CN103964440B - A kind of preparation method extracting silicon carbide from the urethane of packaged silicon carbide - Google Patents
A kind of preparation method extracting silicon carbide from the urethane of packaged silicon carbide Download PDFInfo
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- CN103964440B CN103964440B CN201410185492.6A CN201410185492A CN103964440B CN 103964440 B CN103964440 B CN 103964440B CN 201410185492 A CN201410185492 A CN 201410185492A CN 103964440 B CN103964440 B CN 103964440B
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Abstract
The invention discloses a kind of preparation method extracting silicon carbide from the urethane of packaged silicon carbide, its process is: (1) is being enclosed with the polyurethane waste material of silicon carbide in the first beaker; (2) acetone and solvent joined in polyurethane waste material and stir, until solution in the first beaker and throw out no longer include considerable change; (3) by throw out and separated from solvent, use clear water washing precipitate, obtain silicon carbide blend, and with the acetone in distillation under vacuum recycling design and DMF; (4) caustic soda is put in the second beaker, adds distilled water, be made into alkali lye; (5) silicon carbide blend that step (3) obtains is added in the alkali lye of step (4), and electric stirring under boil condition, to add throw out (silicon carbide) centrifugation in the second beaker after sour remove portion impurity, clean, dry, namely obtain purer silicon carbide.Present method products obtained therefrom non-corrosiveness and viscosity is low, purity is high, environmental protection, products obtained therefrom serve many purposes.
Description
Technical field
The present invention relates to a kind of preparation method extracting silicon carbide from the urethane of packaged silicon carbide, raw materials used is common caustic soda, phosphoric acid etc., belongs to field of fine chemical, particularly relates to the preparation method that a kind of chemical reaction obtains high-purity carborundum.
Background technology
Silicon carbide mainly contains four large Application Areass, that is: function ceramics, high grade refractory, abrasive material and metallurgical raw material.Because it is of many uses, stable performance, thermal conductivity is high, thermal expansivity is little, wear resisting property is good, is widely applied to every field.The purposes of silicon carbide, has established the domestic and international market of silicon carbide.Believe in the near future, the impact domestic and international market that silicon carbide will be very large.
And the method for producing silicon carbide use is at present comparatively simple, and the purity preparing the silicon carbide drawn is not high, and containing more impurity, the cost of preparation is also higher; And in the preparation, the problem of environmental pollution produced is especially outstanding.Therefore, a kind of method that can solve the generation problems such as the production silicon carbide of prior art must be researched and developed.
Summary of the invention
The object of the invention is to solve in prior art the defect of producing existing for silicon carbide, a kind of preparation method extracting silicon carbide from the urethane of packaged silicon carbide is provided, this preparation method can find out optimised process and the condition thereof of degradation of polyurethane, thus the silicon carbide impelling it to wrap up is out exposed, and then provide foundation for extracting silicon carbide, recycle simple physical method centrifugal separation technique silicon carbide is extracted, then dry.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method extracting silicon carbide from the urethane of packaged silicon carbide, comprises the following steps:
(1) polyurethane waste material being enclosed with silicon carbide of 10-20g is weighed in the first beaker with analytical balance;
(2) measure 10-20ml acetone and 20-50mlDMF solvent, join in polyurethane waste material, stir 0.5-2h, until solution in the first beaker and throw out no longer include considerable change;
(3) by throw out and separated from solvent, use clear water washing precipitate, obtain silicon carbide blend, and with the acetone in distillation under vacuum recycling design and DMF;
(4) weigh the caustic soda of 10-50g in the second beaker with analytical balance, and the distilled water measuring 20-100ml with graduated cylinder is in the second beaker, compound concentration is the alkali lye of 15%-50%;
(5) the silicon carbide blend 5-10g that step (3) obtains is added in the alkali lye of step (4), and electric stirring 4-10h under boil condition, after adding 20-50ml acid remove portion impurity, the throw out (silicon carbide) in the second beaker carried out successively centrifugation, clean, dry, finally namely obtain purer silicon carbide.
Further, in described step (1): the polyurethane waste material of the packaged silicon carbide taken is 15g.
Further, in described step (2): measure 15ml acetone and 30mlDMF solvent, churning time is 1h.
Further, in described step (4): caustic soda amount is 15g, the distillation water yield is 50ml.
Further, in described step (5): silicon carbide blend amount is 5g, the reaction times is 8 hours, and will by alkali lye neutralization until ability centrifugation after becoming neutrality, and the acid that neutralization uses is phosphoric acid.
In sum, utilize a kind of preparation method's tool extracting silicon carbide from the urethane of packaged silicon carbide of the present invention to have the following advantages: to adopt the waste material of certain enterprise to be raw material, in experimentation, equipment is simple, easy to operate, safe and reliable simultaneously; Its preparation method is simple, and the silicon carbide purity obtained is high, and minimum to the pollution of environment, can not affect to some extent the healthy of the people.Simple, feasible, the safety of technique in present method leaching process, products obtained therefrom non-corrosiveness and viscosity is low, purity is high, environmental protection, products obtained therefrom serve many purposes.
Simultaneously, this experiment produces long-living waste material for raw material with certain enterprise domestic, detect analysis by instrument (as infrared, DSC etc.) and learn its main component, on the basis of existing theory, by omnibearing consideration, obtain the Technology of this experiment, belong to environment-friendly type enterprise, this experiment meets the current policies of country, not only environmental protection but also useful.
Embodiment
By specific embodiment given below, the present invention can be had a clear understanding of further.
Embodiment 1
From the urethane of packaged silicon carbide, extract a preparation method for silicon carbide, comprise the following steps:
(1) polyurethane waste material being enclosed with silicon carbide of 15g is weighed in the first beaker with analytical balance;
(2) measure 15ml acetone and 30mlDMF solvent, join in polyurethane waste material, stir 1h, until solution in the first beaker and throw out no longer include considerable change;
(3) by throw out and separated from solvent, use clear water washing precipitate, obtain silicon carbide blend, and with the acetone in distillation under vacuum recycling design and DMF;
(4) weigh the caustic soda of 15g in the second beaker with analytical balance, and the distilled water measuring 50ml with graduated cylinder is in the second beaker, compound concentration is the alkali lye of 30%;
(5) the silicon carbide blend 5g that step (3) obtains is added in the alkali lye of step (4), and electric stirring 8h under boil condition, after adding 35ml phosphoric acid remove portion impurity, the throw out (silicon carbide) in the second beaker is carried out successively centrifugation, clean, dry, and by alkali lye neutralization until ability centrifugation after becoming neutrality, finally to namely obtain purer silicon carbide.
Embodiment 2
From the urethane of packaged silicon carbide, extract a preparation method for silicon carbide, comprise the following steps:
(1) polyurethane waste material being enclosed with silicon carbide of 10g is weighed in the first beaker with analytical balance;
(2) measure 10ml acetone and 20mlDMF solvent, join in polyurethane waste material, stir 0.5h, until solution in the first beaker and throw out no longer include considerable change;
(3) by throw out and separated from solvent, use clear water washing precipitate, obtain silicon carbide blend, and with the acetone in distillation under vacuum recycling design and DMF;
(4) weigh the caustic soda of 10g in the second beaker with analytical balance, and the distilled water measuring 20ml with graduated cylinder is in the second beaker, compound concentration is the alkali lye of 15%%;
(5) the silicon carbide blend 8g that step (3) obtains is added in the alkali lye of step (4), and electric stirring 4h under boil condition, after adding 20ml phosphoric acid remove portion impurity, the throw out (silicon carbide) in the second beaker is carried out successively centrifugation, clean, dry, and by alkali lye neutralization until ability centrifugation after becoming neutrality, finally to namely obtain purer silicon carbide.
Embodiment 3
From the urethane of packaged silicon carbide, extract a preparation method for silicon carbide, comprise the following steps:
(1) polyurethane waste material being enclosed with silicon carbide of 20g is weighed in the first beaker with analytical balance;
(2) measure 20ml acetone and 50mlDMF solvent, join in polyurethane waste material, stir 2h, until solution in the first beaker and throw out no longer include considerable change;
(3) by throw out and separated from solvent, use clear water washing precipitate, obtain silicon carbide blend, and with the acetone in distillation under vacuum recycling design and DMF;
(4) weigh the caustic soda of 50g in the second beaker with analytical balance, and the distilled water measuring 100ml with graduated cylinder is in the second beaker, compound concentration is the alkali lye of 50%;
(5) the silicon carbide blend 10g that step (3) obtains is added in the alkali lye of step (4), and electric stirring 10h under boil condition, after adding 50ml phosphoric acid remove portion impurity, the throw out (silicon carbide) in the second beaker is carried out successively centrifugation, clean, dry, and by alkali lye neutralization until ability centrifugation after becoming neutrality, finally to namely obtain purer silicon carbide.
The above is only preferred embodiment of the present invention, not does any pro forma restriction to technology contents of the present invention.Every above embodiment is done according to technical spirit of the present invention any simple modification, equivalent variations and modification, all still belong in the scope of technical scheme of the present invention.
Claims (5)
1., in a kind of preparation method extracting silicon carbide from the urethane of packaged silicon carbide, it is characterized in that, comprise the following steps:
(1) polyurethane waste material being enclosed with silicon carbide of 10-20g is weighed in the first beaker with analytical balance;
(2) measure 10-20ml acetone and 20-50mlDMF solvent, join in polyurethane waste material, stir 0.5-2h, until solution in the first beaker and throw out no longer include considerable change;
(3) by throw out and separated from solvent, use clear water washing precipitate, obtain silicon carbide blend, and with the acetone in distillation under vacuum recycling design and DMF;
(4) weigh the caustic soda of 10-50g in the second beaker with analytical balance, and the distilled water measuring 20-100ml with graduated cylinder is in the second beaker, compound concentration is the alkali lye of 15%-50%;
(5) the silicon carbide blend 5-10g that step (3) obtains is added in the alkali lye of step (4), and electric stirring 4-10h under boil condition, after adding sour remove portion impurity, the throw out silicon carbide in the second beaker is carried out successively centrifugation, clean, dry, finally namely obtain pure silicon carbide.
2. a kind of preparation method extracting silicon carbide from the urethane of packaged silicon carbide according to claim 1, is characterized in that, in described step (1): the polyurethane waste material of the packaged silicon carbide taken is 15g.
3. a kind of preparation method extracting silicon carbide from the urethane of packaged silicon carbide according to claim 1, is characterized in that, in described step (2): measure 15ml acetone and 30mlDMF solvent, churning time is 1h.
4. a kind of preparation method extracting silicon carbide from the urethane of packaged silicon carbide according to claim 1, is characterized in that, in described step (4): caustic soda amount is 15g, the distillation water yield is 50ml.
5. a kind of preparation method extracting silicon carbide from the urethane of packaged silicon carbide according to claim 1, it is characterized in that, in described step (5): silicon carbide blend amount is 5g, reaction times is 8 hours, and will by alkali lye neutralization until ability centrifugation after becoming neutrality, the acid that neutralization uses is phosphoric acid.
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| CN104449097A (en) * | 2014-12-11 | 2015-03-25 | 江门市绿茵环保科技有限公司 | Novel fireproof thermal insulation coating and preparation method thereof |
| CN104403431A (en) * | 2014-12-11 | 2015-03-11 | 江门市绿茵环保科技有限公司 | Novel thermal insulating paint |
| CN111547725A (en) * | 2020-05-14 | 2020-08-18 | 湖南太子新材料科技有限公司 | Preparation method for extracting silicon carbide from polyurethane wrapped with silicon carbide |
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| CN101817526A (en) * | 2010-04-08 | 2010-09-01 | 浙江源盛硅晶材料有限公司 | Method for recovering polyethylene glycol and silicon carbide from silicon crystal cutting waste liquid |
| CN101941699A (en) * | 2010-09-14 | 2011-01-12 | 东北大学 | Method for reclaiming silicon and silicon carbide from cutting waste materials of monocrystalline silicon and polycrystalline silicon |
| CN102071320A (en) * | 2011-01-24 | 2011-05-25 | 云南临沧鑫圆锗业股份有限公司 | Solar cell germanium substrate slice processing liquid waste treatment process |
| CN102211774A (en) * | 2010-04-02 | 2011-10-12 | 南开大学 | Method for purifying silica micropowder through selective flocculation |
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Patent Citations (4)
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| CN102211774A (en) * | 2010-04-02 | 2011-10-12 | 南开大学 | Method for purifying silica micropowder through selective flocculation |
| CN101817526A (en) * | 2010-04-08 | 2010-09-01 | 浙江源盛硅晶材料有限公司 | Method for recovering polyethylene glycol and silicon carbide from silicon crystal cutting waste liquid |
| CN101941699A (en) * | 2010-09-14 | 2011-01-12 | 东北大学 | Method for reclaiming silicon and silicon carbide from cutting waste materials of monocrystalline silicon and polycrystalline silicon |
| CN102071320A (en) * | 2011-01-24 | 2011-05-25 | 云南临沧鑫圆锗业股份有限公司 | Solar cell germanium substrate slice processing liquid waste treatment process |
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