CN103738980A - Method for preparing high-purity water salt and serial products by using well and rock salt raw material brine - Google Patents
Method for preparing high-purity water salt and serial products by using well and rock salt raw material brine Download PDFInfo
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Abstract
The invention relates to a method for preparing high-purity water salt and serial products by using well and rock salt raw material brine; the high-purity water salt serial products comprise: pharmacopoeia-grade medicinal raw material high-purity water salt, medicinal raw material salt, sub-pharmacopoeia-grade green nutrient and health-care high-purity water salt with organic and inorganic nutrient elements, sub-pharmacopoeia-grade edible high-purity water salt, and sub-pharmacopoeia-grade edible high-purity water salt. The pharmacopoeia-grade medicinal raw material high-purity water salt product is liquid, and can be diluted with deionized water to produce medicinal sodium chloride preparations or normal saline; it is not necessary to produce solid medicinal raw material salt by traditional brine purification, evaporation and crystallization processes, or to produce medicinal sodium chloride preparations or normal saline by diluting medicinal raw material salt with water. The method of the invention adopts ceramic membrane filtration and nanofiltration membrane processing, is low in comprehensive energy consumption, can save a lot of energy, reduce equipment investment and land occupation, reduce production cost to the maximum extent, and is free of salt dust, environmental pollution or corrosion in the production process.
Description
Technical field
The present invention relates to well mine salt raw brine without evaporation production pharmacopeia level high purity water salt series product and preparation method.High purity water salt series product comprise: pharmacopeia level medicinal raw material high purity water salt, medicinal raw material salt, sub-pharmacopeia level add N green nourishing health care high purity water salt (N is organic and inorganic nutritive element), sub-pharmacopeia level for meal high purity water salt (alternative solid edible salt), sub-pharmacopeia level eat with adding iodine high purity water salt.In addition, the solid salt (not dry salt) that utilizes evaporative crystallization technique to produce adds high purity water, through membrane filtration, also can produce high purity water series product.
Background technology
Utilize well mine salt raw brine without evaporation production pharmacopeia level high purity water salt series product and preparation method, now domesticly there is no this type of products production and production method, and well mine salt bittern produces through bittern purifying, vacuum-evaporation the production method that medicinal raw material salt, solid edible Yan Wei domestic production enterprise generally adopt.
One, medicinal raw material salt (medicinal sodium chloride) product and production technology
Medicinal sodium chloride product: be colourless, transparent cube crystallization or white crystallinity powder; Odorless; Taste is salty.This product is easily molten in water, almost insoluble in ethanol.The aobvious sodium salt of the aqueous solution and the muriatic identification of this product.Meet Chinese Pharmacopoeia standard in 2010.
Medicinal raw material salt (medicinal sodium chloride) quality standard is as table 1.
Table 1 medicinal raw material salt quality standard
| Index name | Index |
| Content (NaCl) >= | 99.5% |
| Potential of hydrogen test | Qualified |
| Clarity test | Qualified |
| Iodide test | Qualified |
| Bromide test | Qualified |
| Vitriol (SO4)≤ | 0.002% |
| Barium salt test | Qualified |
| Calcium salt test | Qualified |
| Magnesium (Mg)≤ | 0.001% |
| Potassium (K)≤ | 0.02% |
| Weight loss on drying≤ | 0.50% |
| Iron (Fe)≤ | 0.0003% |
| Heavy metal≤ | 0.00002% |
| Arsenic salt≤ | 0.00004% |
Medicinal sodium chloride production technology:
In well mine salt district, the production technology of medicinal raw material salt generally comprises: mining area gathers former halogen, former halogen purifying treatment, vacuum evaporating crystalization, solventing-out (or getting rid of mother liquor except nitre), dehydration, with secondary steam water of condensation dissolved salt, vacuum-evaporation recrystallize salt, washing, purifying, dehydrate screening, finished product packing production process.Washing, purifying, dehydrate screening, finished product packing and finished stock storage production link and must in meeting the clean room of GMP authentication, carry out.This production technique exists some shortcomings: processing unit is many, operating process is long; Former halogen consumption is large, and energy consumption is high, and production cost is high.Its concrete technology technology is as follows:
(1) rock salt mining area gathers former halogen: fresh water (or saliferous process water) high pressure injects the molten chamber of a bite salt well, and rock salt dissolving, for the bittern containing NaCl, is returned out to former bittern from another mouthful of well.Conventionally in production operation, the Contents of Main Components of former bittern is NaCl>=290g/l, SO
4 2-≤ 15g/l, Ca
2+≤ 1g/l, Mg
2+≤ 1g/l.This technological process has certain cleaning action to the suspended substance in fresh water.
(2) former halogen purifying treatment (calcium-magnesium removing): this technique has three kinds of chemical treatment methods, caustic soda-Method of Soda, lime-soda method, lime-soda ash-carbon dioxide process at present.In the place that has CO_2 Resource, generally adopt lime-soda ash-carbon dioxide process, this processing method cost minimum (22 yuan/ton of salt of caustic soda-Method of Soda, 23.5 yuan/ton of salt of lime-soda method, 13 yuan/ton of salt of lime-soda ash-carbon dioxide process).Three kinds of methods can be used indirect production and continuous production processes.Brine composition after purification is NaCl>=290g/l, SO
4 2-≤ 12g/l, Ca
2+≤ 9mg/l, Mg
2+≤ 1mg/l.In Salt Production, conventionally claim that the bittern after deliming coal is smart halogen.Essence halogen enters vacuum-evaporator unit precipitated sodium chloride crystal.
(3) vacuum evaporating crystalization: vacuum vaporation system is generally four (or five) effect evaporating pot and forms, and every effect evaporating pot carries one or more heating chambers.The steam coming from boiler is passed into heating evaporation essence halogen in I effect heating chamber, I effect evaporator room produce secondary steam and the flash steam of I effect shwoot bucket together with enter into II effect heating chamber, the water of condensation of II effect heating chamber enters II effect balance bucket, steam in balance bucket turns back to the steam inlet of II effect heating chamber, water of condensation enters II effect shwoot bucket, and II effect shwoot bucket is exactly the balance bucket of III effect; The secondary steam that II effect evaporator room produces enters III effect heating chamber, and the water of condensation of III effect heating chamber enters the balance bucket of III effect, and the flash steam producing in the balance bucket of III effect turns back to III effect heating chamber, and water of condensation enters IV effect balance bucket; The secondary steam that III effect evaporator room produces enters IV effect heating chamber, and the secondary steam that IV effect balance bucket produces enters IV effect heating chamber; IV effect water of condensation enters preheater heating low temperature essence halogen, the secondary steam that IV effect evaporator room produces enters mixing condenser, recirculated cooling water enters the secondary steam in mixing condenser cooling mixing condenser simultaneously, and the not condensing in mixing condenser is extracted out by vacuum ejector, forms system vacuum.In evaporation unit, the salt of crystallization and uncrystallized saltcake (mother liquor) carry out separatedly, and salt slurry enters centrifuge dewatering.
(4) centrifuge dehydration: salt slurry enters centrifuge dewatering and generates loose wet salt, and composition is NaCl>=97%, H
2o≤3%.
(5) loose wet salt dissolves: adopt the secondary steam water of condensation wet salt that directly will fall apart in salt container, to form saturated brine and enter secondary vacuum evaporative crystallization (with (three)) changing, after salt slurry is separated with mother liquor in vaporizer, enter physics washing, purifying.
(6) washing, purifying: utilize the saltcake of the dissolving crystallized salt surface attachment of saturated brine in (five), salt slurry enters centrifugal drying screening.
(7) centrifugal drying screening: salt slurry enters centrifuge dewatering, drying bed is dry, vibrosieve, be packaged to be medicinal raw material salt finished product, finished product standard reaches Chinese Pharmacopoeia version quality standard in 2010, NaCl >=99.6%, other constituent content standards are shown in < < Chinese Pharmacopoeia version > > sodium-chlor quality standard in 2010.
(8) finished product packing storage: pack and store by medicinal sodium chloride preparation packaging standard.
Process point (six) to (eight) is carried out material circulation in the clean room that has passed through GMP authentication.Adopt the pharmaceutical salts cost of above-mentioned explained hereafter 800 yuan to 1000 yuan/ton pharmaceutical salts, loose approximately 1.5 tons of/ton of pharmaceutical salts of wet salt consumption, the about 300kg/ ton of consumption mark coal pharmaceutical salts, the about 95kwh/ ton of power consumption pharmaceutical salts.Obviously cost, material consumption and energy consumption are high especially.
Medicinal raw material salt: be colourless, transparent cube crystallization or white crystallinity powder; Odorless; Taste is salty.This product is easily molten in water, almost insoluble in ethanol.The aobvious sodium salt of the aqueous solution and the muriatic identification of this product.Meet Chinese Pharmacopoeia standard in 2010.
Two, solid edible salt and production method
Solid edible salt comprises and adds iodine edible salt and do not add iodine edible salt, is white crystallization or white crystallinity powder; Odorless; Taste is salty, easily molten in water, almost insoluble in ethanol.It is the edible salt through processing that sodium-chlor is main component of take obtaining from seawater, underground rock (ore deposit) salt deposit, natural halogen (salty) water, the main component of edible salt is sodium-chlor (NaCl), contains the elements such as a small amount of moisture content and impurity and other iron, phosphorus, iodine simultaneously.
Solid edible salt production technology is as follows:
(1) utilize the technique of (one) to (four) in above-mentioned background technology one to obtain loose wet salt, composition is NaCl>=97%, H
2o≤3%.
(2) dry packing: loose wet salt enters drying bed inner drying, obtains dry solid salt, and composition is NaCl>=99.1%, H
2o≤0.3%.
(3) add fluffy powder-yellow prussiate of potash: for guaranteeing that product does not lump, need add yellow prussiate of potash to the solid salt of crystallization and prevent caking.Yellow prussiate of potash is hypertoxic product, need in product, add cautiously use.In interpolation standard 10mg/kg.
(4) add iodine edible salt and will add Potassium Iodate or potassiumiodide, before drying bed or after drying bed, with aqueous solution form, add.Interpolation standard 20-50mg/kg.
Three, bittern purifying and except nitre technology
(1) bittern purifying technique
When utilizing well mine salt making from brine for medicinal raw material salt (medicinal sodium chloride) product and solid edible product salt, most of enterprise has adopted brine purifying technique, and main purpose is removed Ca in raw brine composition
2sO
4and MgSO
4deng impurity component, generally there are at present following three kinds of processing methodes:
1. caustic soda adds Method of Soda purification process: MgSO
4+ 2NaOH=Mg (OH)
2↓+Na
2sO
4, CaSO
4++ Na
2cO
3=CaCO
3↓+Na
2sO
4
2. lime adds Method of Soda purification process: MgSO
4+ Ca (OH)
2=Mg (OH)
2↓+CaSO
4, Ca (OH)
2+ Na
2sO
4=2NaOH+CaSO
4, CaSO
4+ Na
2cO
3=CaCO
3↓+Na
2sO
4
3. lime adds soda ash and adds carbon dioxide process purification process: Ca (OH)
2+ MgSO
4=Mg (OH)
2↓+CaSO
4, Ca (OH)
2+ Na
2sO
4=2NaOH+CaSO
4, 2NaOH+CO
2=Na
2cO
3+ H
2o, CaSO
4+ Na
2cO
3=CaCO
3↓+Na
2sO
4
The brine quality obtaining after above-mentioned three kinds of art breading purify is as table 2.
Brine quality after table 2 bittern purifying
| Index name | Index |
| Content (NaCl) >= | 290g/l |
| Ca 2+≤ | 10mg/l |
| Mg 2+≤ | 3mg/l |
| SS≤ | 10 |
| SO 4 2-≤ | 10g/l |
(2) technique of nitrate removal
Technique of nitrate removal is for raw brine composition Na
2sO
4removal, generally have at present following several technique:
1. cold method, except nitre, is utilized NaCl and Na in raw brine
2sO
4the difference of solubleness, adopts the freezing technique of physics, Na
2sO
4with Na
2sO
410H
2o (mirabilite hydrate) separates out.
2. resin method, except nitre, utilizes ion exchange resin absorption exchange SO
4 2-(sulfate ion).
3. barium method is except nitre, Na
2sO
4+ BaCl
2=2NaCl+BaSO
4↓
4. calcium method is except nitre, Na
2sO
4+ CaCl
2=2NaCl+CaSO
42H
2o ↓
5. embrane method, except nitre, is utilized the selective separation function of nanofiltration membrane, and sulfate radical unnecessary in brine circulation system is separated from brine system with the form of sodium sulfate.
Summary of the invention
The present invention proposes a kind of well mine salt raw brine and produces without evaporation product and the preparation method that high purity water salt series product and preparation method, especially these series product Zhong Shui and salt are purified and added nutritive element.High purity water salt series product comprise: pharmacopeia level medicinal raw material high purity water salt (substitute solid medicinal salt), medicinal raw material salt, sub-pharmacopeia level add N green nourishing health care high purity water salt (N is organic and inorganic nutritive element), sub-pharmacopeia level for meal high purity water salt (alternative solid edible salt), sub-pharmacopeia level eat with adding iodine high purity water salt.Medicinal raw material salt utilizes pharmacopeia level medicinal raw material high purity water salt to do raw material, adopts evaporative crystallization technique to produce.
Technical scheme of the present invention is as follows:
1. well mine salt raw brine is without a method for evaporation production pharmacopeia level high purity water salt, and its step is as follows:
1) raw brine that adopts rock salt mining area to produce, utilize Brine Chemistry precipitation purifying method by raw brine purifying to NaCl>=290g/l, SO
4 2-≤ 15g/l, Ca
2+≤ 6ppm, Mg
2+≤ 3ppm, suspended solid SS≤10ppm, and adopt common ceramic membrane filter system to purify;
2) by 1) in the pH value of bittern after purification be adjusted to neutrality, and deionized water is added to wherein dilution, formation NaCl≤250g/l, SO
4 2-≤ 15g/l, Ca
2+≤ 6ppm, Mg
2+the quality of≤3ppm, suspended solid SS≤1ppm;
3) utilize embrane method to remove nitre, utilize the selective separation function of nanofiltration membrane, sulfate radical unnecessary in brine circulation system is separated from brine system with the form of sodium sulfate; Form NaCl≤250g/l, SO
4 2-≤ 0.7g/l, Ca
2+≤ 6ppm, Mg
2+the quality of≤3ppm, suspended solid SS≤1ppm;
4) by the bittern after nanofiltration membrane, add BaCl
2react, further sulfate radical, forms Na
2sO
4≤ 6ppm, BaSO
4+ BaCl
2≤ 3ppm quality; Common ceramic membrane filter system is filtered the qualified pharmacopeia level high purity water salt of output.
Described step 2) deionized water is salt making enterprises secondary steam water of condensation.
Utilize pharmacopeia level high purity water salt of the present invention directly to add deionized water dilution and produce medicinal sodium chloride preparation or physiological saline.
Utilize pharmacopeia level high purity water salt of the present invention to prepare medicinal raw material salt as raw material substitution solid material salt.
The organic or inorganic nutritive element that utilizes pharmacopeia level high purity water salt snack of the present invention to use, preparation improves the sub-pharmacopeia level of product healthy nutritive value green nourishing health care high purity water salt.
Described nutritive element is the inorganic elements of N1 Repone K, magnesium chloride, calcium, zinc, selenium, iron or riboflavin; Or one or more combinations of gourd, fruit and vegetable juice or base of leaf and flesh meal use animals and plants element.
Utilize pharmacopeia level high purity water salt of the present invention to prepare sub-pharmacopeia level meal high purity water salt; Pure water salt after nanofiltration membrane sulfate radical in pharmacopeia level medicinal raw material high purity water salt preparation method, add 60g/l vacuum refining solid salt, add bariumchloride and remove the sulfate radical of the residual 0.7g/l having in pure water salt, adopt common ceramic membrane filter to purify, do not add yellow prussiate of potash; Or utilize the yellow prussiate of potash that do not add that vacuum salt production equipment is produced to refine solid salt, add high-purity water of condensation that vacuum salt making facility produces, solid salt is dissolved into 300-310g/l concentration, enter ceramic membrane filter and purify, do not add the additives such as yellow prussiate of potash.
Utilize pharmacopeia level high purity water salt of the present invention to prepare sub-pharmacopeia level meal with adding iodine high purity water salt; In pharmacopeia level medicinal raw material high purity water salt preparation method, nanofiltration membrane is except pure water salt after nitre, add 60g/l vacuum refining solid salt, add the sulfate radical that bariumchloride is removed the residual 0.7g/l having in pure water salt, membrane filtration is purified, add Potassium Iodate or potassiumiodide 6-12mg/l, do not add yellow prussiate of potash; Or utilize the yellow prussiate of potash that do not add that vacuum salt production equipment is produced to refine solid salt, add the water of condensation that vacuum salt making facility produces, solid salt is dissolved into 300-310g/l concentration, enter membrane filtration and purify, add Potassium Iodate or potassiumiodide 6-12mg/l, do not add other additives of yellow prussiate of potash.
Be described as follows:
One, the production method of pharmacopeia level medicinal raw material high purity water salt, see Fig. 1:
1) raw brine that adopts rock salt mining area to produce, the Brine Chemistry precipitation purifying method of utilizing background technology one (two) by raw brine purifying to NaCl>=290g/l, SO
4 2-≤ 15g/l, Ca
2+≤ 6mg/l (6ppm), Mg
2+≤ 3mg/l (3ppm), suspended solid SS≤10mg/l (10ppm), and adopt common ceramic membrane filter system to purify;
2) according to the requirement of sodium filter membrane technology condition, by 1) in the pH value of bittern after purification be adjusted to neutrality, and deionized water (salt making enterprises can use secondary steam water of condensation) is added wherein and is diluted, formation NaCl≤250g/l, SO
4 2-≤ 15g/l, Ca
2+≤ 6mg/l (6ppm), Mg
2+the quality of≤3mg/l (3ppm), suspended solid SS≤1mg/l (1ppm);
3) utilize the nanofiltration membrane process system of background technology three (two) 5 to remove 2) in part of sulfuric acid radical ion, form NaCl≤250g/l, SO
4 2-≤ 0.6g/l, Ca
2+≤ 6mg/l (6ppm), Mg
2+the quality of≤3mg/l (3ppm), suspended solid SS≤1mg/l (1ppm).By the bittern after nanofiltration membrane, utilize background technology three (two) 3 to add BaCl
2(bariumchloride) reacts, and further sulfate radical, forms Na
2sO
4≤ 6mg/l (6ppm), BaSO
4+ BaCl
2≤ 3mg/l (3ppm) quality.Through common ceramic membrane filter system, filter the qualified medicinal raw material high purity water salt of output again.
Two, medicinal raw material salt production method, see Fig. 2:
Directly with the pharmacopeia level high purity water product salt in summary of the invention one, adopt background technology one (three)～(eight) evaporative crystallization technique to produce medicinal raw material salt.
The present invention and traditional mode of production solid medicinal raw material salt method difference be, raw materials used is pharmacopeia level high purity water product salt, rather than solid material salt.Conventionally medicinal raw material salt be by solid material salt be dissolved in water saturated after, then pass through the processes such as bittern purifying, evaporative crystallization.Medicinal raw material product salt quality of the present invention is higher than Chinese Pharmacopoeia standard in 2010.
Three, sub-pharmacopeia level adds N green nourishing health care high purity water salt production method, sees Fig. 3:
Directly with the pharmacopeia level medicinal raw material high purity water product salt in summary of the invention one, add can the eat organic and inorganic elements of use of N1 or N2.N1 is the inorganic elementss such as Repone K, magnesium chloride, calcium, zinc, selenium, iron and riboflavin, and N2 uses animals and plants element for eating, as gourd, fruit and vegetable juice or base of leaf and flesh etc.
The present invention adopts pharmacopeia level medicinal raw material high purity water product salt, can add arbitrarily the inorganic of the various use of eating and organotrophy element, improves product healthy nutritive value.Quality product is better than QB2020-2003 standard, inferior to pharmacopeia grade standard.
Four, sub-pharmacopeia level meal high purity water salt production method, see Fig. 4 and Fig. 5:
Utilize in the pharmacopeia level medicinal raw material high purity water salt preparation method in summary of the invention one pure water salt after nanofiltration membrane sulfate radical, add about 60g/l vacuum refining solid salt, add bariumchloride and remove the sulfate radical of the residual 0.7g/l having in pure water salt, adopt common ceramic membrane filter to purify, do not add yellow prussiate of potash.Or utilize the yellow prussiate of potash that do not add that vacuum salt production equipment is produced to refine solid salt, add high-purity water of condensation that vacuum salt making facility produces, solid salt is dissolved into 300-310g/l concentration, enter ceramic membrane filter and purify, do not add the additives such as yellow prussiate of potash.
The present invention utilizes pharmacopeia level medicinal raw material high purity water salt and refining solid salt to do raw material, liquid product, and concentration reaches 300-310g/l, does not add the additives such as yellow prussiate of potash.Product of the present invention and the difference of solid edible salt are not add yellow prussiate of potash (hypertoxic additive) and any additive; Be difficult for deliquescence, be easy to store; Impurity is few, instant safety; Salt-free dust in production process, environmentally safe and corrosion; The production of edible salt and Industrial Salt strictly can be separated, be easy to edible salt in strict accordance with < < food safety management way > > stringent regulations.
Five, sub-pharmacopeia level meal, with adding iodine high purity water salt production method, is shown in Fig. 6 and Fig. 7:
Utilize in the pharmacopeia level medicinal raw material high purity water salt preparation method in summary of the invention one nanofiltration membrane except pure water salt after nitre, add about 60g/l vacuum refining solid salt, add bariumchloride and remove the sulfate radical of the residual 0.7g/l having in pure water salt, membrane filtration is purified, add Potassium Iodate or potassiumiodide 6-12mg/l, do not add yellow prussiate of potash.Or utilize the yellow prussiate of potash that do not add that vacuum salt production equipment is produced to refine solid salt, add the water of condensation that vacuum salt making facility produces, solid salt is dissolved into 300-310g/l concentration, enter membrane filtration and purify, add Potassium Iodate or potassiumiodide 6-12mg/l, do not add other additives such as yellow prussiate of potash.
The present invention utilizes pharmacopeia level medicinal raw material high purity water salt and refining solid salt to do raw material, liquid product, and concentration 300-310g/l, does not add yellow prussiate of potash, and adds Potassium Iodate or potassiumiodide, prevents iodine deficiency.
Advantage of the present invention and effect are:
Pharmacopeia level medicinal raw material high purity water product salt is liquid form, deionized water dilution be can directly add and medicinal sodium chloride preparation or physiological saline produced, and do not need to obtain solid medicinal raw material salt through traditional bittern purifying, evaporation and crystal process, then medicinal raw material salt thin up is obtained to medicinal sodium chloride preparation or physiological saline.The inventive method adopts ceramic membrane filter, nanofiltration membrane treatment, and comprehensive energy consumption is low, can save a large amount of energy, reduces facility investment and floor space, reduce production costs on can be largely, and salt-free dust in production process, non-environmental-pollution and corrosion etc.
Accompanying drawing explanation
Fig. 1: medicinal raw material high purity water salt process flow sheet;
Fig. 2: medicinal raw material salt process flow sheet;
Fig. 3: sub-pharmacopeia level adds N green nourishing health care high purity water salt;
Fig. 4: sub-high purity water salt technical process one for pharmacopeia level meal;
Fig. 5: sub-high purity water salt technical process two for pharmacopeia level meal;
Fig. 6: sub-pharmacopeia level meal is with adding iodine high purity water salt technical process one;
Fig. 7: sub-pharmacopeia level meal is with adding iodine high purity water salt technical process two.
Embodiment
One, pharmacopeia level medicinal raw material high purity water product salt and preparation method
Pharmacopeia level medicinal raw material high purity water product salt: colourless, transparent liquid, taste is salty.Main component is sodium-chlor.
Pharmacopeia level medicinal raw material high purity water product salt preparation method:
(1) raw brine that utilizes rock salt mining area to produce.
(2) utilize three kinds of bittern purifying methods wherein a kind of technique by raw brine purifying to NaCl>=290g/l, Na
2sO
4≤ 15g/l, Ca
2+≤ 6mg/l (6ppm), Mg
2+≤ 3mg/l (3ppm), suspended solid SS≤10mg/l (10ppm).Fig. 1 is shown in bittern purifying technical process.
(3) adopt membrane filtration and make bittern pH value be neutral.
(4) utilize vacuum salt production by-product pure water (secondary steam water of condensation) to join in the bittern of (three), form NaCl≤250g/l, SO
4 2-≤ 15g/l, Ca
2+≤ 6mg/l (6ppm), Mg
2+the quality of≤3mg/l (3ppm), suspended solid SS≤1mg/l (1ppm).
(5) utilize nanofiltration membrane by the bittern sulfate radical ion of (four), form NaCl≤250g/l, SO
4 2-≤ 0.7g/l, Ca
2+≤ 6mg/l (6ppm), Mg
2+the quality of≤3mg/l (3ppm), suspended solid SS≤1mg/l (1ppm).
(6) by the bittern after nanofiltration membrane, add BaCl
2(bariumchloride) reacts, and further sulfate radical, forms Na
2sO
4≤ 6mg/l (6ppm), BaSO
4+ BaCl
2≤ 3mg/l (3ppm) quality.
(7) film is purified and is filtered the qualified medicinal raw material high purity water salt (in Table 3) of output.
(8) filling by appropriate containers in the workshop that meets GMP standard is sale of finished goods.
Table 3 pharmacopeia level medicinal raw material high purity water product salt quality
| Index name | Index |
| Content (NaCl)≤ | 250g/l |
| Potential of hydrogen test | Qualified |
| Clarity test | Qualified |
| Iodide test | Qualified |
| Bromide test | Qualified |
| Vitriol (SO4)≤ | 5mg/l |
| Barium salt test | Qualified |
| Calcium salt test | Qualified |
| Magnesium (Mg)≤ | 3mg/l |
| Potassium (K)≤ | 0.05g/l |
| Iron (Fe)≤ | 0.75mg/l |
| Heavy metal≤ | 0.05mg/l |
| Arsenic salt≤ | 0.1mg/l |
| Yellow prussiate of potash≤ | 0 |
Medicinal raw material high purity water salt process flow diagram is shown in Fig. 1.
Two, medicinal raw material salt (sodium-chlor) product and preparation method
Medicinal raw material salt: be colourless, transparent cube crystallization or white crystallinity powder; Odorless; Taste is salty.This product is easily molten in water, almost insoluble in ethanol.The aobvious sodium salt of the aqueous solution and the muriatic identification of this product.Meet Chinese Pharmacopoeia standard in 2010.
Medicinal raw material salt (sodium-chlor) preparation method:
Directly with summary of the invention one pharmacopeia level high purity water product salt, adopt evaporative crystallization technique to produce medicinal raw material salt.Concrete production technology is as follows:
(1) evaporative crystallization: the pharmacopeia level high purity water salt through preheating is pumped into evaporative crystallization in evaporative crystallization tank, obtains medicinal raw material salt slurry, pharmacopeia level high purity water salt washing for this salt slurry.
(2) centrifuge dehydration: salt slurry generates loose wet salt by centrifuge dewatering, and composition is NaCl>=97%, H
2o≤3%.
(3) dry screening: salt slurry sieves by centrifugal drying, formed medicinal raw material salt finished product, finished product standard is Chinese Pharmacopoeia version quality standard in 2010, NaCl >=99.6%, other constituent content standards are shown in < < Chinese Pharmacopoeia version > > sodium-chlor quality standard in 2010.In Table 4.
(4) finished product packing storage: pack and store by medicinal sodium chloride preparation packaging standard.
Table 4 medicinal raw material product salt quality table
| Index name | Index |
| Content (NaCl) >= | 99.5% |
| Potential of hydrogen test: | Qualified |
| Clarity test: | Qualified |
| Iodide test: | Qualified |
| Bromide test: | Qualified |
| Vitriol (SO 4)≤ | 0.002% |
| Barium salt test: | Qualified |
| Calcium salt test: | Qualified |
| Magnesium (Mg)≤ | 0.001% |
| Potassium (K)≤ | 0.02% |
| Weight loss on drying≤ | 0.50% |
| Iron (Fe)≤ | 0.0003% |
| Heavy metal≤ | 0.00002% |
| Yellow prussiate of potash≤ | 0 |
Medicinal raw material salt (sodium-chlor) process flow sheet is shown in Fig. 2.
Three, sub-pharmacopeia level adds N green nourishing health care high purity water product salt and preparation method
Sub-pharmacopeia level adds N green nourishing health care high purity water product salt: transparent liquid, taste is salty, the organic and inorganic elements of the use of can eating in addition.N1 is the inorganic elementss such as Repone K, magnesium chloride, calcium, zinc, selenium, iron and riboflavin and is better than the standards such as calcium enriched nutrient salt QB2238.1-2005, zinc enriched nutrient salt QB2238.2-2005, Selenium-fortified salt QB2238.3-2005, iron fortification nutritional salt QB2238.4-2005, riboflavin enriched nutrient salt QB2238.5-2005, inferior to pharmacopeia grade standard.N2 uses animals and plants element for eating, and as gourd, fruit and vegetable juice or base of leaf and flesh etc., quality is better than QB2020-2003 standard, inferior to pharmacopeia grade standard (in Table 5).
The sub-pharmacopeia level of table 5 adds N green nourishing health care high purity water product salt quality
Sub-pharmacopeia level adds N green nourishing health care high purity water salt preparation method:
The present invention directly adds can the eat organic and inorganic elements of use of N1 or N2 with the pharmacopeia level medicinal raw material high purity water product salt of summary of the invention one.
Process flow sheet is shown in Fig. 3.
Four, sub-pharmacopeia level meal high purity water product salt and preparation method
Sub-pharmacopeia level meal is used high purity water product salt: colourless, transparent liquid, taste is salty.Main component is sodium-chlor, not containing iodine element and yellow prussiate of potash composition.Quality product is in Table 6.
The sub-pharmacopeia level meal high purity water product salt quality of table 6
| Index name | Index |
| Content (NaCl) | 300～310g/l |
| Potential of hydrogen test: | 6-8 |
| Clarity test: | Qualified |
| Vitriol (SO4)≤ | 6mg/l |
| Barium salt test: | Qualified |
| Calcium salt test: | Qualified |
| Magnesium (Mg)≤ | 2mg/l |
| Potassium (K)≤ | 0.05g/l |
| Iron (Fe)≤ | 0.6mg/l |
| Heavy metal≤ | 0.05mg/l |
| Arsenic salt≤ | 0.1mg/l |
| Yellow prussiate of potash≤ | 0 |
Sub-high purity water product salt preparation method for pharmacopeia level meal:
(1) utilize summary of the invention one (five) nanofiltration membrane except pure water salt after nitre, add about 60g/l vacuum refining solid salt, add bariumchloride and remove the residual sulfate radical that is less than 0.7g/l having in pure water salt, membrane filtration is purified, and does not add yellow prussiate of potash.
Process flow sheet is shown in Fig. 4.
(2) utilize the yellow prussiate of potash that do not add that vacuum salt production equipment is produced to refine solid salt, add the water of condensation that vacuum salt making facility produces, solid salt is dissolved into 300-310g/l concentration, enter membrane filtration and purify, do not add the additives such as yellow prussiate of potash.
Process flow sheet is shown in Fig. 5.
Five, sub-pharmacopeia level meal is with adding iodine high purity water product salt and preparation method
Sub-pharmacopeia level meal is with adding iodine high purity water product salt: colourless, transparent liquid, taste is salty.Main component is sodium-chlor, contains iodine element, not containing yellow prussiate of potash composition.Quality product is in Table 7.
The sub-pharmacopeia level meal high purity water product salt quality of table 7
| Index name | Index |
| Content (NaCl) | 300～310g/l |
| Potential of hydrogen test: | 6-8 |
| Clarity test: | Qualified |
| Vitriol (SO4)≤ | 6mg/l |
| Barium salt test: | Qualified |
| Calcium salt test: | Qualified |
| Magnesium (Mg)≤ | 2mg/l |
| Potassium (K)≤ | 0.05g/l |
| Iodine (in I) | 6～12mg/l |
| Iron (Fe)≤ | 0.6mg/l |
| Heavy metal≤ | 0.05mg/l |
| Arsenic salt≤ | 0.1mg/l |
| Yellow prussiate of potash≤ | 0 |
Sub-pharmacopeia level meal is with adding iodine high purity water product salt preparation method:
Method one: utilize summary of the invention one (five) nanofiltration membrane except pure water salt after nitre, add about 60g/l vacuum refining solid salt, add the sulfate radical that bariumchloride is removed the residual 0.7g/l having in pure water salt, membrane filtration is purified, add Potassium Iodate or potassiumiodide 6-12mg/l, do not add yellow prussiate of potash.
Fig. 6 is shown in technical process.
Method two: utilize the yellow prussiate of potash that do not add that vacuum salt production equipment is produced to refine solid salt, add the water of condensation that vacuum salt making facility produces, solid salt is dissolved into 300-310g/l concentration, entering membrane filtration purifies, add Potassium Iodate or potassiumiodide 6-12mg/l, do not add other additives such as yellow prussiate of potash.Quality product is shown in quality standard 7.
Fig. 7 is shown in technical process.
Claims (8)
1. utilize well mine salt raw brine to prepare a method for high purity water salt, it is characterized in that:
1) raw brine that adopts rock salt mining area to produce, utilize Brine Chemistry precipitation purifying method by raw brine purifying to NaCl>=290g/l, SO
4 2-≤ 15g/l, Ca
2+≤ 6ppm, Mg
2+≤ 3ppm, suspended solid SS≤10ppm, and adopt common ceramic membrane filter system to purify;
2) by 1) in the pH value of bittern after purification be adjusted to neutrality, and deionized water is added to wherein dilution, formation NaCl≤250g/l, SO
4 2-≤ 15g/l, Ca
2+≤ 6ppm, Mg
2+the quality of≤3ppm, suspended solid SS≤1ppm;
3) utilize embrane method to remove nitre, utilize the selective separation function of nanofiltration membrane, sulfate radical unnecessary in brine circulation system is separated from brine system with the form of sodium sulfate; Form NaCl≤250g/l, SO
4 2-≤ 0.7g/l, Ca
2+≤ 6ppm, Mg
2+the quality of≤3ppm, suspended solid SS≤1ppm;
4) by the bittern after nanofiltration membrane, add BaCl
2react, further sulfate radical, forms Na
2sO
4≤ 6ppm, BaSO
4+ BaCl
2≤ 3ppm quality; Common ceramic membrane filter system is filtered the qualified pharmacopeia level high purity water salt of output.
2. the method for claim 1, is characterized in that described step 2) deionized water be salt making enterprises secondary steam water of condensation.
3. utilize the pharmacopeia level high purity water salt of claim 1 directly to add deionized water dilution production medicinal sodium chloride preparation or physiological saline.
4. utilize the pharmacopeia level high purity water salt of claim 1 to prepare medicinal raw material salt as raw material substitution solid material salt.
5. the organic or inorganic nutritive element that utilizes the pharmacopeia level high purity water salt snack of claim 1 to use, preparation improves the sub-pharmacopeia level of product healthy nutritive value green nourishing health care high purity water salt.
6. application as claimed in claim 5, is characterized in that described nutritive element is the inorganic elements of N1 Repone K, magnesium chloride, calcium, zinc, selenium, iron or riboflavin; Or one or more combinations of gourd, fruit and vegetable juice or base of leaf and flesh meal use animals and plants element.
7. utilize the pharmacopeia level high purity water salt of claim 1 to prepare sub-pharmacopeia level meal high purity water salt; Pure water salt after nanofiltration membrane sulfate radical in pharmacopeia level medicinal raw material high purity water salt preparation method, add 60g/l vacuum refining solid salt, add bariumchloride and remove the sulfate radical of the residual 0.7g/l having in pure water salt, adopt common ceramic membrane filter to purify, do not add yellow prussiate of potash; Or utilize the yellow prussiate of potash that do not add that vacuum salt production equipment is produced to refine solid salt, add high-purity water of condensation that vacuum salt making facility produces, solid salt is dissolved into 300-310g/l concentration, enter ceramic membrane filter and purify, do not add the additives such as yellow prussiate of potash.
8. utilize the pharmacopeia level high purity water salt of claim 1 to prepare sub-pharmacopeia level meal with adding iodine high purity water salt; In pharmacopeia level medicinal raw material high purity water salt preparation method, nanofiltration membrane is except pure water salt after nitre, add 60g/l vacuum refining solid salt, add the sulfate radical that bariumchloride is removed the residual 0.7g/l having in pure water salt, membrane filtration is purified, add Potassium Iodate or potassiumiodide 6-12mg/l, do not add yellow prussiate of potash; Or utilize the yellow prussiate of potash that do not add that vacuum salt production equipment is produced to refine solid salt, add the water of condensation that vacuum salt making facility produces, solid salt is dissolved into 300-310g/l concentration, enter membrane filtration and purify, add Potassium Iodate or potassiumiodide 6-12mg/l, do not add other additives of yellow prussiate of potash.
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| CN104000166A (en) * | 2014-06-16 | 2014-08-27 | 中国农业大学 | Color function seasoning low-sodium liquid salt and preparing method thereof |
| CN104543933A (en) * | 2015-01-28 | 2015-04-29 | 山东岱岳制盐有限公司 | Method for preparing deep well water salt |
| CN104872614A (en) * | 2015-05-25 | 2015-09-02 | 江苏久吾高科技股份有限公司 | Production process of liquid edible salt |
| CN105166842A (en) * | 2015-08-28 | 2015-12-23 | 山东岱岳制盐有限公司 | Preparation method of deep-well alkalescent table salt |
| CN109928410A (en) * | 2019-04-04 | 2019-06-25 | 山东肥城精制盐厂有限公司 | A kind of pharmaceutical salts process for refining |
| CN113331389A (en) * | 2021-06-23 | 2021-09-03 | 中盐河南盐业物流配送有限公司 | Salt for soy sauce |
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| CN104000166A (en) * | 2014-06-16 | 2014-08-27 | 中国农业大学 | Color function seasoning low-sodium liquid salt and preparing method thereof |
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| CN104543933A (en) * | 2015-01-28 | 2015-04-29 | 山东岱岳制盐有限公司 | Method for preparing deep well water salt |
| CN104872614A (en) * | 2015-05-25 | 2015-09-02 | 江苏久吾高科技股份有限公司 | Production process of liquid edible salt |
| CN104872614B (en) * | 2015-05-25 | 2017-03-15 | 江苏久吾高科技股份有限公司 | A kind of liquid edible technology of threonates |
| CN105166842A (en) * | 2015-08-28 | 2015-12-23 | 山东岱岳制盐有限公司 | Preparation method of deep-well alkalescent table salt |
| CN105166842B (en) * | 2015-08-28 | 2017-09-22 | 山东岱岳制盐有限公司 | The preparation method of deep-well alkalescent edible salt |
| CN109928410A (en) * | 2019-04-04 | 2019-06-25 | 山东肥城精制盐厂有限公司 | A kind of pharmaceutical salts process for refining |
| CN109928410B (en) * | 2019-04-04 | 2021-08-31 | 山东肥城精制盐厂有限公司 | Medicinal salt refining process |
| CN113331389A (en) * | 2021-06-23 | 2021-09-03 | 中盐河南盐业物流配送有限公司 | Salt for soy sauce |
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