CN103030144A - Method for recovering silicon carbide in waste liquid - Google Patents
Method for recovering silicon carbide in waste liquid Download PDFInfo
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- CN103030144A CN103030144A CN2011103014252A CN201110301425A CN103030144A CN 103030144 A CN103030144 A CN 103030144A CN 2011103014252 A CN2011103014252 A CN 2011103014252A CN 201110301425 A CN201110301425 A CN 201110301425A CN 103030144 A CN103030144 A CN 103030144A
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Abstract
The invention relates to a method for recovering silicon carbide in waste liquid, which comprises the following steps of: separating solids and liquid in the waste liquid through filtering, wherein the solids comprise silicon powder and silicon carbide powder; mixing the solids with water to obtain first mixed liquid; removing the silicon powder and the water in the first mixed liquid through centrifugal separation, and reserving first-stage products which mainly comprise the silicon carbide powder; conducting at least one settling separation process to the first-stage products to obtain second-stage products; adding sodium hydroxide solution into the second-stage products and removing sodium metasilicate produced after reaction between the sodium hydroxide and silicon to obtain third-stage products; and removing residual sodium hydroxide and water in the third-stage products to obtain purified silicon carbide. Therefore, the silicon carbide in the waste liquid can be effectively recycled and the economic benefits are very great.
Description
Technical field
The present invention relates to liquid waste disposal, particularly a kind of method of the silicon carbide in can Recycling of waste liquid.
Background technology
In the process of general industry technique; usually can produce and contain the waste liquid that admittedly contains thing; the program of for example cutting silicon crystal block in the photoelectricity industry semiconductor technology; can use line style blade and collocation to be mixed with the cutting fluid of diamond or silicon carbide (being commonly called as silicon carbide) abrasive particle; under the blade high speed rotating, silicon crystal block is cut into silicon; and the fragmentation and the chip that in the process of cutting silicon crystal block, produce; will be mingled in the cutting fluid and build up (in a silicon crystal block cutting waste fluid; silicon loss because of the width of line style blade of 40% is arranged approximately); cause cutting and liquid-solidly contain that thing content is too high can't to be continued to utilize and become waste liquid; finally can only abandon, not only bad for environmental protection and do not meet economic benefit.
Although have in the prior art aforementioned waste liquid is passed through merely filter cloth, attempt removing consolidating in the waste liquid and contain thing, but existing filter-cloth filtering mode can't will contain in the thing than the silicon carbide of tool economic worth by separating in the waste liquid admittedly, and can block filter cloth because admittedly containing thing, causes filter effect not obvious.
Summary of the invention
Technical problem to be solved by this invention provides the method for the silicon carbide in a kind of Recycling of waste liquid, can effectively the silicon carbide in the waste liquid be recycled.
To achieve these goals, the method that the invention provides the silicon carbide in a kind of Recycling of waste liquid may further comprise the steps: (a) separate consolidating in the waste liquid with filter type and contain thing and liquid, this admittedly contains thing and comprises silica flour and carborundum powder; (b) this is contained admittedly thing and water and be mixed into one first mixing liquid; (c) with centrifugation silica flour and water in this first mixing liquid are removed, keeping carborundum powder is main fs product; (d) the fs product is carried out at least one settlement separate program, to obtain the subordinate phase product, wherein this settlement separate program sequentially comprise and add that water mixes, standing sedimentation and remove the step of suspension; (e) add sodium hydroxide solution to the subordinate phase product, sodium hydroxide and pasc reaction generate meta-acid silicon sodium and are removed, and obtain the phase III product; And (f) sodium hydroxide residual in the phase III product and water are removed, obtain the silicon carbide behind the purifying.
Technique effect of the present invention is: the method for the silicon carbide in the Recycling of waste liquid of the present invention is simple, with low cost, and the silicon carbide that reclaims has high purity, can again make an addition in the silicon crystal block cutting fluid as grinding material, except the environmental pollution that can avoid waste liquid to cause, have the effect that resource reclaims concurrently and be rich in economic worth.
Describe the present invention below in conjunction with the drawings and specific embodiments, but not as a limitation of the invention.
Description of drawings
Fig. 1 is the method flow diagram of the silicon carbide in a preferred embodiment of the present invention Recycling of waste liquid;
Fig. 2 is the synoptic diagram of the employed device of filter type of this preferred embodiment of the present invention;
Fig. 3 is the synoptic diagram of the filter type of this preferred embodiment of the present invention.
Wherein, Reference numeral
10 devices, 20 drainage material accommodating barrel
21 drainage materials, 23 liquid
30 drainage material injection roads, 31 waste liquid pipelines
33 reclaim liquid pipeline 35 return lines
40 plate and frame(type)filter press, 41 filter clothes
43 drainage layers, 45 filtration
50 waste liquid accommodating barrel 51 contain thing admittedly
53 waste liquids 60 reclaim the liquid storage barrel
61 reclaim liquid S11～S18 step
Embodiment
Below in conjunction with accompanying drawing structural principle of the present invention and principle of work are done concrete description:
Fig. 1 is the method flow diagram of the silicon carbide in a preferred embodiment of the present invention Recycling of waste liquid.At first carry out step S11, separate consolidating in the waste liquid with filter type and contain thing and liquid, wherein this admittedly contains thing and comprises silica flour and carborundum powder.
In the method for present embodiment, can use device 10 as shown in Figure 2 to filter waste liquid 53, this device 10 mainly includes a drainage material accommodating barrel 20, splendid attire includes the liquid 23 of drainage material 21 such as the silicon crystal block cutting fluid in it, this drainage material accommodating barrel 20 is connected in an entrance that is provided with the plate and frame(type)filter press 40 of filter cloth 41 via a drainage material injection road 30, in addition, one waste liquid accommodating barrel 50 is connected in the entrance of this plate and frame(type)filter press that is provided with filter cloth 41 40 via a waste liquid pipeline 31, these waste liquid accommodating barrel 50 interior splendid attires include the waste liquid 53 that admittedly contains thing 51, the outlet of this plate and frame(type)filter press 40 then reclaims liquid pipeline 33 with one respectively and a return line 35 is connected, this recovery liquid pipeline 33 is communicated in one and reclaims liquid storage barrel 60, and this return line 35 is communicated in this drainage material accommodating barrel 20.In following examples, illustrate with the employed silicon crystal block cutting fluid of photoelectricity industry semiconductor technology, yet in fact be not limited to this.
Cooperation is with reference to figure 2 and Fig. 3, in the present embodiment, the filtration of waste liquid 53 mainly will contain first the liquid 23 of drainage material 21 by a filter cloth 41, make drainage material 21 storehouses be covered in this filter cloth 41 surfaces and form a drainage layer 43, this filter cloth 41 and this drainage layer 43 that is covered in this filter cloth 41 consist of a filtration 45, the waste liquid 53 that again wish is filtered afterwards is coated with the filter cloth 41 of this drainage layer 43 by storehouse, see through this drainage layer 43 and stop that with filter cloth 41 consolidating in the waste liquid 53 contains thing 51, to obtain the relatively recovery liquid 61 of clarification, that is, contain thing 51 and liquid by this filtration 45 to separate consolidating in this waste liquid 53.
Employed drainage material 21 can be diatomite, activated carbon, snake stone flour, ion exchange resin, quartz sand, manganese sand or its mixture in the filter type of the present invention.If when the waste liquid 53 that wish is filtered was the silicon crystal block cutting fluid, then this drainage material 21 was preferably activated carbon.
Please consult again Fig. 2 and Fig. 3, before beginning to filter, make first the clean cutting fluid 23 that is added with drainage material 21 inject the plate and frame(type)filter press 40 that is provided with this filter cloth 41 via this drainage material injection road 30, make cutting fluid 23 flow back to this drainage material accommodating barrel 20 by filter cloth 41 and via this return line 35, after repeatedly circulating, drainage material 21 in this cutting fluid 23 gradually storehouse is covered in this filter cloth 41 surfaces, forms this drainage layer 43 (the better 0.8mm of being not less than of thickness).After the liquid that is refluxed by return line 35 gradually becomes clarified liq, can stop aforementioned circulation, and begin to carry out the filtration step of waste liquid.
During filtration, make and contain the waste liquid 53 that admittedly contains thing 51, via being coated with the filter cloth 41 of drainage layer 43 in these waste liquid pipeline 31 injection plate paper blotter presses 40 and by storehouse, seeing through drainage layer 43 and stop and admittedly contain thing 51, contain thing 51 effectively to filter consolidating in the waste liquid 53.What specify is, activated carbon powder itself as drainage material 21 namely has most holes in one embodiment of this invention, therefore, not only the slit between each activated carbon powder can tackle that larger the consolidating of particle diameter contains thing 51 (being mainly silica flour and carborundum powder) in the waste liquid 53, the hole of each activated carbon powder itself also can be tackled less the consolidating of particle diameter and contain thing 51, at last, the recovery liquid 61 of acquisition can flow to this recovery liquid storage barrel 60 via this recovery liquid pipeline 33.
Will be understood that the filter type of method of the present invention is not limited to use device 10 as shown in Figure 2 to carry out the filtration of waste liquid 53, any filtration unit that carries out solid/liquid separation is all applicable.
Then carry out step S12, this is contained thing 51 admittedly be mixed into one first mixing liquid with water.Preferably, the volume ratio that water and this contain thing 51 admittedly is at least 1.5: 1, and more preferably, the volume ratio that water and this contain thing 51 admittedly is 2: 1.After this admittedly contained thing 51 and water mixes, this contained thing 51 Uniform Dispersion in this first mixing liquid admittedly, in order to carrying out the follow-up component separating operation that admittedly contains thing 51.
Explanation is in addition, if when the drainage material 21 of filtration waste liquid 53 was activated carbon, consolidating after the filtration contains thing 51 can be doped with activated carbon particle.The particle diameter of activated carbon particle is about 50～200 μ m, the particle diameter of silicon is about 0.6～0.8 μ m, the particle diameter of silicon carbide is about 15 μ m, therefore in another embodiment of the present invention, the step that before step S12, comprises in addition a screening activated carbon and silica flour and carborundum powder, for example: after this is admittedly contained thing 51 and add water and mix, the mesh screen that utilization has 300～350 meshes (mesh) sieves, the silica flour that wherein particle diameter is less and carborundum powder can pass through this mesh screen, and the larger activated carbon of particle diameter can't pass through this mesh screen, thus isolating active carbon and silica flour and carborundum powder.
Then carry out step S13, with centrifugation silica flour and water in this first mixing liquid are removed, keeping carborundum powder is main fs product.Centrifugation step can be carried out in a horizontal centrifuge.Wherein, the proportion of silica flour is approximately 2.33, the proportion of carborundum powder is approximately 3.23, carry out when centrifugal, the large and larger carborundum powder of particle diameter of proportion can be got rid of to outer and be separated, the silica flour that proportion and particle diameter are less and water are then stayed internal layer, therefore can utilize centrifugation by isolating in this first mixing liquid take carborundum powder as main fs product.
Then carry out step S14, the fs product carried out at least one settlement separate program, to obtain the subordinate phase product, wherein this settlement separate program sequentially comprise and add that water mixes, standing sedimentation and remove the step of suspension.Preferably, the volume ratio of water and fs product is at least 1.5: 1, is preferably 2: 1, and the time of leaving standstill is at least 15 minutes, is preferably 20 minutes.
Be noted that in addition, in such as photoelectricity industry semiconductor technology, cut in the employed cutting fluid of program of silicon crystal block, wherein usually include solvent, through resulting fs product after above-mentioned filtration and the step such as centrifugal is also remaining except carborundum powder micro-silica flour and solvent arranged.Wherein silica flour has less proportion and particle diameter compared to carborundum powder, is difficult for precipitating in the standing sedimentation process and is suspended in the liquid, can obtain the higher subordinate phase product of silicon carbide purity after suspension is removed.
Will be understood that, can more promote the purity of silicon carbide through the settlement separate program in road the more.In the present embodiment, method of the present invention is after one settlement separate program, and the purity of silicon carbide is to 96wt%; After the settlement separate program in two roads, the purity of silicon carbide is to 98wt%.Be stressed that after settlement separate program more than two roads, the lifting of the purity of silicon carbide becomes less obvious, therefore goodly select only to carry out the settlement separate program in two roads, to reduce time and the cost that reclaims silicon carbide.
Then carry out step S15, add sodium hydroxide solution to the subordinate phase product, sodium hydroxide and pasc reaction generate meta-acid silicon sodium, because the little meeting of its proportion floats over liquid level, can be removed easily, sodium hydroxide can carry out emulsion reaction with solvent in addition, and the gas loss such as generation carbonic acid gas can obtain the higher phase III product of silicon carbide purity by this to atmosphere.
Carry out again step S16, sodium hydroxide residual in the phase III product and water are removed, obtain the silicon carbide behind the purifying.In an embodiment, can use dilute hydrochloric acid and residual sodium hydroxide acid-base neutralisation among the step S16, can remove by this sodium hydroxide residual in the phase III product and adjust its pH value (better pH value is 6.8).Perhaps, also can use a large amount of flushing with clean water phase III products among the step S16, to remove residual sodium hydroxide in the phase III product.After removing sodium hydroxide residual in the phase III product, with centrifugation separating silicon carbide and water (after the water that acid-base neutralisation produces or the flushing with clean water residual water), then carry out the water that a baking step will remain in the carborundum powder surface and remove, namely obtain the silicon carbide behind the purifying.Wherein, centrifugation step can be to carry out in a horizontal centrifuge, but not as limit.
Because the carborundum powder behind the partially desiccated can present the caking shape, the therefore better dispersion steps S17 that carries out in addition baking step after can utilize rotating paddle that the silicon carbide that lumps is broken up and be indivedual silicon carbide powder independently.
After pulverising step, can carry out again one without screen sizing step S18, utilize the airflow blow carborundum powder, the carborundum powder of different-grain diameter can divide and drop on different positions according to its weight size, the carborundum powder that particle diameter is larger can drop on the position of closer distance because having larger weight, the carborundum powder that particle diameter is less can drop on longer-distance position because having less weight.
In the present embodiment, be respectively equipped with three collectors (can establish still less or more collector) in the position of different distance to collect the silicon carbide of three kinds of particle size range, the particle diameter of the silicon carbide that three collectors near and far are collected is respectively greater than 12.4 μ m (1200 orders are following), 9.3-12.4 μ m (1200 orders～1600 orders) and less than 9.3 μ m (more than 1600 orders).Through dispersion steps and without the purity of the carborundum powder after the screen sizing step to 99wt%, product is more accorded with the demands of the market, and value of the product also can improve.
The method of the silicon carbide in the Recycling of waste liquid of the present invention is simple, with low cost, and the silicon carbide that reclaims has high purity, can again make an addition in the silicon crystal block cutting fluid as grinding material, except the environmental pollution that can avoid waste liquid to cause, have the effect that resource reclaims concurrently and be rich in economic worth.
Certainly; the present invention also can have other various embodiments; in the situation that does not deviate from spirit of the present invention and essence thereof; those of ordinary skill in the art work as can make according to the present invention various corresponding changes and distortion, but these corresponding changes and distortion all should belong to the protection domain of the appended claim of the present invention.
Claims (10)
1. the method for the silicon carbide in the Recycling of waste liquid is characterized in that, may further comprise the steps:
(a) separate consolidating in the waste liquid with filter type and contain thing and liquid, this admittedly contains thing and comprises silica flour and carborundum powder;
(b) this is contained admittedly thing and water and be mixed into one first mixing liquid;
(c) with centrifugation silica flour and water in this first mixing liquid are removed, keeping carborundum powder is main fs product;
(d) this fs product is carried out at least one settlement separate program, to obtain the subordinate phase product, wherein this settlement separate program sequentially comprise and add that water mixes, standing sedimentation and remove the step of suspension;
(e) add sodium hydroxide solution to this subordinate phase product, sodium hydroxide and pasc reaction generate meta-acid silicon sodium and are removed, and obtain the phase III product; And
(f) sodium hydroxide and water residual in should the phase III product be removed, and obtain the silicon carbide behind the purifying.
2. the method for the silicon carbide in the Recycling of waste liquid as claimed in claim 1 is characterized in that, utilizes consolidating in this waste liquid of filtration filtering separation to contain thing and liquid in step a.
3. the method for the silicon carbide in the Recycling of waste liquid as claimed in claim 2 is characterized in that, this filtration comprises a filter cloth and a drainage layer.
4. the method for the silicon carbide in the Recycling of waste liquid as claimed in claim 3 is characterized in that, the material of this drainage layer is diatomite, activated carbon, snake stone flour, ion exchange resin, quartz sand, manganese sand or its mixture.
5. the method for the silicon carbide in the Recycling of waste liquid as claimed in claim 1 is characterized in that, water and this volume ratio that admittedly contains thing are at least 1.5: 1 in step b.
6. the method for the silicon carbide in the Recycling of waste liquid as claimed in claim 5 is characterized in that, the volume ratio that water and this contain thing admittedly is 2: 1.
7. the method for the silicon carbide in the Recycling of waste liquid as claimed in claim 1 is characterized in that, carries out centrifugal with a horizontal centrifuge in step c.
8. the method for the silicon carbide in the Recycling of waste liquid as claimed in claim 1 is characterized in that, in steps d, the volume ratio of water and fs product is at least 1.5: 1, and the time of leaving standstill is at least 15 minutes.
9. the method for the silicon carbide in the Recycling of waste liquid as claimed in claim 1 is characterized in that, also comprises a dispersion steps after step f, and the carborundum powder of part caking is broken up.
10. the method for the silicon carbide in the Recycling of waste liquid as claimed in claim 9 is characterized in that, also comprises one without the screen sizing step after dispersion steps, utilizes the airflow blow carborundum powder, and collects the carborundum powder of different-grain diameter at different positions.
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| CN2011103014252A CN103030144A (en) | 2011-09-28 | 2011-09-28 | Method for recovering silicon carbide in waste liquid |
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| CN2011103014252A CN103030144A (en) | 2011-09-28 | 2011-09-28 | Method for recovering silicon carbide in waste liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103303924A (en) * | 2013-06-25 | 2013-09-18 | 佳明新材料科技有限公司 | Silicon carbide micropowder recycling process flow |
| CN109553104A (en) * | 2017-09-27 | 2019-04-02 | 东莞新科技术研究开发有限公司 | The recovery method of silicon carbide in grinding waste slurry |
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| CN101130237A (en) * | 2007-09-11 | 2008-02-27 | 西安交通大学 | Method for recycling silica powder and carborundum powder from cut waste mortar |
| CN102079520A (en) * | 2011-01-12 | 2011-06-01 | 虹京环保有限公司 | Recycling method of silicon carbide |
| CN101033066B (en) * | 2006-03-06 | 2011-06-22 | 张捷平 | Method of recovering silicon carbide micro-powder |
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| CN101033066B (en) * | 2006-03-06 | 2011-06-22 | 张捷平 | Method of recovering silicon carbide micro-powder |
| CN101113029A (en) * | 2006-07-26 | 2008-01-30 | 金柏林 | Treatment recovery method for monocrystalline silicon cutting waste liquor |
| CN101130237A (en) * | 2007-09-11 | 2008-02-27 | 西安交通大学 | Method for recycling silica powder and carborundum powder from cut waste mortar |
| CN102079520A (en) * | 2011-01-12 | 2011-06-01 | 虹京环保有限公司 | Recycling method of silicon carbide |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103303924A (en) * | 2013-06-25 | 2013-09-18 | 佳明新材料科技有限公司 | Silicon carbide micropowder recycling process flow |
| CN109553104A (en) * | 2017-09-27 | 2019-04-02 | 东莞新科技术研究开发有限公司 | The recovery method of silicon carbide in grinding waste slurry |
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Application publication date: 20130410 |