CN101544551A - Method for purifying high-purity organic solvent-acetone for scientific research - Google Patents
Method for purifying high-purity organic solvent-acetone for scientific research Download PDFInfo
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Abstract
The invention relates to a method for purifying a high-purity organic solvent-acetone for scientific research, which comprises the following steps that: acetone as the raw material is adsorbed to remove impurities by an adsorption resin, dried to remove water by a drying agent, rectified by a rectifying still, filtered and packaged to obtain a chromatographic grade and pesticide residue grade acetone product. The method can obtain the chromatographic acetone product with the purity more than 99.9 percent, ensure that the yield is more than 93 percent and the qualification rate is more than 95 percent, can obtain a 50 to 60 percent pesticide residue grade acetone reagent, can meet the application demand of high efficiency liquid chromatography (HPLC) customers on pesticide residue, and fill in the gap of the national production of pesticide residue grade chromatography reagents; and at the same time, compared with the prior method, the method has high product purity, simple and convenient operation and stable operation, and is suitable for mass production.
Description
Technical field
The invention belongs to chemical technology field, relate to the method for purification of organic solvent, especially a kind of method of purification of high-purity organic solvent-acetone for scientific research.
Background technology
The acetone reagent of Xiao Shouing on the market, its acetone content is about 99.5%, wherein contains impurity such as a small amount of unsaturated hydro carbons, water.This kind acetone can not satisfy the needs of related scientific research test, so this kind acetone must be through being further purified, and the standard that makes its every technical indicator all reach chromatographic grade, pesticide-residue-level acetone could be used.
At present, domestic data about acetone purifying aspect, concentrate on the recycling of acetone in the waste liquid mostly, wherein the patent No. is respectively: 200710028462.4, in 200710060107.5 respectively the recovery with regard to acetone in the waste liquid relevant method and apparatus is provided, but be not suitable for the purification of high purity acetone (content 99.5%).
According to the retrieval, the relevant elaboration of domestic further method of purification about high purity acetone reagent is very few, mainly is owing to few through the content of impurity in the acetone of preliminary purification, is difficult in the rectifying impurity is removed, therefore, The present invention be directed to this technical barrier and propose effective solution.
Summary of the invention
The method of purification that the purpose of this invention is to provide a kind of high-purity organic solvent-acetone for scientific research, this method of purification have characteristics such as technology is simple, residue is easily separated, product purity height.
The present invention is by following scheme implementation:
A kind of method of purification of high-purity organic solvent-acetone for scientific research, the step of purification is as follows:
(1) with raw material acetone by adsorption resin column to remove impurity;
(2) acetone after will adsorbing carries out drying, and measures water content;
(3) water content after the drying is carried out rectifying at the acetone of acceptability limit, the rectifying after-filtration promptly obtains chromatographic grade and pesticide-residue-level acetone product.
And described polymeric adsorbent is Amberlite XAD-4, and siccative is anhydrous potassium sulfate or Anhydrous potassium carbonate.
And, described raw material acetone with the 20-80mL/min velocity flow through adsorption resin column.
And, in the described step (3) in the acetone qualified water content ranges be controlled at≤0.2%.
And the described condition that dried acetone is carried out rectifying is: temperature is 100～300 ℃ at the bottom of the rectifying still, and the acetone fluid temperature is 61 ℃～65 ℃ in the still, 55 ℃～57 ℃ of still top temperature, control reflux ratio 1: 3～5.
Advantage of the present invention and positively effect are:
1, the present invention is that 99.5% acetone is raw material, carries out fractionation by adsorption with polymeric adsorbent as sorbent material and remove wherein impurity with content; adopt anhydrous potassium sulfate or Anhydrous potassium carbonate to remove wherein moisture as siccative; obtain the product acetone of purity 99.9% through absorption, drying, rectification and purification; this method of purification is simple; residue is easily separated; the product purity height, stable, be suitable for large-scale production.
2, this method of purification is adsorbed the impurity of removing in the acetone with polymeric adsorbent, promote acetone content to 99.9%, all other indexs all reach the chromatographic grade requirement, yield rate is increased to 90% by original 70%, saved manpower, reduce the consumption of the energy, more be applicable to industrialized production and application, had remarkable economic efficiency.
3, the product produced of this method of purification after testing its every index meet the requirement of chromatographic grade, pesticide residue grade chromatographic acetone, its acetone content is greater than 99.9%, the rate of recovery is greater than 93%, yield rate reaches 95%, wherein can obtain the pesticide-residue-level acetone reagent of 50-60%, this product can satisfy the application demand of client in pesticide residue of high performance liquid chromatography (HPLC), has filled up the blank that the residual level of domestic farming reagent is produced.
Specific embodiment
The invention will be further described below by specific embodiment, and following examples are descriptive, is not determinate, can not limit protection scope of the present invention with this.
Embodiment 1:
A kind of method of purification of high-purity organic solvent-acetone for scientific research, step is as follows:
(1) raw material acetone (content is about 99.5%) is promoted to the adsorption tower top, wherein adsorbs tower height 2M, diameter 10cm, the amount of interior dress polymeric adsorbent is 4/5 of a tower height, the acetone raw material adsorbs with 20mL/min speed; In tower, acetone fully contacts with polymeric adsorbent, unsaturated hydro carbons impurity is adsorbed, detect absorption fluid quality, it (is the technical requirement of the every index advancing color of effluent liquid spectrum level and the residual level of farming that fluid to be adsorbed is up to the standards, its concrete technical requirement sees Table 1) after, next-step operation entered, and the absorption front-end volatiles that impurity is high are removed.
(2) the effusive acetone of above-mentioned adsorption tower is entered drying tower, tower height 2M, diameter 10cm packs into through baking exsiccant anhydrous potassium sulfate, measures the water content of dry back acetone, and moisture controlled enters next-step operation≤0.2% after water content is qualified; If moisture content, illustrates siccative greater than 0.25% o'clock by water saturation, carry out drying treatment after must changing again.
(3) the stainless steel rectifying still that above-mentioned acetone is after drying injected 100L carries out rectifying; utilize heat-conducting oil heating; temperature is 100 ℃ at the bottom of the control stainless steel still; the acetone fluid temperature is 61 ℃ in the still, goes out 55 ℃ of liquid temps, and the control reflux ratio is in the 1:3 fluid; finished product is behind 0.45 μ mNYL filtering with microporous membrane; the bottling sealing promptly obtains qualified chromatographic grade, pesticide-residue-level acetone product (purity 99.9%) under nitrogen protection, and its front-end volatiles are for further processing.
Embodiment 2:
A kind of method of purification of high-purity organic solvent-acetone for scientific research, step is as follows:
(1) raw material acetone (content is about 99.5%) is promoted to the adsorption tower top, absorption tower height 2M, diameter 10cm, the amount of interior dress polymeric adsorbent is 4/5 of a tower height, and the acetone raw material adsorbs with 80mL/min speed, and the absorption fluid enters next-step operation after the assay was approved; And the absorption front-end volatiles that impurity is high are removed.
(2) effluent liquid with above-mentioned adsorption tower enters drying tower, tower height 2M, and diameter 10cm packs into through baking exsiccant Anhydrous potassium carbonate, measures the water content of dry back acetone, and moisture controlled enters next-step operation≤0.2% after water content is qualified; When moisture content greater than 0.25% the time, siccative is described by water saturation, carry out drying treatment after must changing again.
(3) the stainless steel rectifying still that above-mentioned acetone is after drying injected 120L carries out rectifying.Utilize heat-conducting oil heating, temperature is 300 ℃ at the bottom of the control stainless steel still, the acetone fluid temperature is 65 ℃ in the still, go out 57 ℃ of liquid temps, the control reflux ratio was 1: 5 fluid, finished product is behind 0.45 μ mNYL filtering with microporous membrane, and the bottling sealing promptly obtains qualified chromatographic grade, pesticide-residue-level acetone product (purity 99.9%) under nitrogen protection; Its front-end volatiles are for further processing.
The mensuration of the residual level of farming index:
The residual level of farming index: sample except that satisfying the chromatographic grade index, concentrate 300 times after, with detected all the assorted peaks of GC-ECD gas chromatograph (with γ-phenyl-hexachloride ratio of peak) all be lower than 10ng/L, farming is qualified for residual grade.Pass through the high pure acetone that purifying is crossed like this, can obtain the pesticide residue grade chromatographic product acetone of 50-60% through further purification.
Table 1: the technical indicator of raw material, chromatogram, pesticide-residue-level acetone
Claims (5)
1, a kind of method of purification of high-purity organic solvent-acetone for scientific research is characterized in that: the step of purification is as follows:
(1) with raw material acetone by adsorption resin column to remove impurity;
(2) acetone after will adsorbing carries out drying, and measures water content;
(3) water content after the drying is carried out rectifying at the acetone of acceptability limit, the rectifying after-filtration promptly obtains chromatographic grade and pesticide-residue-level acetone product.
2, the method for purification of a kind of high-purity organic solvent-acetone for scientific research according to claim 1 is characterized in that: described polymeric adsorbent is Amberlite XAD-4, and siccative is anhydrous potassium sulfate or Anhydrous potassium carbonate.
3, the method for purification of a kind of high-purity organic solvent-acetone for scientific research according to claim 1 is characterized in that: described raw material acetone with the 20-80mL/min velocity flow through adsorption resin column.
4, the method for purification of a kind of high-purity organic solvent-acetone for scientific research according to claim 1 is characterized in that: in the described step (3) in the acetone qualified water content ranges be controlled at≤0.2%.
5, the method for purification of a kind of high-purity organic solvent-acetone for scientific research according to claim 1, it is characterized in that: the described condition that dried acetone is carried out rectifying is: temperature is 100～300 ℃ at the bottom of the rectifying still, the acetone fluid temperature is 61 ℃～65 ℃ in the still, 55 ℃～57 ℃ of still top temperature, control reflux ratio 1:3～5.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101759537A (en) * | 2010-01-28 | 2010-06-30 | 安徽时联特种溶剂股份有限公司 | Method for producing HPLC-grade acetone |
| CN101973859A (en) * | 2010-10-29 | 2011-02-16 | 上海化学试剂研究所 | Method and device for preparing ultrapure acetone |
| CN102040496A (en) * | 2010-12-29 | 2011-05-04 | 天津市康科德科技有限公司 | Purification method of high-purity organic solvent 4-methyl-2-pentanone |
| CN102040497A (en) * | 2010-12-29 | 2011-05-04 | 天津市康科德科技有限公司 | Purification method of high-purity organic solvent butanone |
| CN102329200A (en) * | 2011-07-19 | 2012-01-25 | 天津基准化学试剂有限公司 | Method for preparing high-voltage electrophoresis reagent acetone |
| CN102417441A (en) * | 2011-12-26 | 2012-04-18 | 天津市康科德科技有限公司 | Method for purifying chromatographic grade organic solvent methyl tertiary butyl ether |
| CN102452892A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Purification method for pesticide residue-grade dichloromethane for extraction |
| CN104119216A (en) * | 2014-08-01 | 2014-10-29 | 苏州市晶协高新电子材料有限公司 | Production method of continuous acetone dehydration |
| CN105175236A (en) * | 2015-09-25 | 2015-12-23 | 江阴润玛电子材料股份有限公司 | Ultra-clean high-purity acetone production method |
| CN113321576A (en) * | 2021-05-31 | 2021-08-31 | 成都市科隆化学品有限公司 | Benzene-free acetone and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101759537A (en) * | 2010-01-28 | 2010-06-30 | 安徽时联特种溶剂股份有限公司 | Method for producing HPLC-grade acetone |
| CN101759537B (en) * | 2010-01-28 | 2014-06-18 | 安徽时联特种溶剂股份有限公司 | Method for producing HPLC-grade acetone |
| CN102452892A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Purification method for pesticide residue-grade dichloromethane for extraction |
| CN101973859A (en) * | 2010-10-29 | 2011-02-16 | 上海化学试剂研究所 | Method and device for preparing ultrapure acetone |
| CN101973859B (en) * | 2010-10-29 | 2014-12-31 | 上海化学试剂研究所 | Method and device for preparing ultrapure acetone |
| CN102040497A (en) * | 2010-12-29 | 2011-05-04 | 天津市康科德科技有限公司 | Purification method of high-purity organic solvent butanone |
| CN102040496A (en) * | 2010-12-29 | 2011-05-04 | 天津市康科德科技有限公司 | Purification method of high-purity organic solvent 4-methyl-2-pentanone |
| CN102329200B (en) * | 2011-07-19 | 2013-08-14 | 天津基准化学试剂有限公司 | Method for preparing high-voltage electrophoresis reagent acetone |
| CN102329200A (en) * | 2011-07-19 | 2012-01-25 | 天津基准化学试剂有限公司 | Method for preparing high-voltage electrophoresis reagent acetone |
| CN102417441A (en) * | 2011-12-26 | 2012-04-18 | 天津市康科德科技有限公司 | Method for purifying chromatographic grade organic solvent methyl tertiary butyl ether |
| CN104119216A (en) * | 2014-08-01 | 2014-10-29 | 苏州市晶协高新电子材料有限公司 | Production method of continuous acetone dehydration |
| CN104119216B (en) * | 2014-08-01 | 2016-02-24 | 苏州市晶协高新电子材料有限公司 | A kind of production method of acetone serialization dehydration |
| CN105175236A (en) * | 2015-09-25 | 2015-12-23 | 江阴润玛电子材料股份有限公司 | Ultra-clean high-purity acetone production method |
| CN113321576A (en) * | 2021-05-31 | 2021-08-31 | 成都市科隆化学品有限公司 | Benzene-free acetone and preparation method thereof |
| CN113321576B (en) * | 2021-05-31 | 2023-06-13 | 成都市科隆化学品有限公司 | Non-propiophenone and preparation method thereof |
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Effective date of registration: 20100108 Address after: Tianjin City, Hebei District Yu Guan Road No. 15 post encoding: 300230 Applicant after: Tianjin Concord science and Technology Co., Ltd. Co-applicant after: National Institute of Metrology, China Address before: Tianjin City, Hebei District Yu Guan Road No. 15 post encoding: 300230 Applicant before: Tianjin Concord Technology Co., Ltd. |
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