TW200804181A - Method of recovering silicon-containing material - Google Patents

Abstract

A method by which a silicon-containing material from which a coolant has been removed is recovered. The method of recovering a silicon-containing material is characterized by comprising the steps of: removing beforehand a water-soluble coolant from a spent slurry resulting from a silicon wafer production process which comprises the water-soluble coolant, abrasive grains, and silicon particles to thereby obtain a solid matter; extracting from the solid matter the water-soluble coolant remaining in the solid matter with a low-boiling organic solvent which has compatibility with the water-soluble coolant and has a lower boiling point than the water-soluble coolant; removing by filtration the low-boiling organic solvent used in the extraction; and recovering the solid matter obtained by the filtration.

Description

200804181 IX. Description of the Invention: [Technical Field of the Invention] The present invention relates to a method for recovering a cut material from a used slurry, which is used for using a multi-wire cutting machine (hereinafter referred to as " MWS (multi wire saw) or a polishing apparatus, for example, when a polycrystalline silicon wafer for a solar cell or a germanium wafer for a semiconductor device is used. [Prior Art] As a method of forming a wafer (thin sheet) from a twin ingot, there is a method of cutting using a wire saw. At this time, generally, it is called a mixture of a slurry and an abrasive. The method of supplying to the cutting part β χ, _ Generally, “re-use”, but the chips and the like are mixed into the slurry every time the slicing is processed, so that the cutting performance of the wire ore is gradually decreased. Containing the chips of Shi Xi, so far, these stone chips are generally disposed of without being used, or, as in the patent literature, the treatment with inorganic acids such as HF (hydrofluoric acid) or filtration and It is collected by a lot of treatments, such as drying, and it is collected. [Patent Document 1: Japanese Patent Laid-Open No. 2001-278612 [Abstract] [Problems to be Solved by the Invention] However, the stone eve contained in the used materials will be used. In the prior art of Reuters, large-scale equipment is required. Moreover, the number of steps is also relatively high and it takes a lot of work. = It is that when using Shiguang oil in the aggregate, oil such as medium oil or diesel oil is needed. Organic solvent, or HF, etc. Acid, etc., the handling of safety equipment or the prevention of environmental pollution requires huge costs. Also, because of the need: heart 119391.doc 200804181 'There is also the cost of the filter is also a cost, therefore, the expectation - an effective and strict, the main reason. However, when the side of the stone used in the & used material is the case where the material in the material is contained as the material containing the stone, the cold of the organic substance contained in the water is used as a problem, for example, Lexington has caused various problems. A... The organic matter is a harmful substance, or it is caused by the adhesion of organic matter in the fine furnace. The slurry of Gekoujing 1 is used as a material containing Shishi, which is heavy I, /' for use. The present invention has been made in view of the above '"main" to reliably remove the coolant. Tianyue Department # developed in the above situation, the method of removing the cerium-containing material from the coolant. /, the mouth of the collection [technical means to solve the problem] The recovery of the stone-containing material of this 杳明, ^ method, which is characterized by the following steps in the fr you have water-soluble coolant, abrasive grain granules to the dream crystal The water-purifying coolant is preliminarily removed from the round material (4), thereby obtaining a low-boiling organic chelating medium which is mutually soluble with respect to the water-soluble coolant and has a lower point than the water-cooling cold component, and the residual residue is extracted from the solid component. The water-soluble coolant in the upper solid fraction is removed by a transition to remove the low/Focus organic solvent used in the extraction, and the solid fraction obtained by filtration is recovered. In the present invention, a low-foam organic solvent which is relatively easy to evaporate is used to extract a water-soluble coolant remaining in the solid fraction, and the extract is removed by using the method.

The use of low; r Fu point organic dissolution sister? έέ I L /, this recovery to remove the water-soluble coolant containing Shishi materials. The solid fraction obtained by the use of ruthenium contains a low-point organic solvent, but the boiling point of the low-boiling organic solvent is relatively low, so that it is easy to remove. The recovered ruthenium-containing material contains a large amount of ruthenium as a raw material for producing hydrogen and 酸 119391.doc 200804181 acid steel or as a method for producing a plurality of ruthenium. Further, the raw materials and the like which can be used in various publications can be used as the raw material of the Ik halothane in the sword & Patent Laid-Open No. 2005-330149. Further, since the material has been removed from the harmful substance of the water-soluble organic substance, or : μ', the problem of dyeing can be avoided. Embodiments of the present invention include the following steps: from at least: a method of receiving a 'characterized' in a polymer used in a stone wafer process::: : agent,:: abrasive particles and dream particles, which obtain a solid content, using a low-boiling organic solvent for a water-soluble cooling agent, a finer than a water-soluble coolant: from, == remaining in the above solid form to form a mouth shape The handle used in the knife is taken, so... The coolant, 11 is recovered by filtration to remove the low-boiling organic solvent used in the extraction. The solid form obtained by the error is described below, and each step will be described in detail. 1 · The solid fraction is obtained in step f2 by using a water-soluble coolant, abrasive grains and the _ = used slurry to remove the water-soluble coolant in advance, thereby obtaining a so-called used slurry Human granules. The slurry contains abrasive grains and the pots are embedded in # + 7, grain-based coolant. The types of abrasive grains are two, including SiC: diamond, boron trioxide, emulsified aluminum, etc. So-called water-soluble The coolant H939I.doc 200804181 is a type of coolant which is mutually soluble in water, and the type thereof is not limited. The water-soluble coolant includes, for example, a water-soluble organic solvent such as ethylene glycol, propylene glycol or polyethylene glycol. The coolant may contain 5% of water to the left and right. In this case, the coolant may be avoided as a dangerous product in the fire protection method. In the second coolant, a dispersion is usually added to disperse the abrasive grains or (4) chips = ( In the present specification, "%" means "weight" as an example of the steps included in the Shihwa wafer manufacturing process, for example, the Shi Xijing sectioning step, or the Shixi wafer Grinding step, etc. The side produced by the time, or the pair of stone eve = ::::, TM. Used - concentration: shape removal method is not limited 'for example, distillation. u field method if the slurry is self-contained The towel gives the water-soluble solid form, the soil, the sun, the ρ θ 1 ^%, and the base, straight":: Steaming can be normal pressure steaming, decompression...: Any one of the museums, according to the viewpoint of energy saving or safety, the car father is good η Ί Ί Ί Ί _ _ x ^ ”, ' It is better ) 'De. The solid part is usually in the form of powder. Raw. The water-soluble coolant that has been bursted is recovered and used for the re-slurry of the slurry = Γ:: two steaming _ can also be separated, filtered, and Steaming (punching away ~ separation and steaming, (2) combining solids, two VT distillation by vaporization or centrifugation to separate the liquid. It can also be distilled only by distillation or centrifugation 119391.doc 200804181 The solid content of the carboxyl group or the % of the liquid may be used in one or more times. The water-soluble coolant may be removed in advance, and more specifically, for example, the following method may be used. In the first method, the water-soluble cooling system J is removed in advance from the used water and the water mash. The slurry is used as the main component by the method of the following steps. Solid fraction, for the dream] The liquid obtained by the separation is centrifuged twice, thereby recovering water = Na One part of the liquid of the main component, the water-soluble coolant is pre-removed by the steaming-house self-test material, and the sample is at least one of the residue of the liquid and the sludge obtained by the two centrifugation. The steps included in the first method will be described in detail. (1) One-time centrifugation step In this step, the solid fraction of the abrasive particles as a main component is recovered by performing i-time centrifugation on the used charge. The 1st centrifugal separation is better by separating i(10)~i and deleting G. The used slurry is separated. The surface is reported to be eight-t-shaped. The knife is separated from the solid 1 and the first liquid. The first solid: The main component of the fraction is abrasive grains. Since the specific gravity of the abrasive grains is generally larger than that of the stone particles, the abrasive grains settle faster than the stone particles. Therefore, if the low-speed centrifugal separation is performed, the abrasive grains will selectively settle. 1 The solid fraction contains more abrasive particles, so the first fraction can be used for the regeneration of the aggregate. On the other hand, the liquid contains mainly water-soluble coolant and bismuth. (2) 2 centrifugation steps H9391.doc -10 - 200804181 In this step, 'by centrifugation The liquid obtained is subjected to two centrifugation to recover a part of the liquid of the water-soluble coolant as a main component. The second centrifugation is preferably carried out by 2_~5_G. If such a speed is higher than 1 time Separate from the high-speed centrifugal separation, the solid fraction that has not settled in the 1st centrifugation will also settle. Therefore, the second liquid is separated into a liquid containing a water-soluble coolant as a main component by two centrifugation (2nd) liquid)

With the sludge as a solid part. The sludge contains τ 3 granules and abrasive grains that have not settled during the first centrifugation. The second liquid φ intervenes, and the excellent to dry also contains abrasive grains and stone granules. The second liquid is usually used for the regeneration of the slurry, and the entire summer is used for the regeneration of the slurry. The mass of the recycled slurry is too large, so it is not good. Therefore, in the present method, only one part of the second liquid # tooth is recovered. The recovered liquid can be used for the regeneration of the slurry. (3) Distillation step

In this step, a sequel to at least one of the liquid residue obtained by centrifuging the HL i 9 A H straw and the sludge is distilled. The sample of the steaming hall may be, for example, (1) only the liquid residue, (2, only the sludge, (3) the residue of the liquid, or any of the mixture of the mud ν, the tea 忒枓It can only contain one part of the sludge. The mud can be defined before the distillation. Suitable. The method of drying is not special. 2. The second method is to remove the water-soluble cooling in advance: the used pulp: The solid fraction is obtained by steaming in the second method, and the agent is used in the slurry from the used slurry to recover the abrasive particles as a main component by one-time centrifugation. H9391.doc 200804181 The water-soluble coolant is removed in advance, and the heart separates at least a part of the liquid obtained. "The error is separated from the following by one step, and the method included in the method of the second method is described. ~ The sample of the library is different from the U method. In the second method, the liquid obtained by the separation of the 'hearts' is separated from the solid by one. The sample of the distillation can be, for example, one of the liquids: And pay the king to serve - the person. Hey, when the liquid - part of the pair The residue of the body can be separated by 2 ^ ^, which can be separated from the sample, and the distilled sample is packaged with the obtained sludge (total amount or part). 2. Extraction step Secondly, the use of the water-soluble coolant has The low-boiling point of the soluble coolant is lower than that of the water...the organic solvent of the stagnation point, and the extract from the above solid content is left in the solid portion of the above-mentioned solid fraction I w ^ ^ I grain-based coolant. The water-soluble coolant remaining in the organic solvent in the boiling point of the Bu Chong m / 溶解 is dissolved at a low level: "The extraction of the sexual coolant can be achieved, for example, by adding the above: to the above solid content, The two are not suitable for the water-soluble coolant, and the boiling point is lower than the water-soluble fast. The type of the organic solvent is not limited, for example, the carbon number is 1 to 6 (preferably 丨) , 2 is a range between any of 4, 5, and 6) alcohol or a ketone having a carbon number of 3 to 6 (preferably a range of η 1 ^) as between == and 6 Specific examples of the alcohol which can be used include methanol, ethanol, isopropanol, and butanol. Specific examples of such a ketone include C11939l.doc -12-200804181 ketone or mercaptoethyl ketone. The low boiling organic solvent may be a plural mixture. Considering other viewpoints, the ratio of the low boiling organic solvent is better. The water-soluble coolant is lower than 5 generations (preferably 6 〇疋, at the point of the flame, 80% (: above, 90. 〇 or above, 70 〇 to the ancient a 1 〇〇〇 or more). At the time, eight have the following two advantages: • It is easy to evaporate the low-stagnation organic solvent remaining in the solid fraction as described below, and; The pure bismuth of the low-boiling organic solvent obtained by distillation is recovered. The water-soluble coolant in the right (4) residual is melted in the low-point organic ridge medium before or after the extraction. Further, the pulverization of the solid component is carried out, and the filtration step is repeated to remove the low-boiling organic solvent used in the extraction. = party = the device used is not limited. If you consider the sheep 4 in mass production, it is better to use a leafhopper. 4 · The cleaning step The low machine preferably comprises the following steps: using the same or different types of low-point organic solvent to be used in the extraction: cold:: wash: = square: surely remove the residue The m ^ \ ..., 隈疋α washing in the water in the solid fraction can be carried out, for example, by a method of using a good organic solvent from the filter paper. Cleaning is more than 2 repeated cleaning process. It is better to carry out the cleaning to the liquid after washing. 219391.doc 200804181 The brightness is below the standard and is μ, which is it. The transparency of the liquid is once dissolved in the amount of the water-soluble coolant, and the amount of the indirect U is sufficient. The partial agent is dissolved in the low-point organic solvent, and the solid component is dissolved in the solid solvent.歹 = Γ 性 cold below. Transparency is determined by using Jis κ 0102 as the basis for the benchmark. For example, the factory can be used for the drainage test method, and the standard is as good as 10 或 Τ δ and 10 或 or 20 咖. It is good for the car father to further include the low-point organic solvent of the liquid obtained by the liquid after the cleaning and the liquid obtained by the cleaning. The organic solvent can be reused for ..., wide medium. The recovered cleaning. #山,, ;夂远水/ The extraction of the gluten coolant or the laughter, the distillation of the liquid obtained by the hunting filter, and the reading of the liquid after the cleaning can be carried out separately or separately. Concentric night body 5 · Drying step Secondly, it is preferable to include Residue in the solid medium to evaporate and dry the solid part. The low-point organic solvent eight organic solvent is relatively easy to evaporate due to the relatively low boiling point. The drying method of the solid knife is the low-freezing point.干燥 Drying can be carried out for natural migration, or combination of heating and subtraction. The various features disclosed in the heating, subtracting/upper embodiment can be combined with each other. When a plurality of features are included in a real shape '(10) Several features can be appropriately taken out, used alone or in combination in the present invention. Consistent Example 1

An embodiment of the present invention will be described with reference to Fig. 1 for a recovery system containing a stone material. Table A A H939l.doc • 14-200804181 & In the present embodiment, a crucible for a solar cell is selected as an object to be processed by using a slurry. The M WS for solar cells used in this embodiment is mainly focused on the production capacity. In one process, four twin ingots (125 Wxl25 Dx400 L) can be processed at one time, and processed into about 3,200 wafers. (125 Wxl25 Dx〇.3 L).

The dressing trough used in the processing of the Japanese Guardian uses a size of about 200 L, and the inside of the trough, the inside of the trough is used to 丨:! The mass ratio is mixed with abrasive grains (specific gravity: 3 · 2 summer). The water/combination cold part agent (specific gravity: 丨). As the water-soluble coolant, the composition is 5% by weight of propylene glycol, 15% by water, or 5% by weight of a dispersant. About 20 kg of solid matter mainly composed of Shi Xi swarf was mixed into the slurry by one processing. 1 · 1 time, 2 times of centrifugation step First, 500 kg (specific gravity: ι·72, 290 L) was used by decanting type centrifugation (called 1 centrifugation, 500 G) The slurry 1 is separated into a liquid 3a and a solid component 3b. Next, the total amount of the liquid 3a was further separated into a liquid 5a and a sludge % by decantation centrifugal sedimentation (referred to as 2 centrifugation, 3 500 G). The total amount of the solid fraction (containing a large amount of abrasive grains) 3b produced by one centrifugation 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, the two are mixed and 'adjusted specific gravity and viscosity', and a new yarn and a new coolant are added to prepare a regenerated slurry. If the regeneration and slicing of the slurry is repeated, the concentration of the crucible contained in the used regrind slurry is divided into about 12%, (4) and about 0. Mud 5b The liquid 5a is not used as the regenerative coolant 6 (remaining Cooling 119391.doc •15, 200804181 agent) 7 production of 100 kg, 80 kg. The amount and composition of the sludge 5b and the remaining coolant 7 were measured. The results are shown in Table 1. [Table 1]

Si SiC coolant metal Other production sludge 60% 20% 18% 1% 1% below 100 kg Residual coolant 13% 5% 80% 1% 1% below 80 kg 2. Distillation step Next, mix with sludge 5b and The sample of the remaining coolant 7 was subjected to vacuum distillation to obtain a liquid 9a and a solid fraction 9b. The vacuum distillation was carried out using a vacuum distillation apparatus (temperature: 160 ° C, finally reaching a vacuum of 10 Ton*). The liquid 9a is 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 9b 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 remaining particles 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% 119391.doc -16- 200804181 3. Stirring, pulverizing step 夂, for solid content 9b was added with a weight ratio of 5 times (49 〇kg) of isopropyl alcohol (hereinafter referred to as "alcohol") 12, and stirred by a ball mill for an hour. The ball mill uses the valley °. For a diameter of 1 m and a length of 1.5 m, 200 20 mm spherical terrarium beads were placed in the liquid' to rotate at 2 〇 RPM. The container is used by applying grease to the inner surface of the stainless steel container, and nitrogen is applied to the shaft center.

The cockroach is captured and the volatile components are known. According to this method, the solid fraction 9b and the alcohol 12 can be stirred, and the solid fraction 9b is pulverized. Thereafter, the particle size distribution of the particles contained in the mixed liquid after the mixing was measured. The particle size measurement is performed by a pulse width distribution meter. The results are shown in Tables 3 and Table 4. It is known that by adding (4) into the solid portion 9b after distillation, the particles having a particle size of more than 1 coffee disappear, and almost all the particles are insufficient in particle diameter. 〇〇 2 faces. The reason for this is considered to be that the coolant remaining in the solid portion 9b of the steam (4) is dissolved in the alcohol so that the particles adhered by the cooling dJ are separated from each other. [Table 4]

Next, filtration was carried out using a leaf filter type filter device. Thereby, the obtained liquid is placed in the vertical closed container, and the horizontal disc-shaped blade is placed in the vertical direction in the vertical direction =:, and the interval between the blades is adjusted by the spacer ring. The above-mentioned leaf crossing type is configured to be the solid portion 15b only. Deposited on the upper surface of the blade, and the liquid 11939I.doc 200804181 body 15a is discharged through the vertical hollow axial direction. The right filter filter device is used to easily clean the solid bifurcation 5b. Further, the leaf filter type filter device is a closed structure. Therefore, it can be preferably used in a method having a washing step using a highly volatile organic solvent such as the alcohol of the present embodiment. The filter cloth of the leaf filter is made of polypropylene. The treatment of the liquid 15a is as follows: 5 - Washing step φ Next, the solid portion 15b deposited on the upper surface of the blade is washed with 3 times (294 kg) of alcohol. The alcohol used for washing uses isopropyl alcohol. The cleaning is carried out by repeating the following steps: • Injecting alcohol from above the solid fraction 15b, passing it through the solid fraction 15b, recovering the alcohol passing through the solid fraction i5b, and injecting it again from above the solid fraction 15b. The compounding step was carried out for 3 hours, whereby the washed liquid 17a and the solid fraction 17b were obtained. The solid content of the solid portion 17b after washing was ΐη·8 kg, containing 28 kg of alcohol. _ Liquid win 15a and liquid 17a were temporarily stored in After collecting the recovery tank, the mixture is further subjected to distillation. The distillation liquid is taken out as the regenerated alcohol 2, and the regenerated alcohol 2 is again used as the stirring or cleaning alcohol. The distillation is carried out at 9 〇〇c, and the condenser is used for recovery. Evaporated liquid. To increase the yield, the temperature of the condenser is set to -0 C. The boiling point of the alcohol (isopropanol) contained in the liquid 15a and the liquid 17a is 82·4 C, and the propylene glycol is 187·85^ Therefore, in the distillation under 9 〇〇c, propylene glycol hardly evaporates, so that a high-purity alcohol can be recovered by distillation. The total weight of the liquid 15a and the liquid 17a is 75 〇kg, and the weight of the regenerated alcohol 21 is 720 kg. The main component of the solid component remaining after distillation is the coolant component H939l.doc -18- 200804181 G (Bing Yi), and contains SiC, Si, metal impurities, and other components as a trace component. 6. Drying step', person Vacuum drying on solid part 17b (4〇 C 10 Torr or less), the liquid hair pieces 19a, thereby obtaining the solid component (iv). ^ ... through the liquid evaporated condenser recovered to the condition of the condenser (TC under the atmospheric pressure. Recovery

The liquid 19a recovered as g is directly used as the regenerated alcohol 21. The amount and composition of the solid fraction 19b were measured. The results are shown in Table $. [Table 5] The above-mentioned (four)' can be used to recover the stone-containing material 23 which does not actually contain a coolant. The cut material 23 contains more w and can be used as a raw material for producing polycrystals. In the present embodiment, the alcohol is recovered from the liquid 15a and the liquid na, and further returned to the alcohol evaporated in the (iv) drying step. Therefore, most of the alcohol used can be recycled for reuse. In the above-mentioned example, the total amount of the liquid 3a which is centrifuged once is subjected to two-person centrifugation, and the mixture as shown in Fig. 2 can be subjected to two times of centrifugation/mixing of the desired portion, and: The liquid plate remains _ mud 5, and the load is removed. In this case, the centrifugal split can be reduced by 2 times.

Further, in the above embodiment, 7 and mixed, as shown in FIG. 3, the sludge 5b is not dried and the remaining sludge is cooled to the dry sludge 5b, and the sludge is 讣 939 939].d〇c • 19- 200804181 7 mix. The effect of this. In this case, the same as in the above embodiment is obtained, and the centrifugal separation is performed once or twice in the above embodiment, but it is also possible to perform only one centrifugal separation, and the liquid 3a is used as a tomb. In this case, there is an advantage that the cost of the device can be reduced. 1. Example 2 The embodiment 2 of the present invention is described with reference to Fig. 5. Example and implementation of the mussel

The difference between 1 and J 1 is that the sample of only 匕3 of the remaining coolant is subjected to steaming and secondary centrifugation steps, and this step is the same as that of the first embodiment, and the description thereof is omitted. In the crucible, the sludge 5b is discarded, and only the remaining coolant 7 is used as a sample for distillation. x ′′ 2. Steaming crane step,,, person, vacuum distillation of the sample containing the remaining coolant 7 to obtain liquid 9a and solid fraction %. Vacuum distillation to enter the same conditions as in the example < The distillation coolant ji was used for the regeneration of the slurry, and the amount and composition of the solid fraction 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. Looking at Table 7, it can be seen that the larger particles from 1 to 10 are the majority. This is considered to be because the particles adhere to each other due to the coolant remaining in the solid portion 9b to become larger particles. 11939l.doc -20- 200804181 [Table 7] 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 10% 20% 33% 32% 5% 3. Stirring and pulverizing step Next, for solid fraction 9b Isopropanol (hereinafter referred to as "alcohol") 12 in an amount of 5 times by weight (64 kg) was stirred by a ball mill for 1 hour. The stirring under the ball mill was carried out under the same conditions as in Example 1. Thereafter, the particle size distribution of the particles contained in the mixed liquid after the stirring was measured. The results are shown in Table 8. Comparing Table 7 and Table 8, it can be seen that particles having a particle diameter of 0.1 mm or more disappear, and the particle diameter of almost all particles is less than 0.02 [Table 8] 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 98% 2 % 0% 0% 0% 4. Filtration step Next, filtration is performed using a leaf filter type filter device. Filtration was carried out under the same conditions as in Example 1. 5. Washing step Next, the solid portion 15b deposited on the blade was washed with 3 times (38.4 kg) of alcohol. The cleaning of the solid fraction 15b was carried out under the same conditions as in Example 1. The solid portion 17b after washing has an overall weight of 13 kg and contains 2 kg of alcohol. After the liquid 15a and the liquid 17a are temporarily stored in the recovery tank, the same is added to 119391.doc -21 - 200804181. The vaporized liquid was taken out as the regenerated alcohol 21. Regeneration was again used as the alcohol for stirring or washing. The distillation is carried out at 9 (TC) to recover the evaporated liquid. To increase the yield, the condensation is produced as 〇t. The total weight of the body 15a and the liquid 17a is iG2 4 kg. ^: The amount is 95 kg. The main component of the solid component remaining after steaming is the coolant. PG' contains Sic, si, metal impurities, and other components as a trace component. 6. Drying step Next, vacuum is applied to the solid fraction 17b. Drying (40t: 10 T〇rr or less), the liquid 19a was bursted 'by taking out the solid fraction (10). Vacuum drying was carried out under the same conditions as in Example 1. The bursting liquid 19a was recovered by a condenser. The condition was set to o °c under normal pressure. The recovered amount was L84 kg. The recovered liquid 19a was directly used as the regenerated alcohol 21. The amount and composition of the solid fraction 19b were measured, and the results are shown in Table 9.

Further, the particle size distribution of the solid fraction 19b was measured. The results are shown in Table 10. [Table 9] [Table 10] Solid content 0.001 mm or more 90% 0.02 mm or more 10% 0.1 mm to _ 1 mm or more 10 mm or more

119391.doc -22- 200804181 The ruthenium-containing material which does not substantially contain a coolant can be recovered by the above steps. 23 Example 3 The Example 3 was carried out under the same conditions as in Example 2. The solid content of the solid fraction 9b after the distillation, the solid fraction 15b after filtration, the solid fraction after washing, and the weight of the coolant contained in the solid fraction 19b after drying were measured. Residual coolant weight is measured by heating each solid to 1 〇 (rc to remove low boiling organic solvents)

The weight is measured after the medium, and thereafter, the amount of change in weight after heating the uranium after heating and removing the coolant at 3 ° C and again, and 3 〇 〇 c, is reset as residual cooling d. The results are shown in the table. As the table η is unknown, the weight of residual coolant can be greatly reduced by filtration and cleaning.

[Table 11]

Example 4 was carried out under the same conditions as in Example 2 except that the washing step was repeated twice. The solid content of the filtered solid portion 151), the solid boring tool after the first cleaning, the solid content after the second cleaning, and the solid content of the solid material after drying 9b were measured. The results are shown in Table i2. As shown in Table 2, the head error is reduced by repeated cleaning to reduce the weight of the residual coolant. [Table 12]

119391 d0l -23-200804181 The application of the present application is hereby incorporated herein by reference. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 shows a ruthenium-containing material recovery system according to a first embodiment of the present invention. Fig. 2 shows a modification of the ruthenium-containing material recovery system of the embodiment i of the present invention. Fig. 3 shows a modification of the ruthenium-containing material recovery system of the first embodiment of the present invention. Fig. 4 is a view showing a modification of the ruthenium-containing material recovery system of the embodiment of the present invention. Fig. 5 shows a ruthenium-containing material recovery system according to a second embodiment of the present invention. [Explanation of main components] 1 Used slurry 3a 1 time after centrifugation of liquid 3b 1 time after centrifugation, solid part 4 Regenerated abrasive grains 5a 2 times of centrifuged liquid 5b 2 times after centrifugation 6 Regeneration coolant 7 Residual coolant 9a Distilled liquid 9b Solid content after steaming 11 Steaming hall coolant 12 Alcohol 15a Transitional liquid 119391.doc -24- 200804181 15b Filtered solids 17a Cleaned liquid 17b Solid content after washing 19a Liquid after drying 19b Solid content after drying 21 Regenerated alcohol 23 Antimony containing material 119391.doc -25-

Claims (1)

200804181 X. Patent Application Scope 1. A method for recovering I-containing materials, which comprises the following steps: 3 Water-based coolant, abrasive particles and granules used in the process ^ u 1 Obtaining the pre-removal of the water-soluble coolant in the solid form, surry), the mutual solubility of the water-soluble coolant and the low boiling point of the water-soluble cold agent are six times open &lt; eight by - cold From the solid fraction, the 7-soluble solvent remaining in the upper portion is extracted and removed by filtration to remove the low-boiling organic solvent used in the extraction. Adding the solid component obtained by filtration to the method of adding 2. The method for recovering the cut material of the claim item is carried out by previously removing the water-soluble slurry from the used material: 7 ^_ by using the method of the following steps The slurry is obtained by sub-centrifugation of the solid fraction 'by the centrifugation separation: body = centrifugation' thereby recovering the water-soluble cold? The body is in the -2th portion, and one of the liquids of the main component is obtained by distilling from the sample in advance by two centrifugation::: the agent 'at least one of the sample's (sludge) . Residual liquid and sludge 3·If requested! In the recovery material of the cerium-containing material, 褚I is a gentleman &amp; ancient, in which the water-soluble coolant is removed in advance from the used pulp. <Water treatment: By using the following steps, the used pulp is used. The material is subjected to centrifugal centrifugation to recover the abrasive grains to 119391.doc 200804181 Cold:: At least a part of the water solubility is removed first. 3, the liquid obtained by one-time centrifugation: the recovery method of the cerium-containing material of the item i: the carbon number of the carbon 2 is 6 or the carbon number is 3 to 6 - the content of the solvent The recovery method of Shixi material, 1 medium: including methanol, ethanol, isopropanol or C-. Low-temperature organic solvent The method for recovering the cerium-containing material of the long term 1, wherein the low boiling w medium has a lower point than the water soluble coolant by 5 (rc or more. _,,,, *, *7), such as the method for recovering the cut material of the requester, wherein Package: After the transition, the borrowing component is cleaned by using the low-boiling organic solvent used in the extraction or the different types of low-foam organic solvent. The solid content of the material is as shown in claim 7. Recycling, raw, raw 4 /, A heavy hard cleaning until the transparency of the liquid after the month wash is based on the main 9. The method for recovering the cerium-containing material as claimed in the claim, the step of: pulverizing the extracted component of the residual water-soluble coolant. Further, in the case of pre-extraction or extraction, the solid-state further includes the following distillation to recover a low boiling point. 1) The method for recovering the cerium-containing material of claim 1, and the step of arranging the organic solvent by the liquid obtained by the filtration. 119391.doc