CN1279034A - Process for preparing edible refined salt from separated salt - Google Patents

Process for preparing edible refined salt from separated salt Download PDF

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Publication number
CN1279034A
CN1279034A CN00112390A CN00112390A CN1279034A CN 1279034 A CN1279034 A CN 1279034A CN 00112390 A CN00112390 A CN 00112390A CN 00112390 A CN00112390 A CN 00112390A CN 1279034 A CN1279034 A CN 1279034A
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China
Prior art keywords
reaction vessel
crystallizing field
mother liquor
salt
sodium chloride
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CN00112390A
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CN1134226C (en
Inventor
林浩宇
刘清山
陈庆
潘向东
王忠学
朱晓东
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Jiangsu Jinqiao Salt Industry Co Ltd
Lianyungang Design And Research Institute Of Ministry Of Chemical Industry
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Jiangsu Jinqiao Salt Industry Co Ltd
Lianyungang Design And Research Institute Of Ministry Of Chemical Industry
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Priority to CNB001123904A priority Critical patent/CN1134226C/en
Publication of CN1279034A publication Critical patent/CN1279034A/en
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Publication of CN1134226C publication Critical patent/CN1134226C/en
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Abstract

A Process for prepared refined edible salt from separated salt includes such steps as adding separated salt into crystallizing region of reactor at uniform speed, while adding aged halogen, bittern and mother liquid, stirring for crystallization reaction, overflowing mother liquid containing small-granularity crystals and other impurities from reactor, discharging the liquid containing big-granularity crystal of sodium chloride and removing mother liquid to obtain solid sodium chloride, which has 0.15-0.25 mm of average granularity and 98.5-99.5% of purity.

Description

Utilize the method for the edible purified salt of separated salt preparation
The present invention relates to a kind of method of recycling separated salt.
In the prior art, separated salt is the waste products of high temp. salt behind high temperature removal sal epsom that chemical enterprises is produced, and its component is NaCl 60-75%, MgSO 44.5 MgCl-14%, 23.2 KCl 0.4-0.7%-4.3%.The method of recycling separated salt is, utilizes sodium-chlor and the difference of other impurity at aspects such as granularity, proportions in the separated salt, adopts swirler to carry out simple physics separation, recovery part sodium-chlor.Its existing problems are: because less in the difference of aspects such as granularity, proportion at sodium-chlor and other impurity, so separating effect is relatively poor, gained article granularity is little, and can not reach edible purified salt standard through washing and starching drying, and the rate of recovery is very low, cost recovery is high.So it is minimum that separated salt is recycled value in the prior art, belongs to waste basically.
The present invention is directed to the prior art deficiency, propose one and utilize separated salt to produce the method for edible purified salt.
Task of the present invention is achieved in that the present invention is a kind of method with the edible purified salt of separated salt preparation, be characterized in volumometer by the reaction vessel crystallizing field, with every cubic metre of volume per hour 3-60 kilograms feed rate at the uniform velocity add separated salt to the crystallizing field of reaction vessel, simultaneously with every cubic metre of volume per hour 0.1-1 cubic metre feed rate at the uniform velocity add old halogen to the crystallizing field of reaction vessel, simultaneously by 2-4 times of old halogen volume add-on, at the uniform velocity adding sodium chloride content to the crystallizing field of reaction vessel is 4-9% bittern, simultaneously by 3-15 times of old halogen volume add-on, at the uniform velocity the crystallizing field to reaction vessel adds circulating 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 and other impurity, upwards overflow reaction vessel from the periphery of crystallizing field, the mother liquor that overflows, after clarifying, use as circulating mother liquor, 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, the sodium chloride crystal of solid phase will be obtained, through washing and starching drying, obtain edible purified salt.
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, with sodium-chlor contained in the mixing salt is crystalline seed, its sodium-chlor xln is grown up, make the sodium-chlor crystallization velocity controlled, help making sodium chloride crystal to be grown up; 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.By sodium chloride crystal in the separated salt is crystal seed, and the big particle diameter sodium chloride crystal of growing up in converting the halogen reaction overcomes fluidic to upthrust under action of gravity, accumulate in the slip of reaction vessel crystallizing field below.This part slip is emitted from the reaction vessel lower part outlet, again it is sloughed mother liquor, can obtain the crystal median size and be 0.15-0.3 millimeter, purity is 90-95% sodium-chlor.Utilize the difference of particle diameter, realize effectively separating of sodium-chlor and other materials in the mixing salt.And convert less crystal and other impurity of part particle diameter in the halogen reaction, upwards overflow by the periphery of crystallizing field with mother liquor.Converting halogen process adding circulating mother liquor, can reduce the degree of supersaturation of reaction vessel crystallizing field first, moreover can regulate the upwards upflow velocity of overflow mother liquor.To have guaranteed to overflow the granularity of crystal grain, big particle diameter crystal is sunk, thin brilliant being overflowed of small particle size.
Purpose of the present invention can also further reach by following scheme.The method of the edible purified salt of aforesaid preparation, 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 10-25%, 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 following scheme.The method of the edible purified salt of aforesaid preparation is characterized in that the overflow mother liquor through settlement separate, obtains fine crystals, returns the substitute of making sal amarum in the bittern chemical technology.Help the recovery of other useful composition in the separated salt.
The present invention compared with prior art adopts method of the present invention to recycle the edible purified salt of separated salt preparation, and it is low that the closed circuit rate of recovery has improved 3-5 times, cost recovery.Make separated salt recycle and be worth and increase.Its product median size reaches 0.15-0.25 millimeter, and purity can reach 98.5-99.5%.Reached the standard of edible purified salt, and mouthfeel is better than common edible purified salt, simultaneously, helps the recovery of other useful composition in the separated salt, three-waste free discharge.
Fig. 1 is a technological process block-diagram of the present invention.
Fig. 2 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. 2, the method with the edible purified salt of separated salt preparation of present embodiment, the volume of reaction vessel crystallizing field (3) is 3.3 cubic metres, at the uniform velocity add sodium chloride content in 75% separated salt with 200 kilograms feed rate per hour to the crystallizing field (3) of reaction vessel, simultaneously at the uniform velocity add old halogen to the crystallizing field (3) of reaction vessel with 3.3 cubic metres feed rate per hour, 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 3 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, 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 (5) from the periphery (4) of crystallizing field (3), the mother liquor that overflows, after clarifying, use as circulating mother liquor, when the solid-liquid weight ratio that contains greater particle size sodium chloride crystal (6) slip when the reaction vessel bottom reaches 25%, its lower part outlet from reaction vessel (7) is emitted, slough the sodium chloride crystal that mother liquor obtains, through washing and starching drying, obtaining purity is 98.5%, median size is 0.16 edible purified salt.
Embodiment two.The following examples continue to describe summary of the invention of the present invention, see Fig. 1, Fig. 2, the method with the edible purified salt of separated salt preparation of present embodiment, the volume of reaction vessel (5) crystallizing field (3) is 4 cubic metres, per hour 100 kilograms feed rate at the uniform velocity adds sodium chloride content in 70% separated salt to the crystallizing field (3) of reaction vessel, per hour 2.5 cubic metres feed rate at the uniform velocity adds old halogen to the crystallizing field (3) of reaction vessel simultaneously, 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 is 6.7% bittern, simultaneously by 5 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, 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, the mother liquor that overflows, after clarifying, use as circulating mother liquor, when the solid-liquid weight ratio that contains greater particle size sodium chloride crystal (6) slip when the reaction vessel bottom reaches 20%, its lower part outlet from reaction vessel (7) is emitted, slough mother liquor, the solid-phase chlorination sodium crystal that obtains is through washing and starching drying, and obtaining purity is 99.3%, median size is 0.18 the edible purified salt of top grade.
Embodiment three.The following examples continue to describe summary of the invention of the present invention, see Fig. 1, Fig. 2, the method with the edible purified salt of separated salt preparation of present embodiment, the volume of reaction vessel (5) crystallizing field (3) is 2 cubic metres, at the uniform velocity add sodium chloride content in 60% separated salt with 6 kilograms feed rate per hour to the crystallizing field (3) of reaction vessel, per hour 0.2 cubic metre feed rate at the uniform velocity adds old halogen to the crystallizing field (3) of reaction vessel simultaneously, 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, simultaneously by 15 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, 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, the mother liquor that overflows, after clarifying, use as circulating mother liquor, when the solid-liquid weight ratio that contains greater particle size sodium chloride crystal (6) slip when the reaction vessel bottom reaches 10%, its lower part outlet from reaction vessel (7) is emitted, slough mother liquor, the solid-phase chlorination sodium crystal that obtains is through washing and starching drying, and obtaining purity is 99.5%, median size is 0.19 the edible purified salt of top grade.
Embodiment four.The following examples continue to describe summary of the invention of the present invention, and in the above-described embodiments, the overflow mother liquor obtains fine crystals through settlement separate, returns the substitute of making sal amarum in the bittern chemical technology.

Claims (3)

1, a kind of method with the edible purified salt of separated salt preparation, it is characterized in that volumometer by reaction vessel (5) crystallizing field (3), with every cubic metre of volume per hour 3-60 kilograms feed rate at the uniform velocity add separated salt to the crystallizing field (3) of reaction vessel, simultaneously with every cubic metre of volume per hour 0.1-1 cubic metre feed rate at the uniform velocity add old halogen to the crystallizing field (3) of reaction vessel, simultaneously by 2-4 times of old halogen volume add-on, at the uniform velocity adding sodium chloride content to the crystallizing field (3) of reaction vessel is 4-9% bittern, simultaneously by 3-15 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, 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), the mother liquor that overflows, after clarifying, use as circulating mother liquor, 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 crystallizing field (3) below, slough mother liquor, the sodium chloride crystal of solid phase will be obtained, through washing and starching drying, obtain edible purified salt.
2, the method for the edible purified salt of preparation 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 10-25%, will emit its lower part outlet (7) again from reaction vessel.
3, the method for the edible purified salt of preparation according to claim 1 is characterized in that the overflow mother liquor through settlement separate, obtains fine crystals, returns the substitute of making sal amarum in the bittern chemical technology.
CNB001123904A 2000-07-10 2000-07-10 Process for preparing edible refined salt from separated salt Expired - Fee Related CN1134226C (en)

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CN1134226C CN1134226C (en) 2004-01-14

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Cited By (3)

* Cited by examiner, † Cited by third party
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
CN104743579A (en) * 2015-03-06 2015-07-01 华东理工大学 Method for salting out and recycling sodium chloride in magnesium hydroxide production process

Cited By (3)

* Cited by examiner, † Cited by third party
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
CN104743579A (en) * 2015-03-06 2015-07-01 华东理工大学 Method for salting out and recycling sodium chloride in magnesium hydroxide production process

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