CN108191697A - A kind of method of synthetic isopropyl hydrazine - Google Patents
A kind of method of synthetic isopropyl hydrazine Download PDFInfo
- Publication number
- CN108191697A CN108191697A CN201711285574.8A CN201711285574A CN108191697A CN 108191697 A CN108191697 A CN 108191697A CN 201711285574 A CN201711285574 A CN 201711285574A CN 108191697 A CN108191697 A CN 108191697A
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- CN
- China
- Prior art keywords
- hydrazine
- reaction
- isopropyl
- isopropyl hydrazine
- hydrazine hydrate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C241/00—Preparation of compounds containing chains of nitrogen atoms singly-bound to each other, e.g. hydrazines, triazanes
- C07C241/02—Preparation of hydrazines
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of methods of synthetic isopropyl hydrazine; this method is that under catalyst action and isopropanol and hydrazine hydrate be alkylated reaction at a certain temperature under the protection of inert gas; generate isopropyl hydrazine; it is after reaction that the organic phase containing isopropyl hydrazine is separated from the water; organic phase rectifying is obtained into isopropyl hydrazine finished product again, which is calgon.Compared with prior art, the present invention is using isopropanol and hydrazine hydrate as raw material, and one-step synthesis method isopropyl hydrazine, reaction step is few, and post processing is simple, and reactivity hazard is small, and high income, production cost is low, and waste discharge is few, is a kind of environmental type production technology.
Description
Technical field
The invention belongs to chemosynthesis technical fields, and in particular to a kind of method of synthetic isopropyl hydrazine.
Background technology
Isopropyl hydrazine is a kind of widely used medicine intermediate and organic synthesis intermediate, has excellent bioactivity
And chemism.Isopropyl hydrazine is also a kind of common anti-tubercular drug and antidepressant and efficient pesticides meter Le Er in itself
Starting material.
According to the literature, isopropyl hydrazine can be used a large amount of by bromo propane and a large amount of excessive hydration hydrazine reactions, post processing
Ether sequential extractions produce.But due to product, solubility is big in hydrazine hydrate, and extraction difficulty is big, and finishing time is long, receives
Rate is low, is unsuitable for producing greatly.And the method that another kind produces isopropyl hydrazine is：Using ethyl carbazate as starting material, first
Generation acetone hydrazone is reacted with acetone, then by acetone hydrazone catalytic hydrogenation, then the protecting group of hydride is removed, finally uses ethyl acetate
Isopropyl hydrazine is made in extractive distillation.The synthetic method craft route is longer, and hydrogenation process is dangerous big, and process conditions requirement is high,
Complex procedures, for yield less than 80%, production cost is high；In addition, due to containing a large amount of organic impurities, recycling in by-product sodium carbonate
Using and environmental protection treatment cost it is higher, easily cause environmental pollution.
Invention content
In order to overcome disadvantages mentioned above of the existing technology, the present invention provides a kind of simple for process, safe operation, reactions
The isopropyl hydrazine new synthetic method that high income, production cost are low, by-product is few, environmentally protective.
The technical solution adopted by the present invention is：Under the protection of inert gas, isopropanol and hydrazine hydrate are made in catalyst
With lower and be alkylated reaction at a certain temperature, isopropyl hydrazine is generated, keeps isopropanol excessive in reaction process, reaction knot
It is after beam that the organic phase containing isopropyl hydrazine is separated from the water, then organic phase rectifying is obtained into isopropyl hydrazine finished product.From organic phase
The isopropanol of the distillation recovery and hydrazine hydrate recycled from water phase, isopropanol and catalyst can continue on for synthetic isopropyl hydrazine.
Abovementioned alkylization reaction used catalyst is calgon.
The specific process step of the technical solution is as follows：Under the protection of inert gas, by isopropanol, hydrazine hydrate and six partially
Sodium phosphate is put into reaction kettle, open stirring, closed reactor when being heated to 80 DEG C, be continuously heating to 110~130 DEG C into
Row alkylated reaction, reaction time are 5~7 hours, and temperature of reaction kettle is down to 80 DEG C after reaction, then will be in reaction kettle
Layer organic phase, which is transferred in rectifying still, carries out rectifying, collects the fraction that temperature is 106~108 DEG C, obtains isopropyl hydrazine finished product.It is above-mentioned
In step, the molar ratio of isopropanol and hydrazine hydrate is 1.5~2: 1, the addition of calgon for hydrazine hydrate quality 10%~
20%, the content of hydrazine hydrate used is more than 95%.Its reaction equation is as follows：
(CH3)2CHOH + NH2NH2·H2O → (CH3)2CHNHNH2 + 2H2O
Compared with prior art, the beneficial effects of the invention are as follows：The present invention is using isopropanol and hydrazine hydrate as raw material, one-step synthesis method
Isopropyl hydrazine, reaction step is few, and post processing is simple, and reactivity hazard is small, high income（With hydrazine hydrate rate of collecting 90% with
On）, production cost is low, and waste discharge is few, is a kind of environmental type production technology.
Specific embodiment
Percentage composition as described below is mass fraction, and all steps are completed under inert gas shielding.
Embodiment 1
Isopropanol 450g, the hydrazine hydrate 260.4g and calgon 38g that content is 96% are put into reaction kettle, open stirring,
Closed reactor when being heated to 80 DEG C, is continuously heating to 120 DEG C, and insulation reaction 7 hours will react kettle temperature after reaction
Degree is down to 80 DEG C, then upper organic phase in reaction kettle is transferred in rectifying still and carries out rectifying, and it is 106~108 DEG C to collect temperature
Fraction obtains isopropyl hydrazine 345.7g.
Embodiment 2
Isopropanol 525g, the hydrazine hydrate 255.1g and calgon 25g that content is 98% are put into reaction kettle, open stirring,
Closed reactor when being heated to 80 DEG C, is continuously heating to 110 DEG C, and insulation reaction 6 hours will react kettle temperature after reaction
Degree is down to 80 DEG C, then upper organic phase in reaction kettle is transferred in rectifying still and carries out rectifying, and it is 106~108 DEG C to collect temperature
Fraction obtains isopropyl hydrazine 339.3g.
Embodiment 3
Isopropanol 600g, the hydrazine hydrate 252.5g and calgon 50g that content is 99% are put into reaction kettle, open stirring,
Closed reactor when being heated to 80 DEG C, is continuously heating to 130 DEG C, and insulation reaction 5 hours will react kettle temperature after reaction
Degree is down to 80 DEG C, then upper organic phase in reaction kettle is transferred in rectifying still and carries out rectifying, and it is 106~108 DEG C to collect temperature
Fraction obtains isopropyl hydrazine 351.5g.
Claims (1)
- A kind of 1. method of synthetic isopropyl hydrazine, it is characterised in that：Following steps are carried out under inert gas shielding：By isopropyl Alcohol, hydrazine hydrate and calgon are put into reaction kettle, open stirring, closed reactor when being heated to 80 DEG C, after of continuing rising Temperature is alkylated reaction to 110~130 DEG C, and the reaction time is 5~7 hours, and temperature of reaction kettle is down to 80 after reaction DEG C, then upper organic phase in reaction kettle is transferred in rectifying still and carries out rectifying, the fraction that temperature is 106~108 DEG C is collected, is obtained Isopropyl hydrazine finished product；In above-mentioned steps, the molar ratio of isopropanol and hydrazine hydrate is 1.5~2: 1, and the addition of calgon is The 10%~20% of hydrazine hydrate quality, the content of hydrazine hydrate used is more than 95%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711285574.8A CN108191697A (en) | 2017-12-07 | 2017-12-07 | A kind of method of synthetic isopropyl hydrazine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711285574.8A CN108191697A (en) | 2017-12-07 | 2017-12-07 | A kind of method of synthetic isopropyl hydrazine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108191697A true CN108191697A (en) | 2018-06-22 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711285574.8A Withdrawn CN108191697A (en) | 2017-12-07 | 2017-12-07 | A kind of method of synthetic isopropyl hydrazine |
Country Status (1)
| Country | Link |
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| CN (1) | CN108191697A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110627677A (en) * | 2019-09-19 | 2019-12-31 | 宜宾海丰和锐有限公司 | Separation and purification method of ketazine hydrazine hydrate byproduct isopropyl hydrazine |
-
2017
- 2017-12-07 CN CN201711285574.8A patent/CN108191697A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110627677A (en) * | 2019-09-19 | 2019-12-31 | 宜宾海丰和锐有限公司 | Separation and purification method of ketazine hydrazine hydrate byproduct isopropyl hydrazine |
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| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180622 |
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| WW01 | Invention patent application withdrawn after publication |