CN110002450A - The processing method that useless silicon mud recycles - Google Patents
The processing method that useless silicon mud recycles Download PDFInfo
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- CN110002450A CN110002450A CN201910027727.1A CN201910027727A CN110002450A CN 110002450 A CN110002450 A CN 110002450A CN 201910027727 A CN201910027727 A CN 201910027727A CN 110002450 A CN110002450 A CN 110002450A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Abstract
The invention discloses the processing method that a kind of useless silicon mud recycles, method is as follows: (1) useless silicon mud is successively placed in first reactive tank, second reactive tank, third reactive tank, fourth reactive tank and fiveth reactive tank in cleaned respectively, the processing step of magnetic separation, cleaning, pickling and cleaning；(2) the useless silicon mud for deriving from step (1) is mixed with the ratio of solid-to-liquid ratio 1:5~50 with deionized water and is tuned into mud, and dispersing agent is added and is dispersed；(3) mud of step (2) will be derived to spray into a reaction chamber with high pressure, in the reaction chamber, which forms silica dioxide granule through oxidation reaction；(4) particle for deriving from step (3) is collected with cyclone, the micron-sized silica powder of high-purity can be obtained；(5) powder that will derive from step (4) carries out grain size grading, can obtain epigranular and the high-purity silicon dioxide powder greater than 99%；In this way, the high-purity silicon dioxide powder can be widely used in industry filling material, useless silicon mud resource can be made to recycle.
Description
Technical field
It is the present invention relates to a kind of processing method that useless silicon mud recycles, in particular to a kind of that useless silicon mud is made after processing
High-purity silicon dioxide powder can be widely used in industry filling material.
Background technique
Currently, useless silicon mud source is that processing procedure generation, such useless silicon mud are cut or ground in semiconductor or solar wafer factory
It is general that without oily and silicon carbide is cut, liquid content is greater than 80%, and there are many methods for being recycled the silicon mud that gives up for industry, such as by
The dry silicon powder for forming low-purity of silicon mud, addition adhesive, it is re-compacted at being formed after silicon heavy stone used as an anchor or high-temperature fusion after evenly mixing
Silico briquette；Method of the invention is to provide a kind of new recovery technology, and the silicon-dioxide powdery purified can be applied to industrial filling
Material.
Summary of the invention
The main object of the present invention is to provide a kind of processing method that useless silicon mud recycles, and can be regenerated as useless silicon mud high-purity
Silicon-dioxide powdery is spent, industry filling material is can be widely used in and uses.
In order to achieve the above object, present invention employs following technological means:
The processing method that a kind of useless silicon mud of the invention recycles, comprising the following steps:
(1) by useless silicon mud be placed in carrier batch be placed in the first reactive tank in, this anti-first answer slot be ultrasonic rinse bath,
Its cleaning condition is 50~200KHz, and scavenging period is 5~15 minutes；Thereafter it is drawn off being placed in the second reactive tank and carries out magnetic
Choosing, magnetic separation time are 5~15 minutes, and the dispersing agent of 3~20%v/v, the dispersing agent is added in second reactive tank before magnetic separation
For alcohols；Thereafter it being drawn off being placed in third reactive tank again and be cleaned with deionized water, scavenging period is 5~15 minutes,
It is drawn off being placed in the 4th reactive tank again after cleaning and carries out pickling, pickling time is 5~15 minutes；Thereafter it is drawn off being placed in
It is cleaned again with deionized water in 5th reactive tank, scavenging period is 15~30 minutes；
(2) the useless silicon mud for deriving from step (1) is mixed with the ratio of solid-to-liquid ratio 1:5~50 with deionized water and is tuned into mud,
And an alcohols is added and is dispersed as dispersing agent, jitter time is 30 minutes or more；
(3) mud of step (2) will be derived to spray into a reaction chamber with high pressure, which is the atmosphere of controllable atmosphere
Furnace, the gas temperature in the atmosphere furnace are 1200 DEG C~1800 DEG C, and in the reaction chamber, which forms dioxy through oxidation reaction
Silicon carbide particle；
(4) particle for deriving from step (3) is collected with cyclone, the micron-sized silicon dioxide powder of high-purity can be obtained
Grain；
(5) powder that will derive from step (4) carries out grain size grading, can obtain epigranular and silicone content is high-purity greater than 99%
Spend silicon-dioxide powdery.
In the processing method that useless silicon mud of the present invention recycles, it is preferred that the silicone content of the useless silicon mud ingredient
It is 90% or more.
In the processing method that useless silicon mud of the present invention recycles, it is preferred that the sour agent of the pickling is inorganic acid, the acid
Agent is the pure phosphoric acid and 35%v/ of the pure hydrochloric acid of 25%v/v, the bright sulfur acid of 10%v/v, the pure nitric acid of 20%v/v, 10%v/v
The mixture of the deionized water of v.
In the processing method that useless silicon mud of the present invention recycles, it is preferred that the alcohols be methanol, ethyl alcohol, ethylene glycol,
One of diethylene glycol, polyethylene glycol, isopropanol or two or more mixtures.
The processing method that the useless silicon mud of the present invention recycles, wherein the gas in the atmosphere furnace is oxygen or air.
The processing method that the useless silicon mud of the present invention recycles, the advantage is that: can easily and rapidly be regenerated as useless silicon mud
High-purity silicon dioxide powder can be widely used in industry filling material and use, so that useless silicon mud is reached optimal recycling and recycle.
Detailed description of the invention
Fig. 1 show the flow chart of present invention method.
Fig. 2 show the parameter list of 1-4 of the embodiment of the present invention and comparative example.
Fig. 3 show the outside drawing of the resulting silicon-dioxide powdery of the embodiment of the present invention 1.
Fig. 4 show the X-ray diffraction crystalline phase figure of 1 gained silica of the embodiment of the present invention.
Specific embodiment
In relation to the present invention for up to above-mentioned use purpose and effect, used technological means is hereby enumerated preferably feasible
Embodiment, and cooperate shown in schema, details are as follows:
Produced by useless silicon mud source is semiconductor or solar wafer factory cut or grind processing procedure, silicone content therein is
90% or more, the processing method that useless silicon mud of the invention recycles, refering to Figure 1, itself the following steps are included:
(1) useless silicon mud carrier batch is placed in be placed in the first reactive tank, which is ultrasonic rinse bath,
Its cleaning condition is 50~200KHz, and scavenging period is 5~15 minutes；Thereafter it is drawn off being placed in the second reactive tank and carries out magnetic
Choosing, magnetic separation time are 5~15 minutes, and the dispersing agent of 3~20%v/v, the dispersing agent is added in second reactive tank before magnetic separation
For alcohols；Thereafter it being drawn off being placed in third reactive tank again and be cleaned with deionized water, scavenging period is 5~15 minutes,
It is drawn off being placed in the 4th reactive tank again after cleaning and carries out pickling, pickling time is 5~15 minutes, which is 25%v/v
Pure hydrochloric acid, the bright sulfur acid of 10%v/v, the pure nitric acid of 20%v/v, the pure phosphoric acid of 10%v/v and the deionized water of 35%v/v
Mixture；Thereafter it is drawn off being placed in the 5th reactive tank and be cleaned again with deionized water, scavenging period is 15~30 points
Clock；
(2) the useless silicon mud for deriving from step (1) is mixed with the ratio of solid-to-liquid ratio 1:5~50 with deionized water and is tuned into mud,
And an alcohols is added and is dispersed as dispersing agent, such as: methanol, ethyl alcohol, ethylene glycol, diethylene glycol, polyethylene glycol, isopropanol
One of them or two or more mixtures, jitter time are 30 minutes or more；
(3) mud of step (2) will be derived to spray into a reaction chamber with high pressure, which is the atmosphere of controllable atmosphere
Furnace, the gas in the atmosphere furnace can be oxygen or air, and the temperature of the gas is 1200 DEG C~1800 DEG C, in the reaction chamber,
The mud forms silica dioxide granule through oxidation reaction；
(4) particle for deriving from step (3) is collected with cyclone, obtains the micron-sized silica powder of high-purity
(as shown in Figure 3)；
(5) powder that will derive from step (4) carries out grain size grading, obtains epigranular and silicone content is high-purity greater than 99%
Spend silicon-dioxide powdery；
In this way, the high-purity silicon dioxide powder can be widely used in industry filling material.
The processing method that the useless silicon mud of the present invention recycles, embodiment is as follows, wherein the parameter of each embodiment is shown in Fig. 2:
Embodiment 1:
(1) useless silicon mud is placed in carrier and batch is placed in the first reactive tank, which is ultrasonic cleaning
Slot, cleaning condition are 50~200KHz, and scavenging period is 10 minutes；Thereafter it is drawn off being placed in the progress magnetic separation of the second reactive tank
10 minutes, the ethylene glycol of 10%v/v was first added as dispersing agent in the second reactive tank before magnetic separation；Thereafter it is drawn off being placed in third
It is cleaned in reactive tank and with deionized water, scavenging period is 10 minutes；Thereafter be drawn off being placed in the 4th reactive tank into
Row pickling 10 minutes, which was by 25%v/v pure hydrochloric acid, 10%v/v bright sulfur acid, the pure nitric acid of 20%v/v, the pure phosphorus of 10%v/v
The mixture of acid and 35%v/v deionized water composition；Thereafter be drawn off being placed in the 5th reactive tank again with deionized water into
Row cleaning 20 minutes；
(2) mud slurry of the useless silicon mud of step (1) with deionized water mixing preparation at solid-to-liquid ratio 1:50 will be derived from, and will be added
Enter ethylene glycol as dispersing agent, jitter time is 30 minutes or more；
(3) slurry is conveyed through heating zone by pumping the conveying speed with 25ml/min by the mud for deriving from step (2)
It after (1000 DEG C), is injected into pyroreaction room and is reacted, reacting indoor temperature is 1400 DEG C, reacts indoor gas
For air, the reaction time is 0.5 hour；
(4) the micron-sized silicon dioxide powder of high-purity can be obtained after collecting the reactant of step (2) via cyclone
Body, shape are circle, and average grain diameter is that (D50) is 54；
(5) powder that will derive from step (4) carries out grain size grading, obtains epigranular and silicone content is high-purity greater than 99%
Spend silicon-dioxide powdery.
The outside drawing and X-ray diffraction crystalline phase figure of resulting silicon-dioxide powdery are as shown in Figures 3 and 4.
Embodiment 2:
(1) useless silicon mud is placed in carrier and batch is placed in the first reactive tank, which is ultrasonic cleaning
Slot, cleaning condition are 50~200KHz, and scavenging period is 10 minutes；Thereafter it is drawn off being placed in the second reactive tank and carries out magnetic
It selects 10 minutes, the ethylene glycol of 10%v/v is added as dispersing agent in the second reactive tank before magnetic separation；Thereafter it is drawn off being placed in third
Cleaning 10 minutes is carried out with deionized water in reactive tank；Thereafter it is drawn off being placed in the 4th reactive tank and carry out pickling 10 minutes,
The acid agent be 25%v/v pure hydrochloric acid, 10%v/v bright sulfur acid, the pure nitric acid of 20%v/v, 10%v/v pure phosphoric acid and 35%v/v go from
The mixture of sub- water composition；Thereafter it is drawn off being placed in the 5th reactive tank again and cleaning 20 minutes is carried out with deionized water again；
(2) mud slurry of the useless silicon mud of step (1) with deionized water mixing preparation at solid-to-liquid ratio 1:40 will be derived from, and will be added
Enter ethylene glycol as dispersing agent, jitter time is 30 minutes or more；
(3) slurry is conveyed through heating zone by pumping the conveying speed with 25ml/min by the mud for deriving from step (2)
It after (1000 DEG C), is injected into pyroreaction room and is reacted, reacting indoor temperature is 1500 DEG C, reacts indoor gas
For oxygen, the reaction time is 0.5 hour；
(4) the micron-sized silicon dioxide powder of high-purity can be obtained after collecting the reactant of step (2) via cyclone
Body, shape are circle.Average grain diameter is that (D50) is 68；
(5) powder that will derive from step (4) carries out grain size grading, obtains epigranular and silicone content is high-purity greater than 99%
Spend silicon-dioxide powdery.
Embodiment 3:
(1) useless silicon mud is placed in carrier and batch is placed in the first reactive tank, which is ultrasonic cleaning
Slot, cleaning condition are 50~200KHz, and scavenging period is 10 minutes；Thereafter it is drawn off being placed in the second reactive tank and carries out magnetic
It selects 10 minutes, the ethylene glycol of 10%v/v is added as dispersing agent in the second reactive tank before magnetic separation；Thereafter it is drawn off being placed in third
Cleaning 10 minutes is carried out with deionized water in reactive tank；Thereafter it is drawn off being placed in the 4th reactive tank and carry out pickling 10 minutes,
The acid agent is inorganic acid, which is 25%v/v pure hydrochloric acid, 10%v/v bright sulfur acid, the pure nitric acid of 20%v/v, the pure phosphorus of 10%v/v
The mixture of acid and 35%v/v deionized water composition；Thereafter be drawn off being placed in the 5th reactive tank again again with deionized water into
Row cleaning 20 minutes；
(2) mud slurry of the useless silicon mud of step (1) with deionized water mixing preparation at solid-to-liquid ratio 1:20 will be derived from, and will be added
Enter ethylene glycol as dispersing agent, jitter time is 30 minutes or more；
(3) slurry is conveyed through heating zone by pumping the conveying speed with 25ml/min by the mud for deriving from step (2)
It after (1000 DEG C), is injected into pyroreaction room and is reacted, reacting indoor temperature is 1600 DEG C, and reacting indoor gas is
Oxygen, reaction time are 0.5 hour；
(4) the micron-sized silicon dioxide powder of high-purity can be obtained after collecting the reactant of step (2) via cyclone
Body, shape are circle, and average grain diameter is that (D50) is 75；
(5) powder that will derive from step (4) carries out grain size grading, obtains epigranular and silicone content is high-purity greater than 99%
Spend silicon-dioxide powdery.
Embodiment 4:
(1) useless silicon mud is placed in carrier and batch is placed in the first reactive tank, which is ultrasonic cleaning
Slot, cleaning condition are 50~200KHz, and scavenging period is 10 minutes；Thereafter it is drawn off being placed in the second reactive tank and carries out magnetic
It selects 10 minutes, the ethylene glycol of 10%v/v is added as dispersing agent in the second reactive tank before magnetic separation；Thereafter it is drawn off being placed in third
Cleaning 10 minutes is carried out with deionized water in reactive tank；Thereafter it is drawn off being placed in the 4th reactive tank and carry out pickling 10 minutes,
The acid agent be 25%v/v pure hydrochloric acid, 10%v/v bright sulfur acid, the pure nitric acid of 20%v/v, 10%v/v pure phosphoric acid and 35%v/v go from
The mixture of sub- water composition；Thereafter it is drawn off being placed in the 5th reactive tank again and cleaning 20 minutes is carried out with deionized water again；
(2) will step from the useless silicon mud of (1) and deionized water mixing preparation at the mud slurry of solid-to-liquid ratio 1:10, and add
Enter ethylene glycol as dispersing agent, jitter time is 30 minutes or more；
(3) slurry is conveyed through heating zone by pumping the conveying speed with 25ml/min by the mud for deriving from step (2)
It after (1000 DEG C), is injected into pyroreaction room and is reacted, reacting indoor temperature is 1700 DEG C, and reacting indoor gas is
Oxygen, reaction time are 0.5 hour；
(4) the micron-sized silicon dioxide powder of high-purity can be obtained after collecting the reactant of step (2) via cyclone
Body, shape are circle, and average grain diameter is that (D50) is 93；
(5) powder that will derive from step (4) carries out grain size grading, obtains epigranular and silicone content is high-purity greater than 99%
Spend silicon-dioxide powdery.
The processing method that useless silicon mud of the invention recycles, by the useless silicon mud of 90% or more silicone content, after first passing through cleaning
It is deployed into mud, then mud is spurted into high temperature reaction stove and is reacted, obtains high-purity (silicone content is greater than 99%) dioxy
SiClx powder can reduce manufacturing process, increase manufacturing speed and yield, the high-purity silicon dioxide powder can be widely used in work
Industry is filled material and is used, and useless silicon mud resource can be made to recycle, great environmental benefit.
Comparative example:
(1) useless silicon mud is placed in carrier and batch is placed in the first reactive tank, which is ultrasonic cleaning
Slot, cleaning condition are 50~200KHz, and scavenging period is 10 minutes；Thereafter it is drawn off being placed in the progress magnetic separation of the second reactive tank
10 minutes, the ethylene glycol of 10%v/v was first added as dispersing agent in the second reactive tank before magnetic separation；Thereafter it is drawn off being placed in third
It is cleaned in reactive tank and with deionized water, scavenging period is 10 minutes；Thereafter be drawn off being placed in the 4th reactive tank into
Row pickling 10 minutes, which was by 25%v/v pure hydrochloric acid, 10%v/v bright sulfur acid, the pure nitric acid of 20%v/v, the pure phosphorus of 10%v/v
The mixture of acid and 35%v/v deionized water composition；Thereafter be drawn off being placed in the 5th reactive tank again with deionized water into
Row cleaning 20 minutes；
(2) mud slurry of the useless silicon mud of step (1) with deionized water mixing preparation at solid-to-liquid ratio 1:50 will be derived from, and will be added
Enter ethylene glycol as dispersing agent, jitter time is 30 minutes or more；
(3) slurry is conveyed through heating zone by pumping the conveying speed with 25ml/min by the mud for deriving from step (2)
It after (1000 DEG C), is injected into pyroreaction room and is reacted, reacting indoor temperature is 500 DEG C, reacts indoor gas
For air, the reaction time is 0.5 hour；
(4) silicon-dioxide powdery can be obtained after collecting the reactant of step (2) via cyclone, shape is not advise
Lateral plate shape, average grain diameter are that (D50) is 19-128.
In conclusion the present invention has reached desired use purpose and effect really, and more ideal, real compared with the prior art
With, but, above-described embodiment is specifically described for presently preferred embodiments of the present invention, and the embodiment is not to limit
Fixed claim of the invention, it is such as other without departing from the equivalent change completed under disclosed technological means
With modification, it is intended to be limited solely by the claim that the present invention is covered.
Claims (4)
1. a kind of processing method that useless silicon mud recycles, which comprises the following steps:
(1) useless silicon mud is placed in carrier batch to be placed in the first reactive tank, anti-first to answer slot be ultrasonic rinse bath for this, clear
Washing condition is 50~200KHz, and scavenging period is 5~15 minutes；Thereafter it is drawn off being placed in the second reactive tank and carries out magnetic separation,
The magnetic separation time is 5~15 minutes, and the dispersing agent of 3~20%v/v is added in second reactive tank before magnetic separation, which is alcohol
Class；Thereafter it is drawn off being placed in third reactive tank again and be cleaned with deionized water, scavenging period is 5~15 minutes, cleaning
It is drawn off being placed in the 4th reactive tank again afterwards and carries out pickling, pickling time is 5~15 minutes；Thereafter it is drawn off being placed in the 5th
It is cleaned again with deionized water in reactive tank, scavenging period is 15~30 minutes；
(2) the useless silicon mud for deriving from step (1) is mixed with the ratio of solid-to-liquid ratio 1:5~50 with deionized water and is tuned into mud, and added
Enter an alcohols to be dispersed as dispersing agent, jitter time is 30 minutes or more；
(3) mud of step (2) will be derived to spray into a reaction chamber with high pressure, which is the atmosphere furnace of controllable atmosphere,
Gas temperature in the atmosphere furnace is 1200 DEG C~1800 DEG C, and in the reaction chamber, which forms titanium dioxide through oxidation reaction
Silicon particle；
(4) particle for deriving from step (3) is collected with cyclone, obtains the micron-sized silica powder of high-purity；
(5) powder that will derive from step (4) carries out grain size grading, obtains epigranular and high-purity two of the silicone content greater than 99%
Silica powder.
2. the processing method that useless silicon mud recycles as described in claim 1, which is characterized in that the sour agent of the pickling is inorganic
Acid, the acid agent be the pure hydrochloric acid of 25%v/v, the bright sulfur acid of 10%v/v, the pure nitric acid of 20%v/v, 10%v/v pure phosphoric acid with
And the mixture of the deionized water of 35%v/v.
3. the processing method that useless silicon mud recycles as described in claim 1, which is characterized in that the alcohols is methanol, ethyl alcohol, second
One of glycol, diethylene glycol, polyethylene glycol, isopropanol or two or more mixtures.
4. the processing method that useless silicon mud recycles as described in claim 1, which is characterized in that the gas in the atmosphere furnace is oxygen
Gas or air.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112919477A (en) * | 2021-03-12 | 2021-06-08 | 成信实业股份有限公司 | Silicon dioxide regeneration method of semiconductor waste silicon mud |
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| CN112919477B (en) * | 2021-03-12 | 2023-11-03 | 成信实业股份有限公司 | Silicon dioxide regeneration method of semiconductor waste silicon mud |
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