CN105253891A - Method for removing gas-liquid inclusion in quartz sand by using microwave bursting method - Google Patents
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- CN105253891A CN105253891A CN201510743301.8A CN201510743301A CN105253891A CN 105253891 A CN105253891 A CN 105253891A CN 201510743301 A CN201510743301 A CN 201510743301A CN 105253891 A CN105253891 A CN 105253891A
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Abstract
The invention discloses a method for removing gas-liquid inclusion in quartz sand by using a microwave bursting method. Microwave power is the most significant factor which can affect the removal effect of the gas-liquid inclusion in quartz sand, and the scientific and precise method comprises the following steps: putting primarily purified quartz sand in microwave radiation of which the microwave power is 2100-2700w, and treating for 1-3 hours when the temperature of microwave treatment is kept being 700-900 DEGC. A great number of tests show that the gas-liquid inclusion removal effect of a quartz sand material treated by using the method disclosed by the invention is good, gas-liquid inclusion can be even completely removed, and the high-purity quartz sand can meet the requirement of being a crystal substitute product. The method is good in environmental friendliness, simple to operate, stable and reliable in process and applicable to industrial large-scale production.
Description
Technical field
The present invention relates to quartz sand technical field of purification, more specifically, relates to the processing method that a kind of microwave decrepitation method removes gas liquid inclusion in quartz sand.
Background technology
Along with developing rapidly of high-tech area, particularly in the development of aeronautical technology, nuclear power industry and electronic industry, more and more higher to the requirement of silica glass material purity.The demand adapting to these fields is exploited in highly purified mineral crystal ore deposit in large quantities.But along with petering out of mineral crystal resource, impel people to explore new raw material of quartz glass mineral and substitute mineral crystal.In late 1970s, developed country starts to explore the road replacing crystal ore deposit with common quartz mine.To the nineties in 20th century, the common quartz such as Kemmochi is processed into the raw material powder of high-grade silica glass.And China's research is in this respect started late, technology is backwardness relatively, and quartz raw material purity is not high, therefore makes great efforts the purity improving quartz sand, has become the important topic in China's industry.
Compared with mineral crystal, except containing except a large amount of impurity in quartz mine, also containing a large amount of gas liquid inclusions.After preliminary impurity cleaning, most impurity is removed, but part gas liquid inclusion also exists, and does not also reach the purity demand of high-tech area.The method of current raising quartz sand material purity mainly adopts difference of corrosion method and thermal spalling method, but removal effect is limited, and complex operation.Report according to data: quartz sand has the selectivity of its uniqueness by microwave heating, this is because the material that specific inductivity is large heats up little faster than specific inductivity, the specific inductivity of silicon-dioxide is less than the specific inductivity of water, during microwave heating, water molecules in gas liquid inclusion produces very large pressure at interface, inclusion is burst, reaches the object removing gas liquid inclusion.The Chinese patent application being 201110040475.X as number of patent application provides gas liquid inclusion and Impurity removal method in the production of a kind of glass sand, quartz sand is placed in microwave field, microwave frequency range is 300MHz ~ 300GHz, gas liquid inclusion and impurity is made to be heated rapid temperature increases to more than 1000 DEG C (more high better) by selectivity, be incubated 2 ~ 30 minutes, then cool rapidly, then quartz sand is applied plus load, destroy gas liquid inclusion or impurity is peeled off, poor effect.This can only prove that the method for the gas liquid inclusion using microwave decrepitation method to remove in quartz sand is feasible, be devoted for years to based on the applicant and study in quartz sand purifying, find that treatment process condition nuance all may cause huge purification effect difference, so be necessary to seek accurate microwave processes that is more stable, better effects if, the purifying for quartz sand provides the technical guarantee that can actually apply.
Summary of the invention
The technical problem that the present invention will solve is not enough for existing quartz sand purification technique, especially removes the deficiency of gas liquid inclusion technical scheme in quartz sand for microwave decrepitation method, provides the processing method of gas liquid inclusion in a kind of efficient removal quartz sand.
Goal of the invention of the present invention is achieved by the following technical programs:
The invention provides the processing method that a kind of microwave decrepitation method removes gas liquid inclusion in quartz sand, that the quartz sand of preliminary purification to be placed in microwave power be 2100 ~ 2700w microwave radiation, during maintenance microwave treatment, temperature is 700 ~ 900 DEG C simultaneously, time is process under the condition of 1 ~ 3h, and the quartz sand of described preliminary purification is the quartz sand material of preliminary purification.
The quartz sand of described preliminary purification utilizes existing traditional technology to be obtained through thick broken, sorting, calcining, screening by quartz mine.Described quartz mine is the gas liquid inclusion being rich in water, and namely in described gas liquid inclusion, liquid component is mainly the quartz mine of water.
Preferably, the quartz sand of described preliminary purification is the quartz sand material through preliminary purification.
The most preferred scheme of the present invention is that the quartz sand of preliminary purification to be placed in microwave power be 2400w microwave radiation, and when keeping microwave treatment, temperature is 800 DEG C simultaneously, and the time is process under the condition of 1h.
The present invention provides simultaneously and prepares the good glass sand of gas liquid inclusion removal effect based on described processing method.
Beneficial effect of the present invention:
The present invention is directed to the deficiency of existing quartz sand purification technique, especially remove for microwave decrepitation method the deficiency that quartz sand gas liquid inclusion removes technology, provide a kind of simple, efficient, stable microwave decrepitation method efficiently to remove the processing method of gas liquid inclusion in quartz sand.
Studying for a long period of time, combination on basis is creative to be analyzed, and the applicant sums up and obtains, and quartz sand sample is after microwave treatment, and different microwave conditions is different to the effect removing gas liquid inclusion.Be 2400w in conjunction with lot of experiments determination microwave power of the present invention, holding temperature is 800 DEG C, and it is best that soaking time is that the condition of 1h removes gas liquid inclusion effect.Its reason is:
In microwave field, the hydroxy water in quartz sand and the material in gas liquid inclusion there occurs reaction.Existing Research Literature shows: the existence form of proton in quartz sand has following several form:
（1）≡S
i-OH;
（2）≡S
i-H;
（3）HO-OH;
(4) H
2o and H
2.
Hydrogen molecule and water great majority are present in quartz sand in gas liquid inclusion with physical form, and its mechanism is:
（1）S
iO
2+H
2→S
iO+H
2O;
（2）HO-OH+S
iO→≡S
i-OH+H
2O;
（3）≡S
i-OH+≡S
i-H→≡S
i-S
i≡+H
2O;
（4）≡S
i-OH+≡S
i-H→S
i-O-S
i+H
2。
Reaction occurs along with the change of temperature, and while reaction occurs, alpha-quartz sand is transformed into β-quartz sand, and its lattice passage increases, and the water that reaction is formed can be assembled along passage, forms the inclusion varied in size.And the climbing speed of temperature and the height of temperature affect very large on the removal of water molecules.The specific inductivity of silicon-dioxide is much smaller than water, and containing a large amount of water in gas liquid inclusion, temperature rises fast, and water is constantly vaporized, and makes in whole inclusion system entropy increase, reacts continuous forward to carry out; Also make to produce very big pressure in gas liquid inclusion, burst at quartz sand surface, along with the discharge of gas, inclusion crackle slowly heals again.Thus under microwave action, remove inclusion in quartz sand crystal and hydroxy water has certain effect.Key is to determine best microwave power, holding temperature and soaking time, ensures that reaction reaches the required condition point removing inclusion and hydroxy water.
The present invention is summed up best microwave power, holding temperature and soaking time and is verified further by orthogonal experiment, the quartz sand gas liquid inclusion removal effect processing gained under present invention process condition is stable and best, can reach basic removal, gained glass sand meets the requirement as crystal ore deposit substitute.Present invention process environmental friendliness, simple to operate, process stabilizing is reliable, is applicable to industrialized production.
Accompanying drawing explanation
Quartz sand sample infrared spectrogram before and after Fig. 1 process.
Figure 21 sample polarized light microscopy figure.
Figure 32 sample polarized light microscopy figure.
Figure 43 sample polarized light microscopy figure.
Figure 54 sample polarized light microscopy figure.
Figure 65 sample polarized light microscopy figure.
Figure 76 sample polarized light microscopy figure.
Figure 87 sample polarized light microscopy figure.
Figure 98 sample polarized light microscopy figure.
Figure 109 sample polarized light microscopy figure.
Figure 111 No. 0 sample polarized light microscopy figure.
Figure 12 is without microwave treatment quartz sand and sample 2 thermogravimetric analysis figure.
Figure 13 is without the X diffractogram of microwave treatment quartz sand and sample 2.
Embodiment
The present invention is further described below in conjunction with the drawings and specific embodiments.For convenience of description, reagent, instrument and equipment etc. that the following embodiment of the present invention adopts exemplify as follows, but therefore do not limit the present invention, other reagent, instrument, equipment and method unless stated otherwise, the reagent all used with reference to this area routine, instrument, equipment and method.
Main raw material: the quartz sand powder that Nanjing produces.
Laboratory apparatus and equipment: RWS microwave Multi-function experimental stove (Zhong Sheng heat energy company limited of Hunan Province), quartz crucible with cover, electronic balance, loft drier, Fourier infrared spectrograph, Leica polarizing microscope is seen, X-ray diffractometer, thermogravimetric analyzer, inductive coupling plasma emission spectrograph, 721 spectrophotometers.
Sample characterization: adopt Fourier infrared spectrograph to observe the content of water molecules in quartzy sand sample gas liquid inclusion; With the change of the microscopic morphology of gas liquid inclusion in the quartzy sand sample of Leica polarized light microscope observing after microwave acid dipping process; Thermogravimetric analyzer and X-ray diffractometer is adopted to analyze the crystal formation of quartz sand sample.
Embodiment 1
Quartz sand powder being placed in microwave power is 2400w microwave radiation, and during maintenance microwave treatment, temperature is 800 DEG C simultaneously, and the time is process under the condition of 1h.
Embodiment 2
Quartz sand powder being placed in microwave power is 2400w microwave radiation, and during maintenance microwave treatment, temperature is 700 DEG C simultaneously, and the time is process under the condition of 2h.
Embodiment 3
Quartz sand powder being placed in microwave power is 2100w microwave radiation, and during maintenance microwave treatment, temperature is 800 DEG C simultaneously, and the time is process under the condition of 3h.
Embodiment 4
Quartz sand powder being placed in microwave power is 2700w microwave radiation, and during maintenance microwave treatment, temperature is 800 DEG C simultaneously, and the time is process under the condition of 2h.
Embodiment 5
Quartz sand powder being placed in microwave power is 2700w microwave radiation, and during maintenance microwave treatment, temperature is 900 DEG C simultaneously, and the time is process under the condition of 1h.
Embodiment 6
Quartz sand powder being placed in microwave power is 2700w microwave radiation, and during maintenance microwave treatment, temperature is 700 DEG C simultaneously, and the time is process under the condition of 3h.
Embodiment 7
Quartz sand powder being placed in microwave power is 2400w microwave radiation, and during maintenance microwave treatment, temperature is 900 DEG C simultaneously, and the time is process under the condition of 3h.
Embodiment 8
Quartz sand powder being placed in microwave power is 2100w microwave radiation, and during maintenance microwave treatment, temperature is 900 DEG C simultaneously, and the time is process under the condition of 2h.
Embodiment 9
Quartz sand powder being placed in microwave power is 2100w microwave radiation, and during maintenance microwave treatment, temperature is 700 DEG C simultaneously, and the time is process under the condition of 1h.
Embodiment 10 orthogonal test is verified
The present embodiment utilizes L9 (3
4) orthogonal table carry out gas liquid inclusion minimizing technology in quartz sand of the present invention orthogonal test checking.With microwave power, microwave treatment time, microwave treatment temperature be major influence factors A, B and C, select the Three factors-levels L9 (3 of orthogonal
3), verify by as shown in table 2:
Table 1 orthogonal test factor and level
| Level | A | B | C |
| 1 | 2100 | 1 | 700 |
| 2 | 2400 | 2 | 800 |
| 3 | 2700 | 3 | 900 |
Table 2 orthogonal design table
| Experiment numbers | A | B | C |
| 1 | 2100 | 1 | 700 |
| 2 | 2400 | 1 | 800 |
| 3 | 2700 | 1 | 900 |
| 4 | 2400 | 2 | 700 |
| 5 | 2700 | 2 | 800 |
| 6 | 2100 | 2 | 900 |
| 7 | 2700 | 3 | 700 |
| 8 | 2100 | 3 | 800 |
| 9 | 2400 | 3 | 900 |
Note: factor A is microwave power (W), factor B microwave treatment time (h), factor C microwave treatment temperature (DEG C).
Embodiment 11 examination and test of products
(1) under Fourier infrared spectrograph, undressed sample No. 10 samples (raw material is without microwave treatment quartz sand) and orthogonal test 1-9 sample are detected, as shown in Figure 1: as seen from Figure 1, at wave band 3000 ~ 3600cm
-1in scope, there is not infrared absorption peak in No. 2 samples substantially; And 1,3,4,5,7,8, No. 9 sample exists area and the intensity of infrared absorption peak, and be more or less the same with the absorption peak area of base-material and intensity, the absorption peak area of No. 6 samples and intensity maximum.It can thus be appreciated that: the effect of the removal gas liquid inclusion of No. 2 quartz sand samples is best.
(2) be the removal effect of gas liquid inclusion in further comparative sample, utilize Leica polarizing microscope to observe 1 ~ No. 9 sample and unprocessed quartz sand 10, as shown in Fig. 2 ~ 11, be followed successively by the polarisation figure that different quartz sand amplifies 500 times.Visible: No. 2 samples have few small volume gas liquid inclusion to exist, and the crackle on its surface substantially heals and entirety does not have atrament; 3,4,5, No. 9 samples have the gas liquid inclusion of a small amount of small volume and many little slight cracks, and its surface exists many cracks, has less atrament; Gas liquid inclusion containing a large amount of different volumes size in No. 10 base-materials, the crack on its surface is few, and there is a large amount of atraments on its surface; And 1,6,7, No. 8 sample surfaces has many cracks, all contain the gas liquid inclusion of a large amount of small volumes, and be distributed in around crack, there is less atrament on surface.The effect further illustrating the removal gas liquid inclusion of No. 2 quartz sand samples is best, and gained quartz sand quality is the highest.
(4) adopt thermogravimetric analyzer and X-ray diffractometer to analyze the crystal formation of quartz sand sample before and after microwave treatment, analytical results is distinguished as shown in Figure 12,13:
Figure 12 is the thermogravimetric analysis figure of quartz sand without microwave treatment and lower No. 2 samples of optimal conditions.As seen from Figure 12: the two has endotherm(ic)peak at about 500 DEG C; C place is significantly less than No. 2 without the temperature reaching baseline after the quartz sand weightlessness of microwave treatment; The steep of curve 1 is greater than curve 2; Both have endotherm(ic)peak after 1500 DEG C.Quartz sand curve 1 without microwave treatment is because containing a large amount of gas liquid inclusions in base-material, cause temperature rise rate to be accelerated; Because the particle of the existence of gas liquid inclusion and quartz sand is comparatively large, the temperature reaching baseline after causing quartz sand weightlessness is low.No. 2 curves of microwave treatment are because of sample through microwave treatment, and in quartz sand, gas liquid inclusion content is few, particle is little, and temperature rise rate is slower than 1 curve; Gas liquid inclusion reduces, and the temperature reaching baseline after quartz sand weightlessness is high.Known: quartz sand generation crystal conversion in microwave explosion process.
Figure 13 is the X diffractogram of quartz sand without microwave treatment and No. 2 samples.(in figure, 1 is without microwave treatment as seen from Figure 13; 2 is No. 2 that cross through microwave treatment): No. 2 samples are about 24.64 time, and two peak-to-peak values are little, and 54.64 time, peak value is little; Base-material is about 24.64 time, and two peak values are large, and 54.64 time, peak value is large; Two diffractograms just show difference in shape at diffraction peak number, angle position relative intensity order so that diffraction; By contrasting with standard map, illustrate that the former is β-quartz sand; No. 2 samples are ɑ-quartz sand.Further illustrate and change at microwave explosion process quartz sand crystal formation.This is because under microwave heating condition, in quartz sand, gas liquid inclusion explosion, makes quartz sand particle less; Also make the fracture of quartz sand crystal generation key, make to detach crystal with the hydroxy water of silica bound, cause the crystal habit of quartz sand to change; And base-material does not do microwave treatment, there is not any crystal conversion in crystal.
Claims (2)
1. a microwave decrepitation method removes the processing method of gas liquid inclusion in quartz sand, it is characterized in that, be that the quartz sand of preliminary purification to be placed in microwave power be 2100 ~ 2700w microwave radiation, when keeping microwave treatment, temperature is 700 ~ 900 DEG C simultaneously, and the time is process under the condition of 1 ~ 3h.
2. microwave decrepitation method removes the processing method of gas liquid inclusion in quartz sand according to claim 1, and it is characterized in that, the power of described microwave radiation processing is 2400w, and described microwave treatment temperature is 800 DEG C, and described microwave treatment time is 1h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112010317A (en) * | 2020-09-14 | 2020-12-01 | 昆明理工大学 | Method for purifying quartz sand by microwave-vacuum combined roasting |
| CN115872408A (en) * | 2022-10-19 | 2023-03-31 | 北京理工大学 | Quartz sand purification method based on thermal plasma jet |
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| JP2004210548A (en) * | 2002-12-26 | 2004-07-29 | Fujikura Ltd | Method of manufacturing quartz glass |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112010317A (en) * | 2020-09-14 | 2020-12-01 | 昆明理工大学 | Method for purifying quartz sand by microwave-vacuum combined roasting |
| CN115872408A (en) * | 2022-10-19 | 2023-03-31 | 北京理工大学 | Quartz sand purification method based on thermal plasma jet |
| CN115872408B (en) * | 2022-10-19 | 2023-08-11 | 北京理工大学 | Quartz sand purification method based on thermal plasma jet |
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