CN103159191A - Preparation method of hydroxylamine salt - Google Patents
Preparation method of hydroxylamine salt Download PDFInfo
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- CN103159191A CN103159191A CN2013100974998A CN201310097499A CN103159191A CN 103159191 A CN103159191 A CN 103159191A CN 2013100974998 A CN2013100974998 A CN 2013100974998A CN 201310097499 A CN201310097499 A CN 201310097499A CN 103159191 A CN103159191 A CN 103159191A
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Abstract
The invention relates to a preparation method of a hydroxylamine salt. The existing preparation process of the hydroxylamine salt is complex, the production safety needs to be enhanced and the product stability is poorer. The invention adopts the following technical scheme: firstly well preparing an appropriate amount of acid solution and oxime according to the molar ratio that C=NOH: H is 1: (1-1.3), wherein the mass fraction of the acid solution is 10%-35%; and adding the solution which is well prepared in the first step into a rectifying tower, controlling the absolute pressure of the rectifying tower at 0.095-0.1MPa and keeping the temperature of a tower kettle at 20-130 DEG C to perform distillation, controlling the tower top reflux ratio at 0-4, timely separating fractions, controlling the reflux ratio of the tower kettle at 0-100, circulating part of kettle liquid, and finally concentrating, crystallizing, filtering and drying a product to get the high-quality solid hydroxylamine salt. According to the preparation method disclosed by the invention, the efficiency of the rectifying tower is improved, the reaction rate is promoted, the using quantity of the raw materials is saved, the quality of a crude finished product is optimized, and the organic residues are overcome; and the process flow is short, the raw materials are saved, the yield is high, the product quality is stable, the post-treatment is simple, and the preparation method is environment-friendly.
Description
Technical field
The invention belongs to technical field of fine chemical synthesis, particularly a kind of preparation method of hydroxylammonium salt.
Background technology
Hydroxylammonium salt is purposes Chemicals very widely.Oxammonium sulfate and phosphatic hydroxylamine be mainly for the production of hexanolactam, agricultural chemicals etc.; Oxammonium hydrochloride mainly is used as the raw material of the compound probabilities such as medicine, spices, dyestuff.
At present, the method for preparing oxammonium sulfate mainly contains nitric oxide reduction method, acetoxime method, hydrolysis method etc.; The method for preparing phosphatic hydroxylamine mainly contains hydrogenation catalyst reduction method and hydrolysis method etc.; The method for preparing oxammonium hydrochloride mainly contains Nitromethane 99Min. hydrolysis method, acetoxime method, disulfonic acid ammonium salt hydrolysis method etc.This class methods ubiquity technical process is numerous and diverse, unstable product quality, post-processed difficulty, the drawback such as yield is low.
Publication number is to be described to a kind of production technique take Raschig process as basic route in the application documents " method for preparing solid hydroxylamine hydrochloride " of CN 1751986A, the hydroxylamine sulfate solution of utilizing oxammonium sulfate, ammonium sulfate, sulfuric acid, water to form is raw material, obtain the azanol complex compound by the extraction agent complexometric extraction, use successively again the oxammonium hydrochloride aqueous solution (or hydroxylamine sulfate solution) neutralization, the above-mentioned azanol complex compound of dilute hydrochloric acid back extraction to obtain the new oxammonium hydrochloride aqueous solution, obtain the product solid hydroxylamine hydrochloride after evaporative crystallization.Use this technology can effectively utilize Raschig process fluid sulphuric acid azanol, but technical process is complicated, adds auxiliary agent many, the finished product hydroxylammonium salt contains organic residue, and waste liquid contains a large amount of acid and organism, and post-processed is complicated.
Publication number is to be described in the application documents " oxime hydrolysis reaction and infiltration evaporation membrane sepn lotus root are closed the technology preparation of hydroxylamine by one-step method " of CN 101100293A to utilize oxime hydrolysis reaction and infiltration gasification film separation coupling technique preparation of hydroxylamine by one-step method, although using this technology to make the oxime hydrolysis efficiency is 80%, but infiltration vaporization membrane module is complicated, cost is higher, life-span is limited, and owing to using excessive strong acid and toluene, the actual industrial feasibility is not high.
Publication number is to be described in rectifying tower in the application documents " method of hydroxylammonium salt " of CN 101497433A, reaction that ketoxime is hydrolyzed in acidic solution generates hydroxylammonium salt and ketone, in time discharge from the ketone of rectifying tower tower top output, the crystallization of cooling reactor liquid, filter, washing, drying obtains the hydroxylammonium salt solid.Use this technical matters flow process simple, but this method can't prepare high-quality oxammonium sulfate, the hydroxylammonium salt that obtains contains organic residue, and in system, excessive acid-utilising rate is low again can't reuse.
Above-mentioned document shows, technique is simple, production safety, product is stable, trash is few, environmental friendliness, and save energy is the direction that following hydroxylammonium salt preparation technology probes into.Therefore, be badly in need of existing hydroxylammonium salt preparation technology is improved or develop new production line.
Summary of the invention
The present invention is directed to above-mentioned defective, a kind of preparation method of hydroxylammonium salt is provided, utilize a kind of rectification and hydrolization technology that refluxes at the bottom of tower that contains, according to reflux ratio at the bottom of the proportioning adjusting tower of raw material oxime and acid, reflux ratio increases cyclic part still liquid along with sour increment, improve the acid-utilising rate, thereby improve the column efficiency of rectifying tower operate continuously, promoted speed of reaction, optimized thick final product quality.This operational path is simple, flow process is short, and product purity is high, and aftertreatment is light, and yield is high and cost is relatively low.
For this reason, the present invention takes following technical scheme, a kind of preparation method of hydroxylammonium salt, oxime and acid are added in rectifying tower with certain proportioning, and adjusting tower head tower still reflux ratio is distinguished in the reaction that is hydrolyzed of the pressure and temperature of controlling rectifying tower, the knockout tower tops, circulation tower reactor liquid, the extraction bottom product, this product obtains high-quality hydroxylammonium salt through concentrated, crystallization, filtration, drying.
Concrete steps are as follows:
The first step: oxime (C=NOH) in molar ratio: acid (H) is 1:(1 ~ 1.3), be ready to appropriate acid solution and oxime.Described oxime is acetoxime, Diacetylmonoxime, and the methyl-propyl ketoxime, methyl isobutyl ketoxime,, described acid is phosphoric acid, sulfuric acid, hydrochloric acid, the massfraction of acid solution is (10% ~ 35%).
Second step: the ready solution of the first step is added in rectifying tower, controlling rectifying tower is to distill under 20 ~ 130 ℃ at absolute pressure 0.095 ~ 0.1MPa and tower reactor temperature, controlling the tower top reflux ratio is 0 ~ 4, timely separate fraction, controlling the tower reactor reflux ratio is 0 ~ 100, cyclic part still liquid, the circulation fluid entrance can be at feed position co-altitude or upper-lower position, the extraction bottom product.
The 3rd step: product concentrates, crystallization, filtration, drying obtain high-quality solid hydroxylammonium salt.
Described ketoxime is acetoxime, Diacetylmonoxime, methyl-propyl ketoxime, methyl isobutyl ketoxime.
Described mineral acid is hydrochloric acid, sulfuric acid or phosphoric acid.
Described proportioning is molar ratio: oxime (C=NOH): acid (H) is 1:(1 ~ 1.3).
At the bottom of described tower, reflux ratio is the tower reactor circulation fluid and the ratio of tower reactor Produced Liquid, and span of control is (0 ~ 100), and with the direct ratio that is controlled to of proportioning raw materials acid, namely sour increment reflux ratio increases.
The pressure of described control rectifying tower is normal pressure or decompression, and decompression refers to that absolute pressure is (0.095 ~ 0.1MPa).
Hydroxylammonium salt preparation method of the present invention, use a kind of rectification and hydrolization technology that refluxes at the bottom of tower that contains, according to reflux ratio size at the bottom of the proportioning adjusting tower of raw material oxime and acid, cyclic part tower reactor liquid, raw material fully is hydrolyzed in rectifying tower obtains hydroxylammonium salt and ketone, realized in the situation that in rectifying tower the little large excessive reaction-ure conversion-age of acid high, Reaction Separation is carried out simultaneously.Improve efficiency of rectification tower, promoted speed of reaction, saved the raw material consumption, optimized thick final product quality, overcome organic residue.This technical process is short, and raw material is economized, and yield is high, constant product quality, and aftertreatment is simple, and environmental friendliness.
Compared with prior art, the technology of the present invention has following remarkable advantage:
1. the present invention innovates a kind of rectification and hydrolization technology that refluxes at the bottom of tower that contains, and according to reflux ratio at the bottom of the proportioning adjusting tower of raw material oxime and acid, reflux ratio is the tower reactor circulation fluid and the ratio of tower reactor Produced Liquid, and span of control is (0 ~ 100), increases along with the increment of acid.Cyclic part still liquid improves the acid-utilising rate, thereby improves the column efficiency of rectifying tower operate continuously, has promoted speed of reaction, has optimized thick final product quality.
2. this process using tower reactor part still liquid refluxes and coordinates the top separation to carry out simultaneously, for the reversible characteristics of this technique hydrolysis reaction, by controlling the reflux ratio of tower top and tower reactor, cyclic part still liquid in the time of separate fraction has realized that transformation efficiency is high in the situation that the little large excessive speed of reaction of acid is fast, hydrolysis degree is complete, thick finished product purity is good, constant product quality, process operation safety.
3. the aftertreatment of this technique is simple, through suitably processing, but ketone reuse oxime processed, the azanol mother liquor can be used derived product processed, and acid solution can be used agricultural chemicals processed, energy-saving and emission-reduction, environmental friendliness.
4. finished product purity is high, does not contain organic residue.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1
Press oxime and 10% sulfuric acid mol ratio than being 1:0.5, taking purity to be 99.9% acetoxime 73.2 grams, 10% sulfuric acid 490 grams, use dropping funnel to add rectifying tower from the middle part simultaneously with the speed of 2ml/s and distill, controlling temperature is 50 ~ 60 ℃, and absolute pressure is 0.09MPa, controlling the tower top reflux ratio is that 100(is total reflux), after 15 minutes, then to regulate the tower top reflux ratio be 1, and the tower reactor reflux ratio is 5, part still liquid returns to the rectifying section of rectifying tower, sampling analysis is collected respectively in the circulation hydrolysis.Recording liquid of top of the tower PH is 7, and tower bottoms is 0.1% through dehydrated alcohol extraction post analysis organic phase oxime content.Final concentration kettle liquid obtains solid sulphuric acid azanol 160 grams after crystallization, filtration, drying.Yield is 97%, and transformation efficiency is 95%.
Embodiment 2
Press oxime with 10% sulfuric acid mol ratio than being 1:0.5, take purity and be 99.9% acetoxime 73.2 grams, 10% sulfuric acid 490 grams use dropping funnel to add rectifying tower from the middle part simultaneously with the speed of 2ml/s and distill, controlling temperature is 50 ~ 60 ℃, absolute pressure is 0.09MPa, and controlling the tower top reflux ratio is that 100(is total reflux), after 15 minutes, regulating the tower top reflux ratio is 1 again, the tower reactor reflux ratio is that 0(does not namely circulate), collect respectively sampling analysis.Recording liquid of top of the tower PH is 7, and tower bottoms is 2.8% through dehydrated alcohol extraction post analysis organic phase oxime content.Final concentration kettle liquid obtains solid sulphuric acid azanol 151.2 grams after cooling, crystallization, filtration, drying.Yield is 97%, and transformation efficiency is 92%.
Embodiment 3
Press oxime and 20% hydrochloric acid mol ratio than being 1:1, taking purity to be 99.9% acetoxime 73.2 grams, 20% hydrochloric acid 365 grams, use dropping funnel to add rectifying tower from the middle part simultaneously with the speed of 2ml/s and distill, controlling temperature is 50 ~ 60 ℃, and absolute pressure is 0.09MPa, controlling the tower top reflux ratio is that 100(is total reflux), after 15 minutes, then to regulate the tower top reflux ratio be 0.5, and the tower reactor reflux ratio is 8, part still liquid returns to the rectifying section of rectifying tower, sampling analysis is collected respectively in the circulation hydrolysis.Recording liquid of top of the tower PH is 6.5, and tower bottoms is 0.3% through dehydrated alcohol extraction post analysis organic phase oxime content.Final concentration kettle liquid obtains solid hydroxylamine hydrochloride 66.6 grams after cooling, crystallization, filtration, drying.Yield is 96%, and transformation efficiency is 95.7%.
Embodiment 4
Press oxime with 20% hydrochloric acid mol ratio than being 1:1, take purity and be 99.9% acetoxime 73.2 grams, 20% hydrochloric acid 365 grams use dropping funnel to add rectifying tower from the middle part simultaneously with the speed of 2ml/s and distill, controlling temperature is 50 ~ 60 ℃, absolute pressure is 0.09MPa, and controlling the tower top reflux ratio is that 100(is total reflux), after 15 minutes, regulating the tower top reflux ratio is 0.5 again, the tower reactor reflux ratio is that 0(does not namely circulate), collect respectively sampling analysis.Recording liquid of top of the tower PH is 6.8, and tower bottoms is 2.8% through dehydrated alcohol extraction post analysis organic phase oxime content.Final concentration kettle liquid obtains solid hydroxylamine hydrochloride 62.9 grams after cooling, crystallization, filtration, drying.Yield is 90.5%, and transformation efficiency is 91.8%.
Embodiment 5
Press oxime and 20% phosphoric acid molar ratios than being 1:0.35, taking purity to be 99.9% acetoxime 73.2 grams, 20% phosphatase 11 71.5 grams, use dropping funnel to add rectifying tower from the middle part simultaneously with the speed of 2ml/s and distill, controlling temperature is 70 ~ 80 ℃, and absolute pressure is 0.08MPa, controlling the tower top reflux ratio is that 100(is total reflux), after 25 minutes, then to regulate the tower top reflux ratio be 2, and the tower reactor reflux ratio is 4, part still liquid returns to the feed zone of rectifying tower, sampling analysis is collected respectively in the circulation hydrolysis.Recording liquid of top of the tower PH is 7.0, and tower bottoms is 0.4% through dehydrated alcohol extraction post analysis organic phase oxime content.Final concentration kettle liquid obtains solid phosphoric acid azanol 166.5 grams after cooling, crystallization, filtration, drying.Yield is 97.3%, and transformation efficiency is 97%.
Embodiment 6
Press oxime with 20% phosphoric acid molar ratios than being 1:0.35, take purity and be 99.9% acetoxime 73.2 grams, 20% phosphatase 11 71.5 grams use dropping funnel to add rectifying tower from the middle part simultaneously with the speed of 2ml/s and distill, controlling temperature is 70 ~ 80 ℃, absolute pressure is 0.08MPa, and controlling the tower top reflux ratio is that 100(is total reflux), after 25 minutes, regulating the tower top reflux ratio is 2 again, the tower reactor reflux ratio is that 0(does not namely circulate), collect respectively sampling analysis.Recording liquid of top of the tower PH is 6.4, and tower bottoms is 3.9% through dehydrated alcohol extraction post analysis organic phase oxime content.Final concentration kettle liquid obtains solid phosphoric acid azanol 178.2 grams after cooling, crystallization, filtration, drying.Yield is 90.5%, and transformation efficiency is 90.2%.
Embodiment 7
Hydrochloric acid mol ratio by oxime and 33% is 1:1.02, takes purity and be 99.9% Diacetylmonoxime 87.2 grams, 33% hydrochloric acid 110.6 grams, use dropping funnel to add rectifying tower from the middle part simultaneously with the speed of 3ml/s and distill, controlling temperature is 90 ~ 100 ℃, and absolute pressure is 0.8MPa, controlling the tower top reflux ratio is that 100(is total reflux), after 30 minutes, then to regulate the tower top reflux ratio be 1, and the tower reactor reflux ratio is 3, part still liquid returns to the feed zone of rectifying tower, sampling analysis is collected respectively in the circulation hydrolysis.Recording liquid of top of the tower PH is 7.0, and tower bottoms is 0.5% through dehydrated alcohol extraction post analysis organic phase oxime content.Final concentration kettle liquid obtains solid hydroxylamine hydrochloride 67.8 grams after cooling, crystallization, filtration, drying.Yield is 97.5%, and transformation efficiency is 97%.
Embodiment 8
Hydrochloric acid mol ratio by oxime and 33% is 1:1.02, take purity and be 99.9% Diacetylmonoxime 87.2 grams, 33% hydrochloric acid 110.6 grams use dropping funnel to add rectifying tower from the middle part simultaneously with the speed of 3ml/s and distill, controlling temperature is 90 ~ 100 ℃, absolute pressure is 0.8MPa, and controlling the tower top reflux ratio is that 100(is total reflux), after 30 minutes, regulating the tower top reflux ratio is 1 again, the tower reactor reflux ratio is that 0(does not namely circulate), collect respectively sampling analysis.Recording liquid of top of the tower PH is 6.5, and tower bottoms is 4.2% through dehydrated alcohol extraction post analysis organic phase oxime content.Final concentration kettle liquid obtains solid hydroxylamine hydrochloride 64.1 grams after cooling, crystallization, filtration, drying.Yield is 92.1%, and transformation efficiency is 91.5%.
Embodiment 9
Hydrochloric acid mol ratio by oxime and 25% is 1:1.03, take purity and be 99.8% methyl isobutyl ketoxime 115.4 grams, 25% hydrochloric acid 150.39 grams, using dropping funnel to add rectifying tower from the middle part simultaneously with the speed of 4ml/s distills, controlling temperature is 90 ~ 100 ℃, absolute pressure is 0.09MPa, controlling the tower top reflux ratio is that 100(is total reflux), after 40 minutes, then to regulate the tower top reflux ratio be 1.5, and the tower reactor reflux ratio is 3, part still liquid returns to the stripping section of rectifying tower, sampling analysis is collected respectively in the circulation hydrolysis.Recording liquid of top of the tower PH is 7.0, and tower bottoms is 0.2% through dehydrated alcohol extraction post analysis organic phase oxime content.Final concentration kettle liquid obtains solid hydroxylamine hydrochloride 68.3 grams after cooling, crystallization, filtration, drying.Yield is 98.3%, and transformation efficiency is 98%.
Embodiment 10
Hydrochloric acid mol ratio by oxime and 25% is 1:1.03, take purity and be 99.8% methyl isobutyl ketoxime 115.4 grams, 25% hydrochloric acid 150.39 grams use dropping funnel to add rectifying tower from the middle part simultaneously with the speed of 4ml/s and distill, controlling temperature is 90 ~ 100 ℃, absolute pressure is 0.09MPa, and controlling the tower top reflux ratio is that 100(is total reflux), after 40 minutes, regulating the tower top reflux ratio is 1.5 again, the tower reactor reflux ratio is that 0(does not namely circulate), collect respectively sampling analysis.Recording liquid of top of the tower PH is 6.0, and tower bottoms is 3.9% through dehydrated alcohol extraction post analysis organic phase oxime content.Final concentration kettle liquid obtains solid hydroxylamine hydrochloride 65.1 grams after cooling, crystallization, filtration, drying.Yield is 93.7%, and transformation efficiency is 93%.
Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Claims (3)
1. the preparation method of a hydroxylammonium salt, it is characterized in that oxime and acid are added in rectifying tower with certain proportioning, the reaction that is hydrolyzed of the pressure and temperature of controlling rectifying tower, difference adjusting tower head tower still reflux ratio, the knockout tower tops, circulation tower reactor liquid, the extraction bottom product, this product obtains high-quality hydroxylammonium salt through concentrated, crystallization, filtration, drying.Be specially:
The first step: oxime (C=NOH) in molar ratio: acid (H) is 1:(1 ~ 1.3), be ready to appropriate acid solution and oxime, the massfraction of acid solution is (10% ~ 35%),
Second step: the ready solution of the first step is added in rectifying tower, controlling rectifying tower is to distill under 20 ~ 130 ℃ at absolute pressure 0.095 ~ 0.1MPa and tower reactor temperature, controlling the tower top reflux ratio is 0 ~ 4, timely separate fraction, controlling the tower reactor reflux ratio is 0 ~ 100, cyclic part still liquid, and the circulation fluid entrance can be at feed position co-altitude or upper-lower position, the extraction bottom product
The 3rd step: product concentrates, crystallization, filtration, drying obtain high-quality solid hydroxylammonium salt.
2. the preparation method of a kind of hydroxylammonium salt according to claim 1, is characterized in that described ketoxime is acetoxime, Diacetylmonoxime, cyclohexanone-oxime, methyl isobutyl ketoxime.
3. the preparation method of a kind of hydroxylammonium salt according to claim 1, is characterized in that described acid is hydrochloric acid, sulfuric acid or phosphoric acid.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104925768A (en) * | 2014-03-19 | 2015-09-23 | 湖北航天化学技术研究所 | Hydroxylamine nitrate crystal preparation method |
| CN105314610A (en) * | 2014-08-04 | 2016-02-10 | 余立新 | Preparation method for hydroxylammonium chloride |
| CN105315139A (en) * | 2014-08-04 | 2016-02-10 | 余立新 | Processing method for ketoxime type silane byproduct ketoxime salt |
| CN105384656A (en) * | 2015-10-23 | 2016-03-09 | 中石化南京工程有限公司 | Cyclohexanone oxime synthesis method |
| CN105540559A (en) * | 2016-01-28 | 2016-05-04 | 苏州市吴赣药业有限公司 | Method for improving quality of oxammonium hydrochloride and raising yield of oxammonium hydrochloride |
| CN105731401A (en) * | 2016-03-25 | 2016-07-06 | 巨化集团技术中心 | Device and method for producing hydroxylamine hydrochloride |
| CN105752954A (en) * | 2016-03-25 | 2016-07-13 | 巨化集团技术中心 | Method for purifying hydroxylamine hydrochloride |
| CN105776159A (en) * | 2016-01-28 | 2016-07-20 | 张玲 | Method for producing hydroxylamine hydrochloride through continuous method |
| CN106829893A (en) * | 2017-03-20 | 2017-06-13 | 临沭县华盛化工有限公司 | The method that HAS is produced using continuous vacuum distillation |
| CN106946234A (en) * | 2017-03-09 | 2017-07-14 | 北京化工大学 | A kind of preparation method of HAS |
| CN107539966A (en) * | 2017-09-29 | 2018-01-05 | 江苏艾科维科技有限公司 | The preparation method of HAS |
| CN109133015A (en) * | 2018-10-22 | 2019-01-04 | 江苏长青农化股份有限公司 | A kind of preparation method of hydroxylamine hydrochloride |
| CN109250694A (en) * | 2018-08-24 | 2019-01-22 | 北京化工大学 | A method of hydroxylamine hydrochloride is prepared using hydrogen chloride dry gas |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101250112A (en) * | 2008-03-18 | 2008-08-27 | 台州市知青化工有限公司 | Method for producing 1-p-methylphenyl ethylamine |
| CN101497433A (en) * | 2009-03-08 | 2009-08-05 | 宁波欧迅化学新材料技术有限公司 | Method for preparing hydroxylammonium salt |
-
2013
- 2013-03-25 CN CN201310097499.8A patent/CN103159191B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101250112A (en) * | 2008-03-18 | 2008-08-27 | 台州市知青化工有限公司 | Method for producing 1-p-methylphenyl ethylamine |
| CN101497433A (en) * | 2009-03-08 | 2009-08-05 | 宁波欧迅化学新材料技术有限公司 | Method for preparing hydroxylammonium salt |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104925768A (en) * | 2014-03-19 | 2015-09-23 | 湖北航天化学技术研究所 | Hydroxylamine nitrate crystal preparation method |
| CN105314610A (en) * | 2014-08-04 | 2016-02-10 | 余立新 | Preparation method for hydroxylammonium chloride |
| CN105315139A (en) * | 2014-08-04 | 2016-02-10 | 余立新 | Processing method for ketoxime type silane byproduct ketoxime salt |
| CN105315139B (en) * | 2014-08-04 | 2017-08-29 | 余立新 | A kind of processing method of ketoxime type silane by-products ketoxime salt |
| CN105384656A (en) * | 2015-10-23 | 2016-03-09 | 中石化南京工程有限公司 | Cyclohexanone oxime synthesis method |
| CN105540559A (en) * | 2016-01-28 | 2016-05-04 | 苏州市吴赣药业有限公司 | Method for improving quality of oxammonium hydrochloride and raising yield of oxammonium hydrochloride |
| CN105776159A (en) * | 2016-01-28 | 2016-07-20 | 张玲 | Method for producing hydroxylamine hydrochloride through continuous method |
| CN105731401A (en) * | 2016-03-25 | 2016-07-06 | 巨化集团技术中心 | Device and method for producing hydroxylamine hydrochloride |
| CN105752954A (en) * | 2016-03-25 | 2016-07-13 | 巨化集团技术中心 | Method for purifying hydroxylamine hydrochloride |
| CN106946234B (en) * | 2017-03-09 | 2019-07-30 | 北京化工大学 | A kind of preparation method of hydroxyl sulfate |
| CN106946234A (en) * | 2017-03-09 | 2017-07-14 | 北京化工大学 | A kind of preparation method of HAS |
| CN106829893A (en) * | 2017-03-20 | 2017-06-13 | 临沭县华盛化工有限公司 | The method that HAS is produced using continuous vacuum distillation |
| CN107539966A (en) * | 2017-09-29 | 2018-01-05 | 江苏艾科维科技有限公司 | The preparation method of HAS |
| CN109250694A (en) * | 2018-08-24 | 2019-01-22 | 北京化工大学 | A method of hydroxylamine hydrochloride is prepared using hydrogen chloride dry gas |
| CN109250694B (en) * | 2018-08-24 | 2020-12-11 | 北京化工大学 | Method for preparing hydroxylamine hydrochloride by using hydrogen chloride dry gas |
| CN109133015A (en) * | 2018-10-22 | 2019-01-04 | 江苏长青农化股份有限公司 | A kind of preparation method of hydroxylamine hydrochloride |
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