ℃ pure water, filtrate enters filtrate through the filter cloth of vacuum adhesive tape type filter and collects jar, and filter cake then is a water content at 5% pie silicon carbide;
The silicon carbide filter cake enters through rotary conveyor and carries out thermal dehydration in the electrically heated baking oven, and temperature is controlled at 80 ℃, heats 3 hours, makes the silicon carbide water ratio be lower than 0.1%; Silicon carbide powder enters air classifier by gravity or pull of vacuum,,, pack after screening out large particulate matter after within the needed scope through the size distribution of air classifier control finished product silicon carbide through the 40um vibratory screening apparatus, the finished product silicon carbide micro-powder;
The liquid that obtains after the cutting fluid solid-liquid separation, moisture content is 60%, polyoxyethylene glycol cutting fluid content is 40%, under the condition that keeps 25 ℃ of temperature, add discoloring agent and flocculating aids in the liquid: discoloring agent is that gac, flocculating aids are diatomite, the two additional proportion is 10: 1, and with carrying out solid-liquid separation in the plate and frame(type)filter press, liquid portion enters next procedure:
Isolated liquid, moisture content is 60%, polyoxyethylene glycol cutting fluid content is 20%, carry out decolorization filtering once more, under the condition that keeps 25 ℃ of temperature, add discoloring agent and flocculating aids in the liquid once more: discoloring agent is a gac, flocculating aids is a diatomite, the two additional proportion is 10: 1, and with carrying out solid-liquid separation in the separating centrifuge, liquid portion enters next procedure once more:
It is 1um, 5um, three kinds of placed in-line deep bed filter of precision of 10um that isolated liquid is squeezed into precision, filters; Filtrate is squeezed into ion exchange system under 20 ℃, carry out the absorption and the exchange of zwitterion, and the polyoxyethylene glycol cutting fluid water content that obtains is 60%, and specific conductivity is at 0.1us; Wherein, ion exchange system comprises big sun bed and big cloudy bed, and big sun bed adopts the 200CNA strong acid cation resin; Big cloudy bed adopts the 900CL strong base anion resins, and the part by weight of big sun bed, big cloudy bed is 1: 2.
Through the polyoxyethylene glycol cutting fluid aqueous solution of ion-exchange, squeeze into the vacuum quadruple effect evaporator through pump, temperature is controlled at 70 ℃, vacuum degree control is at 0.01MPa, after first three level evaporation, the water-content in the polyoxyethylene glycol cutting fluid is 5%, behind relay tank, enter quadruple effect vacuum pan pipe evaporator, temperature is controlled at 70 ℃, and vacuum degree control is removed moisture and other low-boiling-point substances in the cutting fluid at 0.01MPa, moisture content is 0.1%, and can obtains finished product polyoxyethylene glycol cutting fluid.
Embodiment 2
The silicon chip cutting waste fluid 2000g that weighs uses agitator to stir, and controls its temperature at 60 ℃, adds 1200g distilled water, and the ratio that water adds is squeezed into the cutting waste fluid that is mixed with water in the pressure filter 60%, and pressure-controlling is at 6bar; Pressure filter is under this pressure, carry out solid-liquid separation: solids such as the silicon carbide of the overwhelming majority, silicon, iron are stayed and are formed filter cake in the filter cloth, and the polyoxyethylene glycol cutting fluid of the overwhelming majority and water see through filter cloth formation filtrate, obtain the 120g solid, 1600g liquid: comprised most silicon carbide in the solid, silicon and small amounts of iron; All polyoxyethylene glycol have been comprised in the liquid, moisture and micro-silicon carbide, silicon;
The solid that the process solid-liquid separation obtains, additional proportion is 60 ℃ of pure water of 5 times, after the stirring, utilizes band filter elimination moisture, it is 30% calcium hydroxide that its solid that obtains adds concentration at normal temperatures, reacted 4 hours, and squeezed in the scraper plate settling vessel and separate, during owing to separation, the difference of proportion, light filter residue is a water glass, and heavy filter residue is the silicon carbide that contains impurity, respectively from difference outlet discharging;
The silicon carbide that contains impurity that obtains after separating adds concentration under 60 ℃ temperature be 30% hydrochloric acid, reacted 4 hours, squeezes in the horizontal centrifuge and separate, because when separating, the difference of proportion, heavy filter residue silicon carbide fails to be convened for lack of a quorum and leaches from discharge port, obtains the silicon carbide stream of water ratio 80%;
The cleaning of silicon carbide, the silicon carbide stream of water ratio 80% is squeezed into vacuum adhesive tape type filter, utilize 60 ℃ pure water or tap water washing silicon carbide, filtrate enters filtrate through the filter cloth of vacuum adhesive tape type filter and collects jar, and filter cake then is a water content at 30% pie silicon carbide;
The pure water that in pie silicon carbide, adds 60 ℃ once more, make its water content reach 80%, squeeze into vacuum adhesive tape type filter once more, utilize 60 ℃ pure water washing silicon carbide, filtrate enters filtrate collection jar through the filter cloth of vacuum adhesive tape type filter, filter cake then is a water content at 30% pie silicon carbide, the pure water that in pie silicon carbide, adds 60 ℃ once more, make its water content reach 80%, squeeze into vacuum adhesive tape type filter once more, utilize 60 ℃ pure water washing silicon carbide, filtrate enters filtrate through the filter cloth of vacuum adhesive tape type filter and collects jar, and filter cake then is a water content at 30% pie silicon carbide;
Dry silicon carbide, the silicon carbide filter cake enters through rotary conveyor and carries out thermal dehydration in the steam baking oven, temperature is controlled at 110 ℃, 10 hours heat-up times, make the silicon carbide water ratio be lower than 0.1%, silicon carbide powder enters air classifier by gravity or pull of vacuum, through the size distribution of air classifier control finished product silicon carbide after within the needed scope, pack after process 100um vibratory screening apparatus screens out large particulate matter, get the finished product silicon carbide micro-powder.
Liquid filtering, the liquid that obtains after the cutting fluid solid-liquid separation, moisture content is 80%, polyoxyethylene glycol cutting fluid content is 20%, under the condition that keeps 60 ℃ of temperature, add discoloring agent and flocculating aids in the liquid: discoloring agent is that gac, flocculating aids are diatomite, and the two additional proportion is 10: 1, carry out solid-liquid separation with candle filter, liquid portion enters next procedure:
Isolated liquid, moisture content is 80%, polyoxyethylene glycol cutting fluid content is 40%, carry out decolorization filtering once more, under the condition that keeps 60 ℃ of temperature, add discoloring agent and flocculating aids in the liquid once more: discoloring agent is a gac, flocculating aids is a diatomite, the two additional proportion is 10: 1, carries out solid-liquid separation with candle filter once more, and liquid portion enters next procedure:
Isolated liquid is squeezed into the deep bed filter that precision is 10um, filters, and filtrate is squeezed into ion exchange system under 35 ℃, carries out the absorption and the exchange of zwitterion, and the polyoxyethylene glycol cutting fluid water content that obtains is 80%, and specific conductivity is at 30us; Wherein, ion exchange system comprises big sun bed and big cloudy bed, and big sun bed adopts the 200CNA strong acid cation resin; Described big cloudy bed adopts the 900CL strong base anion resins, and the part by weight of big sun bed, big cloudy bed is 1: 2.Through the polyoxyethylene glycol cutting fluid aqueous solution of ion-exchange, squeeze into the vacuum quadruple effect evaporator through pump, temperature is controlled at 135 ℃, vacuum degree control is at 0.09MPa, after first three level evaporation, the water-content in the polyoxyethylene glycol cutting fluid is 35%, behind relay tank, enter quadruple effect vacuum pan pipe evaporator, temperature is controlled at 135 ℃, and vacuum degree control is removed moisture and other low-boiling-point substances in the cutting fluid at 0.09MPa, moisture content is 0.9%, and can obtains finished product polyoxyethylene glycol cutting fluid.
Embodiment 3
The silicon chip cutting waste fluid 2000g that weighs uses agitator to stir, and controls its temperature at 60 ℃, adds 400g distilled water, and the ratio that water adds is squeezed into the cutting waste fluid that is mixed with water in the pressure filter 40%, and pressure-controlling is at 6bar; Pressure filter is under this pressure, carry out solid-liquid separation: solids such as the silicon carbide of the overwhelming majority, silicon, iron are stayed and are formed filter cake in the filter cloth, and the polyoxyethylene glycol cutting fluid of the overwhelming majority and water see through filter cloth formation filtrate, obtain the 120g solid, 1600g liquid: comprised most silicon carbide in the solid, silicon and small amounts of iron; All polyoxyethylene glycol have been comprised in the liquid, moisture and micro-silicon carbide, silicon;
The solid that the process solid-liquid separation obtains, additional proportion is 60 ℃ of pure water of 5 times, after the stirring, utilizes band filter elimination moisture, it is 30% potassium hydroxide that its solid that obtains adds concentration at normal temperatures, reacted 4 hours, and squeezed in the scraper plate settling vessel and separate, during owing to separation, the difference of proportion, light filter residue is a water glass, and heavy filter residue is the silicon carbide that contains impurity, respectively from difference outlet discharging;
The silicon carbide that contains impurity that obtains after separating adds concentration under 60 ℃ temperature be 30% nitric acid, reacted 4 hours, squeezes in the horizontal centrifuge and separate, because when separating, the difference of proportion, heavy filter residue silicon carbide fails to be convened for lack of a quorum and leaches from discharge port, obtains the silicon carbide stream of water ratio 80%;
The cleaning of silicon carbide is squeezed into vacuum adhesive tape type filter with the silicon carbide stream of water ratio 80%, utilizes 60 ℃ pure water washing silicon carbide, and filtrate enters filtrate through the filter cloth of vacuum adhesive tape type filter and collects jar, and filter cake then is a water content at 30% pie silicon carbide;
The tap water that in pie silicon carbide, adds 60 ℃ once more, make its water content reach 80%, squeeze into vacuum adhesive tape type filter once more, utilize 60 ℃ tap water washing silicon carbide, filtrate enters filtrate through the filter cloth of vacuum adhesive tape type filter and collects jar, and filter cake then is a water content at 30% pie silicon carbide.The pure water that in pie silicon carbide, adds 60 ℃ once more, make its water content reach 80%, squeeze into vacuum adhesive tape type filter once more, utilize 60 ℃ pure water washing silicon carbide, filtrate enters filtrate through the filter cloth of vacuum adhesive tape type filter and collects jar, and filter cake then is a water content at 30% pie silicon carbide
Dry silicon carbide, the silicon carbide filter cake enters through rotary conveyor and carries out thermal dehydration in the Oil fuel dry box, temperature is controlled at 110 ℃, 10 hours heat-up times, make the silicon carbide water ratio be lower than 0.1%, silicon carbide powder enters air classifier by gravity or pull of vacuum, through the size distribution of air classifier control finished product silicon carbide after within the needed scope, pack after process 80um vibratory screening apparatus screens out large particulate matter, get the finished product silicon carbide micro-powder.
Liquid filtering, the liquid that obtains after the cutting fluid solid-liquid separation, moisture content is 80%, polyoxyethylene glycol cutting fluid content is 40%, under the condition that keeps 60 ℃ of temperature, add discoloring agent and flocculating aids in the liquid: discoloring agent is that gac, flocculating aids are diatomite, and the two additional proportion is 10: 1, carry out solid-liquid separation with plate and frame(type)filter press, liquid portion enters next procedure:
Isolated liquid, moisture content is 80%, polyoxyethylene glycol cutting fluid content is 40%, carry out decolorization filtering once more, under the condition that keeps 60 ℃ of temperature, add discoloring agent and flocculating aids in the liquid once more: discoloring agent is that gac, flocculating aids are diatomite, and the two additional proportion is 10: 1, carry out solid-liquid separation with plate and frame(type)filter press once more, liquid portion enters next procedure:
It is the 0.5um deep bed filter that isolated liquid is squeezed into precision, filters, and filtrate is squeezed into ion exchange system under 28 ℃, carries out the absorption and the exchange of zwitterion, and the polyoxyethylene glycol cutting fluid water content that obtains is 80%, and specific conductivity is at 10us; Wherein, ion exchange system comprises big sun bed and big cloudy bed, and big sun bed adopts the 200CNA strong acid cation resin; Big cloudy bed adopts the 900CL strong base anion resins, big sun bed, the part by weight of big cloudy bed is 1: 2, the polyoxyethylene glycol cutting fluid aqueous solution through ion-exchange, squeeze into the vacuum quadruple effect evaporator through pump, temperature is controlled at 125 ℃, vacuum degree control is at 0.06MPa, after first three level evaporation, the water-content in the polyoxyethylene glycol cutting fluid is 15%, behind relay tank, enter quadruple effect vacuum pan pipe evaporator, temperature is controlled at 125 ℃, and vacuum degree control is removed moisture and other low-boiling-point substances in the cutting fluid at 0.06MPa, moisture content is 0.6%, and can obtains finished product polyoxyethylene glycol cutting fluid.
Embodiment 4
The silicon chip cutting waste fluid 2000g that weighs uses agitator to stir, and controls its temperature at 50 ℃, adds 1000g distilled water, and the ratio that water adds is squeezed into the cutting waste fluid that is mixed with water in the pressure filter 50%, and pressure-controlling is at 6bar; Pressure filter is under this pressure, carry out solid-liquid separation: solids such as the silicon carbide of the overwhelming majority, silicon, iron are stayed and are formed filter cake in the filter cloth, and the polyoxyethylene glycol cutting fluid of the overwhelming majority and water see through filter cloth formation filtrate, obtain the 1200g solid, 1600g liquid: comprised most silicon carbide in the solid, silicon and small amounts of iron; All polyoxyethylene glycol have been comprised in the liquid, moisture and micro-silicon carbide, silicon;
The solid that the process solid-liquid separation obtains, additional proportion is 50 ℃ of pure water of 3 times, after the stirring, utilizes band filter elimination moisture, it is 20% calcium hydroxide that its solid that obtains adds concentration at normal temperatures, reacted 3 hours, and squeezed in the horizontal centrifuge and separate, during owing to separation, the difference of proportion, light filter residue is a water glass, and heavy filter residue is the silicon carbide that contains impurity, respectively from difference outlet discharging;
The silicon carbide that contains impurity that obtains after separating adds concentration under 50 ℃ temperature be 20% hydrochloric acid, reacted 3 hours, squeezes in the horizontal centrifuge and separate, because when separating, the difference of proportion, heavy filter residue silicon carbide fails to be convened for lack of a quorum and leaches from discharge port, obtains the silicon carbide stream of water ratio 70%;
The cleaning of silicon carbide, the silicon carbide stream of water ratio 70% is squeezed into vacuum adhesive tape type filter, utilize 50 ℃ tap water washing silicon carbide, filtrate enters filtrate through the filter cloth of vacuum adhesive tape type filter and collects jar, and filter cake then is a water content at 20% pie silicon carbide;
The tap water that in pie silicon carbide, adds 50 ℃ once more, make its water content reach 70%, squeeze into vacuum adhesive tape type filter once more, utilize 50 ℃ tap water washing silicon carbide, filtrate enters filtrate collection jar through the filter cloth of vacuum adhesive tape type filter, filter cake then is a water content at 20% pie silicon carbide, the tap water that in pie silicon carbide, adds 50 ℃ once more, make its water content reach 70%, squeeze into vacuum adhesive tape type filter once more, utilize 50 ℃ tap water washing silicon carbide, filtrate enters filtrate through the filter cloth of vacuum adhesive tape type filter and collects jar, and filter cake then is a water content at 20% pie silicon carbide;
Dry silicon carbide, the silicon carbide filter cake enters through rotary conveyor and carries out thermal dehydration in the electrically heated baking oven, temperature is controlled at 90 ℃, 8 hours heat-up times, make the silicon carbide water ratio be lower than 0.1%, silicon carbide powder enters air classifier by gravity or pull of vacuum, through the size distribution of air classifier control finished product silicon carbide after within the needed scope, pack after process 80um vibratory screening apparatus screens out large particulate matter, get the finished product silicon carbide micro-powder;
Liquid filtering, the liquid that obtains after the cutting fluid solid-liquid separation, moisture content is 70%, polyoxyethylene glycol cutting fluid content is 30%, under the condition that keeps 50 ℃ of temperature, add discoloring agent and flocculating aids in the liquid: discoloring agent is that gac, flocculating aids are diatomite, and the two additional proportion is 10: 1, carry out solid-liquid separation with plate and frame(type)filter press, liquid portion enters next procedure:
Isolated liquid, moisture content is 70%, polyoxyethylene glycol cutting fluid content is 30%, carry out decolorization filtering once more, under the condition that keeps 40 ℃ of temperature, add discoloring agent and flocculating aids in the liquid once more: discoloring agent is that gac, flocculating aids are diatomite, and the two additional proportion is 10: 1, carry out solid-liquid separation with plate and frame(type)filter press once more, liquid portion enters next procedure:
It is 1um filter stick formula strainer that isolated liquid is squeezed into precision, filters, and filtrate is squeezed into ion exchange system under 35 ℃, carries out the absorption and the exchange of zwitterion, and the polyoxyethylene glycol cutting fluid water content that obtains is 80%, and specific conductivity is at 20us; Wherein, ion exchange system comprises big sun bed and big cloudy bed, and big sun bed adopts the 200CNA strong acid cation resin; Big cloudy bed adopts the 900CL strong base anion resins, and the part by weight of big sun bed, big cloudy bed is 1: 2.
Through the polyoxyethylene glycol cutting fluid aqueous solution of ion-exchange, squeeze into the vacuum quadruple effect evaporator through pump, temperature is controlled at 100 ℃, vacuum degree control is at 0.08MPa, after first three level evaporation, the water-content in the polyoxyethylene glycol cutting fluid is 25%, behind relay tank, enter quadruple effect vacuum pan pipe evaporator, temperature is controlled at 100 ℃, and vacuum degree control is removed moisture and other low-boiling-point substances in the cutting fluid at 0.08MPa, moisture content is 0.7%, and can obtains finished product polyoxyethylene glycol cutting fluid.
Should be noted that at last: above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; although the present invention is had been described in detail with reference to the foregoing description; those of ordinary skill in the field are to be understood that: the technician reads after the present specification still and can make amendment or be equal to replacement the specific embodiment of the present invention, but these modifications or change all do not break away within the claim protection domain that the present patent application awaits the reply.
Claims (8)
1. method that reclaims silicon carbide and polyoxyethylene glycol cutting fluid from silicon chip cutting waste fluid may further comprise the steps:
1), silicon chip cutting waste fluid is stirred, control its temperature at 25-60 ℃, add entry in waste liquid, the ratio that water adds is the 1-60% of cutting waste fluid cumulative volume, then carries out solid-liquid separation under 0.5-6bar pressure, obtains solid and liquid:
2), in the solid that step 1) obtains, adding quality is the 1-5 10-60 ℃ of water doubly of solid masses, after the stirring, remove by filter moisture, it is 0.5-30% alkali lye that the solid that obtains adds concentration at normal temperatures, reacts after 0.5-4 hour, separate, obtain water glass and the silicon carbide that contains impurity;
3), with step 2) silicon carbide that contains impurity that obtains, under 10-60 ℃ temperature, adding concentration is the mineral acid of 0.5-30%, react after 0.5-4 hour, separates, the silicon carbide that obtains water ratio 10-80% flows;
4) the silicon carbide flow vacuum of the water ratio 10-80% that step 3) is obtained utilizes 10-60 ℃ water washing silicon carbide after filtering, and the cake moisture after the washing is at 5-30%; So repeat 3 times, the cake moisture after the washing that obtains is at 5-30%;
5) the silicon carbide filter cake that step 4) is obtained dewaters under 80-110 ℃ of condition, dewaters after 3-10 hour, obtains the silicon carbide water ratio and is lower than 0.1% powder; Silicon carbide powder is sieved, screen out the silicon carbide micro-powder that gets product behind the large particulate matter;
6), with the liquid that step 1) obtains, be controlled under temperature 25-60 ℃ the condition, in liquid, add discoloring agent and flocculating aids, carry out solid-liquid separation, obtain solid and liquid; Equal conditions, the liquid that separation is obtained is once more behind the decolorization filtering, carry out solid-liquid separation, separate the liquid that obtains and pass through strainer, filtrate is passed through ion exchange system under 20-35 ℃, carry out the absorption and the exchange of zwitterion, the polyoxyethylene glycol cutting fluid water content that obtains is at 60-80%, and specific conductivity is at 0.1-30us;
7), with step 6) through the polyoxyethylene glycol cutting fluid of ion-exchange, in 70-135 ℃, evaporate under the 0.01-0.09MPa vacuum tightness, the water-content in the polyoxyethylene glycol cutting fluid after the evaporation is at 5-35%; Then, evaporate under the 0.01-0.09MPa vacuum degree condition in 70-135 ℃, in order to removing moisture and other low-boiling-point substances in the cutting fluid, in moisture content during at 0.1-0.9%, the can polyoxyethylene glycol cutting fluid that gets product.
2. method according to claim 1 is characterized in that described step 2) in alkali lye be to be selected from a kind of in sodium hydroxide, calcium hydroxide and the potassium hydroxide.
3. method according to claim 1 is characterized in that mineral acid in the described step 3) is to be selected from a kind of in sulfuric acid, hydrochloric acid and the nitric acid.
4. method according to claim 1 is characterized in that discoloring agent is for being selected from gac in the described step 6); Described flocculating aids is to be selected from a kind of in diatomite and the perlite.
5. method according to claim 1 is characterized in that described step 6) strainer is that to be selected from precision be the placed in-line deep bed filter of one or several precision, in the filter stick formula strainer one or both among 0.5um, 1um, 5um, the 10um.
6. method according to claim 1 is characterized in that described step 6) intermediate ion exchange system comprises big sun bed, big cloudy bed; Described big sun bed adopts the 200CNA strong acid cation resin; Described big cloudy bed adopts the 900CL strong base anion resins.
7. method according to claim 6 is characterized in that the part by weight of described big sun bed, big cloudy bed is 1: 2.
8. method according to claim 1 is characterized in that described finished product silicon carbide, and carborundum content is at 90-99%; Described finished product polyoxyethylene glycol cutting fluid, the content of its polyoxyethylene glycol is at 98-100%.
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