CN102452892B - Purification method for pesticide residue-grade dichloromethane for extraction - Google Patents
Purification method for pesticide residue-grade dichloromethane for extraction Download PDFInfo
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- CN102452892B CN102452892B CN201010514089.5A CN201010514089A CN102452892B CN 102452892 B CN102452892 B CN 102452892B CN 201010514089 A CN201010514089 A CN 201010514089A CN 102452892 B CN102452892 B CN 102452892B
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Abstract
The present invention discloses a purification method for pesticide residue-grade dichloromethane for extraction. According to the method, an adsorbent adsorbing treatment is firstly performed to remove impurities, wherein the boiling point of the impurities is close to the boiling point of dichloromethane; a drying agent is adopted to remove water; after drying, treatments of refining and purifying are performed to obtain the finished product. According to the present invention, the dichloromethane with the content of 99.5% is adopted as the raw material; after treatments of adsorbing, drying and refining, the pesticide residue-grade dichloromethane with the purity more than 99.8% is obtained, and the yield is more than 80%, wherein various technical indicators meet the requirements of the pesticide residue-grade dichloromethane. The pesticide residue-grade dichloromethane purified by the method of the present invention has high purity, and the interference on the organic matter determination due to the impurities in the dichloromethane can be eliminated so as to improve the repeatability and the accuracy of the organic matter determination in the water. The pesticide residue-grade dichloromethane purified by the method of the present invention is particularly adopted as the extraction solvent for the organic matter analysis in the water, and the interference on the organic matter analysis due to the impurities in the dichloromethane can be effectively eliminated.
Description
Technical field
The present invention relates to extraction solvent used in Analysis of Organic Substances in the method for purification, particularly water quality of the residual level methylene dichloride of a kind of agriculture, effectively can to remove in methylene dichloride impurity to the interference of Analysis of Organic Substances.
Background technology
The organism kinds that occurring in nature exists is various; some organism has acute or chronic, direct or indirect intoxicating effect to human body; what have can also be accumulated in the DNA structure that organization internal changes cell; " three cause " (carcinogenic, teratogenesis, mutagenesis) is produced to human body; serious harm HUMAN HEALTH; organism environmental pollution and residue problem, cause concern and the attention of countries in the world, thus analysis and identification organic pollutant to protection of the environment and people ' s health significant.
Because in most sample, organic content is low, extraction comparison is difficult.People mostly first by sample after pre-treatment enrichment is concentrated, then carry out qualitative and quantitative analysis by analytical technology.At present, the technology such as liquid-liquid extraction, Solid-Phase Extraction is mainly contained for Sample Pretreatment Technique.Methylene dichloride is a kind of widely used organic solvent, also be important extraction agent, in organic mensuration, play very important effect, China's standard method " the mensuration vapor-phase chromatography of GB/T 14552-1993 water and soil quality organophosphorus pesticide " etc. is exactly adopt methylene dichloride as extraction solvent.General dichloromethane extraction process be sample under condition of different pH with dichloromethane extraction repeatedly, combining extraction liquid concentrated several times, then adopt different instrument to analyze.Because current commercially available analytical pure or chromatographically pure dichloromethane solvent are still containing some impurity, and these impurity also have larger response in instrument after being concentrated several times, the repeatability of analytical results and accuracy are had a great impact, therefore should be purified before use, after dichloromethane solvent concentrates several times after purifying, just be can be used as extraction agent through instrument testing without component residue impurity.
Summary of the invention
For the deficiency that analytical pure methylene dichloride exists in organic substance extraction process, the invention provides the method for purification of the residual level methylene dichloride of the agriculture used in a kind of organic substance extraction process, the methylene dichloride purity that the inventive method obtains is high, and object product yield is high, easy and simple to handle.
The method of purification of pesticide residue-grade dichloromethane for extraction of the present invention comprises following content: first methylene dichloride raw material carries out adsorption treatment, sorbent material is gac or 5A molecular sieve, methylene dichloride after adsorption treatment carries out drying treatment, dried methylene dichloride distills, the light constituent of distillation removing raw materials quality mark 2% ~ 10% and the heavy constituent of raw materials quality mark 2 ~ 10%, collect middle runnings and be extracted with the residual level methylene dichloride of agriculture.
In the inventive method, methylene dichloride raw material is commercially available analytical pure methylene dichloride, or chromatographic pure dichloromethane etc., the quality purity of general methylene dichloride is about 99.5%.
In the inventive method, adsorption treatment adopts conventional adsorption column, and loaded by sorbent material in adsorption column, methylene dichloride raw material carries out adsorption cleaning process by adsorption column to methylene dichloride.Sorbent material is commercially available gac or 5A molecular sieve etc., and the granularity of sorbent material is generally 20 ~ 40 orders.Methylene dichloride raw material is generally every 50mL sorbent material (30 ~ 50) mL/min methylene dichloride raw material by the flow velocity of sorbent material.Impurity in sorbent material or in adsorption column enters methylene dichloride, and will carry out purifying treatment before sorbent material and adsorption column use, or a small amount of material first flowed out is abandoned, the material abandoned is generally 10% ~ 100% of sorbent material volume.
In the inventive method, drying siccative is anhydrous sodium sulphate, adopts the dry post that siccative is housed, and after dry, the water content control of methylene dichloride is in≤0.01% (quality).
In the inventive method, distillation can adopt batch distillation, also can adopt continuous still battery, and distillation temperature is 50 ~ 60 DEG C.
In the method for purification of a kind of pesticide residue-grade dichloromethane for extraction of the present invention, the impurity that key is (1) adopts adsorbent removing close with methylene dichloride boiling point, siccative dewaters, improve repeatability and the accuracy of Analysis of Organic Substances in water quality, light, the last running of distillation removing containing impurity.(2) the methylene dichloride product purity of the present invention's purification is high, easy and simple to handle, and product recovery rate is high.In the method for purification of pesticide residue-grade dichloromethane for extraction of the present invention, through adsorbent, siccative dewaters, the residual level methylene dichloride of agriculture that purity is greater than 99.8% can be obtained after refining, product yield is greater than 80%, and wherein all technical all reaches the requirement of the residual level methylene dichloride of agriculture, is specially adapted to the extraction solvent that Analysis of Organic Substances in water quality is used, effectively can remove impurity in methylene dichloride and, to the interference of Analysis of Organic Substances, greatly improve accuracy and the repeatability of analytic process.
Embodiment
Set forth technical scheme of the present invention below in conjunction with embodiment, but be not limited to the embodiment of the present invention.
Embodiment 1
(1) raw material methylene dichloride (analytical pure) 500mL is added in adsorption column, (φ 20mm × 350mm, lower end has cock to control) in, 2/3rds sorbent materials are filled in adsorption column, in 200 DEG C of oven dry after sorbent material cleans with distilled water, methylene dichloride flows through the adsorption column that sorbent material is housed with 20mL/min flow velocity, discard the 20mL solution first flowed out.
(2) methylene dichloride adsorbed through adsorption column is added (φ 20mm × 350mm in dry post, lower end has cock to control) in, 2/3rds siccative are filled in dry post, siccative anhydrous sodium sulphate is through 500 DEG C of oven dry, methylene dichloride flows through the adsorption column that sorbent material is housed with 20mL/min flow velocity, discard the 20mL solution first flowed out, control water content≤0.01% of methylene dichloride.
(3) methylene dichloride dried through super-dry post is added in batch distillation device, utilize heating in water bath, bath temperature is 50 DEG C, and it is 10mL/min that control flow check goes out flow velocity, discard lighting end 20mL and last running 20mL, collect outflow middle runnings liquid and be qualified product.
Embodiment 2
(1) raw material methylene dichloride (analytical pure) 600mL is added adsorption column (φ 20mm × 350mm, lower end has cock to control) in, 2/3rds sorbent materials are filled in adsorption column, in 180 DEG C of oven dry after sorbent material cleans with distilled water, methylene dichloride flows through the adsorption column that sorbent material is housed with 30mL/min flow velocity, discard the 20mL solution first flowed out.
(2) methylene dichloride adsorbed through adsorption column is added dry post (φ 20mm × 350mm, lower end has cock to control) in, 2/3rds siccative are filled in dry post, siccative anhydrous sodium sulphate is through 550 DEG C of oven dry, methylene dichloride flows through the adsorption column that sorbent material is housed with 30mL/min flow velocity, discard the 20mL solution first flowed out, control water content≤0.01% of methylene dichloride.
(3) methylene dichloride dried through super-dry post is added in glass rectifier unit, utilize water-bath to add, bath temperature is 60 DEG C, and it is 20mL/min that control flow check goes out flow velocity, discard lighting end 20mL and last running 20mL, collect effluent liquid and be qualified product.
Table 1 agriculture residual level methylene dichloride technical indicator
Claims (4)
1. the method for purification of a pesticide residue-grade dichloromethane for extraction, it is characterized in that comprising following content: first methylene dichloride raw material carries out adsorption treatment, sorbent material is gac or 5A molecular sieve, methylene dichloride after adsorption treatment carries out drying treatment, dried methylene dichloride distills, distillation temperature is 50 ~ 60 DEG C, and the light constituent of distillation removing raw materials quality mark 2% ~ 10% and the heavy constituent of raw materials quality mark 2 ~ 10%, collect middle runnings and be extracted with the residual level methylene dichloride of agriculture; Siccative is anhydrous sodium sulphate, and adopt the dry post that siccative is housed to carry out drying treatment, after dry, the water content of methylene dichloride controls in mass≤0.01%; Methylene dichloride raw material is analytical pure methylene dichloride, or chromatographic pure dichloromethane.
2. in accordance with the method for claim 1, it is characterized in that: before sorbent material and adsorption column use, carry out purifying treatment.
3. in accordance with the method for claim 1, it is characterized in that: during adsorption treatment, a small amount of material first flowed out is abandoned, and the material abandoned is 10% ~ 100% of sorbent material volume.
4. in accordance with the method for claim 1, it is characterized in that: distillation adopts batch distillation, or adopt continuous still battery.
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| CN102452892B true CN102452892B (en) | 2015-01-14 |
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| JP2014221727A (en) * | 2013-05-13 | 2014-11-27 | 昭和電工株式会社 | Dichloromethane purification method and method of producing difluoromethane using the same |
| CN106365943B (en) * | 2016-08-31 | 2019-02-12 | 中国船舶重工集团公司第七一八研究所 | A kind of preparation method of the residual grade benzene of agriculture |
| CN109374794A (en) * | 2018-09-20 | 2019-02-22 | 福建中医药大学 | A method of reducing methylene chloride evaporative light scattering detector noise |
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| CN2573497Y (en) * | 2002-09-20 | 2003-09-17 | 史永刚 | Adsorption column for purifying carbon tetrachloride |
| CN101450890A (en) * | 2007-11-30 | 2009-06-10 | 山东方兴科技开发有限公司 | Removal method for recovery of water in dichloroethane |
| CN101544551A (en) * | 2009-05-06 | 2009-09-30 | 天津市康科德科技有限公司 | Method for purifying high-purity organic solvent-acetone for scientific research |
| CN101570484A (en) * | 2009-06-15 | 2009-11-04 | 天津市康科德科技有限公司 | Method for preparing pesticide residue grade chromatographic ethyl acetate |
| CN101781163B (en) * | 2010-01-28 | 2013-03-20 | 安徽时联特种溶剂股份有限公司 | Preparation method of high-purity halogenated hydrocarbon used for liquid chromatogram |
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