CN104402666B - A kind of purification process of MOS level chloroform - Google Patents
A kind of purification process of MOS level chloroform Download PDFInfo
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- CN104402666B CN104402666B CN201410558834.4A CN201410558834A CN104402666B CN 104402666 B CN104402666 B CN 104402666B CN 201410558834 A CN201410558834 A CN 201410558834A CN 104402666 B CN104402666 B CN 104402666B
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Abstract
The invention discloses the purification process of a kind of MOS level chloroform. This purification process includes: chloroform crude product is filtered by (1) through SBA-15 molecular sieve chelate sorbent, obtains filtrate; (2) adopt rectifier unit to carry out rectification described filtrate, obtain rectification liquid; (3) described rectification liquid is carried out ultrafiltration. The purification process of the present invention adopt SBA-15 molecular sieve chelate sorbent be filtered, EtOH in primary industry level chloroform, contained carbonyl impurities, metal ion etc. are had and have very strong absorbability by SBA-15 molecular sieve chelate sorbent, can effectively remove impurity therein, improve the purity of product. By the chloroform after SBA-15 molecular sieve chelate sorbent filters successively through rectification and ultrafiltration, MOS level chloroform can be obtained, simplify operation sequence, ensure that the quality of product and relatively low production cost simultaneously.
Description
Technical field
The present invention relates to the technical field that chloroform purifies, particularly relate to the purification process of a kind of MOS level chloroform.
Background technology
Chloroform is a kind of colourless transparent liquid, has the refractive power sweet, high of special odor, taste, does not fire, matter weight, volatile. Its sterling, to photaesthesia, meets light note and generation Oxidation in air. It is a kind of organic synthesis raw material, is mainly used to produce freon (such as F-21, F-22, F-23), dyestuff and medicine, medically, is commonly used for anesthetis. Additionally, it also acts as antibiotic, spice, oils and fats, resin, the solvent of rubber and extractant. The fire-fighting liquid that may be manufactured without freezing is mixed with carbon tetrachloride. It is additionally operable to the propellant powder of aerosol, corn fumigant and calibration temperature titer. In recent years due to the fast development of electronics industry, MOS level chloroform is often applied to the abluent of electronic industrial products.
In prior art, the purification of high-purity chloroform is all wash after sulphuric acid jolting, calcium chloride distills after alkali alumina post adsorbs after drying and namely obtains final products, shortcoming is complex operation, product exists metal ion, have a strong impact on the purity of product due to the existence of foreign ion, limit industrialization and use.
Summary of the invention
In view of this, the present invention provides the purification process of a kind of MOS level chloroform, and this purification process has simple to operate, and the purity of the refined product obtained through this purification process is higher.
The purification process of a kind of MOS level chloroform, comprises the following steps:
(1) chloroform crude product is filtered through SBA-15 molecular sieve chelate sorbent, obtain filtrate;
(2) adopt rectifier unit to carry out rectification described filtrate, obtain rectification liquid;
(3) described rectification liquid is carried out ultrafiltration, obtain MOS level chloroform.
Here term " molecular sieve chelate sorbent " and term " adsorbent of molecular sieve " generally in the art are same connotation. The chloroform of term " chloroform crude product " i.e. technical grade purity, for instance purity is 95.0～99.0wt%.Molecular sieve chelate sorbent is preferably employing and is through impregnation with method modification, to improve the effect of its filtration, be certainly also adopted by without infusion process modification or additive method is modified. This modified detailed process is, SBA-15 molecular sieve impregnates 24～36h then dry gained in impregnation liquid. Impregnation liquid can be dissolved in the mixed solvent being mixed with 85wt% phosphoric acid, diisobutyl phthalate, isoamyl acetate by 2,4 dinitrophenyl hydrazine, the activated alumina that grinds, then adds obtained by the ultra-pure water of 18.2M Ω .cm. In the component of this impregnation liquid, 2, the mass ratio of 4-dinitrophenylhydrazine and activated alumina is 1:0.7～0.9,2, the amount ratio of 4-dinitrophenylhydrazine and phosphoric acid is 1g:(10～14) ml, 2, the amount ratio of 4-dinitrophenylhydrazine and diisobutyl phthalate is 1g:(1～2) ml, 2, the amount ratio of 4-dinitrophenylhydrazine and isoamyl acetate is 1g:(2～4) ml, the amount ratio of 2,4 dinitrophenyl hydrazine and ultra-pure water is 1g:(6～10) other impregnation liquid of being familiar with of the certain this area of ml are applied equally to this programme.
In rectification, the pressure of its filtration is preferably 0.1～0.15Mpa, and temperature is 30～40 DEG C. Distillation process specifically, first filtrate is inserted in rectifier unit 61～62 DEG C according to reflux ratio be 10:1～3 reflux 0.5～1h, remove front-end volatiles obtain treating rectification liquid; Then, will treat that rectification liquid carries out rectification with the flow velocity of 10～20mL/min. The device of rectification can adopt any device that can be used for distillation operation that this area is general, for instance quartz glass fractionating tower etc.
In ultrafiltration, ultrafiltration adopts hollow fiber ultrafiltration membrane to carry out. The aperture of hollow fiber ultrafiltration membrane, less than 0.02 μm, all can adopt specification well-known to those skilled in the art as its hollow fiber ultrafiltration membrane external diameter and internal diameter.
The purification process of the present invention adopt SBA-15 molecular sieve chelate sorbent be filtered, EtOH in primary industry level chloroform, contained carbonyl impurities, metal ion etc. are had and have very strong absorbability by SBA-15 molecular sieve chelate sorbent, can effectively remove impurity therein, improve the purity of product. By the chloroform after SBA-15 molecular sieve chelate sorbent filters successively through rectification and ultrafiltration, MOS level chloroform can be obtained, simplify operation sequence, ensure that the quality of product and relatively low production cost simultaneously.
Detailed description of the invention
Technical scheme is further illustrated below in conjunction with embodiment.
Embodiment 1
The preparation of SBA-15 molecular sieve chelate sorbent post: take 20g2,4-dinitrophenylhydrazine, 14g activated alumina are dissolved in 240ml85% phosphoric acid, 20ml diisobutyl phthalate, 40ml isoamyl acetate after grinding, add the ultra-pure water composition impregnation liquid of 160ml18.2M Ω .cm, at room temperature 400gSBA-15 molecular sieve is added in this impregnation liquid, filtering after dipping 24h, at 100 DEG C of temperature, dry 16h, namely obtains SBA-15 molecular sieve chelate sorbent 449g, dress post, stand-by.
The purification of chloroform crude product: be that 90.0wt% technical grade chloroform raw material passes into the SBA-15 molecular sieve chelate sorbent that step (1) obtains at 0.15MPa, 40 DEG C of temperature and filters by 1000g content, filtrate is through glass rectifier unit 62 DEG C backflow 1h, adjustment reflux ratio is 10:3, remove front-end volatiles, carrying out rectification with the flow velocity of 20mL/min, collecting essence distillate via hole diameter is that 0.02 μm of hollow fiber ultrafiltration membrane filtration is MOS level chloroform.Your chloroform content 99.61wt% of purification difference, yield 86.32% in this example. After testing, the index such as the moisture in product, non-volatile matter, free acid, chloride, free chlorine, metal ion all meets the standard of MOS level chloroform.
Embodiment 2
The preparation of SBA-15 molecular sieve chelate sorbent post: take 25g2,4-dinitrophenylhydrazine mill, 20g activated alumina are dissolved in 300ml85% phosphoric acid, 37.5ml phthalic acid diisobutyl ester, 75ml isoamyl acetate after grinding in, it is blended into the ultra-pure water composition impregnation liquid of 200ml18.2M Ω .cm, at room temperature 400gSBA-15 molecular sieve is added in this impregnation liquid, filtering after dipping 30h, at 100 DEG C of temperature, dry 16h, namely obtains SBA-15 molecular sieve chelate sorbent 463g, dress post, stand-by.
The purification of chloroform crude product: be that 90.0wt% technical grade chloroform raw material passes into the SBA-15 molecular sieve chelate sorbent that step (1) obtains at 0.125MPa, 35 DEG C of temperature and filters by 1000g content, filtrate is through glass rectifier unit 61.5 DEG C backflow 0.75h, adjustment reflux ratio is 10:2, remove front-end volatiles, carrying out rectification with the flow velocity of 15mL/min, collecting essence distillate via hole diameter is that 0.02 μm of hollow fiber ultrafiltration membrane ultrafiltration is MOS level chloroform. The chloroform content 99.85wt% of purified product in this example, yield 89.52%. After testing, the index such as the moisture in product, non-volatile matter, free acid, chloride, free chlorine, metal ion all meets the standard of MOS level chloroform.
Embodiment 3
The preparation of SBA-15 molecular sieve chelate sorbent post: take 30g2,4-dinitrophenylhydrazine, 27g activated alumina are dissolved in 360ml85% phosphoric acid, 60ml diisobutyl phthalate, 120ml isoamyl acetate after grinding, it is blended into the ultra-pure water composition impregnation liquid of 240ml18.2M Ω .cm, at room temperature 400gSBA-15 molecular sieve is added in this impregnation liquid, filtering after dipping 36h, at 100 DEG C of temperature, dry 16h, namely obtains SBA-15 molecular sieve chelate sorbent 469g, dress post, stand-by.
The purification of chloroform crude product: be that 90.0wt% technical grade chloroform raw material passes into the SBA-15 molecular sieve chelate sorbent that step (1) obtains at 0.1MPa, 30 DEG C of temperature and filters by 1000g content, filtrate is through glass rectifier unit 61 DEG C backflow 0.5h, adjustment reflux ratio is 10:1, remove front-end volatiles, carrying out rectification with the flow velocity of 10mL/min, collecting essence distillate via hole diameter is that 0.02 μm of hollow fiber ultrafiltration membrane ultrafiltration is MOS level chloroform. The content 99.91wt% of chloroform, yield 90.12% in the chloroform product of purification obtained in this example. After testing, the index such as the moisture in product, non-volatile matter, free acid, chloride, free chlorine, metal ion all meets the standard of MOS level chloroform.
Specific performance such as following table by the purified product of embodiment 1～3:
Owing to the numerical range of each technological parameter involved in the present invention can not all embody in the above-described embodiments, as long as but the completely envisioned any numerical value fallen in this numerical range above-mentioned of those skilled in the art all can implement the present invention, certainly also includes the combination in any of occurrence in some numerical rangies. Herein, for the consideration of length, eliminating and provide the embodiment of occurrence in certain one or more numerical range, this is not to be construed as the insufficient disclosure of technical scheme.
Applicant states, the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment, but the invention is not limited in above-mentioned detailed process equipment and technological process, namely do not mean that the present invention has to rely on above-mentioned detailed process equipment and technological process could be implemented.The equivalence of each raw material of product of the present invention, it will be clearly understood that any improvement in the present invention, is replaced and the interpolation of auxiliary element, concrete way choice etc. by person of ordinary skill in the field, all falls within protection scope of the present invention and open scope.
Claims (7)
1. the purification process of a MOS level chloroform, it is characterised in that comprise the following steps:
(1) chloroform crude product is filtered through SBA-15 molecular sieve chelate sorbent, obtain filtrate;
(2) adopt rectifier unit to carry out rectification described filtrate, obtain rectification liquid;
(3) described rectification liquid is carried out ultrafiltration, obtain MOS level chloroform;
Wherein, molecular sieve chelate sorbent described in step (1) is by SBA-15 molecular sieve impregnates 24～36h then dry gained in impregnation liquid;
Wherein, described impregnation liquid is be dissolved in the mixed solvent being mixed with 85wt% phosphoric acid, diisobutyl phthalate, isoamyl acetate by 2,4 dinitrophenyl hydrazine, the activated alumina that grinds, then adds obtained by the ultra-pure water of 18.2M Ω .cm.
2. purification process according to claim 1, it is characterised in that the mass ratio of described 2,4 dinitrophenyl hydrazine and activated alumina is 1:0.7～0.9.
3. purification process according to claim 1, it is characterised in that the amount ratio of described 2,4 dinitrophenyl hydrazine and phosphoric acid is 1g:(10～14) ml;
Preferably, described 2,4 dinitrophenyl hydrazine is 1g:(1～2 with the amount ratio of diisobutyl phthalate) ml;
Preferably, described 2,4 dinitrophenyl hydrazine is 1g:(2～4 with the amount ratio of isoamyl acetate) ml;
Preferably, described 2,4 dinitrophenyl hydrazine is 1g:(6～10 with the amount ratio of ultra-pure water) ml.
4. purification process according to claim 1, it is characterised in that the pressure filtered described in step (1) is 0.1～0.15MPa, and temperature is 30～40 DEG C.
5. purification process according to claim 1, it is characterised in that described in step (1), the purity of chloroform crude product is 95.0～99.0wt%.
6. purification process according to claim 1, it is characterized in that, distillation process described in step (2) specifically, first filtrate is inserted in rectifier unit 61～62 DEG C according to reflux ratio be 10:1～3 reflux 0.5～1h, remove front-end volatiles obtain treating rectification liquid; Then, will treat that rectification liquid carries out rectification with the flow velocity of 10～20mL/min.
7. purification process according to claim 1, it is characterised in that ultrafiltration described in step (3) adopts hollow fiber ultrafiltration membrane, and the aperture of hollow fiber ultrafiltration membrane is less than 0.02 μm.
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| CN112284841A (en) * | 2019-07-25 | 2021-01-29 | 中国科学院沈阳应用生态研究所 | Method for quickly removing ethanol in chloroform |
| CN114394881B (en) * | 2022-01-26 | 2023-02-03 | 南京化学试剂股份有限公司 | Refining method of high-yield high-purity trichloromethane |
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| CN102093160B (en) * | 2010-12-29 | 2013-05-29 | 天津市康科德科技有限公司 | Method for preparing chromatographically-pure trichloromethane |
| CN102303854B (en) * | 2011-07-28 | 2013-05-15 | 国药集团化学试剂有限公司 | Purification method of monopotassium phosphate |
| CN103951543B (en) * | 2014-04-18 | 2016-04-20 | 广东华特气体股份有限公司 | A kind of trifluoromethane purification devices and purification process |
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