CN101570484A - Method for preparing pesticide residue grade chromatographic ethyl acetate - Google Patents
Method for preparing pesticide residue grade chromatographic ethyl acetate Download PDFInfo
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- CN101570484A CN101570484A CNA2009100692533A CN200910069253A CN101570484A CN 101570484 A CN101570484 A CN 101570484A CN A2009100692533 A CNA2009100692533 A CN A2009100692533A CN 200910069253 A CN200910069253 A CN 200910069253A CN 101570484 A CN101570484 A CN 101570484A
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Abstract
The invention relates to a method for preparing pesticide residue grade chromatographic ethyl acetate. The steps are as follows: through adsorption edulcoration by sorbent and polymeric adsorbent; desiccant dehydration; rectification and purification; and filtration, and the qualified product of pesticide residue grade chromatographic ethyl acetate can be obtained. The method utilizes the difference of the ethyl acetate and impurities inside and adopts the preparation method of drying and rectification after adsorption to separate the ethyl acetate from some impurities therein; and after purification, the index (see figure 1) of the pesticide residue grade chromatographic ethyl acetate can be reached. The method has the advantages of short rectification time and 93 to 95 percent of pure chromatography yield, wherein the pure chromatography yield of a pesticide residue grade chromatographic product can be 75 to 85 percent, and the large-scale production of the pesticide residue grade chromatographic ethyl acetate can be formed.
Description
Technical field
The invention belongs to the chemical reagent field, especially a kind of preparation method of pesticide residue grade chromatographic ethyl acetate.
Background technology
In recent years, along with the development of agricultural cience and farming techniques, the kind and the quantity of agricultural chemicals constantly increase, and chemical pesticide has become the main means of prevention and elimination of disease and pests.The generally use of agricultural chemicals causes the pesticidal contamination problem often to take place, and the pesticide residue phenomenon that exceeds standard is quite serious.In the world, for safeguarding domestic economy interests and protection health of people, more and more strict requirement has been proposed sanitary indexs such as pesticide residue in the imported food.The Chinese government is for ensureing people health, implement effective control agricultural chemicals in farm crop produce reasonable use and to the monitoring of residual quantity, to satisfy the needs of foreign trade.
Along with the globalization of market for farm products, the agricultural chemicals residue problem more is subjected to people's attention in the agricultural-food.Compare with advanced country, China is relatively backward aspect the control pesticidal contamination, and agricultural residual monitoring system is also unsound, some areas even blank.Therefore, the preparation method of the residual level of research farming organic solvent has important practical significance to agricultural development.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, provide a kind of and can effectively remove the preparation method that the small amount of impurities, the product purity that are difficult to remove in the ethyl acetate reach farming residual level index and the simple pesticide residue grade chromatographic ethyl acetate of technology.
The objective of the invention is to be achieved through the following technical solutions:
A kind of preparation method of pesticide residue grade chromatographic ethyl acetate, preparation method's step is as follows:
(1) the raw acetic acid ethyl ester is promoted to the adsorption column top, utilizes gravity to flow in the post, control flow velocity 60mL～100mL/min, the interior sorbent material of organic solvent and adsorption column is fully contacted, and absorption impurity wherein, remove the initial flow fluid, fluid is detected;
(2) qualified fluid be will detect and adsorption resin column, flow velocity 50mL～80mL/min flowed into;
(3) the fluid drying tower with step (2) carries out drying, and dry fluid water content is controlled at 0.05%～0.2%;
(4) dried fluid is squeezed into reactor rectifying, utilize heat-conducting oil heating, 120 ℃～200 ℃ of control heat-conducting oil heating temperature, the ethyl acetate fluid temperature is 85 ℃～95 ℃ in the still, goes out 79 ℃～80 ℃ of liquid temps; Reflux ratio 1: 0.5～0.8 is adjusted to 1: 4～and 5, obtain qualified pesticide residue grade chromatographic ethyl acetate product at last;
(5) qualified back finished product stores under nitrogen protection with 0.45 μ mPTFE filtering with microporous membrane, bottling.
And the purity of described raw acetic acid ethyl ester is 99.5%.
And described sorbent material is zeolite, silica gel or activated alumina.
And the length of described adsorption column is 2m, internal diameter 15cm, and the amount of dress sorbent material is 4/5 of a column length.
And described polymeric adsorbent is PC101 or Amberlyst15A.
Advantage of the present invention and positively effect are:
1, the present invention utilizes the difference on ethyl acetate and the contaminant characteristics wherein, adopt the production method of absorption after drying, rectifying, ethyl acetate is separated with some impurity wherein, can reach pesticide residue grade chromatographic ethyl acetate index (seeing Table 1) after the purification, the rectifying time is few, the chromatographically pure productive rate reaches 93%～95%, and wherein the pesticide residue grade chromatographic product reaches 75%～85%, can form the scale production of pesticide residue grade chromatographic ethyl acetate.
2, the present invention takes to adsorb, method dry, rectifying removes wherein impurity, obtain qualified product by setting processing condition rectifying, can obtain the pesticide residue grade chromatographic ethyl acetate of purity 〉=99.9%, chromatographic grade yield 93%～95%, wherein 75%～85% is the residual level of farming, compare the product purity height of this law preparation with ordinary method, equipment configuration is simple, and is stable.
Embodiment
Below content of the present invention is further elaborated by the following example, but these embodiment do not limit protection scope of the present invention.
A kind of preparation method of pesticide residue grade chromatographic ethyl acetate, step is as follows:
(1) content is about 99.5% raw acetic acid ethyl ester and is promoted to zeolite adsorption post (column length 2M, internal diameter 15cm, the dress amount of zeolite be column length 4/5) top, utilize gravity to flow in the post, control flow velocity 60mL～100mL/min, organic solvent is fully contacted with zeolite, and wherein impurity of absorption, remove initial flow fluid (because of beginning time the impurity band in the zeolite can be come out), fluid is detected.
In this adsorption step, except that can using the zeolite adsorption post, can also use the adsorption column of weighting agents such as silica gel, activated alumina.
(2) (wherein polymeric adsorbent is PC101 or Amberlyst15A will to detect qualified fluid inflow adsorption resin column, this adsorption resin column is identical with the zeolite adsorption post), utilize the contact of polymeric adsorbent and organic solvent can adsorb the bigger impurity of uv-absorbing and separate with it, flow velocity 50mL～80mL/min, fluid detects absorbancy near index.
To employed adsorption column (silica gel, zeolite, activated alumina, polymeric adsorbent PC101 or Amberlyst15A) in above two steps, the applicant has carried out choosing test: absorption column length 1.2m, internal diameter 24mm, choose silica gel, zeolite, aluminum oxide and polymeric adsorbent respectively, carry out adsorption test.The result shows that zeolite and polymeric adsorbent effect are relatively good.Further test is found, adopts two kinds of sorbent material associating results of use better.After the absorption of two-stage adsorption column, the content of ethyl acetate 〉=99.7%, light absorption value is high slightly in low band, and high band is near index request.After molecular sieve or hydrolith drying, moisture reaches 0.06%～0.12%, by selected processing condition rectifying, control each point temperature and reflux ratio, after removing front-end volatiles, the ethyl acetate of preparing all meets the chromatogram index, and has 75%～85% to reach agricultural residual level index request.
(3) the fluid drying tower (siccative is molecular sieve or hydrolith) with step (2) carries out drying, and dry fluid water content 0.05%～0.2% is considered as siccative by water saturation greater than 0.2%, carries out drying after the replacing again.
(4) drying back solution is squeezed into the rectifying of 200L reactor, utilizes heat-conducting oil heating, 120 ℃～200 ℃ of control heat-conducting oil heating temperature, and the ethyl acetate fluid temperature is 85 ℃～95 ℃ in the still, goes out 79 ℃～80 ℃ of liquid temps; Reflux ratio 1: 0.5～0.8 is adjusted to 1: 4～5 (all being presented on the instrument controlling box), obtains qualified pesticide residue grade chromatographic ethyl acetate product at last.
(5) qualified back finished product stores under nitrogen protection with 0.45 μ mPTFE filtering with microporous membrane, bottling.
Effect detection:
The pesticide residue grade chromatographic ethyl acetate of producing is in ultraviolet wavelength 254nm～400nm scope (the quartzy cuvette of 1cm, water is made reference), absorbancy satisfies the index request in the table 1, content is greater than 99.9%, and the rate of recovery 93%～95%, yield rate reach 90%～94% approximately.Detect through the residual level of farming: after 300 times of sample concentration, all be lower than the peak height of 10ng/L γ-phenyl-hexachloride with the peak height at detected all the assorted peaks of GC-ECD gas chromatograph, the detection of the residual level of farming reagent is qualified.The pesticide residue grade chromatographic ethyl acetate of this method preparation can satisfy the application demand of client in pesticide residue, has filled up the domestic blank that does not have pesticide residue grade chromatographic ethyl acetate.
Table 1 pesticide residue grade chromatographic ethyl acetate technical indicator
Claims (5)
1, a kind of preparation method of pesticide residue grade chromatographic ethyl acetate is characterized in that: preparation method's step is as follows:
(1) the raw acetic acid ethyl ester is promoted to the adsorption column top, utilizes gravity to flow in the post, control flow velocity 60mL～100mL/min, the interior sorbent material of organic solvent and adsorption column is fully contacted, and absorption impurity wherein, remove the initial flow fluid, fluid is detected;
(2) qualified fluid be will detect and adsorption resin column, flow velocity 50mL～80mL/min flowed into;
(3) the fluid drying tower with step (2) carries out drying, and dry fluid water content is controlled at 0.05%～0.2%;
(4) dried fluid is squeezed into reactor rectifying, utilize heat-conducting oil heating, 120 ℃～200 ℃ of control heat-conducting oil heating temperature, the ethyl acetate fluid temperature is 85 ℃～95 ℃ in the still, goes out 79 ℃～80 ℃ of liquid temps; Reflux ratio 1: 0.5～0.8 is adjusted to 1: 4～and 5, obtain qualified pesticide residue grade chromatographic ethyl acetate product at last;
(5) qualified back finished product stores under nitrogen protection with 0.45 μ m PTFE filtering with microporous membrane, bottling.
2, the preparation method of pesticide residue grade chromatographic ethyl acetate according to claim 1 is characterized in that: the purity of described raw acetic acid ethyl ester is 99.5%.
3, the preparation method of pesticide residue grade chromatographic ethyl acetate according to claim 1 is characterized in that: described sorbent material is zeolite, silica gel or activated alumina.
4, the preparation method of pesticide residue grade chromatographic ethyl acetate according to claim 1 is characterized in that: the length of described adsorption column is 2m, internal diameter 15cm, and the Intake Quantity of sorbent material is 4/5 of a column length.
5, the preparation method of pesticide residue grade chromatographic ethyl acetate according to claim 1 is characterized in that: described polymeric adsorbent is PC101 or Amberlyst15 A.
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| CNA2009100692533A CN101570484A (en) | 2009-06-15 | 2009-06-15 | Method for preparing pesticide residue grade chromatographic ethyl acetate |
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| CNA2009100692533A CN101570484A (en) | 2009-06-15 | 2009-06-15 | Method for preparing pesticide residue grade chromatographic ethyl acetate |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102040455A (en) * | 2010-12-29 | 2011-05-04 | 天津市康科德科技有限公司 | Purification method of chromatographically pure organic solvent cyclohexane |
| CN102417450A (en) * | 2011-12-26 | 2012-04-18 | 天津市康科德科技有限公司 | Method for purifying chromatographic grade butyl acetate |
| 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 |
| CN104693028A (en) * | 2015-03-31 | 2015-06-10 | 太仓沪试试剂有限公司 | Purification method of ethyl acetate |
| CN105037156A (en) * | 2015-07-13 | 2015-11-11 | 苏州晶瑞化学股份有限公司 | Production method for ultra-clean high-purity ethyl acetate |
| CN105085260A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of ethyl acetate for liquid chromatography-mass spectrometer |
| CN112299999A (en) * | 2020-11-13 | 2021-02-02 | 南京化学试剂股份有限公司 | Refining method of high-purity ethyl acetate |
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2009
- 2009-06-15 CN CNA2009100692533A patent/CN101570484A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| CN102040455A (en) * | 2010-12-29 | 2011-05-04 | 天津市康科德科技有限公司 | Purification method of chromatographically pure organic solvent cyclohexane |
| CN102417450A (en) * | 2011-12-26 | 2012-04-18 | 天津市康科德科技有限公司 | Method for purifying chromatographic grade butyl acetate |
| CN105085260A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of ethyl acetate for liquid chromatography-mass spectrometer |
| CN104693028A (en) * | 2015-03-31 | 2015-06-10 | 太仓沪试试剂有限公司 | Purification method of ethyl acetate |
| CN105037156A (en) * | 2015-07-13 | 2015-11-11 | 苏州晶瑞化学股份有限公司 | Production method for ultra-clean high-purity ethyl acetate |
| CN112299999A (en) * | 2020-11-13 | 2021-02-02 | 南京化学试剂股份有限公司 | Refining method of high-purity ethyl acetate |
| CN112299999B (en) * | 2020-11-13 | 2021-07-13 | 南京化学试剂股份有限公司 | Refining method of high-purity ethyl acetate |
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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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Application publication date: 20091104 |