CN100532641C - Method for deactivation of active sodium sand - Google Patents
Method for deactivation of active sodium sand Download PDFInfo
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- CN100532641C CN100532641C CNB2006101342868A CN200610134286A CN100532641C CN 100532641 C CN100532641 C CN 100532641C CN B2006101342868 A CNB2006101342868 A CN B2006101342868A CN 200610134286 A CN200610134286 A CN 200610134286A CN 100532641 C CN100532641 C CN 100532641C
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Abstract
The invention involves the treating method of excessive sodium sand in chemical reaction. An inactivation method for active sodium sand contains: in the protection of inert gas, adding liquid paraffin into the active sodium system, adding water directly to deactivating sodium, after stratification, counteracting the water layer and discharging. The liquid paraffin used in the invention is general industrial liquid paraffin with high boiling point, uneasy bumping and high specific heat, is a good dispersion medium, and can effectively disperse sodium in keeping exclusion with the air; the usage amount of liquid paraffin is reasonable, and can be recycled, low cost; easy to operate and safe; water layer can be discharged directly after treatment, is environmental protection, liquid paraffin is recycled and reused, so this low-cost method of the invention is easy to carried out for industrialization and safe complete deactivating alive sodium effect.
Description
Technical field:
The present invention relates to the treatment process of excessive sodium sand in the chemical reaction.
Background technology:
Sodium is a kind of raw material commonly used in the chemical engineering industry, can be used to carry out polytype reaction.Sodium is spontaneous combustion easily in air, with water meeting vigorous reaction releasing hydrogen gas and even burning.But sodium usually belongs to excess material in reaction, thus how the processing reaction still residual in excessive active sodium, need most Safety Problems in most of exactly reaction of using sodium.The method of existing this type of active sodium of cancellation with Virahol or ethanol and sodium reaction, generates sodium alkoxide earlier normally under the nitrogen protection condition, question response finishes, and adds the sodium alkoxide reaction of water and generation, generates sodium hydroxide and alcohol.The advantage of this process is that whole process reaction is gentle.But this process uses ethanol or Virahol to come cancellation, in the process of sodium alkoxide of Sheng Chenging and water reaction subsequently, though be reduced into alcohol again, because alcohol dissolves each other with water, cause alcohol to recycle, thereby has increased processing cost.In addition, cancellation is carried out in two steps, also makes complex treatment process, and the cycle increases.
Summary of the invention:
The objective of the invention is to solve above-mentioned not enough problem, a kind of method for deactivating of active sodium sand is provided, succinct, safe, the active sodium of cancellation cheaply.
The technical scheme that the present invention is adopted for achieving the above object is as follows: a kind of method for deactivating of active sodium sand; under the protection of rare gas element, in pending active sodium system, add whiteruss, add the active sodium of the direct inactivation of entry; layering behind the inactivation, the discharging of in the water layer and back.
Describedly add entry under 50～500 rev/mins of stirring velocitys, adding entry; temperature is no more than the boiling point of 100 ℃ or organic light constituent in the hierarchy of control; waiting not have gas produces; add water again with pending quality such as system; stir; protection of inert gas is cooling, layering down, and water layer is neutralized to neutral discharging with acid.
Described organic layer steams light constituent, after the industrial sodium hydroxide drying, gets the whiteruss recycling.
The add-on of described whiteruss is the weight more than or equal to sodium in the pending system, less than waiting until in pending system gross weight.
Described whiteruss is the general industry whiteruss, and water content is less than 0.5%.
Described stirring velocity is 100-200 rev/min.
The described speed that adds water by control comes temperature in the hierarchy of control to be no more than the boiling point of 100 ℃ or organic light constituent.
Introduce extraneous cold circulation in the described system inactivation, with hierarchy of control temperature of reaction.
Described inert protective gas is nitrogen or argon gas.
Described neutralization acid is dilute sulphuric acid or dilute hydrochloric acid.
The invention has the beneficial effects as follows: used whiteruss is the general industry whiteruss, and the boiling point height is difficult for bumping; Specific heat is big, is a kind of good dispersion medium, and effectively dispersed activity sodium makes it isolated with air; Its consumption must not be lower than the quality of pending active sodium, is not higher than the system total mass that contains active sodium, if active sodium be dispersed in special heavy-gravity still residual in, then strengthen the whiteruss consumption to the degree that can stir; The whiteruss consumption is reasonable, and can recycle, and cost is low; Best hierarchy of control temperature is no more than 100 ℃ during processing; Outer can the establishing of reactor adds cold circulation, uses during the cycle at needs controlled temperature or urgent need shortening, also can add; Easy and simple to handle, safety; The back water layer that disposes can directly discharge, environmental protection, and whiteruss then recycles and utilizes, so the inventive method cost is low and realize industrialization easily, reaches the effect of the active sodium of safe inactivation.
Embodiment:
Below by specific embodiment the present invention is further detailed, but the present invention is not limited to this.
Embodiment 1:
Contain in the system of have an appointment 50 active sodium of gram and 50 gram toluene to 100 grams, add 50 gram water content less than 0.5% general industry whiteruss, with the nitrogen replacement system, with 0 ℃ of cold circulation cooling reactor, 100 rev/mins of speed stir and drip water down, and the dropping process keeps reactor temperature to be no more than 100 ℃, no longer include the gas generation after 20 minutes and emerge, continue to add 100 gram water, stir half an hour, lower aqueous layer is emitted in the cooling layering, add dilute hydrochloric acid and be neutralized to neutrality, discharging; Organic layer is emitted, steam toluene after, whiteruss is dried to moisture less than 0.5% with industrial sodium hydroxide, be equipped with reuse.
Embodiment 2:
Contain in the system of the active sodium of 50 gram normal hexanes, 50 grams to 100 grams, add 50 gram whiterusss, with the argon replaces system, do not open cold circulation, 200 rev/mins of stirrings drip water down, and the interior temperature of maintenance system is no more than 100 ℃ in the dropping process, no longer includes gas after 45 minutes and generates, continue to add 100 gram water, stir half an hour, lower aqueous layer is emitted in the cooling layering, add dilute sulphuric acid and be neutralized to neutrality, discharging; Organic layer is emitted, and steams hexane, and whiteruss is dried to moisture less than 0.5% with industrial sodium hydroxide, is equipped with reuse.
Embodiment 3:
Contain in the system of have an appointment 40 active sodium of gram and 60 gram toluene to 100 grams, add 60 gram water content less than 0.5% general industry whiteruss, with the nitrogen replacement system, with 0 ℃ of cold circulation cooling reactor, 150 rev/mins of speed stir and drip water down, and the dropping process keeps reactor temperature to be no more than 100 ℃, no longer include the gas generation after 18 minutes and emerge, continue to add 100 gram water, stirred 40 minutes, lower aqueous layer is emitted in the cooling layering, add dilute hydrochloric acid and be neutralized to neutrality, discharging; Organic layer is emitted, steam toluene after, whiteruss is dried to moisture less than 0.5% with industrial sodium hydroxide, be equipped with reuse.
Embodiment 4
Contain in the system of the active sodium of 55 gram normal hexanes, 45 grams to 100 grams, add 90 gram whiterusss, with the argon replaces system, do not open cold circulation, 300 rev/mins of stirrings drip water down, and the interior temperature of maintenance system is no more than 100 ℃ in the dropping process, no longer includes gas after 40 minutes and generates, continue to add 100 gram water, stir half an hour, lower aqueous layer is emitted in the cooling layering, add dilute sulphuric acid and be neutralized to neutrality, discharging; Organic layer is emitted, and steams hexane, and whiteruss is dried to moisture less than 0.5% with industrial sodium hydroxide, is equipped with reuse.
Claims (8)
1; a kind of method for deactivating of active sodium sand; it is characterized in that: under the protection of rare gas element; in pending active sodium system, add whiteruss; the add-on of whiteruss is the weight more than or equal to sodium in the pending system; smaller or equal to pending system gross weight; add the active sodium of the direct inactivation of entry again; add entry under 50～500 rev/mins of stirring velocitys, adding entry; temperature is no more than the boiling point of 100 ℃ or organic light constituent in the hierarchy of control; wait not have gas and produce, add the water with pending quality such as system again, stir; protection of inert gas cooling down behind the inactivation; layering, water layer is neutralized to neutral discharging with acid.
2, the method for deactivating of a kind of active sodium sand according to claim 1, it is characterized in that: organic layer steams light constituent after the layering, whiteruss with the industrial sodium hydroxide drying after, whiteruss recycling.
3, the method for deactivating of a kind of active sodium sand according to claim 1 is characterized in that: whiteruss is the general industry whiteruss, and water content is less than 0.5%.
4, the method for deactivating of a kind of active sodium sand according to claim 1 is characterized in that: adding entry is to add entry under the 100-200 rev/min of stirring velocity.
5, the method for deactivating of a kind of active sodium sand according to claim 1 is characterized in that: the speed that adds water by control comes temperature in the hierarchy of control to be no more than the boiling point of 100 ℃ or organic light constituent.
6, the method for deactivating of a kind of active sodium sand according to claim 1 is characterized in that: introduce extraneous cold circulation in the system inactivation, with hierarchy of control temperature of reaction.
7, the method for deactivating of a kind of active sodium sand according to claim 1 is characterized in that: inert protective gas is nitrogen or argon gas.
8, the method for deactivating of a kind of active sodium sand according to claim 1 is characterized in that: neutralization is dilute sulphuric acid or dilute hydrochloric acid with acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101342868A CN100532641C (en) | 2006-11-13 | 2006-11-13 | Method for deactivation of active sodium sand |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101342868A CN100532641C (en) | 2006-11-13 | 2006-11-13 | Method for deactivation of active sodium sand |
Publications (2)
| Publication Number | Publication Date |
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| CN1952212A CN1952212A (en) | 2007-04-25 |
| CN100532641C true CN100532641C (en) | 2009-08-26 |
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| CNB2006101342868A Active CN100532641C (en) | 2006-11-13 | 2006-11-13 | Method for deactivation of active sodium sand |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105148815A (en) * | 2015-08-19 | 2015-12-16 | 大连理工大学 | Method and device for treating waste sodium/potassium in laboratory |
| CN107214344A (en) * | 2017-05-17 | 2017-09-29 | 成都化润药业有限公司 | A kind of industrial production process of sodium sand |
| CN108311089A (en) * | 2018-02-07 | 2018-07-24 | 西安交通大学 | A kind of bulk metal sodium impurity secure processing device and method |
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2006
- 2006-11-13 CN CNB2006101342868A patent/CN100532641C/en active Active
Non-Patent Citations (2)
| Title |
|---|
| 钠的性质实验的改进. 赵东洋.化学教学，第3期. 2006 |
| 钠的性质实验的改进. 赵东洋.化学教学，第3期. 2006 * |
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| CN1952212A (en) | 2007-04-25 |
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Effective date of registration: 20200515 Address after: 116200 Songhai street, songmudao chemical industry park, Jinpu New District, Dalian City, Liaoning Province Patentee after: Dalian Shuangbo Pharmaceutical Chemical Co., Ltd Address before: 116620, Liaoning, Dalian double D port, double D5 street, 18, bio pharmaceutical R & D center, C Patentee before: LIANHUA CHEMISTRY CO., LTD., DALIAN |
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