CN101481361A - Technique of preparing high-purity bentazone raw pesticide - Google Patents
Technique of preparing high-purity bentazone raw pesticide Download PDFInfo
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- CN101481361A CN101481361A CNA2008100190142A CN200810019014A CN101481361A CN 101481361 A CN101481361 A CN 101481361A CN A2008100190142 A CNA2008100190142 A CN A2008100190142A CN 200810019014 A CN200810019014 A CN 200810019014A CN 101481361 A CN101481361 A CN 101481361A
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- dce
- bentazone
- water
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- brine
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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Abstract
The invention discloses a preparation process of a high-purity bentazone without brine waste and dust pollution. The process comprises the following steps: adding a certain amount of bentazone (BTZ) and dichloroethane (DCE) which are washed by water to a three-necked flask to form BTZ-DCE solution, placing the three-necked flask in hot water, slowly heating to 60 DEG C, depressurizing to distill off the DCE, cooling by glass condenser brine, collecting a certain amount of distillate in a round-bottomed flask followed by stop, slowly cooling in water to 35 DEG C, further cooling with brine ice to minus 5 DEG C, centrifuging, washing with a little cold DCE and water, and drying in a vacuum drying oven to obtain the product. The preparation process has the following advantages: no brine waste is generated due to no application of alkali and acid, the crystal is easily dried, no dust pollution is produced, and the process totally meets the scientific development concept of energy-saving and emission-reduction.
Description
Technical field
The present invention relates to a kind of agricultural chemical compound, especially relate to a kind of high-purity bentazone raw pesticide preparation technology's improvement.
Background technology
The preparation technology of the former medicine of bentazone (also claiming bentazone) in the market, what continue to use all is to utilize bentazone (BTZ) ethylene dichloride (DCE) the solution alkali collection acidifying washing of synthesizing after washing, and alkali collection acidizing extraction concentrates, and to wait two kinds of methods, its essence be exactly that impurity is removed in the acidifying of coming together of BTZ-DCE solution alkali.
Owing to all adopt alkali, acid, therefore can produce a large amount of brine wastes in these two kinds of technologies, the pollution of dust is arranged again simultaneously, and purity all is lower than 97%, have only 82% sometimes.
Summary of the invention
The present invention is directed to the technological deficiency of above-mentioned existence, proposed a kind of preparation technology who does not have the high-purity bentazone raw pesticide of brine waste and no dust pollution.
Technical scheme of the present invention is achieved in that the preparation technology of the former medicine of a kind of bentazone, and the step of described technology is as follows:
A certain amount of bentazone, the ethylene dichloride that add in A, the there-necked flask after washing are formed BTZ-DCE solution;
B, place hot water slowly to be warming up to 60 ℃ there-necked flask, decompression steams DCE;
C, after the glass condenser brine refrigeration, stop after in round-bottomed flask, collecting a certain amount of fraction;
D, in water, slowly cool to 35 ℃, be cooled to-5 ℃ with icy salt solution again, centrifugation;
E, a small amount of cold DCE and the water washing of usefulness get product after the vacuum drying oven drying.
Among the present invention, there-necked flask, glass condenser, round-bottomed flask, vacuum drying oven are all purchased from medical equipment shop, Suzhou City.
Advantage of the present invention is: do not adopt alkali, acid in the technology of the present invention, therefore can not produce a large amount of brine wastes, crystallizing and drying is easy in addition, does not have the pollution of dust, meets the Scientific Outlook on Development of energy-saving and emission-reduction fully.
Description of drawings
Below in conjunction with accompanying drawing the present invention is done further to describe.
Accompanying drawing is a process flow sheet of the present invention.
Specific embodiments
Embodiment one
From accompanying drawing as can be seen, the preparation technology of the former medicine of a kind of bentazone, its processing step is as follows: A, bentazone 75 grams, ethylene dichloride 700 grams that add in there-necked flask after the washing are formed BTZ-DCE solution 775 grams (about 621 liters); B, place hot water slowly to be warming up to 60 ℃ there-necked flask, decompression steams DCE;
C, after the glass condenser brine refrigeration, in 1000 milliliters of round-bottomed flasks, collect fraction and stop for about 440 milliliters;
D, slowly cool to 35 ℃, be cooled to-5 ℃ with icy salt solution again, centrifugation at tap water;
E, a small amount of cold DCE and the water washing of usefulness get product (purity is 〉=97%) after the vacuum drying oven drying.
Embodiment two
From accompanying drawing as can be seen, the preparation technology of the former medicine of a kind of bentazone, its processing step is as follows: A, bentazone 75 grams, ethylene dichloride 700 grams that add in there-necked flask after the washing are formed BTZ-DCE solution 775 grams (about 621 liters); B, place hot water slowly to be warming up to 60 ℃ there-necked flask, decompression steams DCE;
C, after the glass condenser brine refrigeration, in 1000 milliliters of round-bottomed flasks, collect fraction and stop for about 440 milliliters;
D, slowly cool to 35 ℃, be cooled to-5 ℃ with icy salt solution again, centrifugation at well water;
E, a small amount of cold DCE and the water washing of usefulness get product (purity is 〉=97%) after the vacuum drying oven drying.
Embodiment three
From accompanying drawing as can be seen, the preparation technology of the former medicine of a kind of bentazone, its processing step is as follows: A, bentazone 75 grams, ethylene dichloride 700 grams that add in there-necked flask after the washing are formed BTZ-DCE solution 775 grams (about 621 liters); B, place hot water slowly to be warming up to 60 ℃ there-necked flask, decompression steams DCE;
C, after the glass condenser brine refrigeration, in 1000 milliliters of round-bottomed flasks, collect fraction and stop for about 440 milliliters;
D, slowly cool to 35 ℃, be cooled to-5 ℃ with icy salt solution again, centrifugation at mineral water;
E, a small amount of cold DCE and the water washing of usefulness get product (purity is 〉=97%) after the vacuum drying oven drying.
Claims (1)
1. the preparation technology of the former medicine of bentazone, it is characterized in that: the step of described technology is as follows:
A certain amount of bentazone, the ethylene dichloride that add in A, the there-necked flask after washing are formed BTZ-DCE solution;
B, place hot water slowly to be warming up to 60 ℃ there-necked flask, decompression steams DCE;
C, after the glass condenser brine refrigeration, stop after in round-bottomed flask, collecting a certain amount of fraction;
D, in water, slowly cool to 35 ℃, be cooled to-5 ℃ with icy salt solution again, centrifugation;
E, a small amount of cold DCE and the water washing of usefulness get product after the vacuum drying oven drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100190142A CN101481361A (en) | 2008-01-09 | 2008-01-09 | Technique of preparing high-purity bentazone raw pesticide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100190142A CN101481361A (en) | 2008-01-09 | 2008-01-09 | Technique of preparing high-purity bentazone raw pesticide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101481361A true CN101481361A (en) | 2009-07-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008100190142A Pending CN101481361A (en) | 2008-01-09 | 2008-01-09 | Technique of preparing high-purity bentazone raw pesticide |
Country Status (1)
| Country | Link |
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| CN (1) | CN101481361A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924405A (en) * | 2012-11-21 | 2013-02-13 | 合肥星宇化学有限责任公司 | Method for preparing bentazone aqueous agent |
| CN102924404A (en) * | 2012-11-21 | 2013-02-13 | 合肥星宇化学有限责任公司 | Method for preparing bentazone sodium salt powder |
| CN104447618A (en) * | 2014-12-26 | 2015-03-25 | 合肥星宇化学有限责任公司 | Method for purifying bentazon |
| CN105566249A (en) * | 2015-12-29 | 2016-05-11 | 浙江中山化工集团股份有限公司 | Process method for preparing high-content bentazone sodium salt raw drug and bentazone sodium salt raw drug prepared by same |
-
2008
- 2008-01-09 CN CNA2008100190142A patent/CN101481361A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924405A (en) * | 2012-11-21 | 2013-02-13 | 合肥星宇化学有限责任公司 | Method for preparing bentazone aqueous agent |
| CN102924404A (en) * | 2012-11-21 | 2013-02-13 | 合肥星宇化学有限责任公司 | Method for preparing bentazone sodium salt powder |
| CN102924404B (en) * | 2012-11-21 | 2016-01-20 | 合肥星宇化学有限责任公司 | A kind of preparation method of bentazone sodium salt pulvis |
| CN102924405B (en) * | 2012-11-21 | 2016-01-20 | 合肥星宇化学有限责任公司 | A kind of preparation method of bentazone aqua |
| CN104447618A (en) * | 2014-12-26 | 2015-03-25 | 合肥星宇化学有限责任公司 | Method for purifying bentazon |
| CN105566249A (en) * | 2015-12-29 | 2016-05-11 | 浙江中山化工集团股份有限公司 | Process method for preparing high-content bentazone sodium salt raw drug and bentazone sodium salt raw drug prepared by same |
| CN105566249B (en) * | 2015-12-29 | 2019-06-04 | 浙江中山化工集团股份有限公司 | Prepare the process and thus obtained Bentazon sodium salt raw medicine of high-content Bentazon sodium salt raw medicine |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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Application publication date: 20090715 |