CN104649300B - The method of recovery and refining sodium bromide from dipropyl cyanoacetate mixture - Google Patents
The method of recovery and refining sodium bromide from dipropyl cyanoacetate mixture Download PDFInfo
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- CN104649300B CN104649300B CN201310576632.8A CN201310576632A CN104649300B CN 104649300 B CN104649300 B CN 104649300B CN 201310576632 A CN201310576632 A CN 201310576632A CN 104649300 B CN104649300 B CN 104649300B
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Abstract
The present invention proposes from dipropyl cyanoacetate mixture and to reclaim and the method for refining sodium bromide. Comprise step: the dipropyl cyanoacetate mixture containing sodium bromide is filtered, and filter collection sodium bromide dissolves, and adjusting PH with hydrobromic acid is 6～6.5, adds ether and paraffins mixture extractant, is uniformly mixed stratification. Divide water intaking liquid to boil, be cooled to 80 DEG C and add active carbon and diatomite mixing decolorizer, in 50～80 DEG C of decolourings, filter, filtrate spraying is dry, obtains the anhydrous sodium bromide of white powder, and purity is high, and the rate of recovery is high.
Description
Technical field
The present invention relates to from dipropyl cyanoacetate mixture to reclaim and the method for refining sodium bromide.
Background technology
In dipropyl cyanoacetate production process, produce a large amount of accessory substance sodium bromides, ethanol and a small amount of propyl cyanide acetic acidEster, a propyl cyanide sodium acetate, dipropyl cyanoacetic acid sodium etc., also comprise the gas chromatography impurity that raw material brings in product mixturesAnd foreign pigment. Accessory substance sodium bromide is solid matter in mixture, dry again after common employing filtration of past or centrifugationDrying method reclaims. The sodium bromide reclaiming directly replaces industrial sodium bromide to be recycling in and prepares hydrobromic acid, organic bromide as bromineFor alkane etc., in the bromide product of producing like this, often with much impurity, affect subsequent production, as low in yield, purity is not highDeng.
CN101798121B has introduced the method that reclaims sodium bromide from diethyl butylmalonate factory effluent, is about toWaste water is sent in evaporimeter, in evaporimeter, passes into steam and makes waste water evaporation and concentration with Steam Heating waste water, and crystallisation by cooling dividesFrom. the shortcoming of the method is to remove the organic impurities that clean sodium bromide is carried secretly, and the disposable rate of recovery is not high. obtainSodium bromide be two hydrates, easily caking.
CN1616352A has introduced a kind of from trimethoxy benzaldehyde industrial wastewater extraction sodium bromide method, de-by waste waterChromogenic filter, then condensing crystallizing. The method shortcoming is: sodium bromide color impurities and organic impurities can not be removed completely, gained brominationSodium is also dihydrate, easily caking.
Summary of the invention
The object of the invention is to provide a kind of method that reclaims sodium bromide mixture of producing from dipropyl cyanoacetate. MakeCan remove neatly by this method the gas chromatography impurity that sodium bromide is carried secretly, make the sodium bromide of purification and recover reach industrial goodsRequirement, replaces industrial sodium bromide to be directly used in other bromides and produces. Using the sodium bromide of this method purification and recover is anhydride,Purity is high, the rate of recovery is high, technological operation is simple.
Technical scheme of the present invention is: the method for recovery and refining sodium bromide from dipropyl cyanoacetate mixture, itComprise following processing step: the dipropyl cyanoacetate mixture that contains sodium bromide is filtered, and the sodium bromide of filter collection is soluble in water,Adding hydrobromic acid tune pH value is 6～6.5, adds ethers and the agent of alkanes mixture extraction, is uniformly mixed stratification. Water intaking layer, addsHeat boiling more than 30 minutes, is cooled to 80 DEG C, adds active carbon and diatomite mixture decolorizer, 50～80 DEG C of decolourings 0.5～1Hour, filtering, filtrate is spray-dried must white anhydrous thing sodium bromide.
As preferred technical scheme, the boiling point of ethers and alkanes extractant should meet 100 DEG C of following requirements, guarantees addingEnter front can the steaming of decolorizer and remove, so that follow-up decolouring is more complete.
As preferred technical scheme, the boiling point of ethers and alkanes extractant is 60～80 DEG C.
As preferred technical scheme, the weight ratio of ethers and alkanes is 1:0.3～1.
As preferred technical scheme, active carbon and diatomaceous weight ratio are 2:0.5～1.
Adopt the anhydride sodium bromide purity of optimal technical scheme purification and recover of the present invention high, white color.
The sodium bromide solution of the decolouring that employing technical solution of the present invention obtains can be directly used in organic bromide and produce, and receivesRate is high, impurity is few.
Specific implementation method
Embodiment 1
The centrifugal filtration of 2000L dipropyl cyanoacetate mixed liquor is separated, approximately 240 ㎏ sodium bromides of filter collection are dissolved in to 300LIn water, adding hydrobromic acid tune pH value is 6～6.5, stirs 5 minutes, adds propyl ether 20 ㎏, pentane 10 ㎏, 30 points of high degree of agitationClock, stratification. Divide a water intaking layer suction bleacher, the boiling 1 hour that heats up, is cooled to 80 DEG C, adds active carbon and diatomite to mixClose decolorizer (weight ratio 1:0.4) 7 ㎏, keep 75～80 DEG C of decolourings 1 hour, filter. Filtrate spraying is dry, obtains white powderAnhydrous sodium bromide.
Embodiment 2
Sodium bromide 100 ㎏ of collection that centrifugation is filtered are dissolved in to 150 ㎏ water, and adding hydrobromic acid tune pH value is 6～6.5, stirs 5Minute, add propyl ether 6 ㎏ and benzinum 3 ㎏, high degree of agitation 30 minutes, stratification. Divide water intaking layer, suction bleacher, heats upSeethe with excitement 1 hour, be cooled to 80 DEG C, add activated carbon 1 ㎏, diatomite 0.4 ㎏, keeps 75～80 DEG C of decolourings 30 minutes, filters. FilterLiquid adds isopropyl alcohol 54 ㎏, stirs, and drips 10～15 DEG C of concentrated sulfuric acid 200 ㎏, is warming up to 65 DEG C of insulations 3 hours, distillation. Heat up in a steamerFluid washing, with anhydrous sodium sulfate drying, filters to obtain 2-N-Propyl Bromide.
Claims (4)
1. the method for recovery and refining sodium bromide from dipropyl cyanoacetate mixture, is characterized in that, it comprises following workSkill step: the dipropyl cyanoacetate mixture that contains sodium bromide is filtered, and filter collection sodium bromide is soluble in water, adjusts pH with hydrobromic acidValue is 6～6.5, adds ether and the agent of alkanes mixture extraction, is uniformly mixed stratification; Divide water intaking layer ebuillition of heated half littleTime more than, be cooled to 80 DEG C, add active carbon and diatomite mixing decolorizer, in 50～80 DEG C of decolourings, while hot filter, filtrateSpray-dried white anhydrous thing sodium bromide.
2. as claimed in claim 1ly from dipropyl cyanoacetate mixture, reclaim and the method for refining sodium bromide its spyLevy and be that alkanes is pentane, normal hexane or its mixture, ethers is 100 DEG C of following linear of boiling point, and described linear isEthylene-propylene ether, propyl ether, or its mixture.
3. as claimed in claim 1ly from dipropyl cyanoacetate mixture, reclaim and the method for refining sodium bromide its spyLevy and be that the weight ratio of ethers and alkanes is 1:0.3～1.
4. as claimed in claim 1ly from dipropyl cyanoacetate mixture, reclaim and the method for refining sodium bromide its spyLevy and be to mix decolorizer active carbon and diatomaceous weight ratio is 2:0.5～1.
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| CN201310576632.8A CN104649300B (en) | 2013-11-19 | 2013-11-19 | The method of recovery and refining sodium bromide from dipropyl cyanoacetate mixture |
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| CN104649300B true CN104649300B (en) | 2016-05-04 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105858687A (en) * | 2016-06-26 | 2016-08-17 | 潍坊天福化学科技有限公司 | Method for preparing sodium bromide using waste hydrobromic acid |
| CN106365951B (en) * | 2016-08-31 | 2018-12-11 | 濮阳天源生物科技有限公司 | Prepare the recycling technique of 2- N-Propyl Bromide during 2,2- diisopropyl propionitrile |
| CN107337218B (en) * | 2017-07-21 | 2023-04-07 | 浙江华海天诚药业有限公司 | Method for recovering sodium bromide from bromine-containing wastewater |
| CN109456141B (en) * | 2018-11-13 | 2020-04-07 | 湖南兴同化学科技有限公司 | Method for preparing isopropyl bromide from oxadiazon etherification wastewater |
| CN112142588B (en) * | 2020-10-22 | 2022-01-28 | 湖南省湘中制药有限公司 | Recovery of 2-propylmalonic acid and method for preparing valproic acid by using same |
| CN112174169B (en) * | 2020-11-06 | 2022-01-28 | 湖南省湘中制药有限公司 | Method for recovering potassium chloride from high-salt valproate wastewater |
| CN113307289A (en) * | 2021-08-02 | 2021-08-27 | 清大国华环境集团股份有限公司 | Resource recycling method for hazardous waste containing brominated alkanes |
| CN113979452A (en) * | 2021-09-27 | 2022-01-28 | 江苏沃德化工有限公司 | Refining process of byproduct sodium bromide in bronopol synthesis |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1616352A (en) * | 2003-11-12 | 2005-05-18 | 李茂山 | Process for extracting sodium bromide |
| CN101245138A (en) * | 2008-03-21 | 2008-08-20 | 山东兄弟化工科技发展有限公司 | Poly-2,6-dibromobenzene aether and synthesizing process |
| CN101798121A (en) * | 2009-12-25 | 2010-08-11 | 溧阳市永安精细化工有限公司 | Method for recovering and recycling sodium bromide from diethylbutylmalonate waste water |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2006111164A1 (en) * | 2005-04-18 | 2006-10-26 | Jan Procida | Method of producing pure halide salts of alkaline and/or alkaline earth metal resulting from hvdrolytic treatment of halogenous organic waste material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1616352A (en) * | 2003-11-12 | 2005-05-18 | 李茂山 | Process for extracting sodium bromide |
| CN101245138A (en) * | 2008-03-21 | 2008-08-20 | 山东兄弟化工科技发展有限公司 | Poly-2,6-dibromobenzene aether and synthesizing process |
| CN101798121A (en) * | 2009-12-25 | 2010-08-11 | 溧阳市永安精细化工有限公司 | Method for recovering and recycling sodium bromide from diethylbutylmalonate waste water |
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Denomination of invention: Method for recovering and refining sodium bromide from a mixture of dipropylcyanoacetate Effective date of registration: 20230828 Granted publication date: 20160504 Pledgee: Bank of China Limited Shaoyang Branch Pledgor: Hunan Province Xiangzhong Pharmaceutical Co.,Ltd. Registration number: Y2023980054088 |