CN102924323B - Neutralization improvement method for production of oxadiazon - Google Patents
Neutralization improvement method for production of oxadiazon Download PDFInfo
- Publication number
- CN102924323B CN102924323B CN201210477041.0A CN201210477041A CN102924323B CN 102924323 B CN102924323 B CN 102924323B CN 201210477041 A CN201210477041 A CN 201210477041A CN 102924323 B CN102924323 B CN 102924323B
- Authority
- CN
- China
- Prior art keywords
- hour
- production
- stir
- neutralization
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Detergent Compositions (AREA)
Abstract
The invention discloses a neutralization improvement method for the production of oxadiazon, belonging to the filed of fine chemical production. The neutralization improvement method mainly comprises the following steps: neutralizing in a methylbenzene system, washing, separating water and drying. Compared with the traditional process, the neutralization improvement method can increase the yield stably, reduce the wastewater discharge during the production of the oxadiazon, reduce the number of related equipment and operating personnel, and is economical and environment-friendly.
Description
Technical field
The present invention relates to fine chemistry industry technical field of producing, the neutralization specifically belonged in the production of Yi Zhong Evil humulone is improved one's methods.
Background technology
Evil humulone production technique is more, produces at present that most what adopt is the ten step main reactions comprising esterification, nitrated, hydrolysis, etherificate, Fe3+ reduction (or hydrogenating reduction), diazotization, Reduction with Stannous Chloride, neutralization, acidylate, cyclization.Specifically 2; to be starting raw material obtain 2 through esterification, nitrated, hydrolysis, etherificate, Fe3+ reduction (or hydrogenating reduction), diazotization, Reduction with Stannous Chloride to 4-chlorophenesic acid; 4-bis-chloro-5-isopropoxy benzene hydrazine hydrochloride (under be called for short hydrazonium salt); 2 are obtained again through neutralization; the chloro-5-isopropoxide phenylhydrazine of 4-bis-(under be called for short hydrazine), the more former medicine of Evil humulone must be arrived through acidylate, cyclization.Mainly in liquid caustic soda and water, throw hydrazonium salt with operation in tradition, obtain hydrazine through sheet frame (whizzer) discharging, then drop into subsequent processing, produce a large amount of waste water like this, personnel labor intensity is larger.
Summary of the invention
The neutralization that the object of this invention is to provide in the production of Yi Zhong Evil humulone is improved one's methods, and overcome the deficiencies in the prior art, this is improved one's methods and can improve production yield, reduces discharge of wastewater and reduces production cost, economic environmental protection.
The technical solution used in the present invention is as follows:
Principal reaction principle of the present invention:
Neutralization in the production of Yi Zhong Evil humulone is improved one's methods, and comprises the following steps:
1), under whipped state, dry hydrazonium salt is dropped in toluene system;
2) control temperature less than 40 DEG C is 1.1-1.2: 1 slowly add powdered sodium hydroxide according to sodium hydroxide and hydrazonium salt mol ratio;
3) be slowly warmed up to 63-73 DEG C, stir 1 hour;
4) add gauge water, ON cycle water for cooling is to 55-60 DEG C; Stir 1 hour;
5) half an hour is left standstill, layering sub-cloud water;
6) drop into quantitative siccative at 55-60 DEG C and stir 1 hour;
7) filtrate after sheet frame of slightly lowering the temperature enters subsequent processing.
Described siccative is gac.
Compared with the prior art, beneficial effect of the present invention is as follows:
The present invention is compared with Conventional processing methods, and yield promotes steadily, and Mei Dun Evil humulone decreases about 8 tons of discharge of wastewater, and decreases relevant device and operator, reduces labour intensity, reduces production cost.
Embodiment
Neutralization in the production of embodiment 1, Zhong Evil humulone is improved one's methods, and comprises the following steps:
1), under whipped state, dry hydrazonium salt is dropped in toluene system;
2) control temperature less than 40 DEG C, slowly adds quantitative powdered sodium hydroxide, and sodium hydroxide and hydrazonium salt mol ratio are 1.1: 1;
3) be slowly warmed up to 63-73 DEG C, stir 1 hour;
4) add gauge water, ON cycle water for cooling is to 55-60 DEG C; Stir 1 hour;
5) half an hour is left standstill, layering sub-cloud water;
6) drop into qualitative activity charcoal siccative at 55-60 DEG C and stir 1 hour;
7) filtrate after sheet frame of slightly lowering the temperature enters subsequent processing.
Neutralization in the production of embodiment 2, Zhong Evil humulone is improved one's methods, and comprises the following steps:
1), under whipped state, dry hydrazonium salt is dropped in toluene system;
2) control temperature less than 40 DEG C, slowly adds quantitative powdered sodium hydroxide, and sodium hydroxide and hydrazonium salt mol ratio are 1.2: 1;
3) be slowly warmed up to 63-73 DEG C, stir 1 hour;
4) add gauge water, ON cycle water for cooling is to 55-60 DEG C; Stir 1 hour;
5) half an hour is left standstill, layering sub-cloud water;
6) drop into qualitative activity charcoal siccative at 55-60 DEG C and stir 1 hour;
7) filtrate after sheet frame of slightly lowering the temperature enters subsequent processing.
Simultaneous test example: get post and produce same batch of hydrazonium salt and dry, take 6 parts (every part of 80g) stand-by.Test one is improving technique, and test two is former technique
Test one: get 500ml there-necked flask 3 (numbering 1#, 2#, 3#), drop into 300g toluene respectively, stir respectively and drop into the load weighted hydrazonium salt of 80g, get 14g powdered sodium hydroxide three parts, control temperature less than 40 DEG C slowly drops in three flasks respectively, finish and be warmed up to 63 ~ 73 DEG C, stir 1 hour, then 50ml water is added, control temperature stirs 1 hour at 55 ~ 60 DEG C, leaves standstill 30 minutes, and point sub-cloud water drops into 2g gac, stir 1 hour, suction filtration obtains filtrate and weighs sampling detection record respectively;
Test two: get 500ml there-necked flask 3 (numbering 4#, 5#, 6#), drop into 100ml water and 100ml32% liquid caustic soda respectively, under whipped state, drop into 80g hydrazonium salt respectively, stir and be warming up to 55-75 DEG C, add 100ml water immediately, open cooling system simultaneously and be cooled to 0 ~ 12 DEG C, suction filtration, use 100ml water washing, obtain hydrazine, dry sampling detection record of weighing;
Testing data contrast is as follows:
Claims (2)
1. the neutralization in the production of Yi Zhong Evil humulone is improved one's methods, and it is characterized in that, comprises the following steps:
1), under whipped state, 2,4-bis-dry chloro-5-isopropoxy benzene hydrazine hydrochloride are dropped in toluene system;
2) control temperature less than 40 DEG C is 1.1-1.2: 1 slowly add powdered sodium hydroxide according to sodium hydroxide and 2,4-bis-chloro-5-isopropoxy benzene hydrazine hydrochloride mol ratio;
3) be slowly warmed up to 63-73 DEG C, stir 1 hour;
4) add gauge water, ON cycle water for cooling is to 55-60 DEG C; Stir 1 hour;
5) half an hour is left standstill, layering sub-cloud water;
6) drop into quantitative siccative at 55-60 DEG C and stir 1 hour;
7) filtrate after sheet frame of slightly lowering the temperature enters subsequent processing.
2. the neutralization in Yi Zhong Evil humulone production according to claim 1 is improved one's methods, and it is characterized in that: described siccative is gac.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210477041.0A CN102924323B (en) | 2012-11-21 | 2012-11-21 | Neutralization improvement method for production of oxadiazon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210477041.0A CN102924323B (en) | 2012-11-21 | 2012-11-21 | Neutralization improvement method for production of oxadiazon |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102924323A CN102924323A (en) | 2013-02-13 |
| CN102924323B true CN102924323B (en) | 2015-04-01 |
Family
ID=47639286
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210477041.0A Active CN102924323B (en) | 2012-11-21 | 2012-11-21 | Neutralization improvement method for production of oxadiazon |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102924323B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110655477A (en) * | 2019-10-25 | 2020-01-07 | 湖南兴同化学科技有限公司 | Synthesis method of oxadiazon intermediate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4695312A (en) * | 1985-04-03 | 1987-09-22 | Shionogi & Co., Ltd. | 4,5,6,7-tetrahydro-2H-indazole derivatives and herbicides containing them |
| CN1208400A (en) * | 1995-12-29 | 1999-02-17 | 罗狄亚化学公司 | Method for synthesizing aryl hydrazine through reduction of a diazo compound derivative |
| JP2000290267A (en) * | 1999-04-07 | 2000-10-17 | Toray Res Center:Kk | Production of oxadiazolone derivative |
-
2012
- 2012-11-21 CN CN201210477041.0A patent/CN102924323B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4695312A (en) * | 1985-04-03 | 1987-09-22 | Shionogi & Co., Ltd. | 4,5,6,7-tetrahydro-2H-indazole derivatives and herbicides containing them |
| CN1208400A (en) * | 1995-12-29 | 1999-02-17 | 罗狄亚化学公司 | Method for synthesizing aryl hydrazine through reduction of a diazo compound derivative |
| JP2000290267A (en) * | 1999-04-07 | 2000-10-17 | Toray Res Center:Kk | Production of oxadiazolone derivative |
Non-Patent Citations (1)
| Title |
|---|
| 2,4-二氯-5-异丙氧基苯肼的合成;姚益明，徐海亮;《精细化工原料及中间体》;20040831(第8期);第21-22页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102924323A (en) | 2013-02-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104262200B (en) | One recycles waste water and prepares N, N ' production method of-dicyclohexylcarbodiimide | |
| CN105348154A (en) | Method for recycling sulfosalicylic acid from doxycycline production waste liquid | |
| CN108358798A (en) | A kind of method of micro passage reaction synthesis Tarceva intermediate | |
| CN103626240A (en) | Method for preparing ruthenium trichloride with low-concentration complicated ruthenium-containing waste liquid | |
| CN102924323B (en) | Neutralization improvement method for production of oxadiazon | |
| CN100532261C (en) | Process for preparing solid potassium ferrate | |
| CN103360295A (en) | Device and method for preparing perchloromethylmercaptan | |
| CN107083490A (en) | A kind of organic silicon chemical waste residue processing method | |
| CN107253914A (en) | The method that the nitrophenol of 2 amino 4 is prepared using Disperse Blue 2BLN byproduct | |
| CN102795984B (en) | Production method of mixed binary acid with long carbon chain | |
| CN102993131B (en) | Method for utilizing o-chlorocyclohexanol to prepare cyclohexene oxide by cyclization | |
| CN105037204A (en) | Zero-emission production process of N-cyanoethylaniline | |
| CN101723845A (en) | Method for producing m-acetamino-N,N-diethyl aniline | |
| CN105198734B (en) | Method of preparing gallic acid | |
| CN104876856B (en) | A kind of method that Split Method prepares (R) (+) 3 amino piperidine dihydrochloride | |
| CN106238098A (en) | The preparation method of a kind of 1,2,4,5 four substituted ramification of imidazole and catalyst for preparing thereof | |
| CN102527339B (en) | Organic porous gel absorbent, preparation method and application thereof | |
| CN211035755U (en) | Recycling device for oxime amine mother liquor | |
| CN106748912B (en) | A kind of synthesis technology of sodium azulenesulfonate monohydrate | |
| CN102020571A (en) | Preparation method of tetramethylammonium bromide | |
| CN105130920A (en) | Method for recycling formic acid in 3-methyl-4-nitroimino-tetrahydro-1, 3, 5-oxadiazine | |
| CN104744529B (en) | A kind of efficient high yield preparation method being suitable for suitability for industrialized production Gastrodine | |
| CN101716261B (en) | Method for preparing hecogenin | |
| CN100365010C (en) | Ergosterol preparation method | |
| CN103483155A (en) | Method for recovering phenol from diphenyl isophthalate synthesis wash water |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Neutralization improvement method for production of oxadiazon Effective date of registration: 20170621 Granted publication date: 20150401 Pledgee: Hefei SME financing Company limited by guarantee Pledgor: Hefei Xingyu Chemical Co., Ltd. Registration number: 2017340000097 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20180615 Granted publication date: 20150401 Pledgee: Hefei SME financing Company limited by guarantee Pledgor: Hefei Xingyu Chemical Co., Ltd. Registration number: 2017340000097 |