CN102079741A - Novel dewatering and purifying method of ethylene carbonate (EC) - Google Patents
Novel dewatering and purifying method of ethylene carbonate (EC) Download PDFInfo
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- CN102079741A CN102079741A CN2010105987100A CN201010598710A CN102079741A CN 102079741 A CN102079741 A CN 102079741A CN 2010105987100 A CN2010105987100 A CN 2010105987100A CN 201010598710 A CN201010598710 A CN 201010598710A CN 102079741 A CN102079741 A CN 102079741A
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Abstract
The invention relates to a novel dewatering and purifying method of ethylene carbonate (EC). The technical scheme adopted by the invention is as follows: an impurity-removing agent which is insoluble in EC and can absorb the moisture, alcohols and micromolecular impurities in EC is added in EC, wherein the impurity-removing agent can be one or more of spherical low-sodium molecular sieves such as 3A, 4A, 5A, 10X, 13X and the like, activated aluminium oxide, activated carbon, silica gel, calcium oxide, calcium chloride and the like; and the impurity-removing agent accounts for 3%-30% of EC, the temperature of the process is controlled to 40-100 DEG C and the time of the process is 1-10 hours. The invention has the following advantages and positive effects: the impurity-removing agent is added in EC and accounts for 3%-30% of EC, thus EC can be purified efficiently and fast, the process consumes low energy and the aims of increasing the quality and reducing the cost can be realized.
Description
Technical field
The present invention relates to a kind of novel NSC 11801 (EC) dehydrating and removing impurities method.
Background technology
NSC 11801 (EC) is a kind of organic solvent and organic synthesis intermediate of excellent property, have advantages such as boiling point height, toxicity and corrodibility are little, be widely used in fields such as plastics, printing and dyeing, Polymer Synthesizing, gas delivery and electrochemical, on battery industry, can be used as the fine solvent of lithium battery electrolytes.Because the thermostability height of EC, be heated to 200 ℃ just take place a small amount of the decomposition, fusing point is 36.4 ℃, flash-point is 160 ℃, boiling point is 238 ℃, thermal safety and specific inductivity are the highest in existing lithium-ion battery electrolytes organic solvent system, so EC is widely used in the lithium ion battery industry.Along with the emergence of lithium electricity industry, the consumption of EC also increases gradually.
At present, the more of industrial employing is with oxyethane (EO) and CO
2Be raw material direct esterification preparation.Yet, owing in EO and CO2 generation esterification generation EC, also may exist reaction, oxyethane and the reaction of ethylene glycol generation glycol ether and the hydrolysis reaction of EC that the EO hydration generates ethylene glycol.The generation of alcohols and the hydrolysis of NSC 11801 all can bring negative influence to lithium-ion battery electrolytes, and in addition, self has certain moisture NSC 11801, can bring certain influence to the control of lithium-ion battery electrolytes moisture.Therefore before the preparation of carrying out lithium-ion battery electrolytes, must carry out purifying processing to NSC 11801, to such an extent as to satisfy the demand of high-quality lithium ion battery.At present, the mode of the rectifying that numerous electrolytic solution manufacturer all takes is purified to EC, according to statistics, this method is purified and will be obtained cell-grade NSC 11801 EC, yield is greatly about about 88%, and the whole process time is long, has increased certain cost in the electrolytic solution production process.
Summary of the invention
The objective of the invention is to overcome the prior art deficiency, utilize a kind of new technology to NSC 11801 (EC) carry out efficiently, fast, low consumption ground purify (yield can be brought up to more than 95%).
The object of the present invention is achieved like this:
Be to solve the problems referred to above that prior art exists, the technical scheme that the present invention takes is: add in described NSC 11801 and be insoluble to NSC 11801 and can adsorb the wherein cleaner of moisture, alcohols and small molecular weight impurity thereof again; Cleaner can be wherein one or more such as spherical low sodium type molecular sieve such as 3A, 4A, 5A, 10X, 13X, activated alumina, gac, silica gel, calcium oxide, calcium chloride.The add-on of cleaner is 3% ~ 30% of NSC 11801 (EC) amount, and whole process temperature is controlled at 40 ~ 100 ℃, and the time is 1 ~ 10 hour.
Technical process.
In airtight kiln, (experimentize among the moisture＜50ppm, oxygen part＜50ppm),: the NSC 11801 that will liquefy (EC) is inserted (steel cylinder vacuumizes displacement three times with filling high-purity argon gas) in the stainless steel cylinder, add quantitative cleaner, rocked after the sealing 5 minutes, NSC 11801 (EC) is fully contacted with cleaner, putting into 40 ℃ vacuum drying oven leaves standstill after 1 ~ 5 hour and rocked NSC 11801 (EC) moisture, purity and alcohols impurity after sampling analysis is handled again 5 minutes.The said process temperature is controlled at about 40 ~ 100 ℃, and the time is 1 ~ 10 hour, and sampling will promptly obtain the NSC 11801 (EC) of high-quality requirement after detecting and reaching requirement after cleaner and NSC 11801 (EC) filtration.
The NSC 11801 (EC) that liquefaction is good is squeezed in the product jar, the ON cycle pump mixes NSC 11801 (EC), with stainless steel pipes the product jar is linked to each other with the removal of impurities column sealing, with the recycle system NSC 11801 (EC) is constantly circulated between removal of impurities post and product jar, sampling analysis moisture, purity and alcohols impurity after 1 ~ 10 hour circulates.Said process requires the temperature of removal of impurities post preferably to be controlled at 40 ~ 100 ℃, and optimization is controlled at 50 ~ 80 ℃; Require the temperature of product jar preferably to be controlled at 40 ~ 100 ℃, optimization is controlled at 40 ~ 60 ℃; The full cycle pressure process requires to be controlled at 0.01 ~ 0.3Mpa, and optimization is controlled at 0.05 ~ 0.2Mpa.
Advantage of the present invention and positively effect:In NSC 11801 (EC), add cleaner, and cleaner content accounts for 3%～30% of EC weight, can be efficiently, fast, low consumption NSC 11801 (EC) is purified, thus reach the purpose that upgrading is fallen.
Description of drawings
Fig. 1 is NSC 11801 (EC) unstripped gas analysis of hplc figure.
Fig. 2 is gas chromatographic analysis figure after NSC 11801 (EC) removal of impurities.
Embodiment
The present invention is further illustrated with specific embodiment below, but the present invention is not subjected to the qualification of following embodiment.
Embodiment 1.
See Fig. 1 and Fig. 2, NSC 11801 (EC) raw material, purity is 99.91%, and wherein impure ethylene glycol is 53ppm, and Diethylene Glycol is 28ppm, contains moisture 104ppm.Get above-mentioned EC 500g, the 5A molecular sieve of adding 15%, handled 3 hours in 45 ℃, handling back moisture is that 6.3ppm(adopts Metrohm KF-831 type (Switzerland ten thousand is logical) coulomb moisture tester to measure), purity is 99.97%, ethylene glycol is 21ppm, and Diethylene Glycol is that 5ppm(adopts GC-3900 type (U.S.'s Varian) gas chromatograph to measure).
Embodiment 2.
See Fig. 1 and Fig. 2, NSC 11801 (EC), purity are 99.89%, and ethylene glycol is 103ppm, and Diethylene Glycol is 62ppm, moisture 98ppm.Get above-mentioned EC 500g, the 5A molecular sieve of adding 10% and 3% gac, handled 5 hours in 45 ℃, handling back moisture is that 7.4ppm(adopts Metrohm KF-831 type (Switzerland ten thousand is logical) coulomb moisture tester to measure), purity is 99.95%, ethylene glycol is 43ppm, and Diethylene Glycol is that 27ppm(adopts GC-3900 type (U.S.'s Varian) gas chromatograph to measure).
Embodiment 3.
See Fig. 1 and Fig. 2, NSC 11801 (EC), purity are 99.94%, and ethylene glycol is 33ppm, and Diethylene Glycol is 19ppm, moisture 53ppm.Get above-mentioned EC 500g, the 4A molecular sieve of adding 5%, 5% 5A molecular sieve and 5% 13X molecular sieve, handled 2 hours in 45 ℃, handling back moisture is that 5.7ppm(adopts Metrohm KF-831 type (Switzerland ten thousand is logical) coulomb moisture tester to measure), purity is 99.98%, ethylene glycol is 13ppm, and Diethylene Glycol is that 0ppm(adopts GC-3900 type (U.S.'s Varian) gas chromatograph to measure).
Embodiment 4.
See Fig. 1 and Fig. 2, NSC 11801 (EC), purity are 99.89%, and ethylene glycol is 113ppm, and Diethylene Glycol is 27ppm, moisture 46ppm.In the product jar, squeeze into the EC1000Kg that has liquefied, the 5A molecular sieve of adding 10% and 5% 13X molecular sieve in the removal of impurities post, ON cycle pump circulation sampling analysis after 3 hours, handling back moisture is that 5.8ppm(adopts Metrohm KF-831 type (Switzerland ten thousand is logical) coulomb moisture tester to measure), purity is 99.96%, ethylene glycol is 18ppm, and Diethylene Glycol is that 7ppm(adopts GC-3900 type (U.S.'s Varian) gas chromatograph to measure).
The performance test of the finished product.
1, gets 500g NSC 11801 (EC) at kiln with stainless steel cylinder, detect its moisture, purity and alcohols foreign matter content (see figure 1), adding 10%5A molecular sieve and 5%13X molecular sieve are handled (purity and impurity the results are shown in Figure 2) in steel cylinder, and the moisture of NSC 11801 (EC), purity and the variation of alcohols impurity see Table 1 before and after handling.
As can be seen from Table 1, the method for EC dehydrating and removing impurities of the present invention is fast and simple, easy handling, and the product that obtains satisfies the requirement of high-quality cell-grade.
2, with same batch NSC 11801 (EC) 2000Kg, on average handle by different process in two batches after the liquefaction: technology 1, with the mode of traditional rectification under vacuum dewater, removal of impurities purifies; Technology 2 is handled with dehydrating and removing impurities method of the present invention.Table 2 is comparing results of two kinds of art breading.
As can be seen from Table 2, the quality product after two kinds of art breading does not have notable difference, but the yield of technology 2 illustrates that greater than technology 1 the present invention's effect aspect reducing the wastage is obvious.
The above only is a better embodiment of the present invention, so all equivalences of doing according to the described structure of patent claim of the present invention, feature and principle change or modify, is included in the patent claim of the present invention.
Claims (5)
1. the method for a novel NSC 11801 dehydrating and removing impurities is characterized in that: add in NSC 11801 and be insoluble to NSC 11801 and can adsorb the wherein cleaner of moisture, alcohols and small molecular weight impurity thereof again.
2. the method for a kind of novel NSC 11801 dehydrating and removing impurities according to claim 1 is characterized in that: described cleaner is wherein one or more of spherical low sodium type molecular sieve, activated alumina, gac, silica gel, calcium oxide and the calcium chloride of model 3A, 4A, 5A, 10X, 13X.
3. the method for a kind of novel NSC 11801 (EC) dehydrating and removing impurities according to claim 1 is characterized in that: the add-on of described cleaner is 3% ~ 30% of NSC 11801 (EC) amount.
4. the method for a kind of novel NSC 11801 (EC) dehydrating and removing impurities according to claim 1, it is characterized in that: whole removal of impurities process temperature is controlled at 50 ~ 100 ℃, and the time is 1 ~ 10 hour.
5. the method for a kind of novel NSC 11801 (EC) dehydrating and removing impurities according to claim 1, it is characterized in that: whole process temperature is controlled at 40 ~ 100 ℃, and the time is 2 ~ 8 hours.
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| CN2010105987100A CN102079741A (en) | 2010-12-21 | 2010-12-21 | Novel dewatering and purifying method of ethylene carbonate (EC) |
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| CN2010105987100A CN102079741A (en) | 2010-12-21 | 2010-12-21 | Novel dewatering and purifying method of ethylene carbonate (EC) |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105218509A (en) * | 2015-07-12 | 2016-01-06 | 九江学院 | The minimizing technology of ethylene glycol in a kind of NSC 11801 |
| CN105541782A (en) * | 2015-12-18 | 2016-05-04 | 苏州华一新能源科技有限公司 | Vinylene carbonate purifying method |
| CN106279099A (en) * | 2016-08-10 | 2017-01-04 | 东莞市凯欣电池材料有限公司 | A kind of sulfuric acid vinyl ester except water acid reduction method |
| CN108033943A (en) * | 2017-12-19 | 2018-05-15 | 苏振东 | A kind of preparation method of fluorinated ethylene carbonate |
| CN108160039A (en) * | 2017-11-23 | 2018-06-15 | 孝感市锐思新材科技有限公司 | A kind of preparation method of fluorinated ethylene carbonate purification material |
| CN108191811A (en) * | 2017-12-19 | 2018-06-22 | 苏振东 | A kind of direct fluorination prepares the preparation method of fluorinated ethylene carbonate |
| CN108821969A (en) * | 2018-06-14 | 2018-11-16 | 薛利 | A kind of organic solvent purifying device and purification process |
| CN110420943A (en) * | 2019-08-30 | 2019-11-08 | 苏州金宏气体股份有限公司 | A kind of device and method removing solid particle in ultra-pure ethyl orthosilicate steel cylinder |
| CN111100003A (en) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | Crystallization purification process of high-purity ethylene carbonate |
| CN113636999A (en) * | 2021-07-26 | 2021-11-12 | 珠海理文新材料有限公司 | Water removal and crystallization method of vinylene carbonate |
| CN110420943B (en) * | 2019-08-30 | 2024-05-31 | 金宏气体股份有限公司 | Device and method for removing solid particles in ultra-high purity ethyl silicate steel cylinder |
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| CN101717389A (en) * | 2009-10-29 | 2010-06-02 | 张家港市华盛化学有限公司 | Disacidifying and dewatering method of fluoroethylene carbonate |
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Patent Citations (5)
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| JPH0574485A (en) * | 1991-09-13 | 1993-03-26 | Asahi Chem Ind Co Ltd | Nonaqueous electrolyte secondary battery |
| JPH09227550A (en) * | 1996-02-22 | 1997-09-02 | Mitsui Petrochem Ind Ltd | Purification of ethylene carbonate |
| JP2002193892A (en) * | 2000-12-28 | 2002-07-10 | Ube Ind Ltd | Method for producing high-purity carbonate |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105218509B (en) * | 2015-07-12 | 2017-11-10 | 九江学院 | The minimizing technology of ethylene glycol in a kind of ethylene carbonate |
| CN105218509A (en) * | 2015-07-12 | 2016-01-06 | 九江学院 | The minimizing technology of ethylene glycol in a kind of NSC 11801 |
| CN105541782A (en) * | 2015-12-18 | 2016-05-04 | 苏州华一新能源科技有限公司 | Vinylene carbonate purifying method |
| CN106279099A (en) * | 2016-08-10 | 2017-01-04 | 东莞市凯欣电池材料有限公司 | A kind of sulfuric acid vinyl ester except water acid reduction method |
| CN108160039A (en) * | 2017-11-23 | 2018-06-15 | 孝感市锐思新材科技有限公司 | A kind of preparation method of fluorinated ethylene carbonate purification material |
| CN108191811A (en) * | 2017-12-19 | 2018-06-22 | 苏振东 | A kind of direct fluorination prepares the preparation method of fluorinated ethylene carbonate |
| CN108033943A (en) * | 2017-12-19 | 2018-05-15 | 苏振东 | A kind of preparation method of fluorinated ethylene carbonate |
| CN108191811B (en) * | 2017-12-19 | 2020-12-01 | 张甘泉 | Preparation method for preparing fluoroethylene carbonate by direct fluorination |
| CN108033943B (en) * | 2017-12-19 | 2020-12-01 | 张甘泉 | Preparation method of fluoroethylene carbonate |
| CN108821969A (en) * | 2018-06-14 | 2018-11-16 | 薛利 | A kind of organic solvent purifying device and purification process |
| CN111100003A (en) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | Crystallization purification process of high-purity ethylene carbonate |
| CN111100003B (en) * | 2018-10-25 | 2022-08-12 | 中国石油化工股份有限公司 | Crystallization purification process of high-purity ethylene carbonate |
| CN110420943A (en) * | 2019-08-30 | 2019-11-08 | 苏州金宏气体股份有限公司 | A kind of device and method removing solid particle in ultra-pure ethyl orthosilicate steel cylinder |
| CN110420943B (en) * | 2019-08-30 | 2024-05-31 | 金宏气体股份有限公司 | Device and method for removing solid particles in ultra-high purity ethyl silicate steel cylinder |
| CN113636999A (en) * | 2021-07-26 | 2021-11-12 | 珠海理文新材料有限公司 | Water removal and crystallization method of vinylene carbonate |
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Application publication date: 20110601 |