CN101054189B - Method of preparing sea crystal from byproduct salt of refining iminodiacetic acid - Google Patents
Method of preparing sea crystal from byproduct salt of refining iminodiacetic acid Download PDFInfo
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- CN101054189B CN101054189B CN2006100503148A CN200610050314A CN101054189B CN 101054189 B CN101054189 B CN 101054189B CN 2006100503148 A CN2006100503148 A CN 2006100503148A CN 200610050314 A CN200610050314 A CN 200610050314A CN 101054189 B CN101054189 B CN 101054189B
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Abstract
The invention relates to a method for preparing seawater crystal with refined iminodiacetic acid by-product salt and the steps are as follows in order: washing the by-product salt, solving, fine filtering, filtering with various medium, micro-filtering, chelating, secondary fine filtering, recrystallizing, centrifugating and drying, then adding a proportion of MgSO4, MgCl2, CaCl2, KCl and NaS2O3 into the salt to prepare seawater crystal and the proportion is: NaCl 72.3-77.5%, MgSO4 7.5-12%, MgCl2 11.6-13.5%, CaCl2 1.65-1.94%, KCl 1.35-1.64% and NaS2O3 0.001-0.002%, with the total percentage of 100%. The invention uses a method for preparing seawater crystal with refined iminodiacetic acid by-product salt, which is characterized in using by-product NaCl, reducing raw materials cost and protecting the environment, which is a typical clean production process.
Description
Technical field
The present invention relates to a kind of manufacture method of solid seawater, especially relate to a kind of method of preparing sea crystal from byproduct salt of refining iminodiacetic acid.
Background technology
Sea crystal is a kind of composition of salt, is artificial seawater as long as mix with an amount of water, can be used for the breed of hinterland sea-food, overcomes the difficulty of seawater transportation aspect.It is the product of seawater and salt chemical engineering, mainly produces by a series of processes such as seawater or bittern being evaporated, centrifugal, concentrated, it has kept the main component of seawater substantially, is the seawater that has concentrated.Add trace element therein selectively, not only can replenish the part element and the compound that run off in the production process, also make whole prod more be imbued with practicability, as adding selenium, molybdenum etc., not only promote the hydrocoles growth, also can make it towards health, nutrition, comprehensive direction develop more.At present, sea crystal is except that as the industrial raw material, and what the application in fishery was comparatively successful has: the one, and in the river mouth or low salinity area, be used for the shrimp crab and grow seedlings or form.The 2nd, at inland lake area preparation artificial seawater, carry out the seawater seed breeding.The 3rd, be widely used in the demand of recreational fisherieses such as landlocked aquarium to seawater.
In the prior art, the production method of sea crystal mainly contains two, the first utilizes bittern to be raw material, with the bittern evaporation concentration, continue to concentrate after removing calcium sulfate, get the solid phase that approaches element ratio in the seawater, add some elements again, make it reach the ratio of each element in the seawater and make sea crystal.Chinese patent 03138874.4 (production method of solid seawater) discloses a kind of production method of utilizing bittern to produce the solid seawater; it can reduce production costs significantly; reclaim resource; coastal society and ecotope have also been protected; but this method need concentrate; energy consumption is higher, and contains a spot of calcium sulfate, has influence on the quality that fishery is grown seedlings or formed.It two is to utilize the method for natural salt added elements to make sea crystal, the method of utilizing natural salt to produce the seawater element introduced in article in " sea salt lake and chemical industry " the 26th volume second phase " development of the plain product of a seawater " literary composition, the resulting seawater element of this method is mixed with that seawater does not have precipitation, the culture experiment effect is remarkable, but uses this manufactured sea crystal cost higher.
The iminodiethanoic acid production method mainly contains two kinds at present, and a kind of is the iminodiacetonitrile method, and a kind of is diethanolamine method.No matter adopt which kind of method, all have a large amount of salt to produce in the production process of iminodiethanoic acid, this salt will influence quality product as bringing in the product, as bring in the waste water and will cause environmental pollution.
Summary of the invention
The invention discloses a kind of is the method for feedstock production sea crystal with iminodiethanoic acid by-product salt.Above-mentioned purpose of the present invention is mainly solved by following technical proposals: with iminodiethanoic acid by-product salt is the feedstock production sea crystal, its steps in sequence is: with the washing of by-product salt, dissolving, smart filter, multi-medium filtering, micro-filtration, chelating, the smart filter of secondary, recrystallization, centrifugal, drying treatment, a certain proportion of sal epsom of interpolation, magnesium chloride, calcium chloride, Repone K, Sulfothiorine make sea crystal in this salt again.
Prescription of the present invention is as follows, below each component summation equal 100%:
Sodium-chlor: 72.3-77.5%
Sal epsom: 7.5-12%
Magnesium chloride: 11.6-13.5%
Calcium chloride: 1.65-1.94%
Repone K: 1.35-1.64%
Sulfothiorine: 0.001-0.002%
Concrete preparation process is:
The washing of by-product salt: the by-product salt of iminodiethanoic acid adds deionized water and soaked 30 minutes through the mother liquor of suction filtration removal iminodiethanoic acid in the salt after draining, drain mother liquor, adds the deionized water immersion again and drains in 30 minutes;
Dissolving: the salt after water washing is put into the container that band stirs, and is dissolved in water, and makes saturated solution;
Smart filter: above-mentioned saturated solution process accurate filter is removed the solids component in the solution;
Multi-medium filtering: remove viscous substance in the solution with the more medium filter that contains gac again;
Micro-filtration: solution is removed larger molecular organics by millipore filter;
Chelating: remove heavy metal ion through chelate resin tower again;
The smart filter of secondary: remove damaged resin through accurate filter;
Recrystallization: solution through concentrate carry dense, after salting out through crystallization, filtration;
Centrifugal: as to obtain purified salt through centrifugation;
Oven dry: control drying machine or oven temperature obtained product, salts contg 〉=99% in 2～5 hours 90～110 ℃ of oven dry.
The salt that obtains thus can be used for preparing sea crystal, also can be used as pickling of the raw material of saltouing and leather etc., and mother liquor then turns back in the saturated solution and recycles.
In above-mentioned purified salt, press again formula rate add sal epsom, magnesium chloride, calcium chloride, Repone K, Sulfothiorine through mix, packing promptly gets the sea crystal finished product.
Related accurate filter is 20～50 μ m fusion-jet type strainers among the present invention, and millipore filter is that the aperture is the micropore filtering film of 0.1～10 μ m.
Resin involved in the present invention adopts LSC-100 amino acid pattern, CR20 polyamine type, CR11 diglycinee type resin any one or arbitrary combination, and chelate resin tower adopts steel lining low calcium and magnesium rubber material.
Mixed processes described in the present invention adopts double worm mixer or trough type mixing machine, preferred double worm mixer.
As preferably, resin adopts CR20 polyamine type resin.
Sea crystal is inexpensive and easy to use, belong to environmentfriendly products, after the use, both can effectively drive away batrachia and other harmful animals in the fresh water, can effectively suppress water cloud and the numerous life of weeds again, purify water, contain the necessary nutritive ingredient of marine animal, can improve hydrobiont and culture quality, promptly improve resistance against diseases and the surviving rate of marine animal.The present invention adopts the method for preparing sea crystal from byproduct salt of refining iminodiacetic acid; protected environment when having reduced raw materials cost again; resource is utilized effectively, so the present invention having the advantage that cost is low, quality good, help protecting environment, is typical clean production technique.
Description of drawings
Fig. 1 is the chemical equation of iminodiethanoic acid by-product salt among the present invention;
Fig. 2 is a process flow sheet of the present invention.
Embodiment
Below by embodiment, and in conjunction with the accompanying drawings, technical scheme of the present invention is described in further detail.
Embodiment 1: put into the iminodiethanoic acid secondary salt 1500kg of suction filtration bucket, drain mother liquor, add water 300kg, soaked 30 minutes, drain; Add water 300kg again, soak and drained in 30 minutes; The salt water dissolution of draining, the millipore filter of more medium filter, aperture 0.1 a μ m of the accurate filter that solution is 20 μ m by an aperture continuously, a band gac, one are equipped with the adsorption tower of CR20 polyamine type resin, an aperture is the accurate filter of 20 μ m, to remove solid impurity, viscous substance, larger molecular organics and heavy metal ion and damaged resin; The solution that refines is separated out crystallization through concentrating, and separates the mother liquor A and the salt that obtain, and the salt that obtains is sent into pneumatic drier through centrifugal, and 100 ℃ of continuous dryings of controlled temperature obtain salts contg and reach 99%, heavy metal ion content 0.5ppm.Get above-mentioned purified salt 723kg, get sal epsom 120kg, magnesium chloride 124kg, calcium chloride 16.58kg, Repone K 16.4kg, Sulfothiorine 0.02kg again; Above material is dropped into double worm mixer mixed 3 hours, again the material package dress that mixes is got final product.
Embodiment 2: put into the iminodiethanoic acid secondary salt 1500kg of suction filtration bucket, drain mother liquor, add water 300kg, soaked 30 minutes, drain; Add water 300kg again, soak and drained in 30 minutes; The salt water dissolution of draining, adding mother liquor A mixes, the accurate filter of the more medium filter of the accurate filter that mixing solutions is 50 μ m by an aperture continuously, a band gac, the micropore filtering film of aperture 10 μ m, an adsorption tower that CR20 polyamine type resin is housed, aperture 50 μ m is to remove solid impurity, viscous substance, larger molecular organics and heavy metal ion and damaged resin; The solution that refines is separated out crystallization through concentrating, and separates the mother liquor B and the salt that obtain, and the salt that obtains is put into Hotaircirculatingoven through centrifugal, 105 ℃ of oven dry of controlled temperature 3 hours, and content reaches 99%, heavy metal ion content 0.8ppm.Get above-mentioned purified salt 775kg, get sal epsom 75kg, magnesium chloride 116kg, calcium chloride 19.4kg, Repone K 14.59kg, Sulfothiorine 0.01kg again, above no material is dropped into double worm mixer mixed 3 hours, again with the material package dress that mixes.
Embodiment 3
Put into the iminodiethanoic acid secondary salt 1500kg of suction filtration bucket, drain mother liquor, add water 300kg, soaked 30 minutes, drain; Add water 300kg again, soak and drained in 30 minutes; The salt water dissolution of draining, adding mother liquor B mixes, the accurate filter of the more medium filter of the accurate filter that mixing solutions is 30 μ m by an aperture continuously, a band gac, the micropore filtering film of aperture 1 a μ m, an adsorption tower that CR20 polyamine type resin is housed, aperture 25 μ m is to remove solid impurity, viscous substance, larger molecular organics and heavy metal ion and damaged resin; The solution that refines is separated out crystallization through concentrating, and separating the mother liquor cover C that obtains can recycle in continuing treating process, and the salt that obtains is through centrifugal, send into pneumatic drier, 130 ℃ of continuous dryings of controlled temperature obtain salts contg and reach 99%, heavy metal ion content 0.1ppm.Get refining sodium-chlor 750kg, get again and get sal epsom 92.08kg, magnesium chloride 126kg, calcium chloride 18.4kg, Repone K 13.5kg, Sulfothiorine 0.02kg again, above material is dropped into double worm mixer mixed 3 hours, the material package that mixes dress.
At last, should be pointed out that above embodiment only is the more representational example of the present invention.Obviously, technical scheme of the present invention is not limited to the foregoing description, and many distortion can also be arranged.The process for purification described in the invention and the prescription of sea crystal can carry out multiple combination.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (2)
1. the method for a preparing sea crystal from byproduct salt of refining iminodiacetic acid is characterized in that comprising the steps:
A: after the recovery of the by-product salt in the iminodiethanoic acid production process, through the smart filter of washing, dissolving, smart filter, multi-medium filtering, micro-filtration, chelating, secondary, recrystallization, centrifugal, drying treatment, obtain that heavy metal ion content 1ppm is following, its content surpasses 99% purified salt; Detailed process is:
The washing of by-product salt: the by-product salt of iminodiethanoic acid adds deionized water and soaked 30 minutes through the mother liquor of suction filtration removal iminodiethanoic acid in the salt after draining, drain mother liquor, adds the deionized water immersion again and drains in 30 minutes;
Dissolving: the salt after water washing is put into the container that band stirs, and is dissolved in water, and makes saturated solution;
Smart filter: above-mentioned saturated solution is removed solids component in the solution through 20～50 μ m fusion-jet type strainers;
Multi-medium filtering: remove viscous substance in the solution with the more medium filter that contains gac again;
Micro-filtration: solution is removed larger molecular organics by millipore filter;
Chelating: remove heavy metal ion through chelate resin tower again;
The smart filter of secondary: remove damaged resin through 20～50 μ m fusion-jet type strainers;
Recrystallization: solution through concentrate carry dense, after salting out through crystallization, filtration;
Centrifugal: as to obtain salt through centrifugation;
Oven dry: control drying machine or oven temperature are at 80～140 ℃ of oven dry 2～5 hours, purified salt content 〉=99% that obtains;
B: add composition---the sea crystal that sal epsom, magnesium chloride, calcium chloride, Repone K, Sulfothiorine make salt in described purified salt successively, their weight percent is respectively 72.3～85,7.5～14,11.6～14.5,1.65～1.94,1.35～1.64,0.001～0.002.
2. the method for a kind of preparing sea crystal from byproduct salt of refining iminodiacetic acid according to claim 1, it is characterized in that resin is any one of LSC-100 amino acid pattern, CR20 polyamine type, CR11 diglycinee type resin, or arbitrary combination.
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| CN104609444B (en) * | 2015-03-01 | 2016-03-30 | 邱廷刚 | Straightization method produces potassium sulfate and the method for several high level byproduct of by-product |
| CN115490382B (en) * | 2022-09-19 | 2023-08-15 | 自然资源部天津海水淡化与综合利用研究所 | Preparation method of deep sea crystal |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594281A (en) * | 2004-07-05 | 2005-03-16 | 四川省天然气化工研究院 | Process for preparing iminodiacetic acid |
| CN1663945A (en) * | 2004-12-24 | 2005-09-07 | 南京师范大学 | Method for reclaiming diglycolamidic acid from acidified mother liquor of diglycolamidic acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1594281A (en) * | 2004-07-05 | 2005-03-16 | 四川省天然气化工研究院 | Process for preparing iminodiacetic acid |
| CN1663945A (en) * | 2004-12-24 | 2005-09-07 | 南京师范大学 | Method for reclaiming diglycolamidic acid from acidified mother liquor of diglycolamidic acid |
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