CN102584684A - Method for recovering pyridine from waste pyridine hydrochloride and cyclically reutilizing pyridine - Google Patents
Method for recovering pyridine from waste pyridine hydrochloride and cyclically reutilizing pyridine Download PDFInfo
- Publication number
- CN102584684A CN102584684A CN2011103919067A CN201110391906A CN102584684A CN 102584684 A CN102584684 A CN 102584684A CN 2011103919067 A CN2011103919067 A CN 2011103919067A CN 201110391906 A CN201110391906 A CN 201110391906A CN 102584684 A CN102584684 A CN 102584684A
- Authority
- CN
- China
- Prior art keywords
- pyridine
- pyridine hydrochloride
- water
- waste
- hydrochloride
- 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.)
- Pending
Links
Abstract
The invention provides a method for recovering pyridine from waste pyridine hydrochloride for producing chloromethyl isopropyl carbonate and cyclically reutilizing the pyridine. The method comprises the following process steps that: the pyridine hydrochloride and water are placed into a container according to a proportion being 1:2 to be stirred to obtain pyridine hydrochloride water solution, the pyridine hydrochloride water solution and two times of pyridine hydrochloride liquid caustic soda are placed into an enamel reaction kettle to be sufficiently stirred for taking reaction to generate pyridine and sodium chloride water solution, the pyridine and sodium chloride water solution are automatically produced in the still state, the upper layer is water-containing pyridine, the lower layer is sodium chloride water solution, the water-containing pyridine at the upper layer is taken out and is subjected to impurity removal through precipitation, rectification elution is adopted for removing water to obtain finished products, and the sodium chloride water solution is conveyed into a concentration pot to be concentrated to obtain sodium chloride finished products. The finished product pyridine can be used as one ingredient to be conveyed into a chloromethyl isopropyl carbonate production process line to be cyclically utilized for producing chloromethyl isopropyl carbonate. The method has the advantages that the resource waste is reduced, the environment cannot be polluted, meanwhile, the production cost of the chloromethyl isopropyl carbonate is also greatly reduced, and the economic benefits of enterprises are improved.
Description
Technical field
The present invention relates to a kind of method that from the waste pyridine hydrochloride of producing chloromethyl sec.-propyl carbonic ether, reclaims the pyrido cycling and reutilization.
Background technology
In the production process of chloromethyl sec.-propyl carbonic ether, can produce the waste pyridine hydrochloride.After the condensation reaction of chloromethyl sec.-propyl carbonic ether finishes, filter out the waste pyridine hydrochloride, one ton of chloromethyl sec.-propyl of every production carbonic ether will produce 0.9 ton of waste pyridine hydrochloride.As this castoff burning is handled, can generate the phosgene COCl2 of contaminate environment.Burn pyridine hydrochloride and also can cause the waste of resource and the increase of production cost.Bank up pyridine hydrochloride is packed, packing bag subjects to corrosion, also pollutes the environment.A large amount of pyridines is arranged in pyridine hydrochloride.And that pyridine is produced at home is less, most of dependence on import.When international resource is nervous, unstable from external import pyridine, have a strong impact on enterprise production sometimes.
Summary of the invention
The purpose of this invention is to provide a kind of method that from the waste pyridine hydrochloride of producing chloromethyl sec.-propyl carbonic ether, reclaims the pyrido cycling and reutilization.From the waste pyridine hydrochloride, reclaim the waste that the pyrido cycling and reutilization can reduce resource with present method, do not pollute the environment again, also can greatly reduce the production cost of chloromethyl sec.-propyl carbonic ether simultaneously, can improve economic benefit of enterprises.It is low that use present method recovery pyridine also has cost recovery, the advantage that recovery utilization rate is high.
Technical scheme of the present invention is: the method that from chloromethyl sec.-propyl carbonate production waste pyridine hydrochloride, reclaims pyridine.It comprises following process step:
A kind of method that from the waste pyridine hydrochloride, reclaims pyridine; In the process of producing chloromethyl sec.-propyl carbonic ether; After the condensation reaction of chloromethyl sec.-propyl carbonic ether finishes, except that getting chloromethyl sec.-propyl carbonic ether finished product, also remain a large amount of waste pyridine hydrochlorides.One ton of chloromethyl sec.-propyl of every production carbonic ether will produce 0.9 ton of waste pyridine hydrochloride.Filter the waste pyridine hydrochloride with filter cloth and get the solid-like pyridine hydrochloride, the pyridine hydrochloride on the water flushing filter cloth gets the aqueous pyridine hydrochloride again.Above-mentioned solid-like pyridine hydrochloride and aqueous pyridine hydrochloride put into dissolving pan and stir make pyridine hydrochloride be dissolved in water fully to become the pyridine hydrochloride aqueous solution, the add-on of water is two times of solid-like pyridine hydrochloride.The above-mentioned pyridine hydrochloride aqueous solution is sent in the free pot of pyridine, and the adding liquid caustic soda also fully stirs, and the add-on of liquid caustic soda is two times of the pyridine hydrochloride aqueous solution.The pyridine hydrochloride aqueous solution and liquid caustic soda fully react and produce pyridine and sodium chloride aqueous solution in whipping process, and its reaction formula is: pyridine hydrochloride+liquid caustic soda=pyridine+sodium-chlor+water.Its reactive chemistry formula is: C5H5N.HCl+NaOH=C5H5N+NaCl+H2O.The solution of above-mentioned pyridine+sodium-chlor+water is sent in the suction filter, and under static state the solution of pyridine+sodium-chlor+water is divided into automatically, and the upper strata is the pyridine of band water after the layering, and lower floor is a sodium chloride aqueous solution.Isolating must be with the pyridine of water behind lower floor's sodium chloride aqueous solution.Owing to salting out, the pyridine of the free state in the pyridine of band water also can separate and layering with water again.Water layer after separation and the layering is separated the pyridine that just obtains with less water.The pyridine of band less water removed with the precipitator method send into the smart tower that slips behind the impurity and remove Yu Shui with smart slide method and just obtain finished product.With sodium chloride aqueous solution send into concentrating pan concentrate the sodium-chlor finished product, the recyclable about 300Kg sodium-chlor of one ton of chloromethyl sec.-propyl of every production carbonic ether finished product.
A kind of method with the finished product pyridine cycling and reutilization that reclaims is sent into recycling production chloromethyl sec.-propyl carbonic ether in the chloromethyl sec.-propyl carbonate production processing line with the finished product pyridine of above-mentioned recovery as one of raw material.After the condensation reaction of chloromethyl sec.-propyl carbonic ether finishes, filter the waste pyridine hydrochloride that makes new advances again, new waste pyridine hydrochloride is sent into again reclaimed pyrido in the new recovery pyridine program the pyridine cycling and reutilization production chloromethyl sec.-propyl carbonic ether that reclaims.So just can continuously reclaim and cycling and reutilization the waste pyridine hydrochloride.
Advantage of the present invention has provided a kind of method that from the waste pyridine hydrochloride of producing chloromethyl sec.-propyl carbonic ether, reclaims the pyrido cycling and reutilization.From the waste pyridine hydrochloride, reclaim the waste that the pyrido cycling and reutilization had both reduced resource with present method, do not pollute the environment again, also greatly reduced the production cost of chloromethyl sec.-propyl carbonic ether simultaneously, improved economic benefit of enterprises.It is low that use present method recovery pyridine also has cost recovery, the advantage that recovery utilization rate is high.
Embodiment
Embodiment of the present invention is following: the method that from chloromethyl sec.-propyl carbonate production waste pyridine hydrochloride, reclaims pyridine.It comprises following process step:
A kind of method that from the waste pyridine hydrochloride, reclaims pyridine; In the process of producing chloromethyl sec.-propyl carbonic ether; After the condensation reaction of chloromethyl sec.-propyl carbonic ether finishes, except that getting chloromethyl sec.-propyl carbonic ether finished product, also remain a large amount of waste pyridine hydrochlorides.One ton of chloromethyl sec.-propyl of every production carbonic ether will produce 0.9 ton of waste pyridine hydrochloride.Filter the waste pyridine hydrochloride with filter cloth and get the solid-like pyridine hydrochloride, the pyridine hydrochloride on the water flushing filter cloth gets the aqueous pyridine hydrochloride again.Above-mentioned solid-like pyridine hydrochloride and aqueous pyridine hydrochloride put into dissolving pan and stir make pyridine hydrochloride be dissolved in water fully to become the pyridine hydrochloride aqueous solution, the add-on of water is two times of solid-like pyridine hydrochloride.The above-mentioned pyridine hydrochloride aqueous solution is sent in the free pot of pyridine, and the adding liquid caustic soda also fully stirs, and the add-on of liquid caustic soda is two times of the pyridine hydrochloride aqueous solution.The pyridine hydrochloride aqueous solution and liquid caustic soda fully react and produce pyridine and sodium chloride aqueous solution in whipping process, and its reaction formula is: pyridine hydrochloride+liquid caustic soda=pyridine+sodium-chlor+water.Its reactive chemistry formula is: C5H5N.HCl+NaOH=C5H5N+NaCl+H2O.The solution of above-mentioned pyridine+sodium-chlor+water is sent in the suction filter, and under static state the solution of pyridine+sodium-chlor+water is divided into automatically, and the upper strata is the pyridine of band water after the layering, and lower floor is a sodium chloride aqueous solution.Isolating must be with the pyridine of water behind lower floor's sodium chloride aqueous solution.Owing to salting out, the pyridine of the free state in the pyridine of band water also can separate and layering with water again.Water layer after separation and the layering is separated the pyridine that just obtains with less water.The pyridine of band less water removed with the precipitator method send into the smart tower that slips behind the impurity and remove Yu Shui with smart slide method and just obtain finished product.With sodium chloride aqueous solution send into concentrating pan concentrate the sodium-chlor finished product, the recyclable about 300Kg sodium-chlor of one ton of chloromethyl sec.-propyl of every production carbonic ether finished product.
A kind of method with the finished product pyridine cycling and reutilization that reclaims is sent into recycling production chloromethyl sec.-propyl carbonic ether in the chloromethyl sec.-propyl carbonate production processing line with the finished product pyridine of above-mentioned recovery as one of raw material.After the condensation reaction of chloromethyl sec.-propyl carbonic ether finishes, filter the waste pyridine hydrochloride that makes new advances again, new waste pyridine hydrochloride is sent into again reclaimed pyrido in the new recovery pyridine program the pyridine cycling and reutilization production chloromethyl sec.-propyl carbonic ether that reclaims.So just can continuously reclaim and cycling and reutilization the waste pyridine hydrochloride.
Claims (1)
1. method that from the waste pyridine hydrochloride, reclaims the pyrido cycling and reutilization, it is characterized in that: it comprises following process step:
A kind of method that from the waste pyridine hydrochloride, reclaims pyridine; In the process of producing chloromethyl sec.-propyl carbonic ether, after the condensation reaction of chloromethyl sec.-propyl carbonic ether finishes, except that getting chloromethyl sec.-propyl carbonic ether finished product, also remain a large amount of waste pyridine hydrochlorides; One ton of chloromethyl sec.-propyl of every production carbonic ether will produce 0.9 ton of waste pyridine hydrochloride; Filter the waste pyridine hydrochloride with filter cloth and get the solid-like pyridine hydrochloride, the pyridine hydrochloride on the water flushing filter cloth gets the aqueous pyridine hydrochloride again, above-mentioned solid-like pyridine hydrochloride and aqueous pyridine hydrochloride is put into dissolving pan and stirring make pyridine hydrochloride be dissolved in water fully to become the pyridine hydrochloride aqueous solution; The add-on of water is two times of solid-like pyridine hydrochloride; The above-mentioned pyridine hydrochloride aqueous solution is sent in the free pot of pyridine, and the adding liquid caustic soda also fully stirs, and the add-on of liquid caustic soda is two times of the pyridine hydrochloride aqueous solution; The pyridine hydrochloride aqueous solution and liquid caustic soda fully react and produce pyridine and sodium chloride aqueous solution in whipping process; Its reaction formula is: pyridine hydrochloride+liquid caustic soda=pyridine+sodium-chlor+water, and its reactive chemistry formula is: C5H5N.HCl+NaOH=C5H5N+NaCl+H2O, send into the solution of above-mentioned pyridine+sodium-chlor+water in the suction filter; Under static state the solution of pyridine+sodium-chlor+water is divided into automatically; The upper strata is the pyridine of band water after the layering, and lower floor is a sodium chloride aqueous solution, and isolating must be with the pyridine of water behind lower floor's sodium chloride aqueous solution; Again because salting out; Pyridine and the water of the free state in the pyridine of band water also can separate and layering, with separate and layering after water layer separate the pyridine that just obtains with less water, the pyridine of band less water is removed with the precipitator method is sent into the smart tower that slips behind the impurity and remove Yu Shui with smart slide method and just obtain finished product; With sodium chloride aqueous solution send into concentrating pan concentrate the sodium-chlor finished product, the recyclable about 300Kg sodium-chlor of one ton of chloromethyl sec.-propyl of every production carbonic ether finished product;
A kind of method with the finished product pyridine cycling and reutilization that reclaims; The finished product pyridine of above-mentioned recovery is sent into recycling production chloromethyl sec.-propyl carbonic ether in the chloromethyl sec.-propyl carbonate production processing line as one of raw material;, the condensation reaction of chloromethyl sec.-propyl carbonic ether filters the waste pyridine hydrochloride that makes new advances after finishing again; New waste pyridine hydrochloride sent in the new recovery pyridine program again reclaim pyrido the pyridine cycling and reutilization that reclaims is produced chloromethyl sec.-propyl carbonic ether, so just can continuously reclaim also cycling and reutilization the waste pyridine hydrochloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103919067A CN102584684A (en) | 2011-11-22 | 2011-11-22 | Method for recovering pyridine from waste pyridine hydrochloride and cyclically reutilizing pyridine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103919067A CN102584684A (en) | 2011-11-22 | 2011-11-22 | Method for recovering pyridine from waste pyridine hydrochloride and cyclically reutilizing pyridine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102584684A true CN102584684A (en) | 2012-07-18 |
Family
ID=46474015
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011103919067A Pending CN102584684A (en) | 2011-11-22 | 2011-11-22 | Method for recovering pyridine from waste pyridine hydrochloride and cyclically reutilizing pyridine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102584684A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965044A (en) * | 2014-04-04 | 2014-08-06 | 安徽海顺化工有限公司 | Preparation method of chloromethyl isopropyl carbonate |
| CN103992264A (en) * | 2014-04-25 | 2014-08-20 | 上海新华联制药有限公司 | Method for recovering pyridine from aqueous solution |
| CN105330078A (en) * | 2015-09-11 | 2016-02-17 | 安徽金禾实业股份有限公司 | Method for recovering catalyst in B4 workshop section in pyridinium salt production |
| CN112028818A (en) * | 2020-09-26 | 2020-12-04 | 安徽金禾实业股份有限公司 | Method for recovering catalyst pyridine |
| CN113200907A (en) * | 2021-03-19 | 2021-08-03 | 江西欧氏化工有限公司 | Novel treatment method of amination wastewater in monosultap synthesis process |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0243320A1 (en) * | 1986-04-25 | 1987-10-28 | Ciba-Geigy Ag | Process for the dehydratation of mixtures of water and N-heterocyclic compounds |
| CN1370770A (en) * | 2001-02-27 | 2002-09-25 | 天津药业集团有限公司 | Pyridine recovering process |
| CN101538240A (en) * | 2009-03-12 | 2009-09-23 | 浙江升华拜克生物股份有限公司 | Method for recycling solid wastes in carbonate production |
-
2011
- 2011-11-22 CN CN2011103919067A patent/CN102584684A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0243320A1 (en) * | 1986-04-25 | 1987-10-28 | Ciba-Geigy Ag | Process for the dehydratation of mixtures of water and N-heterocyclic compounds |
| CN1370770A (en) * | 2001-02-27 | 2002-09-25 | 天津药业集团有限公司 | Pyridine recovering process |
| CN101538240A (en) * | 2009-03-12 | 2009-09-23 | 浙江升华拜克生物股份有限公司 | Method for recycling solid wastes in carbonate production |
Non-Patent Citations (1)
| Title |
|---|
| 陈爱平，等: "吡啶回收方法的改进", 《江西化工》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965044A (en) * | 2014-04-04 | 2014-08-06 | 安徽海顺化工有限公司 | Preparation method of chloromethyl isopropyl carbonate |
| CN103992264A (en) * | 2014-04-25 | 2014-08-20 | 上海新华联制药有限公司 | Method for recovering pyridine from aqueous solution |
| CN105330078A (en) * | 2015-09-11 | 2016-02-17 | 安徽金禾实业股份有限公司 | Method for recovering catalyst in B4 workshop section in pyridinium salt production |
| CN112028818A (en) * | 2020-09-26 | 2020-12-04 | 安徽金禾实业股份有限公司 | Method for recovering catalyst pyridine |
| CN113200907A (en) * | 2021-03-19 | 2021-08-03 | 江西欧氏化工有限公司 | Novel treatment method of amination wastewater in monosultap synthesis process |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102584684A (en) | Method for recovering pyridine from waste pyridine hydrochloride and cyclically reutilizing pyridine | |
| CN106623370B (en) | Organic silicon slurry slag treatment process and system | |
| CN101391844B (en) | Salting pickled vegetable brine recovery technique | |
| CN106319519B (en) | A kind of method that tin stripping liquid and electrotinning are prepared using spent solder stripper cycle | |
| CN101357903B (en) | Novel technique for preparing 4-formyl amino antipyrine | |
| CN102167956A (en) | Method for recycling and reutilizing rare-earth polishing powder waste residue and waste liquor | |
| CN103991898A (en) | Utilizing method of catalytic coal gasification ash residues | |
| CN102557085A (en) | Method for producing cesium salt and rubidium salt based on zero discharge and continuous extraction | |
| CN103103349A (en) | Method for decomposing bayan obo rare earth ore concentrate by acid and alkali combination at low temperature | |
| CN101104883A (en) | Method for reclaiming indium and tin from ITO waste material by pickling-vulcanization deposition combined technique | |
| CN102392144A (en) | Process method for recovering indium and germanium from germanium concentrate | |
| CN107599234B (en) | A kind of waste aluminium plastic separation recycling technique | |
| CN102659559B (en) | Method for preparing lanthanum cerium oxalate from rare earth polishing powder waste residue | |
| CN102286664B (en) | Method for extracting copper from organic silicon chemical waste residue and recovering extraction liquid | |
| CN101935756B (en) | Method for reclaiming rare-earth and organic phase from third phase of rare-earth extraction | |
| CN102199706B (en) | Method for comprehensively recovering valuable metal in diode core | |
| CN104909489B (en) | A kind of process for producing of trichloro-isocyanuric acid sewage water treatment method | |
| CN105367425A (en) | Purification system for chemical method for preparing BHET monomer from waste PET material | |
| CN106185953B (en) | A kind of large-scale quartz sand pickling impurity removal whitening process | |
| CN103014338A (en) | Method for processing poor organic phase after solvent extraction indium extracting | |
| CN108383142B (en) | Method for producing alumina by recycling regenerated aluminum ash | |
| CN102838632B (en) | Process for continuously producing trimethyl phosphite by using N, N-dimethylaniline | |
| CN102167323A (en) | Silicon recovery method | |
| CN102249891B (en) | Method for recovering and purifying phenylacetic acid | |
| CN103303957A (en) | Method for preparing calcium chloride through carbide slag and hydrochloric acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120718 |