CN1333182A - Process for preparing sodium chloride from old bittern and bitter bittern - Google Patents
Process for preparing sodium chloride from old bittern and bitter bittern Download PDFInfo
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- CN1333182A CN1333182A CN 00112389 CN00112389A CN1333182A CN 1333182 A CN1333182 A CN 1333182A CN 00112389 CN00112389 CN 00112389 CN 00112389 A CN00112389 A CN 00112389A CN 1333182 A CN1333182 A CN 1333182A
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Abstract
The preparation method of sodium chloride by old bittern and bitter bittern is characterized by that according to the volume of crystallizing zone of reaction container defining charging speed, adding old bittern into crystallizing zone of reaction container, at the same time adding bitter bittern whose added quantity is 2-4 times that of old bittern, fully mixing and continuously stirring to make reaction, so that the mother liquor containing partial crystal with smaller grain size and other impurity is overflowed from reaction container, and the slurry containing sodium chloride crystal with larger grain size is discharged from lower outlet of the reaction container, then the mother liquor is removed so as to obtain sodium chloride crystal whose purity is up to 90-95%, its average grain size is 0.15-0.3 mm, and the directly-obtained crude salt is undergone the processes of washing and drying, its purity can be up to 98.5-99.5%.
Description
The present invention relates to a kind of method for preparing sodium-chlor, particularly utilize old halogen and bittern to convert the method that stew in soy sauce is equipped with sodium-chlor.
In the prior art, the method for utilizing old halogen and bittern to extract sodium-chlor is, is that the bittern of 4-9% is converted and closed with old halogen and sodium chloride content, carry out simple agitation, allow its solid particulate separate out naturally, again the solid of separating out is separated, obtain the sal amarum that sodium chloride content has only 70-80%.Its existing problems are: the sodium-chlor granularity that adopts this method to extract is little, and median size is less than 0.1 millimeter, and impurity is many, can not directly use as technical grade sodium-chlor.More anorexia is used.
The present invention is directed to the prior art deficiency, propose the method that a kind of brand-new utilization control reaction conditions prepares high purity chlorination sodium.
Task of the present invention is achieved in that the present invention is that a kind of old halogen and bittern of utilizing converted the method that stew in soy sauce is equipped with sodium-chlor, be characterized in volumometer by the reaction vessel crystallizing field, with every cubic metre of volume per hour the feed rate of 0.1-1 cubic meter at the uniform velocity add old halogen to the crystallizing field of reaction vessel, simultaneously doubly by the 2-4 of old halogen volume add-on, at the uniform velocity the crystallizing field adding sodium chloride content to reaction vessel is the bittern of 4-9%, and carry out the complete mixing flow continuously stirring, convert the halogen crystallization reaction, allow and contain the mother liquor of part particle diameter than small-crystalline and other impurity, upwards overflow reaction vessel from the periphery of crystallizing field, the slip that contains the greater particle size sodium chloride crystal below the reaction vessel crystallizing field is emitted from the lower part outlet of reaction vessel, slough mother liquor, obtain the sodium chloride crystal of solid phase.
The supersaturation that sodium-chlor in the halogen process is converted in utilization of the present invention is crystallization power, by control the input speed and the ratio of raw material in the volume of reaction vessel, the crystallization reaction of converting sodium-chlor in the halogen process is carried out in the crystallizing field of reaction vessel, make the sodium-chlor crystallization velocity controlled, help making sodium chloride crystal to be grown up; Simultaneously, complete mixing flow stirs and can prevent that the local degree of supersaturation of generation is excessive in the crystallizing field, reduces the generation of a large amount of sodium-chlor nucleus, also impels the sodium-chlor grain growth; And rise by the overflow mother liquor and to take away thin crystalline substance of part sodium-chlor and impurity, also help the sodium chloride crystal purification of growing up.The sodium chloride crystal that the granularity that crystallization goes out is bigger under action of gravity, overcomes fluidic to upthrust, accumulates in the slip of reaction vessel crystallizing field below.This part slip is emitted from reaction container bottom, isolate mother liquor, can obtain the crystal median size is the 0.15-0.3 millimeter, and purity is the sodium-chlor of 90-95%.
Purpose of the present invention can also further reach by the following method.The aforesaid method for preparing sodium-chlor, be characterized at the slip that contains the greater particle size sodium chloride crystal that will be below the reaction vessel crystallizing field from the process that the lower part outlet of reaction vessel is emitted, when the solid-liquid weight ratio of being easy to act as reaction vessel bottom slip most reaches 15-35%, again it is emitted from the lower part outlet of reaction vessel.Like this, the material of participating in reaction is had in the reaction vessel crystallizing field and more reasonably stop reaction times and reaction density.
Purpose of the present invention can also further reach by the following method.The aforesaid method for preparing sodium-chlor is characterized in being the upflow velocity of the mother liquor that upwards overflows, is by adjusting the make progress sectional area of overflow channel of reaction vessel crystallizing field periphery, and the upflow velocity that makes the mother liquor that upwards overflows is 2-8 rice per hour.The mother liquor that upwards overflows is controlled at the granularity that such upflow velocity has guaranteed to overflow crystal grain, guarantees to make big particle diameter crystal to sink, thin brilliant being overflowed of small particle size.
Purpose of the present invention can also further reach by the following method.The aforesaid method for preparing sodium-chlor, be characterized in overflowing or slip in isolating mother liquor, after clarifying, by the 1-15 of old halogen volume add-on doubly, at the uniform velocity add the crystallizing field of reaction vessel simultaneously with old halogen, in converting the halogen process, recycle.Converting halogen process adding circulating mother liquor, can reduce the degree of supersaturation of reaction vessel crystallizing field first, moreover can regulate the upflow velocity of overflow mother liquor.
Purpose of the present invention can also further reach by the following method.The aforesaid method for preparing sodium-chlor, when being characterized in converting the halogen crystallization reaction, press the volumometer of reaction vessel crystallizing field, with every cubic metre of volume per hour the feed rate of 0-100 kilogram at the uniform velocity add the mixing salt of the identical sodium chloride content of the ion composition that comprises with bittern to the crystallizing field of reaction vessel at 60-90%.Like this, utilizing and to convert the sodium-chlor supersaturation that is produced in the halogen process and be crystallization power, is crystalline seed with sodium-chlor contained in the mixing salt, makes its crystal growth, utilizes the difference of particle diameter again, realizes effectively separating of sodium-chlor and other materials in the mixing salt.Simultaneously, also promoted to convert crystallisation process in the halogen reaction.
Purpose of the present invention can also further reach by the following method.The aforesaid method for preparing sodium-chlor is characterized in through washing and starching drying, obtaining high grade sodium chloride with obtaining the sodium chloride crystal of solid phase.Like this, can improve its purity.
The present invention compared with prior art, it is big that the sodium-chlor that adopts the inventive method to prepare has grain size number, characteristics such as product purity height, and its median size reaches 0.15---and 0.3 millimeter, the crude salt purity of direct filtration just reaches 90-95%, and product purity after washing and starching drying can reach 98.5-99.5%.Can not only directly use as technical grade sodium-chlor.Also reached food sanitation standard.
Fig. 1 is a process flow sheet of the present invention.
Fig. 2 is the another kind of scheme schema of the present invention.
Fig. 3 is the structural representation of reaction vessel of the present invention.
The following examples have further described summary of the invention of the present invention according to accompanying drawing.
Embodiment one.See Fig. 1, Fig. 3, old halogen of the utilization of present embodiment and bittern are converted in the method that stew in soy sauce is equipped with sodium-chlor, the volume of reaction vessel crystallizing field (3) is 3 cubic metres, at the uniform velocity add old halogen with 3 cubic metres feed rate per hour to the crystallizing field (3) of reaction vessel, simultaneously by 3 times of old halogen volume add-on, at the uniform velocity adding sodium chloride content to the crystallizing field (3) of reaction vessel (5) is 7% bittern, and carry out the complete mixing flow continuously stirring, convert the halogen crystallization reaction, the make progress sectional area of overflow channel (4) of reaction vessel crystallizing field (3) periphery is designed to 1.6 square metres, make the upflow velocity of the mother liquor that upwards overflows be per hour 7.5 meters, allow and contain the mother liquor of part particle diameter than small-crystalline (2) and other impurity, upwards overflow the overflow port (1) of reaction vessel from the periphery of crystallizing field (3), when the solid-liquid weight ratio of the slip that contains greater particle size sodium chloride crystal (6) below the reaction vessel crystallizing field (3) reaches 15%, will emit its lower part outlet (7) from reaction vessel.Slough mother liquor, obtain purity and be 95%, median size is the sodium chloride crystal of 0.3 millimeter solid phase.
Embodiment two.See Fig. 1, Fig. 3, the following examples continue to describe summary of the invention of the present invention, old halogen of the utilization of present embodiment and bittern are converted in the method that stew in soy sauce is equipped with sodium-chlor, the volume of reaction vessel (5) crystallizing field (3) is 2 cubic metres, at the uniform velocity add old halogen with 0.2 cubic metre feed rate per hour to the crystallizing field (3) of reaction vessel, simultaneously by 2 times of old halogen volume add-on, at the uniform velocity adding sodium chloride content to the crystallizing field (3) of reaction vessel is 9% bittern, and carry out the complete mixing flow continuously stirring, convert the halogen crystallization reaction, the make progress sectional area of overflow channel (4) of reaction vessel crystallizing field (3) periphery is designed to 1.2 square metres, makes the upflow velocity of the mother liquor that upwards overflows be per hour 0.5 meter.Allow and contain the mother liquor of part particle diameter than small-crystalline (2) and other impurity, upwards overflow the overflow port (1) of reaction vessel from the periphery of crystallizing field, when the solid-liquid weight ratio of the slip that contains greater particle size sodium chloride crystal (6) below the reaction vessel crystallizing field (3) reaches 13%, will emit its lower part outlet (7) from reaction vessel.Slough mother liquor, the purity that obtains solid phase is 94% sodium-chlor.To obtain the sodium chloride crystal of solid phase, through washing and starching drying, obtaining particle diameter is 0.2 millimeter, and purity is 99.5% sodium-chlor.
Embodiment three.See Fig. 1, Fig. 3, the following examples continue to describe summary of the invention of the present invention.Old halogen of the utilization of present embodiment and bittern are converted in the method that stew in soy sauce is equipped with sodium-chlor, the volume of reaction vessel (5) crystallizing field (3) is 4 cubic metres, at the uniform velocity add old halogen with 4 cubic metres feed rate per hour to the crystallizing field (3) of reaction vessel, simultaneously by 4 times of old halogen volume add-on, at the uniform velocity adding sodium chloride content to the crystallizing field (3) of reaction vessel is 4% bittern, simultaneously, by 1 times of old halogen volume add-on, at the uniform velocity the crystallizing field (3) to reaction vessel adds circulating mother liquor, and carry out the complete mixing flow continuously stirring, convert the halogen crystallization reaction, the make progress sectional area of overflow channel (4) of reaction vessel crystallizing field (3) periphery is designed to 2.7 square metres, make the upflow velocity of the mother liquor that upwards overflows be per hour 9 meters, allow and contain the mother liquor of part particle diameter than small-crystalline (2) and other impurity, upwards overflow the overflow port (1) of reaction vessel from the periphery of crystallizing field (3), the mother liquor that overflows recycles in converting the halogen process after clarifying.When the solid-liquid weight ratio of the slip that contains greater particle size sodium chloride crystal (6) below the reaction vessel crystallizing field (3) reaches 38%, will emit its lower part outlet (7) from reaction vessel.Slough mother liquor, obtain the sodium chloride crystal of solid phase.Obtain purity and be the sodium chloride crystal of 94.50% solid phase, through washing and starching drying, obtaining particle diameter is 0.2 millimeter, and purity is 99.4% sodium-chlor.
Embodiment four.See Fig. 2, Fig. 3, the following examples continue to describe summary of the invention of the present invention, old halogen of the utilization of present embodiment and bittern are converted in the method that stew in soy sauce is equipped with sodium-chlor, the volume of reaction vessel (5) crystallizing field (3) is 3 cubic metres, at the uniform velocity add old halogen with 2 cubic metres feed rate per hour to the crystallizing field of reaction vessel, at the uniform velocity adding sodium chloride content to the crystallizing field (3) of reaction vessel by 3 times of old halogen volume add-on simultaneously is 7% bittern, at the uniform velocity add circulating mother liquor by 2 times of old halogen volume add-on simultaneously to the crystallizing field of reaction vessel, make the upflow velocity of the mother liquor that upwards overflows be per hour 6 meters, simultaneously, at the uniform velocity add sodium chloride content 60% with 60 kilograms feed rate per hour to the crystallizing field of reaction vessel, sal epsom content is 13%, content of magnesium chloride is 5%, KCE content is in 0.3% the settlement separate fine crystals that goes out from the overflow mother liquor, and carry out the complete mixing flow continuously stirring, convert the halogen crystallization reaction, allow and contain the mother liquor of part particle diameter than small-crystalline (2) and other impurity, upwards overflow the overflow port (1) of reaction vessel from the periphery of crystallizing field, the mother liquor that overflows recycles after clarification.When the solid-liquid weight ratio of the slip that contains greater particle size sodium chloride crystal (6) below the reaction vessel crystallizing field reaches 25%, will emit its lower part outlet (7) from reaction vessel.Slough mother liquor, the purity that obtains solid phase is 93.5% solid-phase chlorination sodium crystal, and through washing and starching drying, obtaining median size is 0.18 millimeter, and purity is 99.3% sodium-chlor.
Embodiment five.See Fig. 2, Fig. 3, the following examples continue to describe summary of the invention of the present invention.Old halogen of the utilization of present embodiment and bittern are converted in the method that stew in soy sauce is equipped with sodium-chlor, the volume of reaction vessel (5) crystallizing field is 3 cubic metres, at the uniform velocity add old halogen with 2 cubic metres feed rate per hour to the crystallizing field (3) of reaction vessel, simultaneously by 3 times of old halogen volume add-on, at the uniform velocity adding sodium chloride content to the crystallizing field of reaction vessel is 6.8% bittern, simultaneously, by 2.5 times of old halogen volume add-on, at the uniform velocity, make the upflow velocity of the mother liquor that upwards overflows be per hour 7.5 meters to the circulating mother liquor of crystallizing field adding after clarification of reaction vessel.Simultaneously, with per hour 150 kilograms feed rate to the crystallizing field of reaction vessel at the uniform velocity add sodium chloride content 75%, sal epsom content 0.3%, content of magnesium chloride 2%, KCE content is at 12% the tail salt that produces with producing potassium chloride from carnallite.And carry out the complete mixing flow continuously stirring, and convert the halogen crystallization reaction, allow and contain the mother liquor of part particle diameter than small-crystalline (2) and other impurity, upwards overflow the overflow port (1) of reaction vessel from the periphery of crystallizing field, the mother liquor that overflows is made circulating mother liquor and is used after clarification.When the solid-liquid weight ratio of the slip that contains greater particle size sodium chloride crystal (6) below the reaction vessel crystallizing field reaches 25%, its lower part outlet from reaction vessel (7) is emitted, obtain purity and be 93% solid-phase chlorination sodium crystal, through washing and starching drying, obtaining median size is 0.15 millimeter, and purity is 98.5% sodium-chlor.
Embodiment six.See Fig. 2, Fig. 3, the following examples continue to describe summary of the invention of the present invention, old halogen of the utilization of present embodiment and bittern are converted in the method that stew in soy sauce is equipped with sodium-chlor, the volume of reaction vessel (5) crystallizing field (3) is 5 cubic metres, at the uniform velocity add old halogen with 1 cubic metre feed rate per hour to the crystallizing field of reaction vessel, simultaneously by 2 times of old halogen volume add-on, at the uniform velocity adding sodium chloride content to the crystallizing field of reaction vessel is 8.5% bittern, simultaneously, by 15 times of old halogen volume add-on, crystallizing field (3) to reaction vessel at the uniform velocity adds circulating mother liquor, in converting the halogen process, make the upflow velocity of the mother liquor that upwards overflows be per hour 6 meters, simultaneously, at the uniform velocity add sodium chloride content 90% with 500 kilograms feed rate per hour to the crystallizing field of reaction vessel, vitriolate of tartar content is 0.5%, KCE content is produced the by-product salt of vitriolate of tartar at 1.3% mirabilite method, and carry out the complete mixing flow continuously stirring, convert the halogen crystallization reaction, allow and contain the mother liquor of part particle diameter than small-crystalline (2) and other impurity, upwards overflow the overflow port (1) of reaction vessel from the periphery of crystallizing field, when the solid-liquid weight ratio of the slip that contains greater particle size sodium chloride crystal (6) below the reaction vessel crystallizing field reaches 35%, to emit its lower part outlet (7) from reaction vessel, slough mother liquor, isolating mother liquor recycles after clarification with the mother liquor that overflows in the slip.Obtain purity and be 95% solid-phase chlorination sodium crystal, through washing and starching drying, obtain median size 0.14 and be millimeter, purity is 99.3% sodium-chlor.
Claims (6)
1, a kind of old halogen and bittern of utilizing converted the method that stew in soy sauce is equipped with sodium-chlor, it is characterized in that volumometer by reaction vessel (5) crystallizing field (3), with every cubic metre of volume per hour the crystallizing field (3) of feed rate to reaction vessel (5) of 0.1-1 cubic meter at the uniform velocity add old halogen, simultaneously doubly by the 2-4 of old halogen volume add-on, at the uniform velocity crystallizing field (3) the adding sodium chloride content to reaction vessel (5) is the bittern of 4-9%, and carry out the complete mixing flow continuously stirring, convert the halogen crystallization reaction, allow and contain the mother liquor of part particle diameter than small-crystalline (2) and other impurity, upwards overflow reaction vessel (5) from the periphery (4) of crystallizing field (3), to emit from the lower part outlet (7) of reaction vessel at the slip that contains greater particle size sodium chloride crystal (6) of reaction vessel (5) crystallizing field (3) below, slough mother liquor, obtain the sodium chloride crystal of solid phase.
2, the method for preparing sodium-chlor according to claim 1, it is characterized in that will be from the process that the lower part outlet (7) of reaction vessel is emitted at the slip that contains greater particle size sodium chloride crystal (6) of reaction vessel (5) crystallizing field (3) below, when the solid-liquid weight ratio of being easy to act as reaction vessel bottom slip most reaches 15-35%, will emit its lower part outlet (7) again from reaction vessel.
3, the method for preparing sodium-chlor according to claim 1, the upflow velocity that it is characterized in that the mother liquor that upwards overflows, be by adjusting the make progress sectional area of overflow channel (4) of reaction vessel crystallizing field periphery, the upflow velocity that makes the mother liquor that upwards overflows is 2-8 rice per hour.
4, the method for preparing sodium-chlor according to claim 1, it is characterized in that overflowing or slip in isolating mother liquor, after clarifying, by the 1-15 of old halogen volume add-on doubly, at the uniform velocity add the crystallizing field of reaction vessel simultaneously, in converting the halogen process, recycle with old halogen.
5, according to claim 1 and the 4 described methods that prepare sodium-chlor, when it is characterized in that converting the halogen crystallization reaction, press the volumometer of reaction vessel crystallizing field, with every cubic metre of volume per hour the feed rate of 0-100 kilogram at the uniform velocity add the mixing salt of the identical sodium chloride content of the ion composition that comprises with bittern to the crystallizing field of reaction vessel at 60-90%.
6, the method for preparing sodium-chlor according to claim 1 is characterized in that through washing and starching drying, obtaining high grade sodium chloride with obtaining the sodium chloride crystal of solid phase.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001123890A CN1163411C (en) | 2000-07-10 | 2000-07-10 | Process for preparing sodium chloride from old bittern and bitter bittern |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB001123890A CN1163411C (en) | 2000-07-10 | 2000-07-10 | Process for preparing sodium chloride from old bittern and bitter bittern |
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| CN1333182A true CN1333182A (en) | 2002-01-30 |
| CN1163411C CN1163411C (en) | 2004-08-25 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100402426C (en) * | 2006-07-12 | 2008-07-16 | 中蓝连海设计研究院 | Process of preparing refined salt with sodium-containing bittern |
| CN103496719A (en) * | 2013-09-18 | 2014-01-08 | 天津长芦汉沽盐场有限责任公司 | Method for improving granularity and purity of chemical salt byproducts of acrid bittern |
| CN110204127A (en) * | 2019-07-09 | 2019-09-06 | 北京能为科技股份有限公司 | A kind of outside crystal seed method inhibits the system and its orientation scaling method of calcium salt scale |
-
2000
- 2000-07-10 CN CNB001123890A patent/CN1163411C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100402426C (en) * | 2006-07-12 | 2008-07-16 | 中蓝连海设计研究院 | Process of preparing refined salt with sodium-containing bittern |
| CN103496719A (en) * | 2013-09-18 | 2014-01-08 | 天津长芦汉沽盐场有限责任公司 | Method for improving granularity and purity of chemical salt byproducts of acrid bittern |
| CN110204127A (en) * | 2019-07-09 | 2019-09-06 | 北京能为科技股份有限公司 | A kind of outside crystal seed method inhibits the system and its orientation scaling method of calcium salt scale |
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| Publication number | Publication date |
|---|---|
| CN1163411C (en) | 2004-08-25 |
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