CN1140474C - Method for denirifying from hydrazine hydrate salt mud - Google Patents

Method for denirifying from hydrazine hydrate salt mud Download PDF

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CN1140474C
CN1140474C CNB001129694A CN00112969A CN1140474C CN 1140474 C CN1140474 C CN 1140474C CN B001129694 A CNB001129694 A CN B001129694A CN 00112969 A CN00112969 A CN 00112969A CN 1140474 C CN1140474 C CN 1140474C
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hydrazine hydrate
salt slurry
caustic soda
sodium
present
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CNB001129694A
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CN1274685A (en
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赖中胜
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Abstract

The present invention relates to a method for removing nitrogen from hydrazine hydrate salt slurry. The present invention is characterized in that sodium hydroxide solution containing saturated sodium chloride is soaked to replace hydrazine hydrate salt slurry so that nitrogenous substances in the salt slurry are separated from solid substances. When the method provided by the present invention is used, the nitrogenous components in the hydrazine hydrate salt slurry are effectively removed so that sodium chloride, sodium carbonate and hydrazine hydrate in the salt slurry are utilized, energy sources are saved, the environment is protected, and all the effective components are sufficiently recovered and utilized. In addition, the present invention also has the advantages of little investment, simple and convenient operation and favorable recovery benefit.

Description

A kind of method of from hydrazine hydrate salt mud, denitrogenating
The present invention relates to a kind of method of from hydrazine hydrate salt mud, denitrogenating.
Hydrazine hydrate is a kind of important chemical material, is widely used in medicine, the pesticide producing.Mostly the hydrazine hydrate of present stage is to adopt urea hypochlorite oxidation method or ammonia catalytic method technology, the capital obtains by product when producing hydrazine hydrate by aforesaid method: salt slurry, salt slurry is a kind of mixture, wherein contain hydrazine hydrate, sodium hydroxide, composition such as sodium-chlor and nitrogenous thing, if produce, also can contain the yellow soda ash composition in the salt slurry with urea hypochlorite oxidation method.These compositions in the salt slurry all have utility value, but because the existence of nitrogenous thing, make salt slurry can produce explosive substance in the electrowinning process of caustic soda factory: nitrogen trichloride, this has just limited the use of salt slurry.So if salt slurry is effectively recycled, denitrogenating is a very the key link.Present stage what denitrogenate process using is calcination method, promptly be salt slurry to be calcined denitrogenate, the saline and alkaline mixture after the calcining just can be used as electrolysis with former, auxiliary material.But be to use this method necessary earlier with the salt slurry preheating, in warm, hydrazine hydrate can be discharged in the atmosphere with gas form, does existing following shortcoming like this: the one, wasted the energy; The 2nd, can not recycle hydrazine hydrate; The 3rd, polluted environment; Be exactly complicated operation in addition, investment is big.
The purpose of this invention is to provide a kind of method of denitrogenating to remedy the deficiency of prior art from hydrazine hydrate salt mud, this method can effectively be removed the nitrogenous composition in the hydrazine hydrate salt mud, and sodium-chlor, yellow soda ash, hydrazine hydrate in the salt slurry can be obtained utilizing.
The object of the present invention is achieved like this: a kind of method of denitrogenating from hydrazine hydrate salt mud is characterized in that: get salt slurry, add the caustic soda soln of saturated sodium-chloride that contains of 20%-50% in salt slurry, stir into uniform mixture; The caustic soda soln temperature remains on 20 ℃-100 ℃, and the salt slurry temperature remains on 20 ℃-100 ℃; The quality of caustic soda soln and salt slurry is always than being 0.3: 1-4: 1.Because sodium-chlor is saturated in the caustic soda soln, the solubleness of yellow soda ash is also extremely low, so hydrazine hydrate in the salt slurry and nitrogenous thing will be dissolved in caustic soda soln; And the sodium-chlor in the salt slurry, yellow soda ash will exist with solid form, mixture separation are handled again, and just can obtain the blended solid and the caustic soda mother liquor of sodium-chlor, yellow soda ash; Contain hydrazine hydrate and nitrogenous thing in the caustic soda mother liquor.The caustic soda mother liquor can add in the hydrazine hydrate Production Flow Chart and goes, and also contain certain hydrazine hydrate and nitrogenous thing in the sodium-chlor at this moment, yellow soda ash blended solid, in sodium-chlor, yellow soda ash blended solid, add caustic soda soln again, separating treatment again, obtain the lower sodium-chlor of hydrazine hydrate concentration, yellow soda ash blended solid and caustic soda mother liquor again, repeat the above-mentioned replacement process that embathes, up to the sodium-chlor that obtains meeting the requirements, yellow soda ash blended solid, after carbonization, can do electrolysis again with former, auxiliary material
Method provided by the invention in use can save energy, the protection environment, can also fully recycle each active principle; In addition, it is little that the present invention also has investment, and the operation letter makes, and reclaims profitable advantage.
Below by embodiment, the present invention is further described:
Embodiment 1:
Starting material:
The salt slurry that present embodiment uses is produced the salt slurry that produces in the hydrazine hydrate as urea hypochlorite oxidation method, contain 48.52% sodium-chlor in the salt slurry, 24.53% yellow soda ash, 8.69% sodium hydroxide, 0.4% hydrazine hydrate, 17.86% moisture, nitrogenous thing and other material; Caustic soda soln consists of 4.85% sodium-chlor, 31.178% sodium hydroxide, 63.972% moisture and other material.
Technology:
With 200 gram temperature is that to join 200 gram temperature be in 28 ℃ the hydrazine hydrate salt mud for 30 ℃ caustic soda soln, stir into uniform mixture, the mixture vacuum filtration is separated, obtain mixed once solid 199 grams and caustic soda mother liquor 201 grams of sodium-chlor and yellow soda ash.Contain 0.315% hydrazine hydrate in the caustic soda mother liquor.Also contain 0.085% hydrazine hydrate in the mixed once solid, suction filtration separation again after adding 200 gram caustic soda solns stir in the mixed once solid again, reciprocal like this embathe displacement suction filtration 4 times after, just obtaining nitrogen content is four blended solids of 0.00081% (in ammonia), will just can be used as former, the auxiliary material of electrolysis after the carbonization of four blended solids adding carbonic acid gas.
Embodiment 2:
Starting material:
The salt slurry that present embodiment uses is produced the salt slurry that produces in the hydrazine hydrate as urea hypochlorite oxidation method, contain 48.52% sodium-chlor in the salt slurry, 24.53% yellow soda ash, 8.69% sodium hydroxide, 0.4% hydrazine hydrate, 17.86% moisture, nitrogenous thing and other material; Caustic soda soln consists of 2.1% sodium-chlor, 42.2% sodium hydroxide, 55.7% moisture and other material.
Technology:
With 200 gram temperature is that to join 200 gram temperature be in 90 ℃ the hydrazine hydrate salt mud for 65 ℃ caustic soda soln, stir into uniform mixture, the mixture vacuum filtration is separated, obtain mixed once solid 200 grams and caustic soda mother liquor 200 grams of sodium-chlor and yellow soda ash.Contain 0.31% hydrazine hydrate in the caustic soda mother liquor.Also contain 0.09% hydrazine hydrate in the mixed once solid, suction filtration separation again after adding 200 gram caustic soda solns stir in the mixed once solid again, reciprocal like this embathe displacement suction filtration 4 times after, just obtaining nitrogen content is four blended solids of 0.00083% (in ammonia), will just can be used as former, the auxiliary material of electrolysis after the carbonization of four blended solids adding carbonic acid gas.
Embodiment 3:
Starting material:
The salt slurry that present embodiment uses is produced the salt slurry that produces in the hydrazine hydrate as urea hypochlorite oxidation method, contain 48.52% sodium-chlor in the salt slurry, 24.53% yellow soda ash, 8.69% sodium hydroxide, 0.4% hydrazine hydrate, 17.86% moisture, nitrogenous thing and other material; Caustic soda soln consists of 8% sodium-chlor, 25% sodium hydroxide, 67% moisture and other material.
Technology:
With 130 gram temperature is that to join 200 gram temperature be in 28 ℃ the hydrazine hydrate salt mud for 25 ℃ caustic soda soln, stir into uniform mixture, the mixture vacuum filtration is separated, obtain mixed once solid 199 grams and caustic soda mother liquor 131 grams of sodium-chlor and yellow soda ash.Contain 0.437% hydrazine hydrate in the caustic soda mother liquor.Also contain 0.116% hydrazine hydrate in the mixed once solid, suction filtration separation again after adding 130 gram caustic soda solns stir in the mixed once solid again, reciprocal like this embathe suction filtration 5 times after, just obtaining nitrogen content is five blended solids of 0.00053% (in ammonia), will just can be used as former, the auxiliary material of electrolysis after the carbonization of five blended solids adding carbonic acid gas.
Embodiment 4:
Starting material:
The salt slurry that present embodiment uses is the autogamy salt slurry, contains 83% sodium-chlor in the salt slurry, 2% sodium hydroxide, 0.4% hydrazine hydrate, 14.6% moisture, other material; Caustic soda soln consists of 4.85% sodium-chlor, 31.178% sodium hydroxide, 63.972% moisture and other material.
Technology:
With 30 kilograms of temperature is that to join the double centner temperature be in 28 ℃ the hydrazine hydrate salt mud for 50 ℃ caustic soda soln, stir into uniform mixture, mixture is put into the whizzer centrifugation, when centrifuge speed reaches 550-650 rev/min normal speed, beginning adds 190 kilograms of caustic soda solns continuously and embathes displacement washing continuously in whizzer, washing time is 50 seconds, the centrifugal back sampling analysis that finishes, 220.5 kilograms in 99.5 kilograms of blended solids of resultant sodium chloride-containing and caustic soda mother liquor.The nitrogenous thing that contains 0.0004% (in ammonia) in the blended solid just can be used as former, the auxiliary material of electrolysis after blended solid added the carbonic acid gas carbonization.
Explanation in addition: among the above embodiment, each secondary caustic soda mother liquor can be used as the liquid that embathes of upper level salt slurry or blended solid, so that promote the hydrazine hydrate concentration of a caustic soda mother liquor, saves the caustic soda raw material; Suction filtration round-robin number of times mainly with hydrazine hydrate salt mud in hydrazine hydrate content, solid-to-liquid ratio, blended solid after separating when back and forth embathing in moisture content relevant.

Claims (1)

1, a kind of method of from hydrazine hydrate salt mud, denitrogenating, it is characterized in that: with the caustic soda soln that contains saturated sodium-chloride of 20%-50% concentration, the caustic soda soln temperature remains on 20 ℃-100 ℃, embathe the hydrazine hydrate salt mud of 20 ℃-100 ℃ of displacements with this caustic soda soln, the nitrogenous substances in the salt slurry is separated with solid matter; The quality of caustic soda soln and salt slurry is always than being 0.3: 1-4: 1.
CNB001129694A 2000-05-25 2000-05-25 Method for denirifying from hydrazine hydrate salt mud Expired - Fee Related CN1140474C (en)

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Application Number Priority Date Filing Date Title
CNB001129694A CN1140474C (en) 2000-05-25 2000-05-25 Method for denirifying from hydrazine hydrate salt mud

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CN1140474C true CN1140474C (en) 2004-03-03

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Publication number Priority date Publication date Assignee Title
CN100389892C (en) * 2005-10-13 2008-05-28 宜宾天原股份有限公司 Recovering treatment of hydrated hydrazine by-product saline-alkali by urea method
TWI400200B (en) * 2008-03-28 2013-07-01 An Cheng Lee Process and apparatus of deodorizing and recycling for aluminum dross

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