CN103274432B - A kind of method of hydrazine hydrate by-product sodium carbonate decahydrate through urea comprehensive utilization - Google Patents
A kind of method of hydrazine hydrate by-product sodium carbonate decahydrate through urea comprehensive utilization Download PDFInfo
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- CN103274432B CN103274432B CN201310164695.2A CN201310164695A CN103274432B CN 103274432 B CN103274432 B CN 103274432B CN 201310164695 A CN201310164695 A CN 201310164695A CN 103274432 B CN103274432 B CN 103274432B
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Abstract
The invention provides the method for a kind of hydrazine hydrate by-product sodium carbonate decahydrate through urea comprehensive utilization, the method pulls an oar the Sodium carbonate decahydrate gone out through freezing and crystallizing, heats up, becomes certain density sodium carbonate solution, through filtering and impurity removing, enter carbonating tower and pass into CO
2carry out carbonization, generate sodium bicarbonate, carry out centrifugal, separation at the sodium bicarbonate generated reaction, after drying, obtain sodium bicarbonate.Get wherein a small amount of sodium bicarbonate finished product, join Wyler's process and prepare in hydrazine hydrate solution, control its pH value, caustic soda soln excessive in thick hydrazine solution is neutralized.Beneficial effect of the present invention is: the Sodium carbonate decahydrate comprehensive utilization being originally used as the process of waste product low price, increased substantially the economic worth of by product.More Sodium carbonate decahydrate can be obtained follow-up freezing removing in sodium carbonate link, and improve the concentration of hydrazine hydrate in thick hydrazine, also reduce the consumption of acid in hydrazo-dicarbonamide condensation reaction.
Description
Technical field
The present invention relates to hydrazine hydrate field, be specifically related to the method for a kind of hydrazine hydrate by-product sodium carbonate decahydrate through urea comprehensive utilization.
Background technology
Sodium bicarbonate (NaHCO
3) be important inorganic chemical product, be widely used in the industries such as food fermentation agent, fodder additives, fire-fighting, pharmacy, ore dressing, smelting, tanning, water treatment, especially the fine powder end-use of particle diameter less than 150 μm is wider, and production added value is higher.
NaHCO
3production method mainly contains synthesis method, double decomposition and natural alkaline process etc., and synthesis method is owing to mainly consuming soda ash, and stable and reliable product quality, be the sodium bicarbonate production technology of domestic a large amount of employing.But due to the defect of technique self, existing synthesis method production sodium bicarbonate process energy consumption is large, cost is high, product granularity is large, the market competitiveness is weak, enterprise's productivity effect is low, particularly fine powder and fine powder product proportion very little, can not meet the demand in market, greatly have impact on the development of enterprise.
In Wyler's process hydrazine hydrate production, the Sodium carbonate decahydrate solid that by-product is a large amount of, owing to wherein containing the impurity such as a small amount of urea, hydrazine hydrate, sodium-chlor, suitability for industrialized production can not be directly used in, generally all giving the use occasion very low to sodium carbonate specification of quality as item for disposal process, is a kind of wasting of resources.By the method for Sodium carbonate decahydrate carbonization, can when energy consumption be not high, by simple process in early stage, again through carbonic acid gas carbonization, preparation reaches the sodium bicarbonate commodity of industrial application requirement, both improves added value of product, and additionally reduces Carbon emission, concerning the producer having Wyler's process hydrazine hydrate to react, it is a good method not only having had an economic benefit but also had social benefit.
Summary of the invention
The object of the invention is to the deficiency overcoming prior art existence, and a kind of method that hydrazine hydrate by-product sodium carbonate decahydrate through urea fully utilizes is provided, a kind of by directly utilizing hydrazine hydrate by-product sodium carbonate decahydrate through urea carbonization, prepare sodium bicarbonate, and a small amount of sodium bicarbonate reuse, improve the method for Sodium carbonate decahydrate yield and concentration of hydrazine hydrate.
The object of the invention is to have come by following technical solution.The method of this hydrazine hydrate by-product sodium carbonate decahydrate through urea comprehensive utilization, the method comprises following step:
A. get a certain amount of solid Sodium carbonate decahydrate, through being heated to 50 ~ 100 DEG C, and its mass concentration of water use regulation is 5% ~ 31%;
B. sodium carbonate solution is through sedimentation and filtration, removes impurity wherein, obtains clarification sodium carbonate stock liquid;
C. in sodium carbonate stock liquid, pass into excess carbon dioxide gas, in reaction process, use cooling water control temperature of reaction within the scope of 50 ~ 80 DEG C;
D., after reaction terminates, reaction solution is cooled, filter and washs, after drying, namely obtain sodium bicarbonate sodium bicarbonate.
As preferably, get sodium bicarbonate sodium bicarbonate solid, join in thick hydrazine hydrate solution, add-on is 9 ~ 11 to be as the criterion to control hydrazine hydrate solution pH value terminal, and the reaction of wherein excessive caustic soda soln is generated sodium carbonate; Thick hydrazine solution is through freezing, and be separated, gained solid is Sodium carbonate decahydrate solid, can be used in the raw material of this reaction.
As preferably, other insoluble impuritiess such as Sodium carbonate decahydrate solution needs through post-processing steps such as precipitation, filtrations, the magnesium hydroxide that removing wherein contains.The filtration of this solution can adopt various forms of settling tank, also can adopt millipore filter, fabric filter etc. one or more, the sodium carbonate solution of the clarification of final system.
Beneficial effect of the present invention is: the Sodium carbonate decahydrate comprehensive utilization being originally used as the process of waste product low price, increased substantially the economic worth of by product.Simultaneously, due to juvenile sodium bicarbonate finished product is added in thick hydrazine hydrate solution, neutralize wherein excessive sodium hydroxide, more Sodium carbonate decahydrate can be obtained follow-up freezing removing in sodium carbonate link, and improve the concentration of hydrazine hydrate in thick hydrazine, also reduce the consumption of acid in hydrazo-dicarbonamide condensation reaction.
Embodiment
Below by embodiment, the present invention is further elaborated, and help is understood the present invention by embodiment better, but the present invention is not limited only to following embodiment.
The method of this hydrazine hydrate by-product sodium carbonate decahydrate through urea comprehensive utilization, is characterized in that: the method comprises following step:
A. get a certain amount of solid Sodium carbonate decahydrate, through being heated to 50 ~ 100 DEG C, and its mass concentration of water use regulation is 5% ~ 31%;
B. sodium carbonate solution is through sedimentation and filtration, removes impurity wherein, obtains clarification sodium carbonate stock liquid;
C. in sodium carbonate stock liquid, pass into excess carbon dioxide gas, in reaction process, use cooling water control temperature of reaction within the scope of 50 ~ 80 DEG C;
D., after reaction terminates, reaction solution is cooled, filter and washs, after drying, namely obtain sodium bicarbonate sodium bicarbonate;
E. get sodium bicarbonate sodium bicarbonate solid, join in thick hydrazine hydrate solution, add-on is 9 ~ 11 to be as the criterion to control hydrazine hydrate solution pH value terminal, and the reaction of wherein excessive caustic soda soln is generated sodium carbonate;
F. thick hydrazine solution is through freezing, and be separated, gained solid is Sodium carbonate decahydrate solid, can be used in the raw material of this reaction.
Embodiment 1
Get Sodium carbonate decahydrate solid 100g, heating in beaker, and add a small amount of water dissolution, after it dissolves completely, add water and regulate its concentration to be 20%.By suction filtration, the clarified mother liquor of system.This mother liquor is poured in the flask that band stirs, water-bath cools, bottom it, passes into carbonic acid gas carry out carbonization until reaction terminates.Controlling its temperature of reaction in reaction process is 60 DEG C.Stop logical carbon dioxide, cooling reaction solution to 5 DEG C, filters, and to filter cake cold water washing, weighs, obtain solid sodium bicarbonate 42.3g, with the sodium carbonate rate of collecting for 76% after dry.
Embodiment 2
Get Sodium carbonate decahydrate solid 100g, heating in beaker, and add a small amount of water dissolution, after it dissolves completely, add water and regulate its concentration to be 25%.By suction filtration, the clarified mother liquor of system.This mother liquor is poured in the flask that band stirs, water-bath cools, bottom it, passes into carbonic acid gas carry out carbonization until reaction terminates.Controlling its temperature of reaction in reaction process is 60 DEG C.Stop logical carbon dioxide, cooling reaction solution to 5 DEG C, filters, and to filter cake cold water washing, weighs, obtain solid sodium bicarbonate 45.6g, with the sodium carbonate rate of collecting for 82.2% after dry.
Embodiment 3
Get Sodium carbonate decahydrate solid 100g, heating in beaker, and add a small amount of water dissolution, after it dissolves completely, add water and regulate its concentration to be 30%.By suction filtration, the clarified mother liquor of system.This mother liquor is poured in the flask that band stirs, water-bath cools, bottom it, passes into carbonic acid gas carry out carbonization until reaction terminates.Controlling its temperature of reaction in reaction process is 60 DEG C.Stop logical carbon dioxide, cooling reaction solution to 5 DEG C, filters, and to filter cake cold water washing, weighs, obtain solid sodium bicarbonate 47.2g, with the sodium carbonate rate of collecting for 85.1% after dry.
Embodiment 4
Remove thick hydrazine solution 3000ml, the concentration of hydrazine hydrate recorded wherein is 50.1g/l, and wherein sodium hydrate content is 13.5g/l.This thick hydrazine solution is divided into three parts respectively, every part of 1000ml, in No. 2 samples, is adding sodium bicarbonate 20g, in No. 3 samples, add sodium bicarbonate 30g, stir respectively, carry out freezing after dissolving completely.Three samples are all chilled to 0 DEG C, centrifuging respectively, and analyze concentration of hydrazine hydrate respectively to filtrated stock, result is as follows:
| No. 1 sample | No. 2 samples | No. 3 samples | |
| Concentration of hydrazine hydrate | 52.6g/l | 53.4g/l | 54.2g/l |
The above results shows, after adding a small amount of sodium bicarbonate, the caustic soda soln in original solution and sodium hydrogen carbonate solution react and generate sodium carbonate, after freezing, because crystallize sodium carbonate is with ten crystal water, the overall solution water yield declines to some extent, and its concentration of hydrazine hydrate rises to some extent.Although concentration of hydrazine hydrate ascensional range is not high by the numbers, for the practical situation of hydrazine hydrate lower concentration, the follow-up energy consumption of minimizing and other acids consumption are beneficial in addition.
Finally, it should be pointed out that above example is only the more representational example of the present invention.Obviously, technical scheme of the present invention is not limited to above-mentioned example, can also have many distortion, all distortion that those of ordinary skill in the art can directly derive from content disclosed by the invention or associate, and all should think protection scope of the present invention.
Claims (2)
1. a method for hydrazine hydrate by-product sodium carbonate decahydrate through urea comprehensive utilization, is characterized in that: the method comprises following step:
A. get a certain amount of solid Sodium carbonate decahydrate, through being heated to 50 ~ 100 DEG C, and its mass concentration of water use regulation is 5% ~ 31%;
B. sodium carbonate solution is through sedimentation and filtration, removes impurity wherein, obtains clarification sodium carbonate stock liquid;
C. in sodium carbonate stock liquid, pass into excess carbon dioxide gas, in reaction process, use cooling water control temperature of reaction within the scope of 50 ~ 80 DEG C;
D., after reaction terminates, reaction solution is cooled, filter and washs, after drying, namely obtain sodium bicarbonate sodium bicarbonate;
E. get sodium bicarbonate sodium bicarbonate solid, join in thick hydrazine hydrate solution, add-on is 9 ~ 11 to be as the criterion to control hydrazine hydrate solution pH value terminal, and the reaction of wherein excessive caustic soda soln is generated sodium carbonate; Thick hydrazine solution is through freezing, and be separated, gained solid is Sodium carbonate decahydrate solid, can be used in the raw material of this reaction.
2. the method for hydrazine hydrate by-product sodium carbonate decahydrate through urea according to claim 1 comprehensive utilization, it is characterized in that: in stepb, the filtration of this solution adopts various forms of settling tank, or adopts the one of millipore filter, fabric filter or two kinds.
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| CN104743519B (en) * | 2015-01-21 | 2017-01-18 | 江西省博浩源化工有限公司 | Method for preparing sodium percarbonate from sodium carbonate decahydrate and sodium carbonate mixture |
| CN104528658B (en) * | 2015-01-21 | 2016-11-09 | 江西省博浩源化工有限公司 | A kind of hydrazine hydrate by-product prepares method and the product of SODIUM PERCARBONATE |
| CN108996526B (en) * | 2017-06-07 | 2021-06-22 | 中国科学院过程工程研究所 | Preparation method of large-particle heavy sodium bicarbonate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1796280A (en) * | 2004-12-29 | 2006-07-05 | 陈大元 | Separation of salt and alkali from waste salt and alkali residue in production of hydrazine hydrate and technique of cyclic utilization |
| CN1962444A (en) * | 2006-12-01 | 2007-05-16 | 株洲化工集团诚信有限公司 | Process for producing sodium carbonate using industrial salt dreg |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1796280A (en) * | 2004-12-29 | 2006-07-05 | 陈大元 | Separation of salt and alkali from waste salt and alkali residue in production of hydrazine hydrate and technique of cyclic utilization |
| CN1962444A (en) * | 2006-12-01 | 2007-05-16 | 株洲化工集团诚信有限公司 | Process for producing sodium carbonate using industrial salt dreg |
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