CN105712836A - Method for removing trace water in 3-chloropropene - Google Patents
Method for removing trace water in 3-chloropropene Download PDFInfo
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- CN105712836A CN105712836A CN201410728400.4A CN201410728400A CN105712836A CN 105712836 A CN105712836 A CN 105712836A CN 201410728400 A CN201410728400 A CN 201410728400A CN 105712836 A CN105712836 A CN 105712836A
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- chloropropene
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- ethylene glycol
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Abstract
The invention discloses a method for removing trace water in 3-chloropropene. The method comprises the steps of mixing glycerol and/or ethylene glycol with industrial-grade 3-chloropropene evenly, standing to layer, taking the upper liquid, and distilling to obtain 3-chloropropene. The method has the advantages of simple operation, low cost, safety and environmental protection, and can effectively remove the trace water in 3-chloropropene.
Description
Technical field
The present invention relates to the method for micro-moisture in a kind of elimination 3 chloropropenes, belong to 3 chloropropene industrial production technology fields.
Background technology
At present, on market, the content of high-purity technical grade 3 chloropropene has reached more than 99.3%, water white transparency, the chances are 0.01% for water content (mass fraction), but in this 3 chloropropene, water content still can not fully meet the field such as organosilicon and auxiliary agent for water treatment to the 3 high-quality requirements of chloropropene.In 3 chloropropenes, product quality is had large effect by the height of water content so that it is application is limited to.Therefore, low moisture is one of requirement of high-quality 3 chloropropene.
Japanese Unexamined Patent Publication 2,010 83818 document describes the method using zeolite dehydration, and using the dehydrating tower being filled with zeolite that the material of the gaseous state that water content is more than 1000ppm is carried out dehydration, owing to the material phase specific volume of gas material with liquid has turned over hundred times.In order to comply with industrial requirement, it is necessary to be greatly improved the mass flow of gas material.But, if increasing mass flow, increasing the capacity of dehydrating tower with this together, existing and must use the zeolite as dehydrant in a large number, and then the such problem of regeneration also needing to zeolite.
Japan Patent " dewatering of hydrofluorocompounds or hydrogen chlorocarbon ", disclosed in number of patent application 201180044209.2, a kind of employing makes the water that water vapour condensation becomes liquid even freeze solidification by heat exchanger cooling, remove the dewatering of moisture in material, the product content processed by the method is low, but for the material containing acid, water condensation postadhesion, at heat exchanger surface, can cause heat exchanger corrosion failure, and need substantial amounts of energy consumption with the method dehydration of cooling.
Chinese patent " a kind of 3 chloropropene deacidifications, dewatering ", application number is 201210154786, it is the moisture adopting two kinds of desiccant to absorb in chloropropene, the method brings any new impurity into will not to 3 chloropropenes, the moisture level reaching top grade product of product after processed, but, after desiccant water suction, volumetric expansion, need high-temperature roasting to reduce during recovery, and sintering temperature is high, energy consumption is big, and desiccant meeting variable color, and the unit currently using desiccant is substantially free of recycling, dehydration is relatively costly, the desiccant contaminated environment scrapped.Therefore, the method never adopts in commercial production.
Summary of the invention
For hydrogen chlorocarbon water-eliminating method of the prior art, the defect that particularly 3 chloropropene dehydrating process exist, it is an object of the invention to be in that a kind of simple to operate, low cost, safety and environmental protection, and can effectively remove the method for micro-moisture in 3 chloropropenes.
The invention provides the method for micro-moisture in a kind of elimination 3 chloropropenes, the method is after glycerol and/or ethylene glycol being mixed homogeneously with technical grade 3 chloropropene, stratification, takes supernatant liquid by, after distilling, obtaining 3 chloropropenes.
In elimination 3 chloropropenes of the present invention, the method for micro-moisture also includes following preferred version:
In preferred scheme, technical grade 3 chloropropene is 0.05:1～3:1 with the volume ratio of glycerol and/or ethylene glycol；It most preferably is 0.25:1～1:1.
Preferred scheme is combined by alr mode, or utilizes extraction tower or static mixer to realize.Currently preferred hybrid mode is conducive to liquid-liquid transfer.
In preferred scheme, glycerol and/or ethylene glycol are carry out when temperature is 0～40 DEG C mixing and stratification with technical grade 3 chloropropene.Preferred temperature favorably reduces the volatilization of 3 chloropropenes and is conducive to mixed liquor to be layered.
After preferred scheme goes out high-purity 3 chloropropenes by separated, remaining a small amount of glycerol and/or ethylene glycol directly reclaim and reuse.
Glycerol and ethylene glycol that the present invention adopts are commercially available analytical reagent.
Beneficial effects of the present invention: 1, adopt glycerol or ethylene glycol as deicer first, can effectively remove a small amount of moisture in technical grade 3 chloropropene, it is possible to decrease to below 100ppm, and the 3 chloropropene purity obtained are high, will not introduce impurity.2, adopting the process that glycerol or ethylene glycol dewater simple, equipment requirements is low, and operating condition is gentle.3, glycerol or ethanol can recycle, and use cost is low, does not result in environmental pollution.
Detailed description of the invention
Following example are further intended to present invention is described, rather than limit the scope of the invention.
Embodiment 1
Putting into 100g technical grade 3 chloropropene (moisture 800ppm), 100g glycerol in four-hole boiling flask, at room temperature stir 40min, after static layering, take upper strata 3 chloropropene analysis moisture content, test result water content is 98ppm.By upper solution by simple distillation, obtaining 3 chloropropenes of below water content 50ppm, remaining a small amount of glycerol reclaims and uses.
Embodiment 2
Putting into 100g technical grade 3 chloropropene (moisture 1100ppm), 300g glycerol in four-hole boiling flask, at room temperature stir 20min, after static layering, take upper strata 3 chloropropene analysis moisture content, test result water content is 65ppm.By upper solution by simple distillation, obtaining 3 chloropropenes of below water content 50ppm, remaining a small amount of glycerol reclaims and uses.
Embodiment 3
Putting into 100g technical grade 3 chloropropene (moisture 1100ppm), 200g ethylene glycol in four-hole boiling flask, at room temperature stir 30min, static layering, take upper strata 3 chloropropene analysis moisture content, test result water content is 82ppm.By upper solution by simple distillation, obtaining 3 chloropropenes of below water content 50ppm, remaining a small amount of glycol recovery uses.
Embodiment 4
Glycerol filled by the glass filler tower (tower diameter 30mm) be about 800mm, the volume ratio of glycerol and technical grade 3 chloropropene is 4:1, the charging rate controlling technical grade 3 chloropropene (moisture 800ppm) is 10g/min, analyzing the moisture of tower outlet, test result water content is 72ppm.To analyze tower outlet solution to collect, and by simple distillation, obtain 3 chloropropenes of below water content 50ppm, remaining a small amount of glycerol reclaims and uses.
Embodiment 5
Glycerol filled by the glass filler tower (tower diameter 30mm) be about 800mm, the volume ratio of glycerol and technical grade 3 chloropropene is 2:1, the charging rate controlling technical grade 3 chloropropene (moisture 800ppm) is 5g/min, analyzing the moisture of tower outlet, test result water content is 85ppm.To analyze tower outlet solution to collect, and by simple distillation, obtain 3 chloropropenes of below water content 40ppm, remaining a small amount of glycerol reclaims and uses.
Embodiment 6
Static mixer will fill up glycerol, the volume ratio of glycerol and technical grade 3 chloropropene is 6:1, the charging rate controlling glycerol is 20g/min, the Feed space velocities of technical grade chloropropene (water content is 800ppm) is 10g/min, material static analysis in phase separator by outlet, analyzing the moisture of upper strata 3 chloropropene, test result water content is 78ppm.By upper solution by simple distillation, obtaining 3 chloropropenes of below water content 50ppm, remaining a small amount of glycerol reclaims and uses.
Embodiment 7
Putting into 300g technical grade 3 chloropropene (moisture 1000ppm), 100g ethylene glycol in four-hole boiling flask, at room temperature stir 40min, after static layering, take upper strata 3 chloropropene analysis moisture content, test result water content is 109ppm.By upper solution by simple distillation, obtaining 3 chloropropenes of below water content 50ppm, remaining a small amount of glycol recovery uses.
Claims (5)
1. one kind removes the method for micro-moisture in chlorallylene, it is characterised in that after glycerol and/or ethylene glycol being mixed homogeneously with technical grade chlorallylene, stratification, takes supernatant liquid by, after distilling, obtaining chlorallylene.
2. the method for claim 1, it is characterised in that the volume ratio of technical grade chlorallylene and glycerol and/or ethylene glycol is 0.05:1～3:1.
3. the method for claim 1, it is characterised in that the volume ratio of technical grade chlorallylene and glycerol and/or ethylene glycol is 0.25:1～1:1.
4. the method for claim 1, it is characterised in that described is combined by alr mode, or utilizes extraction tower or static mixer to realize.
5. the method for claim 1, it is characterised in that glycerol and/or ethylene glycol are carry out when temperature is 0～40 DEG C mixing and stratification with technical grade chlorallylene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410728400.4A CN105712836A (en) | 2014-12-03 | 2014-12-03 | Method for removing trace water in 3-chloropropene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410728400.4A CN105712836A (en) | 2014-12-03 | 2014-12-03 | Method for removing trace water in 3-chloropropene |
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| CN105712836A true CN105712836A (en) | 2016-06-29 |
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| CN201410728400.4A Pending CN105712836A (en) | 2014-12-03 | 2014-12-03 | Method for removing trace water in 3-chloropropene |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4244892A (en) * | 1978-02-16 | 1981-01-13 | Guseinov Nazim M O | Process for preparing allyl chloride |
| JPS62286936A (en) * | 1986-06-04 | 1987-12-12 | Showa Denko Kk | Production of allyl chloride |
| CN101880263A (en) * | 2009-05-09 | 2010-11-10 | 中国石油化工集团公司 | Preparation method of epichlorohydrin |
| CN103420781A (en) * | 2012-05-17 | 2013-12-04 | 中国石油化工股份有限公司 | Deacidification and dehydration method of 3-chloropropene |
-
2014
- 2014-12-03 CN CN201410728400.4A patent/CN105712836A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4244892A (en) * | 1978-02-16 | 1981-01-13 | Guseinov Nazim M O | Process for preparing allyl chloride |
| JPS62286936A (en) * | 1986-06-04 | 1987-12-12 | Showa Denko Kk | Production of allyl chloride |
| CN101880263A (en) * | 2009-05-09 | 2010-11-10 | 中国石油化工集团公司 | Preparation method of epichlorohydrin |
| CN103420781A (en) * | 2012-05-17 | 2013-12-04 | 中国石油化工股份有限公司 | Deacidification and dehydration method of 3-chloropropene |
Non-Patent Citations (1)
| Title |
|---|
| 张廷深: "氯丙烯的深度加工与应用", 《中国氯碱》 * |
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Application publication date: 20160629 |