CN105540559A - Method for improving quality of oxammonium hydrochloride and raising yield of oxammonium hydrochloride - Google Patents
Method for improving quality of oxammonium hydrochloride and raising yield of oxammonium hydrochloride Download PDFInfo
- Publication number
- CN105540559A CN105540559A CN201610056595.1A CN201610056595A CN105540559A CN 105540559 A CN105540559 A CN 105540559A CN 201610056595 A CN201610056595 A CN 201610056595A CN 105540559 A CN105540559 A CN 105540559A
- Authority
- CN
- China
- Prior art keywords
- oxammonium hydrochloride
- concentration kettle
- yield
- oxammonium
- mother liquid
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/14—Hydroxylamine; Salts thereof
- C01B21/1463—Concentration
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for improving quality of oxammonium hydrochloride and raising the yield of oxammonium hydrochloride. The method includes the following steps that 1, oxammonium hydrochloride hydrolysate is added into a concentration kettle, and then mother liquid containing oxammonium hydrochloride is added into the concentration kettle; 2, the concentration kettle is heated, the temperature is made to be 60-90 DEG C, and the pressure is made to be 500-1000 Pa till liquid in the concentration kettle generates a crystal substance; 3, the concentration kettle is naturally cooled to 10-30 DEG C, then the concentration kettle is opened to completely discharge filtrate, ethyl alcohol is added into the concentration kettle to wash filter residues, and the filter residues are removed and dried. The previous batch of filtrate is adopted to serve as the mother liquid containing oxammonium hydrochloride and mixed with oxammonium hydrochloride hydrolysate, then heating and cooling crystallization are conducted, in this way, the crystallization point of oxammonium hydrochloride in the mixed liquid can be lowered, precipitation of high-purity oxammonium hydrochloride is facilitated, and the quality of the oxammonium hydrochloride is improved; the low temperature is easy to control, drying by distillation and other extreme situations are avoided, safety of process steps is improved, energy consumption is lowered, and the yield of a product is raised.
Description
Technical field
The invention belongs to organic synthesis field, relate to a kind of synthetic method of oxammonium hydrochloride, be specifically related to a kind of method improving quality of oxammonium hydrochloride and yield.
Background technology
Oxammonium hydrochloride is colorless needle crystals, is a kind of important organic synthesis industrial chemicals, and the main medicine intermediate that is used as is used for pharmaceutical industry.The preparation method of oxammonium hydrochloride has multiple, specifically have as follows: 1, Sodium Nitrite synthesis method (oximate method), water is added reactor, and add Sodium Nitrite under stirring, gradation adds Sodium Pyrosulfite, then sulfuric acid acidation is used, material after acidifying is sent into hydrolysis kettle, adds acetone, then neutralize with liquid caustic soda, neutralizer is distilled, obtains acetoxime; Added in salt oven with hydrochloric acid by acetoxime and react, generate oxammonium hydrochloride and acetone, recover acetone uses, and oxammonium hydrochloride, through concentrated, crystallisation by cooling, centrifugation, drying, gets product; 2, obtain hydrolyzed solution by after Nitromethane 99Min. and hydrochloric acid reaction, reconcentration is with obtained oxammonium hydrochloride crude product; 3, Sodium Nitrite is dissolved in water, and is cooled to 0 DEG C, adds sodium bisulfite and dilute sulphuric acid makes solution reacting by heating, and hydro-oxidation sodium solution, to pH value to 7 ~ 8, steams acetoxime, add that hydrochloric acid is concentrated, decolouring, filtration, reconcentration, cooling, crystallization.
All need in aforesaid method to carry out enrichment step, to obtain oxammonium hydrochloride solid.At present, in concentration technology process, normally qualified hydrolyzed solution suction concentration kettle is carried out negative pressure and concentrate, be concentrated into crystalline state, temperature in the kettle controls at about 120 DEG C.Such processing disadvantages is that temperature is higher, is difficult to accurate control; And need workman's moment observing response still can not allow wherein evaporate to dryness, otherwise can explosion hazard be caused, produce potential safety hazard.
Summary of the invention
The present invention seeks to provide a kind of method improving quality of oxammonium hydrochloride and yield to overcome the deficiencies in the prior art.
For achieving the above object, the technical solution used in the present invention is: a kind of method improving quality of oxammonium hydrochloride and yield, and it comprises the following steps:
A oxammonium hydrochloride hydrolyzed solution adds in concentration kettle by (), then add the mother liquid coming containing oxammonium hydrochloride in described concentration kettle;
B () heats described concentration kettle, make that its temperature is 60 ~ 90 DEG C, pressure is 500 ~ 1000Pa, and to described concentration kettle, liquid produces crystallisate;
C described concentration kettle is naturally cooled to 10 ~ 30 DEG C by (), open emptying filtrate subsequently, adds washing with alcohol filter residue wherein, dry.
Optimally, in step (a), the mass ratio of described oxammonium hydrochloride hydrolyzed solution and described mother liquid coming is 5 ~ 6:1.
Further, the mass ratio of described mother liquid coming and described ethanol is 5 ~ 6:1.
Optimally, in step (b), the mode of described heating is for adopting steam heating; Steam off in step (c) and naturally cooling.
Optimally, in step (c), described filtrate is applied mechanically in the oxammonium hydrochloride hydrolyzed solution of next batch as mother liquid coming.
Because technique scheme is used, the present invention compared with prior art has following advantages: the present invention improves the method for quality of oxammonium hydrochloride and yield, heating is carried out and crystallisation by cooling after mixing with oxammonium hydrochloride hydrolyzed solution as the mother liquid coming containing oxammonium hydrochloride by adopting the filtrate of last batch, can reduce oxammonium hydrochloride like this analyses a little in this mixed solution, be conducive to the precipitation of high-purity hydrochloric acid azanol, improve its quality; And lower temperature is easy to control, and can not produce the egregious cases such as evaporate to dryness, improve the security of processing step, reduce energy consumption, improve the output of product.
Embodiment
Below will the present invention is described in detail by specific embodiment.
Embodiment 1
The present embodiment provides a kind of method improving quality of oxammonium hydrochloride and yield, and it comprises the following steps:
A oxammonium hydrochloride hydrolyzed solution in previous process (adopts raw material to be that Nitromethane 99Min. and hydrochloric acid reaction obtain by (), and carry out purifying, oxammonium hydrochloride hydrolyzed solution qualified after testing, the production technique of hydrolyzed solution is prior art) 2800kg adds in concentration kettle, then mother liquid coming (filtrate after crystallization for producing in the last batch) 550kg added in described concentration kettle containing oxammonium hydrochloride mixes;
B () heating concentration kettle, makes that its temperature is 85 DEG C, pressure is 800Pa, to liquid in concentration kettle produces crystallisate (namely in concentration kettle liquid rise crystallisate);
C concentration kettle is naturally cooled to 30 DEG C by (), open the emptying filtrate of valve of concentration kettle subsequently, adds ethanol 100kg and wash filter residue in concentration kettle, collects filter residue and is dried at 60 DEG C, obtain 2000kg oxammonium hydrochloride, purity 99%.
Embodiment 2
The present embodiment provides a kind of method improving quality of oxammonium hydrochloride and yield, and it comprises the following steps:
A oxammonium hydrochloride hydrolyzed solution 3000kg in previous process adds in concentration kettle by (), then mother liquid coming (filtrate after crystallization for producing in the last batch) 600kg added in described concentration kettle containing oxammonium hydrochloride mixes;
B () heating concentration kettle, makes that its temperature is 90 DEG C, pressure is 1000Pa, to liquid in concentration kettle produces crystallisate (namely in concentration kettle liquid rise crystallisate);
C concentration kettle is naturally cooled to 10 DEG C by (), open the emptying filtrate of valve of concentration kettle subsequently, adds ethanol 100kg and wash filter residue in concentration kettle, collects filter residue and is dried at 80 DEG C, obtain 1800kg oxammonium hydrochloride, purity 96%.
Embodiment 3
The present embodiment provides a kind of method improving quality of oxammonium hydrochloride and yield, and it comprises the following steps:
A oxammonium hydrochloride hydrolyzed solution 3000kg in previous process adds in concentration kettle by (), then mother liquid coming (filtrate after crystallization for producing in the last batch) 500kg added in described concentration kettle containing oxammonium hydrochloride mixes;
B () heating concentration kettle, makes that its temperature is 60 DEG C, pressure is 500Pa, to liquid in concentration kettle produces crystallisate (namely in concentration kettle liquid rise crystallisate);
C concentration kettle is naturally cooled to room temperature by (), open the emptying filtrate of valve of concentration kettle subsequently, adds ethanol 85kg and wash filter residue in concentration kettle, collects filter residue and is dried at 70 DEG C, obtain 1900kg oxammonium hydrochloride, purity 97%.
Embodiment 4
The present embodiment provides a kind of method improving quality of oxammonium hydrochloride and yield, and it comprises the following steps:
A oxammonium hydrochloride hydrolyzed solution 3000kg in previous process adds in concentration kettle by (), then mother liquid coming (filtrate after crystallization for producing in the last batch) 1000kg added in described concentration kettle containing oxammonium hydrochloride mixes;
B () heating concentration kettle, makes that its temperature is 85 DEG C, pressure is 800Pa, to liquid in concentration kettle produces crystallisate (namely in concentration kettle liquid rise crystallisate);
C concentration kettle is naturally cooled to 30 DEG C by (), open the emptying filtrate of valve of concentration kettle subsequently, adds ethanol 100kg and wash filter residue in concentration kettle, collects filter residue and is dried at 60 DEG C, obtain 1500kg oxammonium hydrochloride, purity 90%.
Embodiment 5
The present embodiment provides a kind of method improving quality of oxammonium hydrochloride and yield, and it comprises the following steps:
A oxammonium hydrochloride hydrolyzed solution 3000kg in previous process adds in concentration kettle by (), then mother liquid coming (filtrate after crystallization for producing in the last batch) 300kg added in described concentration kettle containing oxammonium hydrochloride mixes;
B () heating concentration kettle, makes that its temperature is 90 DEG C, pressure is 1000Pa, to liquid in concentration kettle produces crystallisate (namely in concentration kettle liquid rise crystallisate);
C concentration kettle is naturally cooled to 10 DEG C by (), open the emptying filtrate of valve of concentration kettle subsequently, adds ethanol 100kg and wash filter residue in concentration kettle, collects filter residue and is dried at 80 DEG C, obtain 1600kg oxammonium hydrochloride, purity 92%.
Above-described embodiment is only for illustrating technical conceive of the present invention and feature; its object is to person skilled in the art can be understood content of the present invention and implement according to this; can not limit the scope of the invention with this; all equivalences done according to spirit of the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (5)
1. improve a method for quality of oxammonium hydrochloride and yield, it is characterized in that, it comprises the following steps:
A oxammonium hydrochloride hydrolyzed solution adds in concentration kettle by (), then add the mother liquid coming containing oxammonium hydrochloride in described concentration kettle;
B () heats described concentration kettle, make that its temperature is 60 ~ 90 DEG C, pressure is 500 ~ 1000Pa, and to described concentration kettle, liquid produces crystallisate;
C described concentration kettle is naturally cooled to 10 ~ 30 DEG C by (), open emptying filtrate subsequently, adds washing with alcohol filter residue wherein, dry.
2. the method for raising quality of oxammonium hydrochloride according to claim 1 and yield, is characterized in that: in step (a), and the mass ratio of described oxammonium hydrochloride hydrolyzed solution and described mother liquid coming is 5 ~ 6:1.
3. the method for raising quality of oxammonium hydrochloride according to claim 1 and 2 and yield, is characterized in that: the mass ratio of described mother liquid coming and described ethanol is 5 ~ 6:1.
4. the method for raising quality of oxammonium hydrochloride according to claim 1 and yield, is characterized in that: in step (b), and the mode of described heating is for adopting steam heating; Steam off in step (c) and naturally cooling.
5. the method for raising quality of oxammonium hydrochloride according to claim 1 and yield, is characterized in that: in step (c), and described filtrate is applied mechanically in the oxammonium hydrochloride hydrolyzed solution of next batch as mother liquid coming.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610056595.1A CN105540559A (en) | 2016-01-28 | 2016-01-28 | Method for improving quality of oxammonium hydrochloride and raising yield of oxammonium hydrochloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610056595.1A CN105540559A (en) | 2016-01-28 | 2016-01-28 | Method for improving quality of oxammonium hydrochloride and raising yield of oxammonium hydrochloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105540559A true CN105540559A (en) | 2016-05-04 |
Family
ID=55820197
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610056595.1A Pending CN105540559A (en) | 2016-01-28 | 2016-01-28 | Method for improving quality of oxammonium hydrochloride and raising yield of oxammonium hydrochloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105540559A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1751986A (en) * | 2005-08-04 | 2006-03-29 | 浙江大学 | Method of preparing solid hydroxylamine hydrochloride |
| CN101172591A (en) * | 2007-10-08 | 2008-05-07 | 江苏康祥集团公司 | Method for producing sodium hypophosphite |
| CN101659402A (en) * | 2009-09-15 | 2010-03-03 | 山东兴辉化工有限公司 | Method for improving quality of oxammonium hydrochloride |
| CN202223911U (en) * | 2011-08-22 | 2012-05-23 | 山东兴辉化工有限公司 | Hydroxylamine hydrochloride salifying concentration evaporating system |
| CN103159191A (en) * | 2013-03-25 | 2013-06-19 | 浙江圣安化工有限公司 | Preparation method of hydroxylamine salt |
| CN103253819A (en) * | 2013-04-22 | 2013-08-21 | 潍坊沃尔特化学有限公司 | Device and production technology for treating ternary-monomer wastewater and extracting sodium sulfate |
| CN105271143A (en) * | 2015-11-20 | 2016-01-27 | 山东兴辉化工有限公司 | Recycling and treatment technology for hydroxylamine hydrochloride mother liquor |
-
2016
- 2016-01-28 CN CN201610056595.1A patent/CN105540559A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1751986A (en) * | 2005-08-04 | 2006-03-29 | 浙江大学 | Method of preparing solid hydroxylamine hydrochloride |
| CN101172591A (en) * | 2007-10-08 | 2008-05-07 | 江苏康祥集团公司 | Method for producing sodium hypophosphite |
| CN101659402A (en) * | 2009-09-15 | 2010-03-03 | 山东兴辉化工有限公司 | Method for improving quality of oxammonium hydrochloride |
| CN202223911U (en) * | 2011-08-22 | 2012-05-23 | 山东兴辉化工有限公司 | Hydroxylamine hydrochloride salifying concentration evaporating system |
| CN103159191A (en) * | 2013-03-25 | 2013-06-19 | 浙江圣安化工有限公司 | Preparation method of hydroxylamine salt |
| CN103253819A (en) * | 2013-04-22 | 2013-08-21 | 潍坊沃尔特化学有限公司 | Device and production technology for treating ternary-monomer wastewater and extracting sodium sulfate |
| CN105271143A (en) * | 2015-11-20 | 2016-01-27 | 山东兴辉化工有限公司 | Recycling and treatment technology for hydroxylamine hydrochloride mother liquor |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2018113478A1 (en) | Method for producing lithium hydroxide monohydrate using lithium carbonate as raw material | |
| JP2015501331A (en) | Method for producing taurine | |
| CN106045879B (en) | Method for preparing cyanoacetic acid | |
| CN106632080A (en) | Flucytosine manufacturing process | |
| CN101607892B (en) | Method for producing sodium citrate | |
| CN101723773B (en) | Method for preparing high purity N-acetyl-DL-amino acid | |
| CN103508974B (en) | A kind of method processing adjacent sulfonamide benzoic acid methyl esters crystalline mother solution | |
| CN115521231B (en) | Environment-friendly clean preparation method of taurine | |
| CN112457270A (en) | Preparation method of dichloro pentachloromethyl thiazole | |
| CN105540559A (en) | Method for improving quality of oxammonium hydrochloride and raising yield of oxammonium hydrochloride | |
| CN110563699A (en) | Post-treatment purification method of fluoro pranoprazan intermediate | |
| CN103755625B (en) | A kind of clean method preparing high purity pyridine hydrochloride | |
| CN110759806A (en) | Preparation method of 2-chloro-4-fluorotoluene | |
| CN113307774B (en) | Method for recovering imidazole from imidazole hydrochloride wastewater | |
| CN103539745A (en) | Preparation method of secnidazole | |
| CN1309698C (en) | Purifying process of 3,4,5-trimethoxyl benzoic acid | |
| CN110590564B (en) | Method for synthesizing 2, 4-dichloroaniline by continuous chlorination process | |
| CN111233835A (en) | Preparation and purification method of 5- (2-fluorophenyl) -1- (pyridine-3-ylsulfonyl) -1H-pyrrole-3-formaldehyde | |
| CN106831513A (en) | The preparation method of thioacetic acid potassium | |
| CN107778160B (en) | Preparation method of 3,4,5, 6-tetrafluorophthalic acid | |
| CN101619015B (en) | Technology for producing inositol by glucose biomimetic method | |
| CN110172038B (en) | Process for preparing analgin magnesium by one-pot method | |
| CN101125815B (en) | Chemical synthesis method for ethyl 6-chloro-6-oxohexanoate | |
| CN112125811A (en) | Preparation method of amantadine | |
| CN113372247A (en) | Preparation method of sodium isethionate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160504 |