TW200804182A - Method for recovering silicon-containing material - Google Patents

Abstract

To provide a method for recovering a silicon-containing material from which a coolant is removed. In the method for recovering a silicon-containing material, a water-soluble coolant is preliminarily removed from a used slurry in manufacturing processes of silicon wafers, the slurry containing at least a water-soluble coolant, abrasive grains and silicon grains to obtain a solid portion, the water-soluble coolant remaining in the solid portion is extracted from the solid portion by using a low boiling point organic solvent having compatibility with the water-soluble coolant and a boiling point lower than that of the coolant, the low boiling point organic solvent used for the extraction is removed by centrifugal separation, and a solid portion obtained by the centrifugal separation is recovered.

Description

200804182 IX. Description of the Invention: [Technical Field] The present invention relates to a method for recovering a stone-containing material from a used slurry, which is used for using a multi-wire cutting machine ( Hereinafter, it is referred to as "MWS (multi wire saw)" or a polishing apparatus, and for example, a solar cell, a polysilicon wafer, or a germanium wafer for a semiconductor device can be manufactured. [Prior Art]

As a method of forming a wafer (thin sheet) from a slicing ingot, there is a method of cutting using a wire saw, and in this case, generally, a mixture of a slurry and a coolant is called to be supplied to the slurry. The method of cutting the part. Further, in general, the slurry is repeatedly used, but the chips and the like are mixed into the slurry each time the slicing is processed, and the cutting performance of the wire ore is gradually lowered. The used slurry contains Shishi's chips, and the chips have been disposed of directly without being used, or, as shown in the patent document, the treatment with inorganic acids such as HF (hydrofluoric acid) has been carried out. Or it can be recovered by performing many processes such as filtration and drying. Patent Document 1: Japanese Patent Laid-Open Publication No. 2001-278612 [Draft of the Invention] [Problems to be Solved by the Invention] However, in the prior art in which the used stone is contained in the used slurry, large-scale equipment is required. Moreover, the number of steps is also large and it takes a lot of work. In particular, when mineral oil is used in the aggregate, it is necessary to use kerosene or wood oil for petroleum, organic solvent, or Hf to calculate the chemical acid, etc., and the handling of safety equipment or environmental pollution requires a huge cost. H9392.doc 200804182 Therefore, the cost of filtering has become the main reason for the increase in costs. Therefore, it is desirable to effectively treat the side of the used material in the aggregate. However, when the used slurry is used as the stone-containing material, the coolant of the organic substance contained in the pulp, and the pulp sometimes causes various problems. The problem is, for example, the generation of an organic substance-based harmful substance or contamination due to adhesion of an organic substance in a refining furnace. Therefore, it is important to remove the cooling as a cutting material. The present invention is based on the above-mentioned circumstances, and provides a method for recovering and removing the content of the coolant; [Technical means for solving the problem] The method for recovering a cut material according to the present invention includes the steps of: preliminarily removing water-soluble from a material used in a process containing at least a water-soluble coolant, a wire, and (4) a wafer. a coolant which is obtained by using a low-boiling organic solvent having a mutual purity and a boiling point lower than that of the water-soluble coolant for the water-soluble coolant, and extracting the water-soluble coolant remaining in the solid portion from the solid content The low-point organic solvent used in the extraction is removed by centrifugation and the solid fraction obtained by centrifugation is recovered. In the present invention, the low-point organic solvent which is relatively easy to evaporate is used to extract the pure water coolant remaining in the _zone, and the low-point organic solvent used in the extraction is removed and removed. The solid material obtained by cutting the material 1 (4) of the coolant contains a low-point organic solvent, but the (four) point organic solvent has a relatively low Buddha point and is therefore easy to remove. 119392.doc 200804182 Among the cerium-containing materials recovered, there are more sputum in the bamboo, and it can be used as a raw material for the production of hydrogen and sodium citrate, or as a raw material for the production of A, raw, and gas. It can be used as a raw material for manufacturing-money by the method disclosed in Japanese Patent Laid-Open Publication No. Hei. Further, since the material has been removed from the water-soluble coolant, it is possible to avoid the problem that organic substances are harmful substances, and the organic substances in the secondary refining furnace are contaminated. [Embodiment]

The method for recovering a cut material according to an embodiment of the present invention, comprising the steps of: pre-removing a slurry towel used in a process towel from a stone wafer containing at least a water-soluble coolant, abrasive grains, and a stone particle a water-soluble coolant, thereby obtaining a solid component, using a low-boiling organic solvent having mutual solubility to a water-soluble coolant and having a boiling point lower than that of the water-soluble coolant, and extracting water-soluble cooling remaining in the solid component from the solid component The agent removes the low-boiling organic solvent used in the extraction by centrifugation, and recovers the solid fraction obtained by centrifugation. Hereinafter, each step will be described in detail. 1. Solid fraction obtaining step First, a solid content is obtained by previously removing a water-soluble coolant from a slurry which has been used in the process from a slurry containing at least a water-soluble coolant, abrasive grains and bismuth particles. The used slurry refers to a mixture of granules in the slurry. There is no limitation on the type of the water-soluble coolant D-abrasive which contains the abrasive particles and the division thereof, and includes, for example, SiC, diamond, and 〇81^(:(^1^301: 〇11 119392.doc 200804182 ed. 6, cubic The water-soluble cooling means a coolant having mutual solubility with respect to water, and the type thereof is not limited. The water-based coolant includes, for example, ethylene glycol, propylene glycol or polyethylene glycol. A water-soluble organic solvent. X, a water-soluble coolant may contain about 5% to 15% of water. In this case, the coolant can be prevented from becoming a dangerous thing in the fire protection method. Particles or Si chips dispersing agent (bentonite), etc. (about several %). In the present specification, "%" means 〇/〇I.

Examples of the steps included in the Shihwa wafer process include, for example, a Shi Xijing ingot slicing step or a dream wafer polishing step. The so-called Shiki particles are, for example, tantalum chips generated when a tantalum ingot is sliced to form a tantalum wafer, or abrasive scraps generated when the wafer is polished. The concentration of ruthenium in the used slurry is, for example, 10% or more. The solid content is obtained by previously removing the water-soluble coolant from the used slurry. The method for removing the water-soluble coolant is not limited, and is, for example, distillation. The method of distillation is not limited as long as it is a method of evaporating a water-soluble coolant from a used slurry to obtain a solid fraction. The distillation may be any of atmospheric distillation, vacuum distillation, and vacuum distillation, and is preferably vacuum (10 Torr or less) distillation from the viewpoint of energy saving or safety. The solid form is usually in the form of a powder. Preferably, the evaporated water soluble coolant is recovered for slurry regeneration. The removal of the water-soluble coolant can be carried out by centrifugation or by enthalpy in addition to distillation. It can be carried out by (1) combining centrifugal separation and distillation, (2) combining, and considering steaming. It can be distilled by distillation or centrifugation to obtain 119392.doc 200804182. It is also possible to distill only the boring tool which is separated by distillation or centrifugation. Centrifugation or filtration can be carried out in the used slurry. (4) Removal of the water-soluble coolant can be carried out, for example, by the following method. 1 -1 · The first method

In the method of Yudi 1 'pre-water-soluble cooling from the used slurry __ includes the following steps: the solid component of the used material is separated by centrifugation (4) (four) particles as a main component, The liquid obtained by centrifugation is centrifuged twice to recover a portion of the liquid containing the water-soluble coolant as a main component, and the water-soluble coolant is preliminarily removed from the sample by the steaming chamber. At least one of the residue of the liquid obtained and the sludge is separated by centrifugation. Hereinafter, the steps included in the first method will be described in detail. (1) 1 centrifugation step

The solid fraction or the solid fraction obtained by distilling the liquid or the liquid can be carried out once in a plurality of times. More specifically, in this step, the solid content of the abrasive grains as a main component is recovered by centrifugation of the above-mentioned used slurry. The first centrifugal separation is preferably carried out at 100 to 1000 G. The used slurry was separated into a first solid fraction and a first liquid by one centrifugal separation. The main component of the J-solid component is abrasive grains. Since the specific gravity of the abrasive grains is generally larger than that of the granules, the abrasive grains settle faster than the granules. Therefore, if low-speed centrifugation is carried out, the abrasive grains selectively settle. Since the first solid fraction contains a large amount of abrasive grains, the first solid fraction can be used for the regeneration of the slurry. On the other hand, the first liquid mainly contains a water-soluble coolant and a stone particle. 119392.doc 200804182 (2) Two-time centrifugation step In this step, a liquid obtained by one-time centrifugation is partially recovered by a centrifugal separation of a portion of a liquid containing a water-soluble coolant as a main component. The second centrifugation is preferably carried out at 2 〇〇〇 to 5 〇〇〇 G. If such a centrifugal separation is carried out at a speed higher than one centrifugal separation, the solid portion which has not settled in the centrifugal separation also settles. Therefore, the second liquid is separated by two centrifugations.

The liquid (second liquid) in which the body is separated into a water-soluble coolant as a main component is separated from the solid as a solid. It contains the stone particles in the mud, and the abrasive grains that have not settled in the centrifugal separation. The second liquid also contains abrasive grains and stone particles. The second liquid is usually used for the regeneration of the slurry, but if the total amount is directly used for the regeneration of the slurry, the mass ratio of the ruthenium of the regenerated slurry is too large. Therefore, in this method, only the portion of the liquid of the 2nd is recovered. The recovered liquid can be used for the regeneration of the slurry. Distillation step In this step, at least one of the residual material and the sludge of the liquid obtained by centrifuging the human by the 7 ^ hunting

The test of Mm 枓 is carried out for distillation. Samples of the distillation Examples Disk #, p 4 (2) only sludge, and (3) any of the liquid residues. The sample may contain only the - part limit. Into the ruthenium distillate for drying. There is no particular method for drying. 1β"2. Method 2 In the second method, the solvent is preliminarily removed by using a method including the following steps in the slurry from the used slurry: by using the used slurry. H9392.doc 200804182 It is expected! Sub-centrifugation to recover the abrasive particles as a main component. The water-soluble coolant is preliminarily removed from the test sample by steaming, and the sample contains: at least a part of the liquid obtained by centrifugation. g is explained by the steps included in the second method. ^ The method of the second method, the square of the tomb distillation, the + away from the ..., the method of preparation and the method of the brother 1 are common. In the second method, the sample of the steaming hall is different from the first method. In the second method, the sample obtained by the sub-centrifugal separation, which is obtained by distilling the sample from the time of the first day, and the sample of the v-cutting distillation, for example, may be (1) the liquid-eight (7) liquid. Any of them. Further, when the residue of the liquid is subjected to two corrections, the residue of the liquid can be subjected to two centrifugation to be carried out; and the sample obtained therein contains (4) (total amount or - part) obtained thereby. 〇2·Extraction step secondly, the water-soluble coolant has a mutual solubility (four) point lower than that of the water-soluble cold agent, and the water-soluble coolant extracted from the solid content in the solid portion . In the present specification, "extraction" m is carried out in a water-soluble cooled boiling point organic solvent remaining in the above solid portion. The extraction of the low water-soluble coolant can be carried out, for example, by adding the above-mentioned low-boiling organic solvent to the upper (four) form and stirring the both. When the water-soluble coolant is mutually soluble and has a boiling point lower than that of the water-soluble coolant, the type of the low-boiling organic solvent is not limited, and for example, it is a carbon number of 1 to 6 (preferably, in the case of (8) Any two of the ketones in the range of alcohol or carbon number 3, preferably in the range between any of 3, 4, 5 and 6. Specific examples of the above-mentioned alcohol include methanol, ethanol, and 119392.doc -12-200804182 propanol or butanol. Specific examples of the film include acetone or methyl ethyl ketone. The low '/fu point organic solvent may be a mixture of a plurality of organic solvents. In view of other viewpoints, the low-boiling organic solvent is more entangled than the water-soluble coolant by 50 ° C or more (preferably 6 (rc or more, 7 (rc or more, ribs or more, 90 C or more or i〇〇). In the case of above, there are two advantages in that it is easy to evaporate the low-boiling organic solvent remaining in the solid fraction obtained by centrifugation as described below, and by centrifuging

When the liquid to be supplied is subjected to distillation to recover a low-boiling organic solvent, it is easy to increase the purity of the low-boiling organic solvent obtained by the retorting. In order to dissolve the water-soluble cooling effect remaining in the target fraction + in the low-boiling organic solvent towel, before the extraction or the extraction, the crucible further includes a step of pulverizing the solid component. 3. Centrifugation step Next, the method of removing the low-boiling organic solvent used in the extraction by centrifugal separation or the apparatus used therein is not limited. Preferably, the centrifugal separation is carried out at 3,000 G or more (preferably 4000 G or more, 5000 G or more _ 〇 G or more, 7000 G or more, or 8000 G or more). Further, the following steps may be further included: one or more (preferably two or more, three or more, four or more, five or more, or six or more), and the use of the above-mentioned low-boiling organic solvent The same or different kinds of (four) point organic solvents, from the point of departure. The knife extracts the water-soluble 14 cold portion d remaining in the solid portion from the solid portion obtained, and removes the low-point organic solvent used in the extraction by centrifugation, and recovers the m-shaped obtained by centrifugation. Minute. In other words, the extraction and centrifugation steps can be repeated. The upper limit of the number of repetitions is not limited to 119392.doc -13- 200804182. It is generally considered that if the extraction is repeated, the extraction and centrifugation may be repeated in the solid fraction φ. Water soluble coolant. The conditions of different extractions and centrifugation are carried out under different conditions, and the same conditions can be used to further reduce the liquid of the burdock of the organic solvent of the Buddha's point. The recovered low-boiling organic solvent can be reused for the extraction of residual water-soluble coolant. After 4, the drying step 〃 the car is good, including the evaporation of the μ, ▲ agent remaining in the solid fraction and the money-shaped step Γ 点 有机 organic solvent == machine solvent because the boiling point is relatively low and relatively easy The Wanqing, which can evaporate the low-boiling organic solvent in the solid fraction, is not limited. The soot is decompressed and dried. For nature, it is also used for heating or two deaths: the various features disclosed in the embodiment can be combined with each other. "The solid scorpion scorpion contains a plurality of special 0 0 0 ^. Zhou Tian obtains one or a plurality of special traits, which are used alone or in combination in the present invention. Embodiment 1 Embodiment of the present invention is made using FIG. Fig. 1 shows the recovery system of the shishi material of the present embodiment. In the present embodiment, the solar ray is used as the object for slicing the slurry. example

The MWS used for solar cells used by Mwe+J is mainly focused on production capacity. & day μ, - in human processing, it can be used for 4 Shi Xijing ingots (125 Wxl25 Dx40〇L1 push processing, processing to 3200 pieces) Wafers on the left and right (125 Wxl25 Dx〇3 L) 119392.doc 14 200804182 The slurry tank used in the processing is about 200 L. The slurry contained in the tank is mixed with a mass ratio of 1:1. Particles (specific gravity: 3 2 i) and water-soluble coolant (specific gravity: 丨). The water-soluble coolant is composed of propylene glycol 80%, water IS%, and dispersant 5%. It is about 2 藉 by one processing. “The solids with swarf chips are mixed into the slurry. 1 · 1 time, 2 times of centrifugation steps First, 500 kg by decanting type centrifugation (called { centrifugation, 500 G) (Specific gravity: ι·72, 29〇L) The used slurry 1 is separated into a liquid 3a and a solid component 3b. Next, the liquid 3a is further separated by sedimentation centrifugation (referred to as 2 centrifugation, 3500 G). The total amount is separated into liquid 5a and sludge 5b. The solid produced by centrifugation by centrifugation The total amount of 3b2 (containing a large amount of abrasive grains) is recovered as the regenerated abrasive grains 4, and a part (30%) of the liquid 5a produced by the two centrifugation is recovered as the regenerated coolant 6, and the two are mixed. Adjusting the specific gravity and viscosity 'Adding new abrasive grains and new coolant to make recycled aggregate. If the slurry is regenerated and sliced, the concentration of the used crucible contained in the used aggregate and recycled slurry is about 12%. (4) or so. Age mud 5b, liquid 5a is not used as regenerative coolant flavor (remaining coolant port generation weight is 10 0 kg, 80 kg, respectively, guess, σ 8 is 疋 sludge and residual coolant The amount and composition of 7 are shown in the table. 耆H9392.doc -15- 200804182 [Table l] Si SiC coolant metal Other production amount of sludge 60% 20% 18% 1% 1% or less 100 kg Remaining coolant 13% 5% 80% 1% 1% or less 80 kg 2. Distillation step Next, the sample mixed with the sludge 5b and the remaining coolant 7 was subjected to vacuum distillation to obtain a liquid 9a and a solid fraction 9b. Vacuum distillation was used. Vacuum distillation unit (temperature: 160 ° C, finally reaching true The liquid 9a was used as a distillation coolant 11 for the regeneration of the slurry. The amount and composition of the solid fraction 9b were measured. The results are shown in Table 2. [Table 2]

Si SiC coolant Metal Other production amount Solid content 60.7% 28.4% 7.4% 1.8% 1.8% or less 98 kg The particle size distribution of the solid fraction of 9 b was measured. In the particle size measurement, particles of 10 mm or more, 1 mm or more and 0.1 mm or more are first separated by using a sieve, and then the particle diameter of the particles of the residue is measured using a particle size distribution meter. The results are shown in Table 3. It can be seen from Table 3 that larger particles of about 1 to 10 mm are dominant. The reason for this is considered to be that the fine particles adhere to each other due to the coolant remaining in the solid portion 9b, and become larger particles. [Table 3] 0.001 mm or more, 0.02 mm or more, 0.1 mm or more, 1 mm or more, 10 mm or more, solid content, 15%, 20%, 28%, 32%, 5% 3. Stirring, centrifugation step, followed by adding 10 times for solid fraction 9b (980) Ignol (hereinafter referred to as "alcohol") 12 of kg) was stirred for 30 minutes. Thereafter, solid liquid separation was carried out by centrifugation (8000 G) 119392.doc -16 - 200804182. Thereby, the liquid 15a and the solid component i5b are obtained. The solid fraction 15b was again subjected to stirring under the same conditions, and the centrifugation, separation, agitation, and centrifugation steps were all carried out 5 times. The total weight of the solid fraction i5b after the end of the 5 scrambling and centrifugation steps was 111.8 kg, containing 28 kg of alcohol. The liquid 15a after centrifugation is distilled. The distilled liquid was taken as the regenerated alcohol... The regenerated alcohol 19 was again used as the mixing alcohol. The steaming system was fed at 90 ° and the evaporating liquid was recovered using a condenser. To increase the yield, the temperature of the condenser is set to 〇. Hey. The boiling point of the alcohol (isopropyl alcohol) contained in the liquid 15a was 82.4. (:, propylene glycol is 187.85. (:. Therefore, 90. (In the next distillation, propylene glycol hardly evaporates, and high-purity alcohol can be recovered by distillation. The total weight of liquid i5a recovered in 5 centrifugation is 4872 kg. The weight of the regenerated alcohol 19 is 4500 kg. The main component of the solid residue remaining after distillation is the coolant component PG (propylene glycol), which contains Sic, §丨, metal impurities and other components as trace components. Step Next, the solid portion 17b is subjected to drying (heating for 1 hour), and the solid portion 17b is obtained by evaporating the liquid 17a. The evaporated liquid 17a is recovered by the condenser. The conditions of the condenser are set to be constant. The amount of recovery was 25 kg. The recovered liquid 17a was directly used as the regenerated alcohol 19. The amount and composition of the solid fraction 17b were measured. The results are shown in Table 4. 119392.doc •17- 200804182 [ Table 4]

Si SiC coolant Metal Other production amount Solid content 69.59% 26.58% Almost 0% 2.00% 1.83% 83.8 kg Further, the particle size distribution of the solid fraction 17b was measured. The particle size measurement was carried out using a particle size distribution meter. The results are shown in Table 5. Comparing Table 3 with Table 5, it was found that the particles having a particle diameter of 〇 · 1 mm or more disappeared by adding the alcohol 12 to the solid portion 9b after distillation and stirring, and the particle diameter of almost all the particles was less than 0.1 mm. The reason is considered to be that the coolant remaining in the solid portion 9b after the distillation is dissolved in the alcohol, and the particles adhered by the coolant are separated from each other. [Table 5] 0.001 mm or more 0.02 mm or more 0.1 mm or more 1 mm or more 10 mm or more Solid fraction 85% 15% 0% 0% 0% By the above procedure, the ruthenium-containing material which does not actually contain the coolant can be recovered. The cerium-containing material 21 contains a large amount of cerium and can be used as a raw material for producing polycrystalline germanium or halogenated smoldering. In the present embodiment, the alcohol is recovered from the liquid 15 a after centrifugation, and the alcohol evaporated in the drying step is also recovered. Therefore, most of the alcohol used can be recovered and reused. In the above embodiment, the total amount of the liquid 3a for one centrifugal separation is subjected to two centrifugation, and as shown in Fig. 2, only the components required to obtain the regenerated coolant 6 are subjected to two centrifugation, and the liquid 3a is used. The residue is mixed with the mud 5b and distilled. In this case, the load of centrifugal separation can be reduced twice. Further, in the above embodiment, the sludge 5b is not dried and mixed with the remaining coolant 7, as shown in FIG. 3, after the sludge 5b is dried, the sludge 5b and the remaining 119392.doc -18-200804182 are also used in this case. The same amount of the coolant 7 as that of the above embodiment was obtained and mixed. Etc. Further, in the above embodiment, centrifugation was performed once or twice, but it is also possible to carry out centrifugation only once, and the liquid 3a is used as a sample for distillation. In this case, there is an advantage that the cost of the device can be reduced. Embodiment 2 Embodiment 2 of the present invention will be described with reference to Fig. 5 . This embodiment and implementation

The difference in Example 1 was that the sample containing only the remaining coolant was dropped. ..., M times, and 2 times of centrifugation steps Since this step is the same as that of the embodiment i, the description is omitted. Among them, the sludge 5b was discarded, and only the remaining coolant 7 was used as a sample for distillation. X 2 2 · steaming step. Secondly, the sample containing the remaining coolant 7 was subjected to vacuum distillation to obtain the night body 9a and the solid fraction %. Vacuum distillation was carried out under the same conditions as in the example " The agent 11 was used for the regeneration of the slurry. The amount and composition of the solid knife 9b were measured. The results are shown in Table 6. [Table 6]

The particle size distribution of the solid fraction 9b was measured. The results are shown in Table 7. As can be seen from Table 7, the larger particles of about (7) mm are dominant. The reason for this is considered to be that the fine particles adhere to each other due to the coolant remaining in the solid portion 9b, and become larger particles. H9392.doc -19- 200804182 [Table 7] m ττλ 0.001 mm or more 0.02 mm or more 〇·1 mm or more 1 mm or more 10 mm or more Solid content 10% [20% 33% 32% 5% 3. Stirring, centrifugation step Next, 1 part by volume (128 kg) of isopropyl alcohol (hereinafter referred to as "alcohol") 12 was added to the solid portion 9b for 30 minutes. Thereafter, the mixture was separated by centrifugation (8 〇〇〇 (7), and the liquid i5a and the solid fraction were obtained. The solid fraction 15b was again stirred and centrifuged under the same conditions. The stirring and centrifugation steps were all carried out. 5 times. The total weight of the solid fraction 15b after the completion of the 5 stirring and centrifugation steps is 14 kg, containing 3 kg of alcohol. The liquid 15a after centrifugation is distilled. The distilled liquid is taken as the regenerated alcohol 19. Reuse The regenerated alcohol 19 is used as a stirring alcohol, and the distillation is carried out at 9 Ό C, and the evaporated liquid is recovered by using a condenser. To increase the yield, the temperature of the condenser is set to 〇 ° C. The liquid recovered in 5 centrifugation i5a The total weight is 632 kg. The weight of the regenerated alcohol 19 is 550 kg. The main component of the solid content remaining after distillation is the coolant component PG, which contains SiC, Si, metal impurities, and other components as trace components. Next, the solid portion 17b is subjected to a drying (look: heating for 1 hour) treatment to evaporate the liquid 17a, thereby obtaining a solid fraction 17b. The evaporated liquid is recovered by a condenser. The conditions were set to 常 under normal pressure. (: The recovery amount was 2.5 kg. The recovered liquid 17a was directly used as the regenerated alcohol 19. The amount and composition of the solid fraction 119392.doc -20-200804182 17b were measured. The results are shown in Table 8. [Table 8]

Si SiC coolant metal 詈 solid content 72% 14% approximately 0% 7% _7% 11kg Further, the particle size distribution of the solid fraction 17b was measured. The results are shown in Table 9. [Table 9] 0.001 mm or more 0.02 mm or more 0.1 mm or more 1 mm or more 1 Π mm l'2 l· Solid content 85% 15% 0% IV illili is human 0% The above steps can be used to recover that the coolant is not actually contained. Containing Shi Xi material 2

Example 3 Example 3 was carried out under the same conditions as in Example 1 except that the weight of the alcohol added during the stirring was halved (i.e., the amount of 5 Torr and the number of times of the disruption and centrifugation were changed). The weight of the coolant contained in each of the fractions 9b and the solid fraction 15b after each centrifugation is separated. The weight of the residual coolant is heated to (10) by removing each solid fraction, and the weight is measured after removing the low organic solvent. 3 _ says that the weight is measured by heating and removing the coolant at 300 c, and the weight change of 3 〇〇 ° Γ ^ Μ , and C heating is used as the weight of the residual agent, thereby proceeding. The results are shown in Table 10. As shown in Table 10, the weight of the residual coolant was reduced by repeating the stirring and centrifugation. The number of stirring and centrifugation can be referred to Table 10. It is appropriately determined according to the use of the bismuth-containing material. Usually it is sufficient if it is carried out twice. 119392.doc -21 - 200804182 [Table ίο] 1 time 2 times 3 times 4 times 5 times 6 times 7 times weight (g) 1280 205 33 53 0.844 0.135 0.022 0.003 This application is for Japanese application 1^〇 .2006-75174 (Application Date: November 3, 2006) claims priority, the content of which is incorporated herein by reference. FIG. 1 is a Fig. 2 shows a modification of the ruthenium-containing material recovery system of the embodiment of the present invention. Fig. 3 shows a modification of the ruthenium-containing material recovery system of the embodiment of the present invention. FIG. 4 shows a 矽 of the embodiment of the present invention. Modification of Material Recovery System FIG. 5 shows a ruthenium-containing material recovery system according to Embodiment 2 of the present invention. [Explanation of Main Element Symbols] 1 Used slurry 3a Solid solution after centrifugation of liquid 3b after one centrifugation 4 Regenerated abrasive grains 5a 2 times after centrifugation of liquid 5b 2 times after centrifugation, solids 6 Regenerated coolant 7 Remaining coolant 9a Distilled liquid 9b Distilled solids 11 Distillation coolant 119392.doc -22- 200804182 12 Alcohol 15a Liquid 15b after centrifugation Solid fraction after centrifugation 17a Liquid 17b after drying Solid fraction after drying 19 Regenerated alcohol 21 Antimony containing material 119392.doc -23-

Claims (1)

200804182 X. Patent application scope: 1. A method for recovering a cut material, which comprises the following steps: Since the water-containing coolant contains at least water-soluble coolant, abrasive grains and granules in the 矽 wafer system = the material is pre-removed from the water, the pure cold solid content is used. a low-boiling organic solvent of a water-soluble cold component, extracting a water-soluble coolant remaining in the solid component from the solid component, and removing the low-boiling organic solvent used in the extraction by centrifugation, and then hunting The solid fraction obtained by centrifugation is recovered. 2. The method for recovering a material of the item 1 wherein the pre-removal of the water-soluble coolant from the used poly-polymer is carried out by a method comprising the steps of: using the used slurry by 1 ~ knife away and recover the abrasive particles as the solid shape of the knife, the fine! The liquid obtained by the secondary centrifugation is subjected to a second portion, and the water-soluble coolant is removed in advance from the steaming sample: ^ _, and the sample contains a tank which is obtained by centrifuging the liquid from the knife. Residual and at least one of the sludge. 3. The method according to claim 1, wherein the water-soluble coolant system (4) is pre-removed from the used slurry, and the method includes the following steps: The amount of material is pushed and transferred. The water is collected by centrifugal centrifugation for 1 time. The solid content of the main component is 119392.doc 200804182, and the water-soluble cold part agent is removed in advance from the sample by distillation. At least a portion of the liquid obtained is separated by centrifugation. 4. The method for recovering a ruthenium-containing material according to claim 1, further comprising the step of: using one or more of the following steps: using a low-material organic solvent of the same or different type as the low-point organic solvent, and obtaining a solid form by centrifugation The water-soluble coolant remaining in the above solid fraction is extracted, and the low-boiling organic solvent used in the extraction of the extract is removed by centrifugation, and the solid fraction obtained by centrifugation is recovered. 5. Recycling method of the cerium-containing material of claim 1 Perform centrifugal separation. Among them, 3000 G or more °· as the request item σπ 料 ^-------- dissimilar agent includes an alcohol having a carbon number of 1 to 6 or a ketone having a carbon number of 3 to 6. 7. The recovery of the cerium-containing material of claim 1 , the agent comprising methanol, ethanol, & C 2 method wherein the low-point organic propylene or propylene. 8. For the recovery method of the stone-containing material of the claim 1, the solid-shaped dry-baked beef obtained by the separation of the heart, will be recovered by the material of the cut material according to claim 1:; It is divided by centrifugation, and further includes, for example, a low boiling organic solvent. The liquid of the waiter is distilled and returned. 119392.doc