CN102275940B - Method for low-temperature hydrolysis of silicon tetrachloride - Google Patents
Method for low-temperature hydrolysis of silicon tetrachloride Download PDFInfo
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- CN102275940B CN102275940B CN 201110213568 CN201110213568A CN102275940B CN 102275940 B CN102275940 B CN 102275940B CN 201110213568 CN201110213568 CN 201110213568 CN 201110213568 A CN201110213568 A CN 201110213568A CN 102275940 B CN102275940 B CN 102275940B
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- silicon tetrachloride
- filtrate
- hydrolysis
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Abstract
The invention discloses a method for the low-temperature hydrolysis of silicon tetrachloride, which comprises: hydrolyzing gasified silicon tetrachloride; subjecting a mixture obtained after hydrolysis to pressure filtration; delivering filtrate to a hydrolysis tower, hydrolyzing silicon tetrachloride till the HCl mass concentration in the filtrate reaches 20 to 30 percent and obtaining hydrochloric acid; grinding filter cakes till there are not blocks; washing ground mixture with water and pulping; performing secondary pressure filtration, returning part of filtrate to the hydrolysis tower to hydrolyze the silicon tetrachloride, neutralizing the other part of filtrate and discharging the part of neutralized filtrate into a waste water tank; and drying and flashing the filter cakes obtained b secondary pressure filtration, and obtaining the final silicon dioxide product by cyclonic separation. In the invention, the equipment requirement is low, the energy consumption is low and pollution is little; the silicon tetrachloride is hydrolyzed more fully; the blockage of pipe lines due to silica gel accumulation and uncontrollable flow rate is avoided; and the service life of the equipment is prolonged.
Description
Technical field
The present invention relates to a kind of low temperature hydrolysis method of silicon tetrachloride.
Background technology
Silicon tetrachloride is the middle by product of production of polysilicon, and polysilicon is the needed main raw material of electronic industry and photovoltaic industry, and in the production of polysilicon, one ton of polysilicon of every production just needs to process 15 tons silicon tetrachloride, and treatment capacity is very large.Undressed silicon tetrachloride is a kind of chemical substance with severe corrosive, is heated or meets the water decomposition heat release, emits poisonous corrosive fume, and is very big to environmental hazard.
Along with the world and China's theCourse of PV Industry, the solar cell demand is increasing, and polysilicon output increases year by year, and environmental problem and resource utilization issue that silicon tetrachloride as by-product brings become increasingly conspicuous.There are not good solution and approach in industry all the time.The harmless treatment of silicon tetrachloride becomes one of bottleneck of restriction polysilicon development.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of low temperature hydrolysis method of silicon tetrachloride.
For solving the problems of the technologies described above, the technical solution used in the present invention may further comprise the steps:
(1) silicon tetrachloride liquid is joined in the vaporizer, with the silicon tetrachloride that the heat-conducting oil heating vaporizer obtains vaporizing, the temperature of described thermal oil is 170-190 ℃.
(2) silicon tetrachloride of described vaporization is passed into carry out bubbling hydrolysis under the liquid in the hydrolysis tower, liquid level is conveyed into the mixture after the hydrolysis in the surge tank at 2-3 rice in the mixture after obtaining being hydrolyzed, tower.
The hydrolysis tower drain pipe vertically enters surge tank.
(3) be transported to the one-level barrier film undercurrent pressure filter from surge tank with the mixture of pump after with described hydrolysis and carry out the press filtration first time, obtain filter cake and filtrate, described filtrate is delivered in the hydrolysis tower silicon tetrachloride is hydrolyzed, until the mass concentration of HCl reaches 20-30% in the gained filtrate, obtain hydrochloric acid.
(4) described filter cake being delivered to colloidal mill is ground to without block existence.
(5) mixture after grinding in the step (4) is conveyed into the water that adding 8-12 doubly measures in the making beating tank, the processing of washing, pull an oar.
(6) mixture after described washing, the making beating is delivered to secondary diaphragm undercurrent pressure filter and carries out the press filtration second time, obtain filter cake and filtrate, filtrate again joins hydrolysis tower silicon tetrachloride is hydrolyzed, the amount of filtrate that joins hydrolysis tower will make in the tower liquid level between 2-3 rice, residual filtrate be delivered in the neutralization tank and after drain into wastewater disposal basin.
(7) filter cake that the secondary press filtration is obtained is delivered to two blade dryers and carries out preliminarily dried, and drying machine adopts 170-190 ℃ heat-conducting oil heating, and be 15-45 minute time of drying, obtains the filter cake of preliminarily dried.
(8) filter cake of described preliminarily dried is conveyed into flash dryer and carries out drying treatment, until the filter cake temperature is 80-90 ℃, air outlet temperature is 70-80 ℃, obtains the silicon-dioxide raw product.
(9) described silicon-dioxide raw product is carried out cyclonic separation, obtain final silica product.
Cover made of plastic covers one-level barrier film undercurrent pressure filter, and only from bottom belt mouth air intake, the HCl that will overflow and chlorine hold up and takes away, carries out discharging after one-level washing, the secondary soda lye wash.
The beneficial effect that adopts technique scheme to produce is:
(1) silicon tetrachloride adopts low temperature hydrolysis technique, to equipment require lowly, energy consumption is low.
(2) bubbling hydrolysis and maintenance liquid level are 2-3 rice under the liquid, make hydrolyzing silicon tetrachloride more abundant.
(3) the present invention changes into hydrochloric acid and silicon-dioxide with the by product in the production of polysilicon, has reduced production cost.
(4) the hydrolysis tower drain pipe vertically enters surge tank, and line clogging and the flow having avoided silica gel to gather causing are uncontrollable.
(5) cover made of plastic covers pressure filter, and only from bottom belt mouth air intake, the HCl that will overflow and chlorine hold up and takes away, then by the one-level washing, through discharging after the secondary soda lye wash, can accomplish zero waste gas emission again, has reduced pollution.
(6) for the second time press filtration has reduced the content of hydrochloric acid in the silicon-dioxide, has both guaranteed the purity of product, has reduced again the corrosion to drying plant, has prolonged the work-ing life of the postorder equipment such as flash dryer.
Embodiment
Embodiment 1:
(1) silicon tetrachloride liquid is joined in the vaporizer silicon tetrachloride that obtains vaporizing with 170 ℃ heat-conducting oil heating vaporizers.
(2) silicon tetrachloride of vaporization is passed into carry out under the liquid bubbling hydrolysis in the hydrolysis tower, liquid level is put into surge tank at 2.5 meters with the mixture after the hydrolysis in the mixture after obtaining being hydrolyzed, tower.The hydrolysis tower drain pipe vertically enters surge tank.
(3) be transported in the one-level barrier film undercurrent pressure filter with the mixture of pump after with described hydrolysis and carry out the press filtration first time, obtain the good filter cake of press filtration and filtrate, described filtrate is delivered in the hydrolysis tower silicon tetrachloride is hydrolyzed, until the mass concentration of HCl reaches 25% in the gained filtrate, obtain hydrochloric acid.
(4) described filter cake being delivered to colloidal mill is ground to without block existence.
(5) mixture after grinding in the step (4) is conveyed into the water that adds 10 times of amounts in the making beating tank, the processing of washing, pull an oar.
(6) mixture after described washing, the making beating is delivered to secondary diaphragm undercurrent pressure filter and carries out the press filtration second time, obtain filter cake and filtrate, filtrate again joins hydrolysis tower silicon tetrachloride is hydrolyzed, the amount of filtrate that joins hydrolysis tower will make that liquid level is 2.5 meters in the tower, residual filtrate be delivered in the neutralization tank and after drain into wastewater disposal basin.
(7) filter cake that for the second time press filtration is obtained is delivered to two blade dryers and carries out preliminarily dried, and drying machine adopts 170 ℃ heat-conducting oil heating, and be 30 minutes time of drying, obtains the filter cake of preliminarily dried.
(8) filter cake of described preliminarily dried is conveyed into flash dryer and carries out drying treatment, until the filter cake temperature is 85 ℃, air outlet temperature is 75 ℃, obtains the silicon-dioxide raw product.
(9) described silicon-dioxide raw product is carried out cyclonic separation, obtain final silica product.
Cover made of plastic covers one-level barrier film undercurrent pressure filter, and only from bottom belt mouth air intake, the HCl that will overflow and chlorine hold up and takes away, carries out discharging after one-level washing, the secondary soda lye wash.
Embodiment 2:
(1) silicon tetrachloride liquid is joined in the vaporizer silicon tetrachloride that obtains vaporizing with 190 ℃ heat-conducting oil heating vaporizers.
(2) silicon tetrachloride of vaporization is passed into carry out under the liquid bubbling hydrolysis in the hydrolysis tower, liquid level is put into surge tank at 2 meters with the mixture after the hydrolysis in the mixture after obtaining being hydrolyzed, tower.The hydrolysis tower drain pipe vertically enters surge tank.
(3) be transported in the one-level barrier film undercurrent pressure filter with the mixture of pump after with described hydrolysis and carry out the press filtration first time, obtain the good filter cake of press filtration and filtrate, described filtrate is delivered in the hydrolysis tower silicon tetrachloride is hydrolyzed, until the mass concentration of HCl reaches 20% in the gained filtrate, obtain hydrochloric acid.
(4) described filter cake being delivered to colloidal mill is ground to without block existence.
(5) mixture after grinding in the step (4) is conveyed into the water that adds 8 times of amounts in the making beating tank, the processing of washing, pull an oar.
(6) mixture after described washing, the making beating is delivered to secondary diaphragm undercurrent pressure filter and carries out the press filtration second time, obtain filter cake and filtrate, filtrate again joins hydrolysis tower silicon tetrachloride is hydrolyzed, the amount of filtrate that joins hydrolysis tower will make that liquid level is 2 meters in the tower, residual filtrate be delivered in the neutralization tank and after drain into wastewater disposal basin.
(7) filter cake that for the second time press filtration is obtained is delivered to two blade dryers and carries out preliminarily dried, and drying machine adopts 190 ℃ heat-conducting oil heating, and be 15 minutes time of drying, obtains the filter cake of preliminarily dried.
(8) filter cake of described preliminarily dried is conveyed into flash dryer and carries out drying treatment, until the filter cake temperature is 80 ℃, air outlet temperature is 70 ℃, obtains the silicon-dioxide raw product.
(9) described silicon-dioxide raw product is carried out cyclonic separation, obtain final silica product.
Cover made of plastic covers one-level barrier film undercurrent pressure filter, and only from bottom belt mouth air intake, the HCl that will overflow and chlorine hold up and takes away, carries out discharging after one-level washing, the secondary soda lye wash.
Embodiment 3:
(1) silicon tetrachloride liquid is joined in the vaporizer silicon tetrachloride that obtains vaporizing with 180 ℃ heat-conducting oil heating vaporizers.
(2) silicon tetrachloride of vaporization is passed into carry out under the liquid bubbling hydrolysis in the hydrolysis tower, liquid level is put into surge tank at 3 meters with the mixture after the hydrolysis in the mixture after obtaining being hydrolyzed, tower.The hydrolysis tower drain pipe vertically enters surge tank.
(3) be transported in the one-level barrier film undercurrent pressure filter with the mixture of pump after with described hydrolysis and carry out the press filtration first time, obtain the good filter cake of press filtration and filtrate, described filtrate is delivered in the hydrolysis tower silicon tetrachloride is hydrolyzed, until the mass concentration of HCl reaches 30% in the gained filtrate, obtain hydrochloric acid.
(4) described filter cake being delivered to colloidal mill is ground to without block existence.
(5) mixture after grinding in the step (4) is conveyed into the water that adds 12 times of amounts in the making beating tank, the processing of washing, pull an oar.
(6) mixture after described washing, the making beating is delivered to secondary diaphragm undercurrent pressure filter and carries out press filtration second time, a filtrate part comes back to hydrolysis tower silicon tetrachloride is hydrolyzed, residual filtrate be delivered in the neutralization tank with after drain into wastewater disposal basin.
(7) filter cake that for the second time press filtration is obtained is delivered to two blade dryers and carries out preliminarily dried, and drying machine adopts 180 ℃ heat-conducting oil heating, and be 45 minutes time of drying, obtains the filter cake of preliminarily dried;
(8) filter cake of described preliminarily dried is conveyed into flash dryer and carries out drying treatment, until the filter cake temperature is 90 ℃, air outlet temperature is 80 ℃, obtains the silicon-dioxide raw product.
(9) described silicon-dioxide raw product is carried out cyclonic separation, obtain final silica product.
Cover made of plastic covers one-level barrier film undercurrent pressure filter, and only from bottom belt mouth air intake, the HCl that will overflow and chlorine hold up and takes away, carries out discharging after one-level washing, the secondary soda lye wash.
Claims (3)
1. the low temperature hydrolysis method of a silicon tetrachloride is characterized in that may further comprise the steps:
(1) silicon tetrachloride liquid is joined in the vaporizer, with the silicon tetrachloride that the heat-conducting oil heating vaporizer obtains vaporizing, the temperature of described thermal oil is 170-190 ℃;
(2) silicon tetrachloride of described vaporization is passed into carry out bubbling hydrolysis under the liquid in the hydrolysis tower, liquid level is conveyed into the mixture after the hydrolysis in the surge tank at 2-3 rice in the mixture after obtaining being hydrolyzed, tower;
(3) from surge tank, be transported in the one-level barrier film undercurrent pressure filter with the mixture of pump after with described hydrolysis and carry out the press filtration first time, obtain filter cake and filtrate, described filtrate is delivered in the hydrolysis tower silicon tetrachloride is hydrolyzed, until the mass concentration of HCl reaches 20-30% in the gained filtrate, obtain hydrochloric acid;
(4) described filter cake being delivered to colloidal mill is ground to without block existence;
(5) mixture after grinding in the step (4) is conveyed into the water that adding 8-12 doubly measures in the making beating tank, the processing of washing, pull an oar;
(6) mixture after described washing, the making beating is delivered to secondary diaphragm undercurrent pressure filter and carries out the press filtration second time, obtain filter cake and filtrate, filtrate again joins hydrolysis tower silicon tetrachloride is hydrolyzed, the amount of filtrate that joins hydrolysis tower will make in the tower liquid level between 2-3 rice, residual filtrate be delivered in the neutralization tank and after drain into wastewater disposal basin;
(7) filter cake that for the second time press filtration is obtained is delivered to two blade dryers and carries out preliminarily dried, and drying machine adopts 170-190 ℃ heat-conducting oil heating, and be 15-45 minute time of drying, obtains the filter cake of preliminarily dried;
(8) filter cake of described preliminarily dried is conveyed into flash dryer and carries out drying treatment, until the filter cake temperature is 80-90 ℃, air outlet temperature is 70-80 ℃, obtains the silicon-dioxide raw product;
(9) described silicon-dioxide raw product is carried out cyclonic separation, obtain final silica product.
2. a kind of low temperature hydrolysis method of silicon tetrachloride as claimed in claim 1, it is characterized in that cover made of plastic covers one-level barrier film undercurrent pressure filter, only from bottom belt mouth air intake, the HCl that will overflow and chlorine hold up and take away, carry out discharging after one-level washing, the secondary soda lye wash.
3. a kind of low temperature hydrolysis method of silicon tetrachloride as claimed in claim 1 is characterized in that the hydrolysis tower drain pipe vertically enters surge tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110213568 CN102275940B (en) | 2011-07-28 | 2011-07-28 | Method for low-temperature hydrolysis of silicon tetrachloride |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110213568 CN102275940B (en) | 2011-07-28 | 2011-07-28 | Method for low-temperature hydrolysis of silicon tetrachloride |
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| CN102275940A CN102275940A (en) | 2011-12-14 |
| CN102275940B true CN102275940B (en) | 2013-01-23 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102515178B (en) * | 2011-12-23 | 2014-08-20 | 李晓武 | Method for producing white carbon black by using silicon tetrachloride as raw material through titration method |
| CN102515104B (en) * | 2012-01-09 | 2013-12-18 | 河北科技大学 | Method for preparing hydrogen chloride and silicon dioxide by hydrolyzing silicon tetrachloride in organic solvent |
| CN103420381B (en) * | 2012-05-15 | 2015-03-25 | 天华化工机械及自动化研究设计院有限公司 | Method for recycling disposal of silicon tetrachloride slag slurry produced in polycrystalline silicon production and device thereof |
| CN105236414A (en) * | 2015-09-21 | 2016-01-13 | 太仓市金锚新材料科技有限公司 | Silicon tetrachloride recycling method |
| CN106644660B (en) * | 2016-11-21 | 2020-04-28 | 天津大学 | Sample pretreatment device and method for measuring content of trace phosphorus impurities in chlorosilane |
| CN106564933A (en) * | 2016-11-22 | 2017-04-19 | 云南临沧鑫圆锗业股份有限公司 | Preparation method of low-chloride high-purity germanium dioxide |
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| DE102004024500A1 (en) * | 2004-05-18 | 2005-12-15 | Degussa Ag | Flame hydrolytically produced silicon-titanium mixed oxide powder |
| CN101941678B (en) * | 2009-07-07 | 2012-09-05 | 自贡市中通货运中心 | Treatment method of silicon tetrachloride |
| CN101940898B (en) * | 2010-09-26 | 2012-09-19 | 河北科技大学 | Method for recycling silicon tetrachloride |
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