CN101289165A - Method for preparing sodium chloride crystal without agglomeration - Google Patents
Method for preparing sodium chloride crystal without agglomeration Download PDFInfo
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- CN101289165A CN101289165A CNA2007100489094A CN200710048909A CN101289165A CN 101289165 A CN101289165 A CN 101289165A CN A2007100489094 A CNA2007100489094 A CN A2007100489094A CN 200710048909 A CN200710048909 A CN 200710048909A CN 101289165 A CN101289165 A CN 101289165A
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- salt
- ferrocyanide
- saturated brine
- yellow prussiate
- sodium chloride
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention discloses a preparation method of a non-caking sodium chloride crystal, which is formed by adding ferrocyanide into saturated brine to be evaporated, concentrated and crystallized, wherein, the ferrocyanide is added when the saturated brine begins to crystallize, thus the crystal form of the salt that is dissolved out for the first time does not change, and only absorbs some ferrocyanide on the surface thereof; the ferrocyanide mainly forms an isolating layer between the crystals, and avoids forming salt bridge between the crystals, thus greatly reducing the content of the ferrocyanide in the salt dissolved out for the first time to be less than or equal to 8 mg/L and at the same time effectively controlling the main participation of the ferrocyanide to change the shape of the sodium chloride crystal; after the branch-structured or star-structured crystals are formed, only a little ferrocyanide is absorbed on the surface of the crystals, thereby effectively reducing the content of the ferrocyanide in the salt dissolved out later to be 3mg/Kg on average, which accords with the requirements in GB5461-2003 national standards.
Description
Technical field
The present invention relates to the salt manufacturing technology, especially relate to the purified salt manufacturing technology of artificial method of evaporating.
Background technology
Sodium-chlor is one of important basic chemical raw materials, also is indispensable chemical among the human lives, is most widely used general, most important a kind of inorganic salt product.
Salt is inhomogeneous because of its particle, causes shortcomings such as salt dissolution rate caking not of uniform size and easy.Along with improving constantly of people's life idea, also more and more higher to the requirement of salt, for overcoming the above problems, develop the inexorable trend that salt uniform particles, tap density is little, dissolution rate is fast salt become market development, and very urgent.Branch salt mainly has the following advantages: 1, prevented from caking; 2, uniform particles, fineness are good, have good mixed characteristic to be easy to and other material thorough mixing with other thinner material, can be used as the salt carrier of many kinds salt, have solved the problem of common salt mixture homogeneity difference; 3, density is little, surface-area is big, does not also become sticky even absorb portion of water.4, dissolution rate is good, than fast 2～3 times of general common cubes sodium-chlor; 5, whiteness height; 6, abroad some tropic countries is mainly from this salt of Britain's import, and after this products production success, branch salt can be used for exporting, and solves the present situation of domestic no branch salt.
The purposes of branch salt is also quite extensive, is the best product that replaces present edible salt, because branch salt not only possesses all characteristics of purified salt, but also has possessed some characteristics that are better than purified salt.Branch salt good fluidity, dissolution rate and fast can lump together more equably with seasonings.As foodstuff additive, branch salt can be mixed in the food equably, when handling sheepskin and calf skin with branch salt, can reduce the consumption of salt greatly, and therefore, branch salt is the new variety of a salt that serves many purposes.
Especially in the preparation process of purified salt,, normally in bittern, add additive sodium chloride crystal is improved, to reach the purpose that forms the dendroid sodium chloride crystal for preventing caking.In " sea lake salt and the chemical industry " first phase the 35th volume of publishing in 2006, " Study on Sodium Chloride Dendrite " literary composition by name is disclosed, wherein the additive types of Xuan Zeing has glucose, sucrose, sodium formiate, glycerine, 163BR, oleic acid etc., mainly be to glucose and 163BR as additive to sodium chloride crystal improvement done deep research.
Chinese patent CN1172852C discloses a kind of " non-caking sodium chloride crystals, the method for preparing them and their application in electrolytic process ", mainly be that the metal complex that adds hydroxyl polycarboxylic acid mixture in sodium chloride solution prevents to lump as additive, but the cost of this mode is higher.
Chinese patent CN1267020C discloses a kind of " preventing the novel process of purified salt caking ", it is to adopt yellow prussiate (yellow prussiate of soda or yellow prussiate of potash) with trace to add pH value in the saturated brine after the making with extra care of 7-9, making concentration is the feed liquid of 1.0～3.0 mg/litre (in yellow prussiate of soda or yellow prussiate of potash), enter in the evaporative crystallizer so that 0.2～0.4 kg of water/hour rising evaporation capacity carries out evaporation concentration, control its pulp density≤10% (volumetric ratio), can be prevented the purified salt of caking, yellow prussiate of potash content≤10 milligram/kilogram in the purified salt.Though it has solved the cost problem of additive, but the yellow prussiate residual quantity in finished product salt is too much, from embodiment as can be seen, though it can reach the standard of national requirements≤10mg/Kg, but the form that is cyanide group in a large number is present in the finished product salt, objectively also there is bigger dispute, no matter adopt vacuum-evaporation still to adopt atmospheric evaporation, added yellow prussiate of potash so long as advance in jar saturated brine, no matter be a salt discharge or gradation salt discharge, yellow prussiate of potash content is all very high in first salt of separating out, be far longer than 10%, its basic reason is to participate in the yellow prussiate of potash that crystal changes except containing in first salt of separating out, after it is separated out because the crystalline adsorptive power is very strong, also in its surface adsorption a lot of yellow prussiate of potash, the phenomenon of the unit's of causing crystal yellow prussiate of potash too high levels takes place, and does not meet national standard.Therefore, how effectively to reduce the research topic that the content of yellow prussiate in finished product salt becomes current hot topic.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art and providing a kind of is the method for additive evaporation salt manufacturing with the yellow prussiate, the content of yellow prussiate is extremely low in the finished product salt that this method is prepared, and the content of the yellow prussiate in the first salt discharge is also lower.
In general, the crystallization of sodium-chlor is a very complicated process, singly do not need additive, and have a lot of parameters control crystalline to grow up, such as the concentration of slip in the amount of additive in the middle of the evaporative crystallization condition, evaporation capacity, the vaporizer, the pH value of bittern etc.Each condition all is the important factor that influences the branch salt formation.In the middle of these factors, it is generally acknowledged that the concentration of saturated solution when most importantly evaporating influences crystalline, still, up to now, do not see as yet this additive of yellow prussiate residual quantity in finished product salt is studied.
In contriver's research process, be surprised to find, the addition manner of this additive of yellow prussiate is to influence its residual quantity in finished product salt, analyses the major cause in the salt especially for the first time.
The object of the present invention is achieved like this:
A kind of preparation method of non-caking sodium chloride crystals is that yellow prussiate is made an addition in the saturated brine, and evaporating, concentrating and crystallizing forms, and wherein, yellow prussiate adds when the saturated brine crystallization begins.
Wherein, in order to guarantee to produce crystallization effect preferably, good conditions is to guarantee the content of yellow prussiate of potash in saturated brine in the 2mg/L-10mg/L scope, and the control solid-to-liquid ratio is in the 13-15% scope, and the pH value of saturated brine is in the 7-10 scope.
Principle of the present invention is: add yellow prussiate when the saturated brine crystallization after, owing to the yellow prussiate negatively charged ion has stronger adsorption at the salt crystal surface of growth, can suppress the generation of nucleus and sodium-chlor crystallization and the growth of size and shape, dissolved sodium-chlor presents hypersaturated state around an xln, just because of dissolved sodium-chlor is in hypersaturated state around xln, crystal edge crystal preferred growth, thereby satisfied the peculiar condition of branch salt crystal growth, how process of growth can be summarized, evaporative process initial crystallization shape remains cube structure, because the plane of crystal crystalline form is incomplete, the cubic salt crystal plane is evenly growth continuously, begin to suppress the growth of plane of crystal to critical volume (size) yellow prussiate ion, at this moment growth only occurs in crystalline edge and recessed teat branch usually, and the final crystallization of growth that edge and recessed teat divide forms branch or star structure.
The present invention has following advantage than prior art:
Because having adopted when saturated brine begins crystallization, the present invention adds additive, the crystalline form of the salt of separating out does not for the first time change as yet, just in its surface adsorption some yellow prussiate of potash, these yellow prussiates mainly form sealing coat between crystal, avoided the formation of salt bridge between the crystal, thereby the content of yellow prussiate in the salt of separating out is for the first time reduced greatly, for≤8mg/L; Simultaneously, analyse after the salt for the first time, the solid-to-liquid ratio of control feed liquid is at 13-15%, the content that keeps yellow prussiate in the crystallization phase feed liquid can be controlled yellow prussiate effectively and mainly participate in changing the sodium chloride crystal shape at 2mg/L-10mg/L, after branch or star structure are crystal formation, its surperficial adsorbed yellow prussiate of potash seldom, thereby effectively reduce the content of separating out the yellow prussiate in the salt subsequently, average out to 3mg/Kg meets the requirement of GB5461-2003 national standard.
Embodiment
Below in conjunction with drawings and Examples the present invention is further described:
Embodiment 1: will be through the purified saturated brine, adjusting its pH value is 7, add 3 liters of saturated brines in the forced crystallization device, evaporation capacity be 0.2 ton of water/hour, pressure-0.08MPa, evaporation feed temperature be evaporation concentration under 75 ℃ the condition, when saturated brine begins crystallization, in crystallizer, add the yellow prussiate of potash of 6mg and mix, continuously feeding, intermittently salt discharge, input speed is 400 milliliters/hour, solid-to-liquid ratio is 13% in the crystallization control device.The wet salt of discharging is concave surface and the star tree dendritic crystal that contains yellow prussiate of potash 3 mg/litre after dehalogenation, drip washing, oven dry, be finished product, the tap density of this finished product is 0.8 gram/cubic centimetre, dissolution rate is 2 times of common purified salt, the sticking water yield is 2 times of common purified salt, and the content of just analysing yellow prussiate of potash in the salt is 6 mg/litre.
Embodiment 2: will be through the purified saturated brine, adjusting its pH value is 10, add 3 liters of saturated brines in the forced crystallization device, evaporation capacity be 0.3 ton of water/hour, pressure-0.08MPa, evaporation feed temperature be evaporation concentration under 70 ℃ the condition, when saturated brine begins crystallization, in crystallizer, add the yellow prussiate of soda of 30mg and mix, continuously feeding, intermittently salt discharge, input speed is 450 milliliters/hour, solid-to-liquid ratio is 15% in the crystallization control device.The wet salt of discharging is concave surface and the star tree dendritic crystal that contains yellow prussiate of soda 6 mg/litre after dehalogenation, drip washing, oven dry, be finished product, the tap density of this finished product is 0.7 gram/cubic centimetre, dissolution rate is 2.5 times of common purified salt, the sticking water yield is 2.5 times of common purified salt, and the content of just analysing yellow prussiate of soda in the salt is 8 mg/litre.
Embodiment 3: will be through the purified saturated brine, adjusting its pH value is 8, add 3 liters of saturated brines in the forced crystallization device, evaporation capacity be 0.3 ton of water/hour, pressure-0.09MPa, evaporation feed temperature be to evaporate evaporation concentration under 75 ℃ the condition, when saturated brine begins crystallization, in crystallizer, add the yellow prussiate of potash of 15mg and mix, continuously feeding, intermittently salt discharge, input speed is 420 milliliters/hour, solid-to-liquid ratio is 14% in the crystallization control device.The wet salt of discharging is concave surface and the star tree dendritic crystal that contains yellow prussiate of potash 3 mg/litre after dehalogenation, drip washing, oven dry, be finished product, and the tap density of this finished product is 0.75 gram/cubic centimetre, and dissolution rate is 2 of a common purified salt.2 times, the sticking water yield is 2.2 times of common purified salt, and the content of just analysing yellow prussiate of potash in the salt is 5 mg/litre.
Claims (4)
1, a kind of preparation method of non-caking sodium chloride crystals is that yellow prussiate is made an addition in the saturated brine, and evaporating, concentrating and crystallizing forms, and it is characterized in that yellow prussiate adds when the saturated brine crystallization begins.
2,, it is characterized in that the content of yellow prussiate is 2mg/L-10mg/L in the saturated brine according to the method for claim 1.
3, according to the method for claim 1, the pH value that it is characterized in that saturated brine is 7-10.
4, according to the method for claim 1, the solid-to-liquid ratio of saturated brine is 13-15% when it is characterized in that evaporative crystallization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100489094A CN101289165B (en) | 2007-04-20 | 2007-04-20 | Method for preparing sodium chloride crystal without agglomeration |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100489094A CN101289165B (en) | 2007-04-20 | 2007-04-20 | Method for preparing sodium chloride crystal without agglomeration |
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| CN101289165A true CN101289165A (en) | 2008-10-22 |
| CN101289165B CN101289165B (en) | 2012-04-18 |
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| CN2007100489094A Expired - Fee Related CN101289165B (en) | 2007-04-20 | 2007-04-20 | Method for preparing sodium chloride crystal without agglomeration |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102099295A (en) * | 2009-06-02 | 2011-06-15 | 阿克佐诺贝尔化学国际公司 | Non-caking salt composition, preparation process and use thereof |
| CN104473125A (en) * | 2014-12-15 | 2015-04-01 | 自贡市轻工业设计研究院有限责任公司 | Application of sorbitol in dendritic salt preparation process |
| CN110357127A (en) * | 2019-06-28 | 2019-10-22 | 孝感广盐华源制盐有限公司 | A kind of anti-caking eats the production method of sodium chloride |
| CN112919501A (en) * | 2021-02-02 | 2021-06-08 | 浙江舟山远东海盐制品有限责任公司 | Production process of square cone type crystal salt |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2642335A (en) * | 1949-02-23 | 1953-06-16 | Ici Ltd | Production of three-dimensional dendritic sodium chloride crystals |
| CN1267020C (en) * | 2003-12-23 | 2006-08-02 | 国家海洋局天津海水淡化与综合利用研究所 | New process for preventing refinery salt from caking |
-
2007
- 2007-04-20 CN CN2007100489094A patent/CN101289165B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102099295A (en) * | 2009-06-02 | 2011-06-15 | 阿克佐诺贝尔化学国际公司 | Non-caking salt composition, preparation process and use thereof |
| CN104803398A (en) * | 2009-06-02 | 2015-07-29 | 阿克佐诺贝尔化学国际公司 | Non-caking salt composition, preparation process and use thereof |
| CN104803398B (en) * | 2009-06-02 | 2022-08-23 | 阿克佐诺贝尔化学国际公司 | Anti-caking salt composition, preparation method and application thereof |
| CN104473125A (en) * | 2014-12-15 | 2015-04-01 | 自贡市轻工业设计研究院有限责任公司 | Application of sorbitol in dendritic salt preparation process |
| CN110357127A (en) * | 2019-06-28 | 2019-10-22 | 孝感广盐华源制盐有限公司 | A kind of anti-caking eats the production method of sodium chloride |
| CN112919501A (en) * | 2021-02-02 | 2021-06-08 | 浙江舟山远东海盐制品有限责任公司 | Production process of square cone type crystal salt |
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| CN101289165B (en) | 2012-04-18 |
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