CN113666347A - Regeneration treatment method of hydrazine hydrate hydrochloride - Google Patents
Regeneration treatment method of hydrazine hydrate hydrochloride Download PDFInfo
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- CN113666347A CN113666347A CN202110986217.4A CN202110986217A CN113666347A CN 113666347 A CN113666347 A CN 113666347A CN 202110986217 A CN202110986217 A CN 202110986217A CN 113666347 A CN113666347 A CN 113666347A
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- Prior art keywords
- hydrazine hydrate
- hydrate hydrochloride
- hydrochloride
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- water
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- 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
- C01B21/16—Hydrazine; Salts thereof
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- 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
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- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a regeneration treatment method of hydrazine hydrate hydrochloride, which comprises the following steps: (1) when the purity of the hydrazine hydrate hydrochloride is lower than 90%, collecting the hydrazine hydrate hydrochloride; (2) dissolving the collected hydrazine hydrate hydrochloride in water, adding a polar solvent into the water under the stirring condition, then continuing stirring for 10-30min, carrying out solid-liquid separation, and drying the solid obtained by separation to obtain the regenerated hydrazine hydrate hydrochloride. The invention adds the polar solvent into the aqueous solution of hydrazine hydrate hydrochloride to destroy the solubility balance of the aqueous solution of hydrazine hydrate hydrochloride so as to separate out hydrazine hydrate hydrochloride crystals, and the aim of removing impurities is achieved by a solid-liquid separation technology; the purity of the obtained regenerated hydrazine hydrate hydrochloride is 99-99.8%, the aim of regeneration treatment of the hydrazine hydrate hydrochloride is effectively achieved, and the recycling efficiency of the hydrazine hydrate hydrochloride is improved.
Description
Technical Field
The invention belongs to the technical field of hydrazine hydrate hydrochloride regeneration, and particularly relates to a regeneration treatment method of hydrazine hydrate hydrochloride.
Background
Hydrazine hydrate hydrochloride is an intermediate product in the process of producing methyl hydrazine by using a hydrazine hydrate method, can be subjected to alkylation reaction with methanol under specific conditions to obtain methyl hydrazine hydrochloride, so that the methyl hydrazine is further obtained, and can be recycled for multiple times, but the impurities contained in the hydrazine hydrate hydrochloride gradually increase along with the increase of the cycle number, wherein the impurities such as iron, p-dimethylhydrazine, trimethylhydrazine and the like are most prominent, and the hydrazine hydrate contains mechanical impurities carried in raw materials, which influence the recycling rate of the hydrazine hydrate and reduce the efficiency of generating the methyl hydrazine; it is necessary to regenerate the intermediate hydrazine hydrate hydrochloride to reduce the content of impurities therein and to increase the concentration of the hydrazine hydrate salt.
At present, hydrazine hydrate hydrochloride with excessive cycle times cannot be used due to high impurity content, and can only be replaced by hydrazine hydrate or be treated by a third party organization as solid waste, but the cost of the two treatment methods is high.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a regeneration treatment method of hydrazine hydrate hydrochloride, which is characterized in that a polar solvent is added into aqueous solution of the hydrazine hydrate hydrochloride to form crystals to be separated from impurities, and the method has the advantages of simple operation, low cost and good economical efficiency.
A regeneration treatment method of hydrazine hydrate hydrochloride comprises the following steps:
(1) when the purity of the hydrazine hydrate hydrochloride is lower than 90%, collecting the hydrazine hydrate hydrochloride;
(2) dissolving the collected hydrazine hydrate hydrochloride in water, adding a polar solvent into the water under the stirring condition, then continuing stirring for 10-30min, carrying out solid-liquid separation, and drying the solid obtained by separation to obtain the regenerated hydrazine hydrate hydrochloride.
Preferably, the polar solvent is acetonitrile, methanol, ethanol or dichloromethane.
Preferably, in step (2), the ratio of hydrazine hydrate hydrochloride to water is 1g (0.3-1) mL, and the volume ratio of water to polar solvent is 1: (5-20).
Preferably, the drying conditions are: the drying temperature is 80-100 ℃, and the drying time is 6-10 h.
Preferably, the regenerated hydrazine hydrate hydrochloride has a purity of 99 to 99.8%.
The hydrazine hydrate hydrochloride is an intermediate product in the process of producing the methylhydrazine by using a hydrazine hydrate method in the prior art.
The invention has the advantages that:
(1) the invention adds the polar solvent into the aqueous solution of hydrazine hydrate hydrochloride to destroy the solubility balance of the aqueous solution of hydrazine hydrate hydrochloride so as to separate out the crystals of hydrazine hydrate hydrochloride, and achieves the purpose of removing impurities by a solid-liquid separation technology.
(2) By the method, the purity of the obtained regenerated hydrazine hydrate hydrochloride is 99-99.8%, the aim of regeneration treatment of the hydrazine hydrate hydrochloride is effectively fulfilled, and the recycling efficiency of the hydrazine hydrate hydrochloride is improved.
Detailed Description
In the process of preparing the methylhydrazine by using a hydrazine hydrate method, the hydrazine hydrate is converted into the methylhydrazine through four steps of salification, methylation, neutralization and displacement and distillation. In the whole process, the hydrazine hydrate amount used in the neutralization and replacement step is far greater than the amount of the replaced methylhydrazine, so that the hydrazine hydrate hydrochloride amount in the re-salifying step is continuously accumulated, and part of redundant hydrazine hydrate hydrochloride needs to be periodically discharged out of a production system, so that the safety production is ensured.
Raw materials: the hydrazine hydrate hydrochloride adopted in the embodiment of the invention is an intermediate product in the process of producing the methyl hydrazine by using a hydrazine hydrate method, the purity is 85 percent, and the hydrazine hydrate hydrochloride contains the following impurities: 5.3 percent of ethyl hydrazine, 7.9 percent of p-dimethylhydrazine and 1.8 percent of other impurities.
The present invention will be further illustrated by the following specific examples of the above-mentioned raw material treatment.
Example 1
Dissolving 300g of the raw material hydrazine hydrate hydrochloride in 300mL of water, slowly adding 1500mL of acetonitrile into the raw material under the stirring condition, then continuing stirring for 10 minutes, performing suction filtration, and performing vacuum drying on a solid material obtained by suction filtration at 90 ℃ for 8 hours to obtain 240 g of regenerated hydrazine hydrate hydrochloride, wherein the purity is 99.5% and the yield is 93.6%.
Example 2
Dissolving 300g of the raw material hydrazine hydrate hydrochloride in 300mL of water, slowly adding 1500mL of methanol into the raw material under the stirring condition, then continuing stirring for 10 minutes, performing suction filtration, and performing vacuum drying on a solid material obtained by suction filtration at 90 ℃ for 8 hours to obtain 238 g of regenerated hydrazine hydrate hydrochloride with the purity of 99.1% and the yield of 92.5%.
Example 3
Dissolving 300g of the raw material hydrazine hydrate hydrochloride in 300mL of water, slowly adding 1500mL of ethanol under the stirring condition, then continuing stirring for 10 minutes, performing suction filtration, and performing vacuum drying on the solid material obtained by suction filtration at 90 ℃ for 8 hours to obtain 242 g of regenerated hydrazine hydrate hydrochloride with the purity of 99.2% and the yield of 94.1%.
Example 4
In a reaction kettle, 300kg of the raw material hydrazine hydrate hydrochloride is dissolved in 150L of water, 1500L of methanol is slowly added into the raw material hydrazine hydrate hydrochloride under the condition of stirring, then the stirring is continued for 20 minutes, the suction filtration is carried out, the solid material obtained by the suction filtration is dried in vacuum for 6 hours at 100 ℃, and 240kg of regenerated hydrazine hydrate hydrochloride is obtained, the purity is 99.3 percent, and the yield is 93.46 percent.
Example 5
Dissolving 600kg of the raw material hydrazine hydrate hydrochloride in 200L of water in a reaction kettle, slowly adding 1200L of acetonitrile into the mixture under the condition of stirring, then continuing stirring for 10 minutes, performing suction filtration, and performing vacuum drying on the solid material obtained by suction filtration at 90 ℃ for 8 hours to obtain 490kg of regenerated hydrazine hydrate hydrochloride, wherein the purity is 99.3 percent and the yield is 95.41 percent.
Example 6
In a reaction kettle, 600kg of the raw material hydrazine hydrate hydrochloride is dissolved in 480L of water, 2600L of dichloromethane is slowly added into the raw material under the condition of stirring, then the stirring is continued for 30 minutes, the suction filtration is carried out, the solid material obtained by the suction filtration is dried in vacuum for 10 hours at 80 ℃, and 480kg of regenerated hydrazine hydrate hydrochloride is obtained, the purity is 99.5 percent, and the yield is 93.65 percent.
Claims (5)
1. A regeneration treatment method of hydrazine hydrate hydrochloride is characterized in that: the method comprises the following steps:
(1) when the purity of the hydrazine hydrate hydrochloride is lower than 90%, collecting the hydrazine hydrate hydrochloride;
(2) dissolving the collected hydrazine hydrate hydrochloride in water, adding a polar solvent into the water under the stirring condition, then continuing stirring for 10-30min, carrying out solid-liquid separation, and drying the solid obtained by separation to obtain the regenerated hydrazine hydrate hydrochloride.
2. The method for reprocessing hydrazine hydrate hydrochloride according to claim 1, wherein: the polar solvent is acetonitrile, methanol, ethanol or dichloromethane.
3. The method for reprocessing hydrazine hydrate hydrochloride according to claim 2, wherein: in the step (2), the ratio of the hydrazine hydrate hydrochloride to the water is 1g (0.3-1) mL, and the volume ratio of the water to the polar solvent is 1: (5-20).
4. The method of claim 3 for reprocessing hydrazine hydrate hydrochloride wherein: the drying conditions are as follows: the drying temperature is 80-100 ℃, and the drying time is 6-10 h.
5. The method of claim 4 for reprocessing hydrazine hydrate hydrochloride wherein: the purity of the regenerated hydrazine hydrate hydrochloride is 99-99.8%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110986217.4A CN113666347A (en) | 2021-08-26 | 2021-08-26 | Regeneration treatment method of hydrazine hydrate hydrochloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110986217.4A CN113666347A (en) | 2021-08-26 | 2021-08-26 | Regeneration treatment method of hydrazine hydrate hydrochloride |
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| CN113666347A true CN113666347A (en) | 2021-11-19 |
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| CN202110986217.4A Pending CN113666347A (en) | 2021-08-26 | 2021-08-26 | Regeneration treatment method of hydrazine hydrate hydrochloride |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2921834A (en) * | 1957-01-31 | 1960-01-19 | Merck & Co Inc | Process for preparing metal selenides |
| CN101239919A (en) * | 2008-01-11 | 2008-08-13 | 南京工业大学 | Synthetic method of aromatic diamine monomer |
| CN103130687A (en) * | 2013-03-19 | 2013-06-05 | 湖南斯派克材料科技有限公司 | Preparation method of methyl hydrazinocarboxylate |
| CN106865512A (en) * | 2015-12-11 | 2017-06-20 | 天津市科密欧化学试剂有限公司 | A kind of preparation method of top pure grade hydrazine hydrochloride |
| CN112973406A (en) * | 2019-12-13 | 2021-06-18 | 湖北富博化工有限责任公司 | Resource utilization and treatment method for nitromethane waste gas |
-
2021
- 2021-08-26 CN CN202110986217.4A patent/CN113666347A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2921834A (en) * | 1957-01-31 | 1960-01-19 | Merck & Co Inc | Process for preparing metal selenides |
| CN101239919A (en) * | 2008-01-11 | 2008-08-13 | 南京工业大学 | Synthetic method of aromatic diamine monomer |
| CN103130687A (en) * | 2013-03-19 | 2013-06-05 | 湖南斯派克材料科技有限公司 | Preparation method of methyl hydrazinocarboxylate |
| CN106865512A (en) * | 2015-12-11 | 2017-06-20 | 天津市科密欧化学试剂有限公司 | A kind of preparation method of top pure grade hydrazine hydrochloride |
| CN112973406A (en) * | 2019-12-13 | 2021-06-18 | 湖北富博化工有限责任公司 | Resource utilization and treatment method for nitromethane waste gas |
Non-Patent Citations (1)
| Title |
|---|
| 李飞等: "《药物化学实验》", 31 May 2019, 华中科技大学出版社 * |
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