CN109319752A - A kind of preparation method of hydrazine sulfate - Google Patents
A kind of preparation method of hydrazine sulfate Download PDFInfo
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- CN109319752A CN109319752A CN201811401811.7A CN201811401811A CN109319752A CN 109319752 A CN109319752 A CN 109319752A CN 201811401811 A CN201811401811 A CN 201811401811A CN 109319752 A CN109319752 A CN 109319752A
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- hydrazine
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- hydrazine sulfate
- sulfuric acid
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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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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of preparation methods of hydrazine sulfate, are related to chemosynthesis technical field, the preparation method successively include (1) in the presence of a catalyst, benzophenone is placed in reactor, uniform stirring, while stabilization is continually fed into ammonia and air, obtains benzophenone connection nitrogen；(2) surfactant and water are added under strongly acidic conditions, reaction is hydrolyzed, alkali neutralization is added to obtain hydrazine hydrate；(3) the obtained hydrazine sulfate of the concentrated sulfuric acid is added into hydrazine hydrate and obtains product hydrazine sulfate through crystallisation by cooling, suction filtration, washing, drying.Operation of the present invention is simple, and pollution is small, and product purity is high, reduces the generation of objectionable impurities, solves pollution problem, greatly reduces the consumption of the cost and resource of production, and product quality reaches excellent pure grade standard, is suitble to the needs of scale industrial production.
Description
Technical field
The present invention relates to chemosynthesis technical fields, and in particular to a kind of preparation method of hydrazine sulfate.
Background technique
Hydrazine sulfate (N2H4·H2SO4) also known as sulphuric acid leaching, toxic, sterling is colourless squamous crystal or rhomboidal crystal,
It is tasteless, it is soluble in hot water, less to be dissolved in cold water, stable in the air, vulnerable to alkali or oxidant effect, moisture absorption is weak, has strong
Strong reduction.
Hydrazine sulfate is widely used, pharmaceutically for manufacturing isoniazid, anhydrous hydrazine, Dipasic and nitrofurazone etc.；On dyestuff
For manufacturing azodicarbonamide, azodiisobutyronitrile etc.；Agriculturally it is used for insecticide, bactericidal agent, malic acid hydrazine, plant growth
Inhibitor；The foaming agent that can be used as plastics and rubber is also used for analytical reagent, Blood laboratory and by separating polonium etc. in tellurium.
The preparation of hydrazine sulfate, industrially commonly use urea method, by urea, sodium hypochlorite, liquid alkaline, in the presence of potassium permanganate into
Row reaction, is distilled, then carries out neutralization reaction with sulfuric acid, and product is through crystallisation by cooling, filtering, dry obtained hydrazine sulfate finished product；
Or in the presence of animal glue, with sodium hypochlorite make ammonia occur partial oxidation, and in sulfuric acid and generate hydrazine sulfate.In prior art
The purity of the hydrazine sulfate of acquisition is often not satisfactory.
Summary of the invention
Simple, high income and energy-saving and environment-friendly hydrazine sulfate system that the technical problem to be solved in the present invention is to provide a kind of methods
Preparation Method.
The present invention provides a kind of preparation method of hydrazine sulfate, comprising the following steps:
(1) in the presence of a catalyst, benzophenone is placed in reactor, uniform stirring, while stabilization is continually fed into
Ammonia and air obtain benzophenone connection nitrogen；
(2) surfactant and water are added under strongly acidic conditions, reaction is hydrolyzed, alkali neutralization is added to obtain hydrazine hydrate；
(3) the obtained hydrazine sulfate of the concentrated sulfuric acid is added into hydrazine hydrate and obtains product sulphur through crystallisation by cooling, suction filtration, washing, drying
Sour hydrazine.
Preferably, it is zinc system and copper, two kinds of nickel system that catalyst, which is catalyst, in the step (1), they and hexichol
The mass ratio of ketone is respectively 1:120-280 and 1:30-60.
Preferably, at 180-200 DEG C, mixing speed is 500-1000 for whipping temp control in the step (1)
Rev/min.
Preferably, the average ventilation of ammonia and air proportion is 1:3 in the step (2).
Preferably, surfactant is stearic acid or dodecyl benzene sulfonic acid in the step (2).
Preferably, hydrolysising reacting temperature control is at 75-95 DEG C in the step (2).
Preferably, specifically comprising the following steps: in the step (2)
(31) pure water is added in a kettle, is slowly added into 98% sulfuric acid under stirring, cooling, adds, add at 70-80 DEG C
Enter 80% hydrazine hydrate, filter while hot, wherein the mass ratio of pure water, 98% sulfuric acid and 80% hydrazine hydrate is 10:10:4；
(32) filtrate adjusts pH=4-5 using sulfuric acid or hydrazine hydrate, stirs 20-60 minutes, crystallisation by cooling unchanged to pH
To 25 DEG C, centrifuge separation crystallization is washed using dehydrated alcohol, is air-dried at room temperature to obtain finished product.
The beneficial effects of the present invention are: operation of the present invention is simple the present invention provides a kind of preparation method of hydrazine sulfate, it is dirty
Contaminate small, product purity is high, reduces the generation of objectionable impurities, solves pollution problem, greatly reduces the cost and money of production
The consumption in source, product quality reach excellent pure grade standard, are suitble to the needs of scale industrial production.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
The present invention provides a kind of preparation method of hydrazine sulfate, comprising the following steps:
(1) in the presence of a catalyst, benzophenone is placed in reactor, uniform stirring, while stabilization is continually fed into
Ammonia and air obtain benzophenone connection nitrogen；
(2) surfactant and water are added under strongly acidic conditions, reaction is hydrolyzed, alkali neutralization is added to obtain hydrazine hydrate；
(3) the obtained hydrazine sulfate of the concentrated sulfuric acid is added into hydrazine hydrate and obtains product sulphur through crystallisation by cooling, suction filtration, washing, drying
Sour hydrazine.
It is zinc system and copper, two kinds of nickel system, the mass ratio of they and benzophenone that catalyst, which is catalyst, in the step (1)
Respectively 1:120-280 and 1:30-60.
At 180-200 DEG C, mixing speed is 500-1000 revs/min for whipping temp control in the step (1).
The average ventilation of ammonia and air proportion is 1:3 in the step (2).
Surfactant is stearic acid or dodecyl benzene sulfonic acid in the step (2).
Hydrolysising reacting temperature control is at 75-95 DEG C in the step (2).
Specifically comprise the following steps: in the step (2)
(31) pure water is added in a kettle, is slowly added into 98% sulfuric acid under stirring, cooling, adds, add at 70-80 DEG C
Enter 80% hydrazine hydrate, filter while hot, wherein the mass ratio of pure water, 98% sulfuric acid and 80% hydrazine hydrate is 10:10:4；
(32) filtrate adjusts pH=4-5 using sulfuric acid or hydrazine hydrate, stirs 20-60 minutes, crystallisation by cooling unchanged to pH
To 25 DEG C, centrifuge separation crystallization is washed using dehydrated alcohol, is air-dried at room temperature to obtain finished product.Embodiment 1
Embodiment 1
The present invention provides a kind of preparation method of hydrazine sulfate, comprising the following steps:
(1) at catalyst (zinc system and copper, nickel system dosage 8g and 30g)) in the presence of, 1000g benzophenone is placed in instead
It answers in device, uniform stirring is carried out with 500-1000 revs/min of rate at 180-200 DEG C, while stabilization is continually fed into ammonia
And air, wherein the average ventilation of ammonia and air proportion is 1:3, is reacted 4-10 hours, and the hexichol that content is 60% is obtained
Ketone joins nitrogen；
(2) dodecyl benzene sulfonic acid 10g is added, reaction is hydrolyzed, instead in hydrochloric acid 100g, water 1000mL at 75-95 DEG C
It answers 4-10 hours, alkali neutralization is added to obtain hydrazine hydrate；
(3) the obtained hydrazine sulfate of the concentrated sulfuric acid is added into hydrazine hydrate and obtains product sulphur through crystallisation by cooling, suction filtration, washing, drying
Sour hydrazine.
Specifically comprise the following steps: in the step (2)
(31) pure water is added in a kettle, is slowly added into 98% sulfuric acid under stirring, cooling, adds, add at 70-80 DEG C
Enter 80% hydrazine hydrate, filter while hot, wherein the mass ratio of pure water, 98% sulfuric acid and 80% hydrazine hydrate is 10:10:4；
(32) filtrate adjusts pH=4-5 using sulfuric acid or hydrazine hydrate, stirs 20-60 minutes, crystallisation by cooling unchanged to pH
To 25 DEG C, centrifuge separation crystallization is washed using dehydrated alcohol, is air-dried at room temperature to obtain finished product.
Embodiment 2
The present invention provides a kind of preparation method of hydrazine sulfate, comprising the following steps:
(1) at catalyst (zinc system and copper, nickel system dosage 8g and 30g)) in the presence of, 1000g benzophenone is placed in instead
It answers in device, uniform stirring is carried out with 500-1000 revs/min of rate at 180-200 DEG C, while stabilization is continually fed into ammonia
And air, wherein the average ventilation of ammonia and air proportion is 1:3, is reacted 4-10 hours, and the hexichol that content is 60% is obtained
Ketone joins nitrogen；
(2) stearic acid 10g, hydrochloric acid 100g, water 1000mL is added, reaction is hydrolyzed at 75-95 DEG C, reaction 4-10 is small
When, add alkali neutralization to obtain hydrazine hydrate；
(3) the obtained hydrazine sulfate of the concentrated sulfuric acid is added into hydrazine hydrate and obtains product sulphur through crystallisation by cooling, suction filtration, washing, drying
Sour hydrazine.
Specifically comprise the following steps: in the step (2)
(31) pure water is added in a kettle, is slowly added into 98% sulfuric acid under stirring, cooling, adds, add at 70-80 DEG C
Enter 80% hydrazine hydrate, filter while hot, wherein the mass ratio of pure water, 98% sulfuric acid and 80% hydrazine hydrate is 10:10:4；
(32) filtrate adjusts pH=4-5 using sulfuric acid or hydrazine hydrate, stirs 20-60 minutes, crystallisation by cooling unchanged to pH
To 25 DEG C, centrifuge separation crystallization is washed using dehydrated alcohol, is air-dried at room temperature to obtain finished product.
Embodiment 3
The present invention provides a kind of preparation method of hydrazine sulfate, comprising the following steps:
(1) at catalyst (zinc system and copper, nickel system dosage 8g and 30g)) in the presence of, 1200g benzophenone is placed in instead
It answers in device, uniform stirring is carried out with 500-1000 revs/min of rate at 180-200 DEG C, while stabilization is continually fed into ammonia
And air, wherein the average ventilation of ammonia and air proportion is 1:3, is reacted 4-10 hours, and the hexichol that content is 60% is obtained
Ketone joins nitrogen；
(2) dodecyl benzene sulfonic acid 10g is added, reaction is hydrolyzed, instead in hydrochloric acid 120g, water 1200mL at 75-95 DEG C
It answers 4-10 hours, alkali neutralization is added to obtain hydrazine hydrate；
(3) the obtained hydrazine sulfate of the concentrated sulfuric acid is added into hydrazine hydrate and obtains product sulphur through crystallisation by cooling, suction filtration, washing, drying
Sour hydrazine.
Specifically comprise the following steps: in the step (2)
(31) pure water is added in a kettle, is slowly added into 98% sulfuric acid under stirring, cooling, adds, add at 70-80 DEG C
Enter 80% hydrazine hydrate, filter while hot, wherein the mass ratio of pure water, 98% sulfuric acid and 80% hydrazine hydrate is 10:10:4；
(32) filtrate adjusts pH=4-5 using sulfuric acid or hydrazine hydrate, stirs 20-60 minutes, crystallisation by cooling unchanged to pH
To 25 DEG C, centrifuge separation crystallization is washed using dehydrated alcohol, is air-dried at room temperature to obtain finished product.
It is obvious to a person skilled in the art that the present invention is not limited to the details of the exemplary embodiment, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit require rather than it is described illustrate to limit, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (7)
1. a kind of preparation method of hydrazine sulfate, which comprises the following steps:
(1) in the presence of a catalyst, benzophenone is placed in reactor, uniform stirring, while stabilization is continually fed into ammonia
And air, obtain benzophenone connection nitrogen；
(2) surfactant and water are added under strongly acidic conditions, reaction is hydrolyzed, alkali neutralization is added to obtain hydrazine hydrate；
(3) the obtained hydrazine sulfate of the concentrated sulfuric acid is added into hydrazine hydrate and obtains product hydrazine sulfate through crystallisation by cooling, suction filtration, washing, drying.
2. the preparation method of hydrazine sulfate as described in claim 1, which is characterized in that catalyst is catalysis in the step (1)
Agent is zinc system and copper, two kinds of nickel system, and the mass ratio of they and benzophenone is respectively 1:120-280 and 1:30-60.
3. the preparation method of hydrazine sulfate as described in claim 1, which is characterized in that whipping temp controls in the step (1)
At 180-200 DEG C, mixing speed is 500-1000 revs/min.
4. the preparation method of hydrazine sulfate as described in claim 1, which is characterized in that ammonia and air in the step (2)
Average ventilation proportion is 1:3.
5. the preparation method of hydrazine sulfate as described in claim 1, which is characterized in that surfactant is in the step (2)
Stearic acid or dodecyl benzene sulfonic acid.
6. the preparation method of hydrazine sulfate as described in claim 1, which is characterized in that hydrolysising reacting temperature in the step (2)
Control is at 75-95 DEG C.
7. the preparation method of hydrazine sulfate as described in claim 1, which is characterized in that specifically included in the step (2) as follows
Step:
(31) pure water is added in a kettle, is slowly added into 98% sulfuric acid under stirring, cooling, adds, be added at 70-80 DEG C
80% hydrazine hydrate, is filtered while hot, wherein the mass ratio of pure water, 98% sulfuric acid and 80% hydrazine hydrate is 10:10:4；
(32) filtrate adjusts pH=4-5 using sulfuric acid or hydrazine hydrate, stirs 20-60 minutes, crystallisation by cooling to 25 unchanged to pH
DEG C, centrifuge separation crystallization is washed using dehydrated alcohol, is air-dried at room temperature to obtain finished product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811401811.7A CN109319752A (en) | 2018-11-22 | 2018-11-22 | A kind of preparation method of hydrazine sulfate |
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| CN201811401811.7A CN109319752A (en) | 2018-11-22 | 2018-11-22 | A kind of preparation method of hydrazine sulfate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112047312A (en) * | 2020-09-30 | 2020-12-08 | 重庆腾泽化学有限公司 | Preparation method of hydrazine sulfate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102328920A (en) * | 2011-07-11 | 2012-01-25 | 山东曹县斯递尔化工科技有限公司 | Process for preparing hydrazine hydrate by air oxidation method |
| CN106865511A (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 sulfate |
| CN107381523A (en) * | 2017-09-07 | 2017-11-24 | 盐城顺恒化工有限公司 | A kind of preparation method of hydrazine sulfate |
-
2018
- 2018-11-22 CN CN201811401811.7A patent/CN109319752A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102328920A (en) * | 2011-07-11 | 2012-01-25 | 山东曹县斯递尔化工科技有限公司 | Process for preparing hydrazine hydrate by air oxidation method |
| CN106865511A (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 sulfate |
| CN107381523A (en) * | 2017-09-07 | 2017-11-24 | 盐城顺恒化工有限公司 | A kind of preparation method of hydrazine sulfate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112047312A (en) * | 2020-09-30 | 2020-12-08 | 重庆腾泽化学有限公司 | Preparation method of hydrazine sulfate |
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