CN104860275A - Method for removing sodium carbonate from hydrazine hydrate crude solution - Google Patents
Method for removing sodium carbonate from hydrazine hydrate crude solution Download PDFInfo
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- CN104860275A CN104860275A CN201510178280.XA CN201510178280A CN104860275A CN 104860275 A CN104860275 A CN 104860275A CN 201510178280 A CN201510178280 A CN 201510178280A CN 104860275 A CN104860275 A CN 104860275A
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Abstract
The invention discloses a method for removing sodium carbonate from a hydrazine hydrate crude solution. The method comprises the following steps: 1, a urea solution is mixed with sodium hypochlorite, wherein a molar ratio of the urea solution to sodium hypochlorite is 1-2, such that the crude solution obtained by a reaction does not contain sodium hydroxide; 2, a chloride is added into the hydrazine hydrate crude solution; and centrifugal separation is carried out, such that poorly soluble carbonate is separated; 3, the hydrazine hydrate solution with sodium carbonate removed is subjected to membrane filtration, such that cations in the solution are removed. With the method, sodium carbonate in the hydrazine hydrate crude solution is thoroughly removed. The produced poorly soluble carbonate can be directly sold after certain treatments, and can be subjected to a reaction with hydrochloric acid recovered from an ADC process for producing chloride for recycling. When the sodium-carbonate-removed hydrazine hydrate solution is used in a biurea production process, acidic substance addition can be greatly reduced. When the sodium-carbonate-removed hydrazine hydrate solution is used in a hydrazine hydrate production process through evaporation and rectification, evaporation and rectification continuous production is facilitated.
Description
Technical field
The present invention relates to the technical field of removing sodium carbonate, be specifically related to a kind of method removing sodium carbonate in the thick solution of hydrazine hydrate.
Background technology
Produced in the thick solution of hydrazine hydrate containing hydrazine hydrate, sodium carbonate, urea, sodium-chlor and water by Wyler's process.Carbonate content is at 110-150g/L, and conventional method to send in crystallization kettle after thick for hydrazine hydrate solution precooling, is cooled to-2 DEG C--and 0 DEG C; The Sodium carbonate decahydrate of centrifugal removing 60--70%, obtains the hydrazine hydrate solution containing 35-60/L sodium carbonate.If with this solution in production hydrazo-dicarbonamide process, remaining sodium carbonate need consume a large amount of acidic substance, adds the consumption of acidic substance.If produce in hydrazine hydrate process with this solution by evaporation, rectifying, because sodium carbonates' presence can form monohydrated sodium carbonate in evaporative process, there is monohydrated sodium carbonate existence that the heat transfer tube of well heater can be made to block in vaporizer, frequent needs stop producing discharges material, add water purge heater, be unfavorable for like this realizing evaporation, rectifying continuous prodution, purge heater need consume the loss that a large amount of steam causes material simultaneously.
Summary of the invention
Object of the present invention just in order to overcome the deficiency of above-mentioned technology, and provides a kind of method removing sodium carbonate in the thick solution of hydrazine hydrate.
The object of the invention is to have come by following technical solution.The method of sodium carbonate in the thick solution of this removing hydrazine hydrate, the method concrete steps are as follows:
(1), by urea soln with clorox mixing post-heating to 106-135 DEG C, urea: clorox mol ratio is 1-2, reaction generates the thick solution containing hydrazine hydrate, not containing sodium hydroxide in the thick solution making reaction generate, the component in thick solution only has hydrazine hydrate, sodium carbonate, urea, sodium-chlor and water;
(2), in the thick solution of hydrazine hydrate add muriate, realize positively charged ion in muriate and carbanion reacts the carbonate generating indissoluble, go out the carbonate of indissoluble through centrifugation;
(3) hydrazine hydrate solution, after removing sodium carbonate is again through the positively charged ion that membrane filtration removing solution exists, thus the sodium carbonate thoroughly in the thick solution of removing hydrazine hydrate.
Described muriate is magnesium chloride, calcium chloride, bariumchloride, strontium chloride, zinc chloride or Manganous chloride tetrahydrate.
Beneficial effect of the present invention is: the sodium carbonate thoroughly in the thick solution of removing hydrazine hydrate.The carbonate of the indissoluble produced can directly externally be sold through process, and the hydrochloric acid reaction that also can reclaim with ADC operation generates muriate, after concentrated, recycles.Produce in hydrazo-dicarbonamide process if the hydrazine hydrate solution after removing sodium carbonate is used in, significantly reduce adding of acidic substance, reduce the consumption of acidic substance.Produce in hydrazine hydrate process if the hydrazine hydrate solution after removing sodium carbonate is used in by evaporation, rectifying, because no longer including the generation of monohydrated sodium carbonate in evaporative process, the heat transfer tube of well heater no longer blocks, and is so more conducive to realizing evaporation, rectifying continuous prodution.
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 sodium carbonate in the thick solution of this removing hydrazine hydrate of the present invention, the method concrete steps are as follows:
(1), by urea soln with clorox mixing post-heating to 106-135 DEG C, urea: clorox mol ratio is 1-2, reaction generates the thick solution containing hydrazine hydrate, not containing sodium hydroxide in the thick solution making reaction generate, the component in thick solution only has hydrazine hydrate, sodium carbonate, urea, sodium-chlor and water;
(2), in the thick solution of hydrazine hydrate add muriate, realize positively charged ion in muriate and carbanion reacts the carbonate generating indissoluble, go out the carbonate of indissoluble through centrifugation;
(3) hydrazine hydrate solution, after removing sodium carbonate is again through the positively charged ion that membrane filtration removing solution exists, thus the sodium carbonate thoroughly in the thick solution of removing hydrazine hydrate, eliminate the impact that positively charged ion brings to rear operation simultaneously.
As preferably, the muriate added is the carbonate that its positively charged ion and carbanion can produce indissoluble, and described muriate is magnesium chloride, calcium chloride, bariumchloride, strontium chloride, zinc chloride or Manganous chloride tetrahydrate (except the muriate that oxidisability is stronger).Realize the positively charged ions such as the magnesium ion in muriate, calcium ion, barium ion, strontium ion, zine ion, mn ion and carbanion reacts the magnesiumcarbonate, calcium carbonate, barium carbonate, Strontium carbonate powder, zinc carbonate, manganous carbonate etc. that generate indissoluble, the carbonate of indissoluble is gone out through centrifugation, the positively charged ion such as magnesium ion, calcium ion, barium ion, strontium ion, zine ion, mn ion that hydrazine hydrate solution after separation exists in membrane filtration removing solution again, thus thoroughly remove the sodium carbonate in the thick solution of hydrazine hydrate.The carbonate of the indissoluble produced can directly externally be sold through process, and the hydrochloric acid reaction that also can reclaim with ADC operation generates muriate, after concentrated, recycles.
Produce in hydrazo-dicarbonamide process if the hydrazine hydrate solution after removing sodium carbonate is used in, significantly reduce adding of acidic substance, reduce the consumption of acidic substance.Produce in hydrazine hydrate process if the hydrazine hydrate solution after removing sodium carbonate is used in by evaporation, rectifying, because no longer including the generation of monohydrated sodium carbonate in evaporative process, the heat transfer tube of well heater no longer blocks, and is so more conducive to realizing evaporation, rectifying continuous prodution.
Embodiment:
1, Jiang Shui passes in urea Preparation tank, under agitation drops into solid urea, magnesium sulfate heptahydrate catalyzer, and magnesium sulfate add-on is 1.5% of urea amount, is mixed with 360g/L urea soln.
2,32% caustic soda is added water, be formulated as 270-275g/L diluted alkaline, pass into chlorine reaction and produce available chlorine 108g/L, the clorox of sodium hydroxide 124g/L.
3, by urea soln with clorox mixing post-heating to 130 DEG C, reaction generates containing the thick solution of hydrazine hydrate, urea: clorox mol ratio is 1.085.Not containing sodium hydroxide in the thick solution that reaction generates.Component hydrazine hydrate 48g/L in thick solution, sodium carbonate 125g/L, urea 25g/L, sodium-chlor 180g/L, all the other are water.
4, in the thick solution of hydrazine hydrate, add strontium chloride, react with sodium carbonate the Strontium carbonate powder generating indissoluble, go out the Strontium carbonate powder of indissoluble through centrifugation, after treatment direct marketing.
5, be separated the strontium ion of the hydrazine hydrate solution after Strontium carbonate powder again in membrane filtration removing solution, thus thoroughly remove the sodium carbonate in the thick solution of hydrazine hydrate, eliminate the impact that strontium ion brings to rear operation simultaneously.
Claims (2)
1. remove a method for sodium carbonate in the thick solution of hydrazine hydrate, it is characterized in that: the method concrete steps are as follows:
(1), by urea soln with clorox mixing post-heating to 106-135 DEG C, urea: clorox mol ratio is 1-2, reaction generates the thick solution containing hydrazine hydrate, not containing sodium hydroxide in the thick solution making reaction generate, the component in thick solution only has hydrazine hydrate, sodium carbonate, urea, sodium-chlor and water;
(2), in the thick solution of hydrazine hydrate add muriate, realize positively charged ion in muriate and carbanion reacts the carbonate generating indissoluble, go out the carbonate of indissoluble through centrifugation;
(3) hydrazine hydrate solution, after removing sodium carbonate is again through the positively charged ion that membrane filtration removing solution exists, thus the sodium carbonate thoroughly in the thick solution of removing hydrazine hydrate.
2. the method for sodium carbonate in the thick solution of removing hydrazine hydrate according to claim 1, is characterized in that: described muriate is magnesium chloride, calcium chloride, bariumchloride, strontium chloride, zinc chloride or Manganous chloride tetrahydrate.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105036098A (en) * | 2015-09-01 | 2015-11-11 | 青海盐湖工业股份有限公司 | Method for removing sodium carbonate in solution |
| CN105645451A (en) * | 2016-02-25 | 2016-06-08 | 青海盐湖工业股份有限公司 | Method for preparing micropowder-grade light calcium carbonate |
| CN106008278A (en) * | 2016-06-06 | 2016-10-12 | 青海盐湖工业股份有限公司 | Preparation method of biurea |
| CN106044729A (en) * | 2016-06-17 | 2016-10-26 | 青海盐湖工业股份有限公司 | Method for treating byproducts of hydrazine hydrate prepared by aid of urea processes |
| CN106349119A (en) * | 2016-08-26 | 2017-01-25 | 衡阳市锦轩化工有限公司 | Method for co-production of biurea and sodium fluoride |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1046328A (en) * | 1989-04-13 | 1990-10-24 | 成都华西化工研究所 | Alkali cycling process with production of hydrated hydrazine from urea |
-
2015
- 2015-04-15 CN CN201510178280.XA patent/CN104860275A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1046328A (en) * | 1989-04-13 | 1990-10-24 | 成都华西化工研究所 | Alkali cycling process with production of hydrated hydrazine from urea |
Non-Patent Citations (1)
| Title |
|---|
| 郑土英等: "ADC发泡剂生产的清洁技术改进", 《化工生产与技术》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105036098A (en) * | 2015-09-01 | 2015-11-11 | 青海盐湖工业股份有限公司 | Method for removing sodium carbonate in solution |
| CN105645451A (en) * | 2016-02-25 | 2016-06-08 | 青海盐湖工业股份有限公司 | Method for preparing micropowder-grade light calcium carbonate |
| CN106008278A (en) * | 2016-06-06 | 2016-10-12 | 青海盐湖工业股份有限公司 | Preparation method of biurea |
| CN106044729A (en) * | 2016-06-17 | 2016-10-26 | 青海盐湖工业股份有限公司 | Method for treating byproducts of hydrazine hydrate prepared by aid of urea processes |
| CN106349119A (en) * | 2016-08-26 | 2017-01-25 | 衡阳市锦轩化工有限公司 | Method for co-production of biurea and sodium fluoride |
| CN106349119B (en) * | 2016-08-26 | 2018-08-03 | 衡阳市锦轩化工有限公司 | The method of coproduction biruea and sodium fluoride |
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Application publication date: 20150826 |