CN104634641B - Method for separating and purifying quartz in soldering flux or coating - Google Patents
Method for separating and purifying quartz in soldering flux or coating Download PDFInfo
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- CN104634641B CN104634641B CN201510095695.0A CN201510095695A CN104634641B CN 104634641 B CN104634641 B CN 104634641B CN 201510095695 A CN201510095695 A CN 201510095695A CN 104634641 B CN104634641 B CN 104634641B
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Abstract
The invention discloses a method for separating and purifying quartz in a soldering flux or coating. The method comprises the steps of highly enriching the low-content quartz while mineral impurities (especially, fluorite) are decomposed by feeding boric acid, hydrochloric acid and nitric acid; when ferrosilicon exists in the material, separating the ferrosilicon out, namely, selectively separating the ferrosilicon out by hydrofluoric acid in a nitric acid medium under the protection of boric acid to provide a good condition for the further purification of the quartz; after that, repeatedly treating a sample containing the enriched quartz by concentrated phosphoric acid to obtain the quartz with high purity. According to the method, the quartz is protected from being decomposed by feeding the boric acid; the fluorite and the ferrosilicon with relatively high proportion in the soldering flux or the coating are removed in advance, the fluoboric acid is formed by the boric acid and hydrogen fluoride (HF) produced in a reaction of the fluorite and the hydrochloric acid as well as HF which is fed at the later period and is used for dissolving the ferrosilicon, and the ferrosilicon can be selectively dissolved by the fluoboric acid, so that the quartz is reserved. The purity of the separated and purified quartz is more than 99%.
Description
Technical field
The present invention relates to a kind of Separation ＆ Purification method and technology field of chemical substance, more particularly to a kind of solder flux or medicine
The Separation ＆ Purification method of quartz in skin.
Background technology
Quartz is widely used in solder flux or coating material, it is mainly used as stabilising arc and slag making, its addition must be controlled strictly
System, the material composition for separating and purifying solder flux or the quartz in coating to research welding material is of crucial importance.In solder flux or coating
Containing fluorite, magnesia, corundum, marble, wollastonite, quartz, feldspar, Antaciron, ilmenite, iron powder, manganese powder, nickel powder, chromium
The material such as ferroalloy and waterglass.Because quartz content is often relatively low, the separation of quartz, purification difficulty are big, because SPA point
Phosphoric acid generates hydrofluoric acid with fluorite reaction during solution, and hydrofluoric acid can decompose quartz；Simultaneously phosphoric acid is difficult to dissolve Antaciron, right
Quartz purification also can have a negative impact.
For this purpose, present invention boric acid-hydrochloric acid-nitric acid is previously isolated from other mineral matters such as fluorite and alloy from source
Fall, because boric acid defines more stable complex compound with fluorine in pretreatment, enable the safe reservation of quartz.Moreover, weld
Magnesia, marble, wollastonite and some alloys in agent, coating is all dissolved and separates, and enables the quartz richness that content is few
Collection, in order that technique has preferable operability, accuracy and validity, by sampling amount 100g is not less than.With hydrofluoric acid in boric acid
Under protection, selective dissolution falls Antaciron and also provides strong guarantee for quartz purification.
The content of the invention
It is an object of the invention to provide a kind of process for separating and purifying method quartzy in solder flux or coating, by adding boron
Acid-hydrochloric acid-nitric acid enables the quartz of low content highly enriched, when in material while the impure minerals such as fluorite are decomposed
In the presence of having Antaciron, it is necessary to isolate the heavy part containing Antaciron, and under boric acid protection, with less in nitric acid medium
Amount hydrofluoric acid falls Antaciron selective dissolution, and further good condition is provided for quartz, then anti-with SPA
Sample is processed again, obtains highly purified quartz.
In order to reach above-mentioned technique effect, the present invention takes technical scheme below：
A kind of Separation ＆ Purification method of quartz in solder flux or coating, the method is comprised the following steps：
A, pretreatment：Solder flux or coating are weighed, the HCl solution dissolved with boric acid is added, is reacted away contained in solder flux or coating
Fluorite；
B, separate mineral matter and make quartzy enrichment：After the solution reaction of step A relaxes, nitric acid is added in heating, stirring
Under conditions of leach 0.5～1h, then filtering reacting liquid obtain filtrate and insoluble matter 1；
C, process insoluble matter 1：The treatment conditions of repeat step A of insoluble matter 1 and step B are obtained twice insoluble matter 2；
D, separation insoluble matter 2：Insoluble matter 2 in step C is transferred in potter's clay bowl, is sized mixing and is isolated light part and contain
The heavy part of Antaciron；
E, separate Antaciron and make quartzy enrichment：Weight containing Antaciron in step D is partly transferred in beaker,
Add boric acid and nitric acid and heating is completely dissolved boric acid, add HF anti-at interval of one section of set time after boric acid is completely dissolved
Antaciron should be decomposed, finally, add water dilution, clarification, filtering solution to obtain insoluble slag after waiting Antaciron to decompose；
Sample after F, preparation enrichment quartz：Light part in step D is merged with the insoluble slag in step E, Ran Houxi
Wash, filter, drying the sample obtained after enrichment quartz；
G, dissolve residual impurities and purify quartzy sample：First soaked the sample after quartz is enriched with step F with nitric acid, so
The impurity of remaining in SPA and heating for dissolving quartz sample is added afterwards, heating is stopped when phosphoric acid white cigarette is emitted, be allowed to cool, plus
Enter water dilution, clarification, discard filtrate, collect precipitation, the precipitation collected is repeated into aforementioned SPA treatment conditions twice, Ran Houzai
Wash with water, filter, drying precipitation, that is, obtaining the quartz for purifying.
Further technical scheme, HCl solution described in step A is concentrated hydrochloric acid and water by volume 1:1 mixes.
Further technical scheme, the potter's clay bowl is the acidproof potter's clay bowl of inner wall coarse.
Further technical scheme, the sample after the several 5 times of enrichments quartz of the volume described in step G used by SPA
Quality.
Step A adds the HCl solution dissolved with boric acid in solder flux or coating when pre-processing, be for the handle from source
Other mineral matters such as fluorite are previously isolated from, because boric acid can form more stable complex compound with fluorine, enable quartz safety
Retain.Then in stepb addition nitric acid can be the magnesia in solder flux or coating, marble, wollastonite and some alloys all
Separated and dissolved is fallen, and the quartz for enabling content few is enriched with.HF is added to be in order to remove Antaciron, because HF in step E
First fluoboric acid is formed with acid reaction, fluoboric acid optionally can dissolve Antaciron and quartz is preserved.
The potter's clay bowl is the acidproof potter's clay bowl of inner wall coarse, is because that the acidproof potter's clay bowl of inner wall coarse can be well
The heavy part containing Antaciron in material is isolated, and itself will not be eroded by diluted acid, to the quartzy sample of reaction purification not
Can have a negative impact.
The present invention compared with prior art, with following beneficial effect：
1st, solder flux or the fluorine in coating can be anticipated, prevents from forming Reaction Separations of the HF to quartz；
2nd, the impurity such as Antaciron can well be dissolved on the basis of quartz is not affected；
3rd, the quartzy purity of separating-purifying is more than 99%.
Specific embodiment
With reference to embodiments of the invention, the invention will be further elaborated.
Embodiment 1：
1st, 250ml concentrated hydrochloric acid solutions are measured and the 250ml aqueous solution is made into 1:1 HCl solution 500ml, then weighs
100.0g boric acid adds stand-by after dissolving in HCl solution；
2nd, weigh 100.0g solder flux or coating, add 500ml dissolved with the HCl solution of 100.0g boric acid, react away solder flux or
Contained fluorite in coating, after question response relaxes, adds 50ml nitration acid heats to boil solution and 1h, mistake is leached under conditions of stirring
Filter reactant liquor collects sediment；
3rd, in the sediment circulating repetition step 2 collected step 2 plus HCl solution and nitric acid treatment process mistake afterwards twice
Insoluble matter is collected in filter；
4th, the insoluble matter that step 3 is collected is transferred in the acidproof potter's clay bowl of inner wall coarse, light part is isolated after sizing mixing
With the heavy part containing Antaciron；
5th, the weight containing Antaciron in step 4 is partly transferred in beaker, adds 5.0g boric acid and 50ml nitric acid simultaneously
Heating is completely dissolved boric acid, and 2mlHF is added at interval of 10min after boric acid is completely dissolved, and 5 HF are added altogether, finally, waits silicon
Ferroalloy adds water dilution, clarification, filtering solution to obtain insoluble slag after having decomposed；
6th, the insoluble slag in the light part and step 5 in step 4 is merged, then washes with water, filters, drying and obtain richness
Sample after collection quartz；
7th, with appropriate nitric acid first the sample wetting being enriched with step 6 after quartz, then by liquid-solid ratio 5:1 adds dense phosphorus
Acid, the impurity of remaining, heating is stopped when phosphoric acid white cigarette is emitted in heating for dissolving quartz sample, allows its natural cooling, is added
The dilution of 1000ml water, clarification, discard filtrate and collect precipitation, and the precipitation of collection is repeated into the aforementioned SPA treatment conditions two of this step
It is secondary, be then washed with water and wash, filter, drying precipitation, that is, obtain the quartz for purifying.
Quartzy purity after separation, purification adopts hydrofluoric acid, hydrochloric acid, the molten sample of perchloric acid, and inductively coupled plasma is former
Sub- emission spectrometer (ICP-AES) is surveyed the method for solution impurity and carries out test analysis, the quartzy purity data after being purified
As a result table, as shown in table 1.
Table 1：Quartzy purity testing result data table after purification
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this
Bright preferably embodiment, embodiments of the present invention are simultaneously not restricted to the described embodiments, it should be appreciated that people in the art
Member can be designed that a lot of other modification and embodiment, and these modifications and embodiment will fall in principle disclosed in the present application
Within scope and spirit.
Claims (5)
1. in a kind of solder flux or coating quartz Separation ＆ Purification method, it is characterised in that the method is comprised the following steps：
A, pretreatment：Solder flux or coating are weighed, the HCl solution dissolved with boric acid is added, firefly contained in solder flux or coating is reacted away
Stone；
B, separate mineral matter and make quartzy enrichment：After the solution reaction of step A relaxes, nitric acid is added in heating, the bar of stirring
0.5～1h of solution is leached under part, then filtering reacting liquid obtains filtrate and insoluble matter 1；
C, process insoluble matter 1：The treatment conditions of repeat step A of insoluble matter 1 and step B are obtained twice insoluble matter 2；
D, separation insoluble matter 2：Insoluble matter 2 in step C is transferred in potter's clay bowl, is sized mixing and is isolated light part and contain ferrosilicon
The heavy part of alloy；
E, separate Antaciron and make quartzy enrichment：Weight containing Antaciron in step D is partly transferred in beaker, is added
Boric acid and nitric acid and heating is completely dissolved boric acid, HF reactions point are added after boric acid is completely dissolved at interval of one section of set time
Solution Antaciron, finally, adds water dilution, clarification, filtering solution to obtain insoluble slag after waiting Antaciron to decompose；
Sample after F, preparation enrichment quartz：Light part in step D is merged with the insoluble slag in step E, is washed out, mistake
Filter, drying obtain being enriched with the sample after quartz；
G, dissolve residual impurities and purify quartzy sample：With nitric acid first the sample wetting being enriched with step F after quartz, Ran Houjia
Enter the impurity of remaining in SPA and heating for dissolving quartz sample, heating is stopped when phosphoric acid white cigarette is emitted, be allowed to cool, add water
Dilution, clarification, discard filtrate, collect precipitation, the precipitation collected is repeated into aforementioned SPA treatment conditions and uses water again twice, then
Washing, filtration, drying precipitation, that is, obtain the quartz for purifying.
2. in a kind of solder flux according to claim 1 or coating quartz Separation ＆ Purification method, it is characterised in that：Step
HCl solution described in A is concentrated hydrochloric acid and water by volume 1:1 mixes.
3. in a kind of solder flux according to claim 1 or coating quartz Separation ＆ Purification method, it is characterised in that：It is described
Potter's clay bowl is the acidproof potter's clay bowl of inner wall coarse.
4. in a kind of solder flux according to claim 1 or coating quartz Separation ＆ Purification method, it is characterised in that：Step
The ratio of sample mass of the addition of SPA described in G with enrichment after quartzy is liquid-solid ratio 5:1.
5. in a kind of solder flux according to claim 1 or coating quartz Separation ＆ Purification method, it is characterised in that：Step
The quartzy purity purified described in G is more than 99%.
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| CN201510095695.0A CN104634641B (en) | 2015-03-04 | 2015-03-04 | Method for separating and purifying quartz in soldering flux or coating |
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| CN104634641B true CN104634641B (en) | 2017-05-10 |
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| CN115888975A (en) * | 2021-09-30 | 2023-04-04 | 深圳市考拉生态科技有限公司 | Preparation method and equipment for purifying quartz from secondary tungsten tailings |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555036A (en) * | 2008-04-07 | 2009-10-14 | 微宏科技（湖州）有限公司 | Method for extracting TiO 2 and SiO 2 in blast furnace slag |
| CN102424393A (en) * | 2011-09-19 | 2012-04-25 | 江苏大学 | Method for synchronously removing multiple impurities from quartz sand |
| CN102621030A (en) * | 2012-03-31 | 2012-08-01 | 武汉钢铁(集团)公司 | Method for determining silicon dioxide in limestone and dolomite by using gravimetric method |
| CN103323451A (en) * | 2013-06-08 | 2013-09-25 | 四川汉龙新材料有限公司 | Determination method of marble and fluorite content in electrode coating |
-
2015
- 2015-03-04 CN CN201510095695.0A patent/CN104634641B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555036A (en) * | 2008-04-07 | 2009-10-14 | 微宏科技（湖州）有限公司 | Method for extracting TiO 2 and SiO 2 in blast furnace slag |
| CN102424393A (en) * | 2011-09-19 | 2012-04-25 | 江苏大学 | Method for synchronously removing multiple impurities from quartz sand |
| CN102621030A (en) * | 2012-03-31 | 2012-08-01 | 武汉钢铁(集团)公司 | Method for determining silicon dioxide in limestone and dolomite by using gravimetric method |
| CN103323451A (en) * | 2013-06-08 | 2013-09-25 | 四川汉龙新材料有限公司 | Determination method of marble and fluorite content in electrode coating |
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Address after: Pixian 610000 Sichuan Province, Chengdu city Chengdu Modern Industrial Avenue North New Area of North Sichuan section of No. 356 Applicant after: Sichuan West metallurgy new material Limited by Share Ltd Address before: Pixian 610000 Sichuan Province, Chengdu city Chengdu Modern Industrial Avenue North New Area of North Sichuan section of No. 356 Applicant before: SICHUAN XIYE NEW MATERIAL CO., LTD. |
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