CN104150487B - A kind of purification process of high-purity silicon processing method - Google Patents

A kind of purification process of high-purity silicon processing method Download PDF

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CN104150487B
CN104150487B CN201410352717.2A CN201410352717A CN104150487B CN 104150487 B CN104150487 B CN 104150487B CN 201410352717 A CN201410352717 A CN 201410352717A CN 104150487 B CN104150487 B CN 104150487B
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hydrochloric acid
washing
purity silicon
processing method
acid solution
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CN104150487A (en
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张又红
陈舒鸣
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QICHUN KAIDI MINING MATERIALS Co Ltd
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QICHUN KAIDI MINING MATERIALS Co Ltd
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Abstract

The present invention relates to a kind of purification process of high-purity silicon processing method, be applied to China's materials processing and purify field.The present invention provides a kind of purification process of high-purity silicon processing method, and including crushing washing and two steps of pickling, adopting hydrochloric acid vapour is that 1-5cm quartz granule reacts purification to particle diameter, SiO in the quartz after purification processes2Purity higher, the method technique is simple, shortens the response time, reduces hydrochloric acid and make consumption, it is adaptable to industrialized production.

Description

A kind of purification process of high-purity silicon processing method
Technical field
The present invention relates to a kind of purification process of high-purity silicon processing method, the present invention relates to a kind of purification process of high-purity silicon processing method, be applied to China's materials processing and purify field.
Background technology
Quartz is a kind of mineral of most study most commonly seen in the earth's crust, and chemical composition is mainly SiO2, submember is Al2O3·Fe2O3, MgO, CaO NaCO K2The compositions such as O, therefore mix SiO at quartz crystallization process2Impurity component in addition, has severely impacted the application in our high-end technology.Tradition purifies the method for quartz and there is salt acid consumption greatly, about the one week problem such as time and length consuming time of reaction needed.
Summary of the invention
For the weak point existed in the problems referred to above, the present invention provides a kind of purification process of high-purity silicon processing method, SiO in the quartz after purification processes2Purity higher, the method technique is simple, shortens the response time, reduces hydrochloric acid and make consumption, it is adaptable to industrialized production.
The present invention provides a kind of purification process of high-purity silicon processing method, it is characterised in that comprise the following steps:
Step 1, crushing washing, first the quartz raw ore material after screening is crushed, after broken, the diameter of material is 1-5, the material input material washing machine after broken is carried out upset friction, injects pure water;
Step 2, pickling, material after broken washing is loaded reaction vessel, shut reaction vessel lid, the water vapour injecting 170 degrees Celsius in container is heated process, stop when container center temperature reaches 120 degrees Celsius supplying gas, whole reaction unit is placed under room temperature, in reaction vessel, hydrochloric acid solution is injected by pipeline, the mass ratio crushing the material after washing and hydrochloric acid solution in container is 100:1, hydrochloric acid solution volatilizees in the container of 120 degrees Celsius and produces hydrochloric acid vapour, material is fumigated four hours with hydrochloric acid vapour, reclaim hydrochloric acid, reaction was injected 1 st pure water at interval of one hour after terminating and is carried out reacted material spraying washing, carry out 6 washings altogether, take out the material after washing, HIGH-PURITY SILICON after being purified.
Described a kind of purification process of high-purity silicon processing method, it is characterised in that described hydrochloric acid solution mass fraction is 36%.
Described a kind of purification process of high-purity silicon processing method, it is characterised in that described material washing machine material is cast steel;The reaction vessel material that described pickling uses is PE plastics.
The invention have the benefit that
1, the present invention is simple to operate, can effectively remove the elements such as ferrum in quartz, aluminum, sodium, titanium, potassium, calcium, and refining effect is good, it is adaptable to industrialized production;
2, the present invention uses the high temp. salt acid vapour impurity to remove in quartz, and the use of high temp. salt acid vapour accelerates reaction process, shortens the response time, and what decrease hydrochloric acid solution makes consumption simultaneously.
3, the reaction vessel material that pickling of the present invention uses is PE plastics, and this Materials Inorganic thing composition is extremely low and quartz is pollution-free.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is described in further detail.But example is not as a limitation of the invention.
Embodiment 1
The quartz of the HIGH-PURITY SILICON after screening is crushed through disintegrating machine, 5-10, crush building stones to put in the material washing machine that cast steel is made and repeatedly rub, injected clear water is stirred, remove raw ore attachment, the water of dirt of draining, it is repeatedly performed several times, until quartz surface free from admixture, earth flows out till clear water until material washing machine.
The material broken washing completed loads in the reaction vessel that PE plastics are made, by seal of vessel, the water vapour injecting 170 degrees Celsius is heated process, stop when the temperature at center reaches 120 degrees Celsius supplying gas, whole reaction unit is placed under room temperature, in reaction vessel, hydrochloric acid solution is injected by pipeline, the mass ratio crushing the material after washing and hydrochloric acid solution in container is 100:1, hydrochloric acid solution volatilizees in the container of 120 degrees Celsius and produces hydrochloric acid vapour, material is fumigated four hours with hydrochloric acid vapour, reclaim hydrochloric acid, reaction was injected 1 st pure water at interval of one hour after terminating and is carried out reacted material spraying washing, carry out 6 washings altogether, take out the material after washing, HIGH-PURITY SILICON after being purified.By the HIGH-PURITY SILICON after comparing tcrude ore diamond stone and purifying it can be seen that the HIGH-PURITY SILICON after purifying by this method is cleaner, pure white, it was demonstrated that effectively removes the impurity in tcrude ore.
Embodiment 2
The quartz of the HIGH-PURITY SILICON after screening is crushed through disintegrating machine, 5-10, crush building stones to put in the material washing machine that cast steel is made and repeatedly rub, injected clear water is stirred, remove raw ore attachment, the water of dirt of draining, it is repeatedly performed several times, until quartz surface free from admixture, earth flows out till clear water until material washing machine.
The material broken washing completed loads in the reaction vessel that PE plastics are made, by seal of vessel, the water vapour injecting 170 degrees Celsius is heated process, stop when the temperature at center reaches 120 degrees Celsius supplying gas, whole reaction unit is placed under room temperature, in reaction vessel, hydrochloric acid solution is injected by pipeline, the mass ratio crushing the material after washing and hydrochloric acid solution in container is 100:1, hydrochloric acid solution volatilizees in the container of 120 degrees Celsius and produces hydrochloric acid vapour, material is fumigated four hours with hydrochloric acid vapour, reclaim hydrochloric acid, reaction was injected 1 st pure water at interval of one hour after terminating and is carried out reacted material spraying washing, carry out 6 washings altogether, take out the material after washing, HIGH-PURITY SILICON after being purified.HIGH-PURITY SILICON after tcrude ore diamond stone and purification is carried out impurity content mensuration respectively, the present embodiment Central Plains iron in ore, aluminum, sodium, titanium, potassium, calcium, magnesium element content respectively 36ppm, 45.6ppm, 22ppm, 8.3ppm, 12ppm, 5.2ppm, 3.5ppm, in the HIGH-PURITY SILICON after purification, above-mentioned impurity content is reduced to 18ppm, 22.6ppm, 12.7ppm, 3.2ppm, 6.5ppm, 1.2ppm, 2.1ppm.

Claims (2)

1. a purification process of high-purity silicon processing method, it is characterised in that comprise the following steps:
Step 1, crushing washing, first quartz raw ore material is crushed, the material diameter after broken is 1-5cm, the material input material washing machine after broken is carried out upset friction, injects pure water;
Step 2, pickling, material after broken washing is loaded reaction vessel, shut reaction vessel lid, the water vapour injecting 170 degrees Celsius in container is heated process, stops when container center temperature reaches 120 degrees Celsius supplying gas, and whole reaction unit is placed under room temperature, injecting hydrochloric acid solution by pipeline in reaction vessel, described hydrochloric acid solution mass fraction is 36%;The mass ratio crushing the material after washing and hydrochloric acid solution in container is 100:1, hydrochloric acid solution volatilizees in the container of 120 degrees Celsius and produces hydrochloric acid vapour, material is fumigated four hours with hydrochloric acid vapour, reclaim hydrochloric acid, reaction was injected 1 st pure water at interval of one hour after terminating and is carried out reacted material spraying washing, carry out 6 washings altogether, take out the material after washing, the HIGH-PURITY SILICON after being purified.
2. a kind of purification process of high-purity silicon processing method according to claim 1, it is characterised in that described material washing machine material is cast steel;The reaction vessel material that described pickling uses is PE plastics.
CN201410352717.2A 2014-07-22 2014-07-22 A kind of purification process of high-purity silicon processing method Active CN104150487B (en)

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CN108584962B (en) * 2018-07-19 2020-05-26 江苏斯力康科技有限公司 Acid steam prepurification metallic silicon process and surface purification equipment
CN111285376A (en) * 2020-04-15 2020-06-16 威海圆环先进陶瓷股份有限公司 Production process for preparing high-purity quartz powder
CN113247913A (en) * 2021-05-24 2021-08-13 曹永华 Quartz purification method for cocoa sea area

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