CN101712479A - Method for preparing sodium sulfite by utilizing total alkali in hydrazine hydrate - Google Patents

Method for preparing sodium sulfite by utilizing total alkali in hydrazine hydrate Download PDF

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CN101712479A
CN101712479A CN200910112210A CN200910112210A CN101712479A CN 101712479 A CN101712479 A CN 101712479A CN 200910112210 A CN200910112210 A CN 200910112210A CN 200910112210 A CN200910112210 A CN 200910112210A CN 101712479 A CN101712479 A CN 101712479A
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hydrazine hydrate
total alkali
utilizing total
produce
sodium sulfite
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CN101712479B (en
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黄绳炀
夏霆
陈世豪
邹福旺
张明坤
黄兵
陈鼎东
吴元金
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FUJIAN PROVINCE SHAOWU CITY RONGFENG CHEMICAL Co Ltd
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FUJIAN PROVINCE SHAOWU CITY RONGFENG CHEMICAL Co Ltd
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Abstract

The invention provides a method for preparing sodium sulfite by utilizing total alkali in hydrazine hydrate, belonging to the technical field of hydrazine hydrate. The method comprises the following steps of: adding one or several kinds of raw materials of SO2 gas, NaHSO3 or Na2S2O5 to a hydrazine hydrate solution until the pH value of the hydrazine hydrate solution is 6.0-7.0, cooling and crystallizing the hydrazine hydrate solution, and then carrying out solid-liquid separation to obtain Na2SO3.7H2O. The invention overcomes the defects of high energy consumption, high cost and the like when the traditional process is used for extracting hydrazine hydrate byproducts and provides the method for preparing the sodium sulfite by utilizing total alkali in the hydrazine hydrate; the whole production process does not have three-waste discharge and has low energy consumption, and the produced products have high additional values.

Description

Utilize the total alkali in the hydrazine hydrate to produce S-WAT
Technical field
The invention belongs to the hydrazine hydrate technical field, more specifically relate to a kind of method of utilizing total alkali in the hydrazine hydrate to produce S-WAT.
Background technology
Hydrazine hydrate is a kind of important fine chemical product, mainly contains 35%, 40%, 80% and 100% plurality of specifications, and its purposes is very extensive, is mainly used in the production whipping agent, as AC whipping agent, OBSH whipping agent; Also be used for pharmaceutical industry, as be used for synthetic vazadrine, the XiLin of muttering of barking; Also can be used for producing sterilant, sterilant, as paclobutrazol, leaf grass agricultural chemicals such as loose.The strong reducing property of hydrazine hydrate in addition can be used as oxygen scavenger, rocket propellant of boiler feed water etc.Hydrazine hydrate traditional processing technology (abbreviation Wyler's process) divides two steps:
(1) clorox preparation:, generate clorox by caustic soda and chlorine reaction below 35 ℃
2NaOH+Cl 2→NaClO+NaCl+H 2O ---------------(1)
(2) hydrazine is synthetic: adopt urea and sodium hypochlorite reaction to generate hydrazine hydrate
H 2NCONH 2+NaClO+2NaOH→H 2NNH 2H 2O+NaCl+Na 2CO 3 ---------(2)
Reaction formula (2) generates in the hydrazine hydrate solution Na 2CO 3, NaCl, also have small amount of N aOH, mainly at present adopt freezing-5 ℃ of methods with Na in the hydrazine hydrate 2CO 3Change into Na 2CO 310H 2The O form is extracted, because of Na 2CO 310H 2O combines a part of water, has correspondingly improved hydrazine hydrate concentration, but this process energy consumption is bigger, the cost height; NaOH still is stored in the hydrazine hydrate solution simultaneously, has both caused wastage of material, increases subsequent production operation processing cost again.
Summary of the invention
The objective of the invention is to be to solve when traditional technology is extracted the hydrazine hydrate byproduct to exist energy consumption big, defectives such as cost height, a kind of method of utilizing total alkali in the hydrazine hydrate to produce S-WAT is provided, and its whole process of production three-waste free discharge, energy consumption are little, the added value of product height that is generated.
The method of utilizing total alkali in the hydrazine hydrate to produce S-WAT of the present invention is: add SO in hydrazine hydrate solution 2Gas, NaHSO 3Or Na 2S 2O 5In one or more raw materials, the pH value that is added to hydrazine hydrate solution is 6.0～7.0, with hydrazine hydrate solution crystallisation by cooling, solid-liquid separation, obtains Na 2SO 37H 2O.
When the present invention utilizes the total alkali in the hydrazine hydrate to produce S-WAT, do not have three waste discharge, it is few to substitute the energy consumption of freezing method extraction byproduct with cooling, especially the NaOH in the hydrazine hydrate is all generated Na 2SO 3, Na 2SO 3End-use extensively is worth height, hydrazine hydrate solution concentration raising rate height, and the raw material sources of employing are extensive, and are cheap, have remarkable economic efficiency and environment protection meaning.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
In the hydrazine hydrate solution that adopts Wyler's process production, add SO 2Gas, NaHSO 3Or Na 2S 2O 5In a kind of, SO 2Gas, NaHSO 3Or Na 2S 2O 5Generate Na with the total alkali reaction in the hydrazine hydrate 2SO 37H 2O, described total alkali are NaOH and Na 2CO 3The pH value that is added to hydrazine hydrate solution is 6.0～7.0, with hydrazine hydrate solution crystallisation by cooling, solid-liquid separation, obtains Na 2SO 37H 2O.
Prove absolutely the present invention below in conjunction with chemical equation:
(1) NaOH in the hydrazine hydrate, NaCO 3With SO 2The gas absorption reaction generates Na 2SO 3, reaction end PH6.0～7.0, the absorption process temperature of reaction is kept 30～55 ℃.
2NaOH+SO 2→Na 2SO 3+H 2O ----------------(3)
NaCO 3+SO 2→Na 2SO 3+CO 2↑ -----------(4)
Or hydrazine hydrate under agitation condition with NaHSO 3Neutralization reaction generates Na 2SO 3, the N-process temperature of reaction is kept 30～50 ℃, reaction end PH 6.0～7.0.
Na 2CO 3+2NaHSO 3→2Na 2SO 3+CO 2↑+H 2O?---------------------(5)
NaOH+NaHSO 3→Na 2SO 3+H 2O -----------------------(6)
Or hydrazine hydrate under agitation condition with Na 2S 2O 5Neutralization reaction generates Na 2SO 3, the N-process temperature of reaction is kept 30～50 ℃, reaction end PH 6.0～7.0.
Na 2S 2O 5+Na 2CO 3→2Na 2SO 3+CO 2↑?---------------------(7)
2NaOH+Na 2S 2O 5→2Na 2SO 3+H 2O -------------------------(8)
(2) above-mentioned Na 2SO 3Feed liquid is through crystallisation by cooling, solid-liquid separation and obtain Na 2SO 37H 2O product and filtrate.The crystallisation by cooling temperature is controlled at 5～33 ℃, and the best is 10～20 ℃.
Na 2SO 3+ 7H 2O → Na 2SO 37H 2O (crystalloid)------------------(9)
(3) filtrate mainly contains NaCl, Na 2SO 3, hydrazine hydrate forms, its moisture content is with Na 2SO 37H 2The O form is taken away, and has correspondingly improved filtrate hydrazine hydrate concentration.
Na 2SO 37H 2O can obtain qualified Na after heating evaporation, crystallization, centrifugal, oven dry 2SO 3Product.
From above technical characterstic as can be seen: when utilizing total alkali the hydrazine hydrate to produce S-WAT, do not have three waste discharge, substituting freezing method with cooling, to extract the byproduct energy consumption few, as extract Na per ton 2SO 37H 2O compares Na 2CO 310H 2O save energy 2.0 * 10 5More than the kilojoule, especially the NaOH in the hydrazine hydrate is all generated Na 2SO 3, Na 2SO 3End-use extensively is worth height, compares Na 2CO 310H 2The added value of product of O improves several times.Hydrazine hydrate solution concentration raising rate is 31-36%, and the raw material sources of employing are extensive, and are cheap, has remarkable economic efficiency and environment protection meaning.
Below be several specific embodiment of the present invention, further specify the present invention, but the present invention be not restricted to this.
Embodiment 1
Inject the 1200ml hydrazine hydrate solution in the 2000ml there-necked flask, its hydrazine hydrate concentration 3.9%, total alkalinity 12% feed SO 2Gas carries out absorption reaction, reaction end PH 6.5.Under agitation condition there-necked flask moved into and fill with in the frozen water enamel basin, ℃ kept 1 hour cooling temperature to 15～20, separates out Na 2SO 37H 2O 435 grams, filtrate 975ml, hydrazine hydrate concentration 5.3% in the filtrate.
Embodiment 2
In the 2000ml there-necked flask, inject the 1200ml hydrazine hydrate solution, its hydrazine hydrate concentration 3.9%, total alkalinity 12%, progressively adding the Sodium Pyrosulfite product under agitation condition reacts, reaction end PH 6.5, then again there-necked flask is moved into and fill with in the frozen water enamel basin, ℃ kept 1 hour cooling temperature to 15～20, separates out Na 2SO 37H 2O 420 grams, filtrate 1015ml, hydrazine hydrate concentration 5.1% in the filtrate.

Claims (6)

1. a method of utilizing total alkali in the hydrazine hydrate to produce S-WAT is characterized in that: add SO in hydrazine hydrate solution 2Gas, NaHSO 3Or Na 2S 2O 5In a kind of, the pH value that is added to hydrazine hydrate solution is 6.0～7.0, with hydrazine hydrate solution crystallisation by cooling, solid-liquid separation, obtains Na 2SO 37H 2O.
2. the method for utilizing total alkali in the hydrazine hydrate to produce S-WAT according to claim 1 is characterized in that: described SO 2Gas, NaHSO 3Or Na 2S 2O 5Generate Na with the total alkali reaction in the hydrazine hydrate 2SO 37H 2O, described total alkali are NaOH and Na 2CO 3
3. the method for utilizing total alkali in the hydrazine hydrate to produce S-WAT according to claim 1, it is characterized in that: the hydrazine hydrate solution temperature of reaction is kept 30～55 ℃.
4. the method for utilizing total alkali in the hydrazine hydrate to produce S-WAT according to claim 1 is characterized in that: the hydrazine hydrate solution of described hydrazine hydrate solution for adopting Wyler's process to produce.
5. the method for utilizing total alkali in the hydrazine hydrate to produce S-WAT according to claim 1, it is characterized in that: described crystallisation by cooling temperature is at 5～33 ℃.
6. the method for utilizing total alkali in the hydrazine hydrate to produce S-WAT according to claim 5, it is characterized in that: described crystallisation by cooling temperature is at 10～20 ℃.
CN2009101122109A 2009-07-09 2009-07-09 Method for preparing sodium sulfite by utilizing total alkali in hydrazine hydrate Expired - Fee Related CN101712479B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103011101A (en) * 2012-12-14 2013-04-03 杭州海虹精细化工有限公司 Method for preparing alkali-free low-salt high-concentration hydrazinium by hydrazine hydrate in urea treatment
CN105399113A (en) * 2015-12-03 2016-03-16 天津长芦汉沽盐场有限责任公司 Method for preparing sodium sulfite solution

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103011101A (en) * 2012-12-14 2013-04-03 杭州海虹精细化工有限公司 Method for preparing alkali-free low-salt high-concentration hydrazinium by hydrazine hydrate in urea treatment
CN105399113A (en) * 2015-12-03 2016-03-16 天津长芦汉沽盐场有限责任公司 Method for preparing sodium sulfite solution

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