CN102452892A - 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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- CN102452892A CN102452892A CN2010105140895A CN201010514089A CN102452892A CN 102452892 A CN102452892 A CN 102452892A CN 2010105140895 A CN2010105140895 A CN 2010105140895A CN 201010514089 A CN201010514089 A CN 201010514089A CN 102452892 A CN102452892 A CN 102452892A
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- methylene dichloride
- dichloromethane
- pesticide residue
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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 used extraction solvent during organism is analyzed in the method for purification, particularly water quality of the residual level of a kind of farming methylene dichloride, can effectively remove the interference that impurity is analyzed organism in the methylene dichloride.
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, and what have can also be accumulated in the dna structure that organization internal changes cell, and human body is produced " three cause " (carcinogenic, teratogenesis, mutagenesis); The serious harm HUMAN HEALTH; Organism environmental pollution and residue problem cause the concern and the attention of countries in the world, so analysis and evaluation organic pollutant are significant to protection environment and people ' s health.
Because organic content is low in most samples, extraction is relatively more difficult.The most elder generation of people after the pre-treatment enrichment concentrates, carries out qualitative and quantitative analysis through analytical technology with sample again.At present, be used for the sample pre-treatments technology and mainly contain technology such as liquid-liquid extraction, SPE.Methylene dichloride is a kind of widely used organic solvent; It also is important extraction agent; In organic mensuration, play important effect, China's standard method " the mensuration vapor-phase chromatography of GB/T 14552-1993 water and soil loamy texture amount organophosphorus pesticide " etc. is exactly to adopt methylene dichloride as extraction solvent.General dichloromethane extraction process be sample under condition of different pH with dichloromethane extraction repeatedly, combining extraction liquid also concentrates several times, adopts different instruments to analyze then.Because present commercially available analytical pure or chromatographically pure dichloromethane solvent still contain some impurity; And these impurity also have bigger response in instrument after concentrating several times; Repeatability and accuracy to analytical results have very big influence; Therefore should it be purified before use, the back dichloromethane solvent of purifying concentrates several times and just not can be used as extraction agent after instrument testing has the composition residual impurity.
Summary of the invention
The deficiency that in the organic substance extraction process, exists to the analytical pure methylene dichloride; The present invention provides the method for purification of the agricultural residual level methylene dichloride that uses in a kind of organic substance extraction process; The methylene dichloride purity that the inventive method obtains is high, and the purpose product yield is high, and is easy and simple to handle.
The method of purification that the present invention extracts with the residual level of farming methylene dichloride comprises following content: the methylene dichloride raw material at first carries out adsorption treatment; Sorbent material is gac or 5A molecular sieve; Methylene dichloride after the adsorption treatment carries out drying treatment; Dried methylene dichloride distills, and the heavy constituent of the light constituent and the raw materials quality mark 2～10% of raw materials quality mark 2%～10% are removed in distillation, collects middle runnings and obtains extraction with the residual level of farming methylene dichloride.
In the inventive method, the methylene dichloride raw material is commercially available analytical pure methylene dichloride, or the chromatographically pure methylene dichloride etc., the quality purity of general methylene dichloride is about 99.5%.
In the inventive method, adsorption treatment adopts conventional adsorption column, and sorbent material is packed in the adsorption column, and the methylene dichloride raw material carries out adsorption cleaning through adsorption column to methylene dichloride to be handled.Sorbent material is commercially available gac or 5A molecular sieve etc., and the granularity of sorbent material is generally 20～40 orders.The methylene dichloride raw material is generally every 50mL sorbent material (30～50) mL/min methylene dichloride raw material through the flow velocity of sorbent material.Impurity in sorbent material or in the adsorption column gets into methylene dichloride, and sorbent material and adsorption column will carry out purifying treatment before using, and perhaps at first effusive a small amount of material is abandoned, and the material of abandoning is generally 10%～100% of sorbent material volume.
In the inventive method, drying uses siccative to be SODIUM SULPHATE ANHYDROUS 99PCT, adopts the dry post that siccative is housed, and the water cut of dry back methylene dichloride is controlled at≤0.01% (quality).
In the inventive method, distillation can be adopted batch distillation, also can adopt continuous still battery, and distillation temperature is 50～60 ℃.
In a kind of method of purification that extracts with the residual level of farming methylene dichloride of the present invention; Key is that (1) adopt adsorbents adsorb to remove the impurity close with the methylene dichloride boiling point; Siccative dewaters, and has improved organism is analyzed in the water quality repeatability and accuracy, and light, the last running that contains impurity is removed in distillation.(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.The present invention extracts in the method for purification with the residual level of farming methylene dichloride, and through adsorbents adsorb, siccative dewaters; Can obtain purity after refining greater than 99.8% agricultural residual grade of methylene dichloride; Product yield is greater than 80%, and wherein each item technical indicator all reaches the requirement of the residual level of farming methylene dichloride, is specially adapted to the used extraction solvent of organism analysis in the water quality; Can effectively remove the interference that impurity is analyzed organism in the methylene dichloride, improve the accuracy and the repeatability of analytic process greatly.
Embodiment
Set forth technical scheme of the present invention below in conjunction with embodiment, but be not limited to the embodiment of the invention.
Embodiment 1
(1) raw material methylene dichloride (analytical pure) 500mL is added in the adsorption column; (φ 20mm * 350mm; There is cock control the lower end) in, fill 2/3rds sorbent materials in the adsorption column, sorbent material cleans the back in 200 ℃ of oven dry with zero(ppm) water; Methylene dichloride is flowed through with the 20mL/min flow velocity adsorption column of sorbent material is housed, and discards at first effusive 20mL solution.
(2) will pass through the methylene dichloride that adsorption column adsorbed and add (φ 20mm * 350mm in the dry post; There is cock control the lower end) in; Fill 2/3rds siccative in the dry post, the siccative SODIUM SULPHATE ANHYDROUS 99PCT is through 500 ℃ of oven dry, and methylene dichloride is flowed through with the 20mL/min flow velocity adsorption column of sorbent material is housed; Discard at first effusive 20mL solution, water cut≤0.01% of control methylene dichloride.
(3) will add in the batch distillation device through the dry methylene dichloride of crossing of super-dry post; Utilize heating in water bath, bath temperature is 50 ℃, and it is 10mL/min that controlling flow goes out flow velocity; Discard lighting end 20mL and last running 20mL, collect outflow middle runnings liquid and be specification product.
Embodiment 2
(1) raw material methylene dichloride (analytical pure) 600mL is added adsorption column (φ 20mm * 350mm; There is cock control the lower end) in; Fill 2/3rds sorbent materials in the adsorption column; Sorbent material cleans the back in 180 ℃ of oven dry with zero(ppm) water, and methylene dichloride is flowed through with the 30mL/min flow velocity adsorption column of sorbent material is housed, and discards at first effusive 20mL solution.
(2) will pass through the methylene dichloride that adsorption column adsorbed and add dry post (φ 20mm * 350mm; There is cock control the lower end) in; Fill 2/3rds siccative in the dry post, the siccative SODIUM SULPHATE ANHYDROUS 99PCT is through 550 ℃ of oven dry, and methylene dichloride is flowed through with the 30mL/min flow velocity adsorption column of sorbent material is housed; Discard at first effusive 20mL solution, water cut≤0.01% of control methylene dichloride.
(3) will add in the glass rectifier unit through the dry methylene dichloride of crossing of super-dry post, and utilize water-bath to add, bath temperature is 60 ℃, and it is 20mL/min that controlling flow goes out flow velocity, discards lighting end 20mL and last running 20mL, collects effluent and is specification product.
The residual level of table 1 farming methylene dichloride technical indicator
Claims (7)
1. one kind extracts the method for purification of using the residual level of farming methylene dichloride; It is characterized in that comprising following content: the methylene dichloride raw material at first carries out adsorption treatment; Sorbent material is gac or 5A molecular sieve, and the methylene dichloride after the adsorption treatment carries out drying treatment, and dried methylene dichloride distills; The heavy constituent of the light constituent and the raw materials quality mark 2～10% of raw materials quality mark 2%～10% are removed in distillation, collect middle runnings and obtain extraction with the residual level of farming methylene dichloride.
2. according to the described method of claim 1, it is characterized in that: the methylene dichloride raw material is the analytical pure methylene dichloride, or the chromatographically pure methylene dichloride.
3. according to the described method of claim 1, it is characterized in that: sorbent material and adsorption column carry out purifying treatment before using.
4. according to the described method of claim 1, it is characterized in that: during adsorption treatment, at first effusive a small amount of material is abandoned, and the material of abandoning is 10%～100% of a sorbent material volume.
5. according to the described method of claim 1, it is characterized in that: siccative is a SODIUM SULPHATE ANHYDROUS 99PCT, adopts the dry post that siccative is housed to carry out drying treatment, and the water cut of dry back methylene dichloride is controlled at≤0.01% (quality).
6. according to the described method of claim 1, it is characterized in that: batch distillation is adopted in distillation, perhaps adopts continuous still battery.
7. according to claim 1 or 6 described methods, it is characterized in that: distillation temperature is 50～60 ℃.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105209413A (en) * | 2013-05-13 | 2015-12-30 | 昭和电工株式会社 | Purification method for dichloromethane, and production method for difluoromethane using said purification method |
| CN106365943A (en) * | 2016-08-31 | 2017-02-01 | 中国船舶重工集团公司第七八研究所 | Preparation method of pesticide residue level benzene |
| 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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| JPS62153248A (en) * | 1985-12-26 | 1987-07-08 | Kyowa Yuka Kk | Purification of ethyl acetate |
| CN2573497Y (en) * | 2002-09-20 | 2003-09-17 | 史永刚 | Adsorption column for purifying carbon tetrachloride |
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| 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 |
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2010
- 2010-10-15 CN CN201010514089.5A patent/CN102452892B/en active Active
Patent Citations (6)
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| JPS62153248A (en) * | 1985-12-26 | 1987-07-08 | Kyowa Yuka Kk | Purification of ethyl acetate |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105209413A (en) * | 2013-05-13 | 2015-12-30 | 昭和电工株式会社 | Purification method for dichloromethane, and production method for difluoromethane using said purification method |
| CN106365943A (en) * | 2016-08-31 | 2017-02-01 | 中国船舶重工集团公司第七八研究所 | Preparation method of pesticide residue level benzene |
| 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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