CN105293523A - Continuous preparation method for production raw material ammonia water of ketazine process hydrazine hydrate - Google Patents
Continuous preparation method for production raw material ammonia water of ketazine process hydrazine hydrate Download PDFInfo
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- CN105293523A CN105293523A CN201510811563.3A CN201510811563A CN105293523A CN 105293523 A CN105293523 A CN 105293523A CN 201510811563 A CN201510811563 A CN 201510811563A CN 105293523 A CN105293523 A CN 105293523A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The present invention belongs to the technical field of ketazine process hydrazine hydrate and aims to provide a continuous preparation method for a production raw material ammonia water of ketazine process hydrazine hydrate. Ammonia water which is stable in concentration is continuously prepared by virtue of liquid ammonia gasification, primary absorption and secondary absorption for being used by a ketazine process hydrazine hydrate production system. The preparation method provided by the present invention uses a densitometer for on-line detection; by combining the liquid ammonia gasification rate and the gasification pressure, the density of ammonia water is automatically controlled at 920-925 kg/m3, and the concentration of ammonia water is 25%, wherein the content of NH4OH content is 340-380 g/l, and the ammonia water content is precisely and stably controlled. Cold and heat exchange required by ammonia water preparation is completed by virtue of a principle that liquid ammonia gasification is endothermic while gas ammonia dissolution is exothermic without heat and cold quantities supplied from outside, so that the energy is saved and the consumption is reduced. By virtue of the secondary absorption, excessive soft water and a small quantity of ammonia are absorbed, so that ammonia is completely absorbed; tail gas emission reaches the standard, diluted ammonia water absorbing ammonia is taken as an absorbent in the primary absorption, and no waste water and liquid waste are produced in the overall production process.
Description
Technical field
The invention belongs to ketazine process hydrazine hydrate technical field, particularly relate to a kind of continuous production method of ketazine process hydrazine hydrate production raw material.
Background technology
Hydrazine hydrate, has another name called: hydrazine hydrate, and chemical formula is N
2h
4h
2o is strong reductant, is important industrial chemicals, is also the raw material of medicine, agricultural chemicals, dyestuff, whipping agent, photographic developer, antioxidant; Produce for feedwater deoxidation, high pure metal, organic compound synthesize and reduce, rare elements is separated, be also used as the manufacture of rocket fuel and explosive, along with the progress of technology, the development of society, the Application Areas of hydrazine hydrate is constantly being widened in recent years.The production method of hydrazine hydrate mainly contains Raschig process, Wyler's process, ketazine process, peroxide passivation and air oxidation process etc.The hydrazine hydrate production method that the present invention mentions is ketazine process, and it adopts acetone, clorox and ammonia react to produce intermediate-ketazine, and hydrazine hydrate is produced in ketazine hydrolysis.Its main chemical reactions equation is:
2NaOH+Cl
2→NaCl+NaClO+H
2O
NH
3+NaClO→NH
2Cl+NaOH
2CH
3COCH
3+NH
3+NH
2Cl+NaOH→(CH
3)
2C＝N-N＝(CH
3)
2C+3H
2O+NaCl
(CH
3)
2C＝N-N＝C(CH
3)
2+3H
2O→N
2H
4·H
2O+2CH
3COCH
3
From above formula, in ketazine process hydrazine hydrate production technique, require that certain density clorox, ammoniacal liquor, acetone enter reactor reaction according to certain ratio, to reduce the generation of side reaction, ensure synthesis yield.And must fluctuation of concentration in process of production as the ammoniacal liquor of one of main raw material, the yield of hydrazine hydrate can be affected; Ammonia concn is too low, and synthesis side reaction increases, and synthesis yield reduces greatly; Ammonia concn is too high, affect the synthetic tower service temperature of hydrazine hydrate, distillation tower service temperature, the operation index of each unit such as hydrolysis pressure, thus reduce the yield of hydrazine hydrate, affect the stationarity of production run simultaneously, also will cause that muriate in hydrazine hydrate product exceeds standard, TOC too high levels etc., and also there is no the prior art of head it off at present.
Therefore, for ensureing hydrazine hydrate building-up reactions yield, ensureing the smooth running of production system, reducing organic impurity in hydrazine hydrate product, how to control ammoniacal liquor continuous seepage, ensure that the precise and stable of ammonia concn becomes crucial.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of continuous production method of ketazine process hydrazine hydrate production raw material ammonia water, prepared ammonia concn is stable, precision is high to use the method to make, and continuous seepage, meet the needs of ketazine process hydrazine hydrate building-up reactions.
The technical solution adopted for the present invention to solve the technical problems is: a kind of continuous production method of ketazine process hydrazine hydrate production raw material ammonia water, comprises the following steps:
(1) liquid ammonia gasification: the liquefied ammonia from anhydrous ammonia tank enters liquid ammonia gasifier by reducing valve adjust flux, carries out liquid ammonia gasification, liquid ammonia gasification flow speed stability, liquid ammonia gasification amount≤2m
3/ h, vapor pressure≤0.4MPa, prepares ammonia;
(2) first order absorption: the ammonia after gasification passes into ammonia first grade absorption tower, the agent of ammonia first order absorption column overhead spray-absorption absorbs ammonia and makes ammoniacal liquor; Adopt densometer to detect ammoniacal liquor density, automatically controlling ammoniacal liquor density by regulating liquid ammonia gasification amount is 920-925kg/m
3, obtain the ammoniacal liquor that concentration is 25%; An obtained high temperature ammoniacal liquor part through liquid ammonia gasifier for liquid ammonia gasification heat, cooling are provided after be back to ammonia first grade absorption tower, another part sends into ammoniacal liquor basin for preparing hydrazine hydrate;
(3) secondary absorbs: ammonia first order absorption column overhead unabsorbed gases all enters ammonia two-level absorption tower, and ammonia two-level absorption tower tower top spray soft water absorbs gas as absorption agent; To the tower reactor liquid part after gas absorption by conduct backflow after interchanger cooling, a part delivers to the absorption agent of ammonia first order absorption top of tower as ammonia first grade absorption tower; Tower top tail gas is up to standard emptying by blow-down pipe, emission intensity speed≤4.9kg/h in tail gas.
Preferably, in described secondary absorption step tail gas, emission intensity speed is 1-3kg/h, ensures that ammonia secondary absorbs rear tail gas index more environmental protection.
The invention has the beneficial effects as follows: by adopting densometer on-line checkingi, the density that collaborative liquid ammonia gasification amount, vapor pressure control ammoniacal liquor is automatically 920-925kg/m
3, with NH
4oH content counts the ammoniacal liquor of 25% concentration of 340 ~ 380g/l, and ammoniacal liquor content obtains precise and stable control; Utilize that liquid ammonia gasification absorbs heat, the principle of gas ammonia exothermic dissolution completes cold and hot exchange required when ammoniacal liquor is produced, provide heat and cold without the need to the external world, energy-saving and cost-reducing; Absorbed by secondary, ensure that excessive soft water and a small amount of ammonia absorb, complete whole absorptions of ammonia, exhaust emissions is up to standard, absorbs the absorption agent of weak ammonia as first order absorption of ammonia, produces in whole production process without waste water, waste liquid.
Ammoniacal liquor the present invention prepared uses in ketazine process hydrazine hydrate production process, make each unit operation indexs such as the synthetic tower service temperature of hydrazine hydrate, distillation tower service temperature, hydrolysis pressure steady, hydrazine hydrate synthesis side reaction minimizing, hydrazine hydrate yield improve.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further described.
Concrete operation step of the present invention: as shown in Figure 1, open the soft water inlet valve of ammonia two-level absorption tower, when the liquid level of ammonia two-level absorption tower reaches 80%, open ammonia two-level absorption tower discharging pump, the soft water of ammonia two-level absorption tower is proceeded to ammonia first grade absorption tower, when ammonia first grade absorption tower liquid level reaches 30%, open anhydrous ammonia tank fluid ammonia valve door, to be entered after vaporizer and ammonia first grade absorption tower ammoniacal liquor out carry out heat exchange by reducing valve adjust flux from the liquefied ammonia of anhydrous ammonia tank and gasify, liquid ammonia gasification amount≤2m
3/ h, vapor pressure≤0.4MPa, ensure liquid ammonia gasification flow speed stability, prepare ammonia; Ammonia after gasification enters ammonia first grade absorption tower and is absorbed by the weak ammonia from ammonia two-level absorption tower, make ammoniacal liquor, if liquid ammonia gasification amount, vapor pressure exceed standard, ammonia speed is too fast, and ammonia absorption effect and specific absorption reduce, and yield reduces, and ammonia speed is too fast, if now soft water flux regulates not in time, ammonia concn will be caused to fluctuate, affect the stability of ammonia concn; Adopt densometer to detect ammoniacal liquor density, automatically controlling ammoniacal liquor density is 920-925kg/m
3, obtain the ammoniacal liquor that concentration is 25%; An obtained high temperature ammoniacal liquor part sends into ammoniacal liquor basin for preparing hydrazine hydrate, another part as circulation fluid through liquid ammonia gasifier for liquid ammonia gasification provide heat, cooling after be back to ammonia first grade absorption tower, at circulation fluid through liquid ammonia gasifier, enter to arrange between ammonia first grade absorption tower 5 DEG C of water coolings coolings, ensure ammonia first grade absorption tower temperature≤25 DEG C, if ammonia first grade absorption tower temperature is too high, ammonia concn can be caused not reach 25%, ammonia two-level absorption tower tower top tail gas ammonia content overproof.
Ammonia first order absorption column overhead unabsorbed gases all enters ammonia two-level absorption tower, and ammonia two-level absorption tower tower top spray soft water absorbs gas as absorption agent; To the tower reactor liquid part after gas absorption by conduct backflow after interchanger cooling, a part delivers to the absorption agent of ammonia first order absorption top of tower as ammonia first grade absorption tower; Tower top tail gas is up to standard emptying by blow-down pipe, and emission intensity speed≤4.9kg/h in tail gas, further, in tail gas, emission intensity speed is 1-3kg/h.
Embodiment 1:
(1) liquefied ammonia from anhydrous ammonia tank enters liquid ammonia gasifier by reducing valve adjust flux, carries out liquid ammonia gasification, liquid ammonia gasification flow speed stability, liquid ammonia gasification amount 2m
3/ h, vapor pressure 0.4MPa, prepares ammonia;
(2) ammonia after gasification passes into ammonia first grade absorption tower, and the agent of ammonia first order absorption column overhead spray-absorption absorbs ammonia and makes ammoniacal liquor; Adopt densometer to detect ammoniacal liquor density, automatically controlling ammoniacal liquor density is 925kg/m
3, obtain the ammoniacal liquor that concentration is 25%; An obtained high temperature ammoniacal liquor part through liquid ammonia gasifier for liquid ammonia gasification heat, cooling are provided after be back to ammonia first grade absorption tower, another part sends into ammoniacal liquor basin for preparing hydrazine hydrate;
(3) ammonia first order absorption column overhead unabsorbed gases all enters ammonia two-level absorption tower, and ammonia two-level absorption tower tower top spray soft water absorbs gas as absorption agent; To the tower reactor liquid part after gas absorption by conduct backflow after interchanger cooling, a part delivers to the absorption agent of ammonia first order absorption top of tower as ammonia first grade absorption tower; Tower top tail gas is up to standard emptying by blow-down pipe, emission intensity speed≤4.9kg/h in tail gas.
Embodiment 2:
(1) liquefied ammonia from anhydrous ammonia tank enters liquid ammonia gasifier by reducing valve adjust flux, carries out liquid ammonia gasification, liquid ammonia gasification flow speed stability, liquid ammonia gasification amount 1m
3/ h, vapor pressure 0.2MPa, prepares ammonia;
(2) ammonia after gasification passes into ammonia first grade absorption tower, and the agent of ammonia first order absorption column overhead spray-absorption absorbs ammonia and makes ammoniacal liquor; Adopt densometer to detect ammoniacal liquor density, automatically controlling ammoniacal liquor density is 920kg/m
3, obtain the ammoniacal liquor that concentration is 25%; An obtained high temperature ammoniacal liquor part through liquid ammonia gasifier for liquid ammonia gasification heat, cooling are provided after be back to ammonia first grade absorption tower, another part sends into ammoniacal liquor basin for preparing hydrazine hydrate;
(3) ammonia first order absorption column overhead unabsorbed gases all enters ammonia two-level absorption tower, and ammonia two-level absorption tower tower top spray soft water absorbs gas as absorption agent; To the tower reactor liquid part after gas absorption by conduct backflow after interchanger cooling, a part delivers to the absorption agent of ammonia first order absorption top of tower as ammonia first grade absorption tower; Tower top tail gas is up to standard emptying by blow-down pipe, emission intensity speed≤1kg/h in tail gas.
Embodiment 3:
(1) liquefied ammonia from anhydrous ammonia tank enters liquid ammonia gasifier by reducing valve adjust flux, carries out liquid ammonia gasification, liquid ammonia gasification flow speed stability, liquid ammonia gasification amount 1.5m
3/ h, vapor pressure 0.3MPa, prepares ammonia;
(2) ammonia after gasification passes into ammonia first grade absorption tower, and the agent of ammonia first order absorption column overhead spray-absorption absorbs ammonia and makes ammoniacal liquor; Adopt densometer to detect ammoniacal liquor density, automatically controlling ammoniacal liquor density is 922kg/m
3, obtain the ammoniacal liquor that concentration is 25%; An obtained high temperature ammoniacal liquor part through liquid ammonia gasifier for liquid ammonia gasification heat, cooling are provided after be back to ammonia first grade absorption tower, another part sends into ammoniacal liquor basin for preparing hydrazine hydrate;
(3) ammonia first order absorption column overhead unabsorbed gases all enters ammonia two-level absorption tower, and ammonia two-level absorption tower tower top spray soft water absorbs gas as absorption agent; To the tower reactor liquid part after gas absorption by conduct backflow after interchanger cooling, a part delivers to the absorption agent of ammonia first order absorption top of tower as ammonia first grade absorption tower; Tower top tail gas is up to standard emptying by blow-down pipe, emission intensity speed 1-3kg/h in tail gas.
Claims (2)
1. a continuous production method for ketazine process hydrazine hydrate production raw material ammonia water, is characterized in that comprising the following steps:
(1) liquid ammonia gasification: the liquefied ammonia from anhydrous ammonia tank enters liquid ammonia gasifier by reducing valve adjust flux, carries out liquid ammonia gasification, liquid ammonia gasification flow speed stability, liquid ammonia gasification amount≤2m
3/ h, vapor pressure≤0.4MPa, prepares ammonia;
(2) first order absorption: the ammonia after gasification passes into ammonia first grade absorption tower, the agent of ammonia first order absorption column overhead spray-absorption absorbs ammonia and makes ammoniacal liquor; Adopt densometer to detect ammoniacal liquor density, automatically controlling ammoniacal liquor density by regulating liquid ammonia gasification amount is 920-925kg/m
3, obtain the ammoniacal liquor that concentration is 25%; An obtained high temperature ammoniacal liquor part through liquid ammonia gasifier for liquid ammonia gasification heat, cooling are provided after be back to ammonia first grade absorption tower, another part sends into ammoniacal liquor basin for preparing hydrazine hydrate;
(3) secondary absorbs: ammonia first order absorption column overhead unabsorbed gases all enters ammonia two-level absorption tower, and ammonia two-level absorption tower tower top spray soft water absorbs gas as absorption agent; To the tower reactor liquid part after gas absorption by conduct backflow after interchanger cooling, a part delivers to the absorption agent of ammonia first order absorption top of tower as ammonia first grade absorption tower; Tower top tail gas is up to standard emptying by blow-down pipe, emission intensity speed≤4.9kg/h in tail gas.
2. the continuous production method of a kind of ketazine process hydrazine hydrate production raw material ammonia water according to claim 1, is characterized in that: in described secondary absorption step tail gas, emission intensity speed is 1-3kg/h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510811563.3A CN105293523A (en) | 2015-11-19 | 2015-11-19 | Continuous preparation method for production raw material ammonia water of ketazine process hydrazine hydrate |
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|---|---|---|---|
| CN201510811563.3A CN105293523A (en) | 2015-11-19 | 2015-11-19 | Continuous preparation method for production raw material ammonia water of ketazine process hydrazine hydrate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107697931A (en) * | 2017-10-31 | 2018-02-16 | 四川锌鸿科技有限公司 | A kind of multistage reverse circulation inhales ammonia process |
| CN111992172A (en) * | 2020-08-03 | 2020-11-27 | 界首市南都华宇电源有限公司 | Collecting device and collecting method for ammonia water preparation |
| CN112299444A (en) * | 2020-10-14 | 2021-02-02 | 营口正源电力配套设备有限公司 | Mobile liquid ammonia recovery ammonia tank replacement equipment and method |
-
2015
- 2015-11-19 CN CN201510811563.3A patent/CN105293523A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107697931A (en) * | 2017-10-31 | 2018-02-16 | 四川锌鸿科技有限公司 | A kind of multistage reverse circulation inhales ammonia process |
| CN107697931B (en) * | 2017-10-31 | 2020-06-30 | 四川锌鸿科技有限公司 | Multistage reverse circulation ammonia absorption process |
| CN111992172A (en) * | 2020-08-03 | 2020-11-27 | 界首市南都华宇电源有限公司 | Collecting device and collecting method for ammonia water preparation |
| CN111992172B (en) * | 2020-08-03 | 2022-04-19 | 界首市南都华宇电源有限公司 | Collecting device and collecting method for ammonia water preparation |
| CN112299444A (en) * | 2020-10-14 | 2021-02-02 | 营口正源电力配套设备有限公司 | Mobile liquid ammonia recovery ammonia tank replacement equipment and method |
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Application publication date: 20160203 |
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