CN109928410A - A kind of pharmaceutical salts process for refining - Google Patents

A kind of pharmaceutical salts process for refining Download PDF

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Publication number
CN109928410A
CN109928410A CN201910270279.8A CN201910270279A CN109928410A CN 109928410 A CN109928410 A CN 109928410A CN 201910270279 A CN201910270279 A CN 201910270279A CN 109928410 A CN109928410 A CN 109928410A
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level
film
liquid
refining
pharmaceutical salts
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CN109928410B (en
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马衍祯
孟强
刘万斌
荆忠山
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Shandong Feicheng Refined Salt Plant Co Ltd
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Shandong Feicheng Refined Salt Plant Co Ltd
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Abstract

The invention discloses a kind of pharmaceutical salts process for refining, the present invention is using natural bittern as raw material, after level-one film process and second level film process, carries out Dual alkali processing, is finally concentrated by evaporation the solid sodium chloride for obtaining meeting pharmacopoeial requirements.Former halogen directly crosses film, pH adjustment and cooling bring cost pressure is avoided, so that compared with the purification that can be achieved with pharmaceutical salts under low operating cost.

Description

A kind of pharmaceutical salts process for refining
Technical field
The present invention relates to a kind of pharmaceutical salts process for refining.Belong to chemical process technical field.
Background technique
Pharmaceutical salts of the invention refer to medicinal sodium chloride, and preparation source can be brine, sea salt or purified salt, wherein Former halogen is from a wealth of sources, and cost of material is low, is to prepare one of optimum feed stock of pharmaceutical salts.But in addition to containing a large amount of in former brine Sodium chloride outside, there are also a small amount of sulfate radical, calcium ion and magnesium ion.Therefore, in pharmaceutical salts production process, need to brine into Row refinement treatment is to remove sulfate radical, calcium ion and magnesium ion therein.
The treatment process of comparative maturity is to first pass through barium chloride method to remove sulfate radical (< 0.1g/l) at present, then by double Alkaline process removes removing calcium and magnesium.There is severe toxicity for barium chloride in the technique, and reagent cost is high.
Applicant attempts selection and barium chloride method is replaced to remove sulfate radical with film process.Film process brine has removal effect Stablize, the advantages that operating cost is low, occupied area is small.Membrane treatment process refer to through the sieve effect of special separation membrane aperture and Each component in former halogen is carried out Selective Separation by the road Nan Xiaoying of film surface charge.The special separation film for selecting suitable aperture, can Make the chloride ion, sodium ion and water molecule energy of brine through film, and sulfate ion, calcium ion and magnesium ion are larger due to partial size And it is trapped.
In order to extend the service life of film, mitigates fouling membrane, first carry out Dual alkali processing and remove calcium ions and magnesium ions in order to avoid generating Precipitating, still, the brine after double alkali process, pH 11-12, temperature is 45-60 DEG C;And to the pH of feed liquid in film operational process (6-8) and temperature (45 DEG C of <) need within the appropriate range.In this way, into increasing pH adjustment and cooling step before film, Undoubtedly increase processing cost.
Summary of the invention
The purpose of the present invention is to overcome above-mentioned the deficiencies in the prior art, provide a kind of pharmaceutical salts process for refining.
To achieve the above object, the present invention adopts the following technical solutions:
A kind of pharmaceutical salts process for refining, specific method is: natural bittern carries out after level-one film process and second level film process Dual alkali processing, is finally concentrated by evaporation and obtains purification medicinal salt.
Preferably, the additive for 2~3ppm being added into natural bittern carries out level-one film process and second level film process, institute again Stating additive is by acrylic acid-acrylic ester-sulfonate terpolymer, ethanol amine, triethylene tetramine, polyglycerol fatty acid Ester, acetic acid hydroxypropyl methylcellulose succinate are obtained by mixing with mass ratio 1:0.2~0.3:0.05~0.08:2~3:0.8~1.
It is further preferred that the additive the preparation method is as follows: acrylic acid-acrylic ester-sulfonate of formula ratio Terpolymer, ethanol amine, triethylene tetramine stir and evenly mix, and it is fine that polyglyceryl fatty acid ester, acetic acid hydroxypropyl first are added while stirring Plain succinate is tieed up, supersonic oscillations are handled 30~40 minutes.
Preferably, the natural bittern is selected from salt lake bittern or subsurface brine.
Preferably, natural bittern obtains level-one dope and the light liquid of level-one through level-one film process, the former separately uses, and the latter enters second level Film process obtains second level dope and the light liquid of second level, the former returns to level-one film process, and the latter enters Dual alkali processing step, then passes through Evaporation and concentration obtains purification medicinal salt." another to use ", which refers to, can be used for the use of other chemical fields, realize waste utilization.
It is further preferred that the technological parameter of level-one film process are as follows: the rate of recovery be 54~70%, operating pressure be 1MPa with Under, average flux is 92~98kg/h;The technological parameter of second level film process are as follows: the rate of recovery is 75~86%, and operating pressure is 0.95MPa is hereinafter, average flux is 110kg/h.
It is further preferred that the natural bittern, after level-one film process, salt content≤10% is the light liquid of level-one, saliferous Measuring > 10% is level-one dope;After second level film process, salt content≤2% is the light liquid of second level, and salt content > 2% is second level Dope;Wherein, salt content refers to these three bivalent ions total mass concentrations of calcic, magnesium, sulfate radical.
It is further preferred that carrying out level-one film process and second level film process using nanofiltration membrane separation plant, nanofiltration membrane is cut Staying molecular weight is 700~800Da.
Still more preferably, the Dual alkali is realized by the way that sodium carbonate and sodium hydroxide is added, wherein sodium carbonate Dosage determines that, to form precipitation of calcium carbonate, the dosage of sodium hydroxide passes through the light liquid of second level by calcium ion content in the light liquid of second level Middle magnesium ion content determines, to form magnesium hydrate precipitate.
Still more preferably, it is added after sodium carbonate and sodium hydroxide stir process 40 minutes, filtering, filtrate is evaporated Concentration, filter residue is that calcium and magnesium mud can export trade.
Preferably, concentration is evaporated using MVR evaporator.
It is further preferred that the process conditions being concentrated by evaporation are as follows: head effect steam pressure: 0.18~0.3Mpa;Steam matter Amount: saturated vapor, the degree of superheat :≤2 DEG C;Liquid level: liquid level stabilizing is controlled the 80% of evaporation tank volume by DCS;In tank Material liquid pH value: 4~5;Solid-to-liquid ratio in tank: 10~30%;Into tank brine turbidity :≤1mg/L;IV effect vaporization chamber vacuum degree: >=- 0.095Mpa。
It is further preferred that being evaporated again after the salting-out agents of 5~8ppm are added into gained filtrate after Dual alkali processing Concentration;The salting-out agents are the mixed liquor of dimethyl ether and acetone, and the two volume ratio is 1:2~3;The process conditions of evaporation and concentration Are as follows: head effect steam pressure: 0.18~0.2Mpa;Quality of steam: saturated vapor, the degree of superheat :≤2 DEG C;Liquid level: pass through DCS Liquid level stabilizing is controlled the 80% of evaporation tank volume;Material liquid pH value in tank: 4~5;Solid-to-liquid ratio in tank: 10~30%;Into tank brine Turbidity :≤1mg/L;IV effect vaporization chamber vacuum degree: >=-0.05Mpa.
It is further preferred that the operation sequence being concentrated by evaporation is as follows:
(1) successively I~IV effect circulating pump of starting, preparation receive each heating room condensed water;
(2) I effect circulation pump startups after, can to I effect heating room for steam, for stream mode are as follows: halt production less than 5 hours can Disposable steam supply;The steam supply to stop production 5~24 hours is in two steps: for the first time for can all supply after 1/2,1 hour;It stops production 24 hours To 72 hours, three steps of steam supply point: for the first time for supplying 1/3 after 1/3,1 hour again, and supplied entirely after 1 hour;It stops production small more than 72 When, steam supply point four steps: for the first time with a small amount of steam preheating heating room, quantity of steam is subject to the room of heating and does not play pressure, supplies after 1 hour 1/3, and all supplied for steam after 1/3 steam, then 1 hour again after 1 hour;
(3) when steam supply, a small amount of steam is first opened, preheating heating room is after 15 minutes, then opens main steam valve according to the above method, finally Close exhaust-valve;When multiple steam supply, also corresponding substep closes exhaust-valve, has finally closed after having supplied vapour;
(4) when I effect heating room not condensing discharge be full steam when, shut in I effect not condensing, condensing is not transferred to length by under Ranking is set;
Notice recirculated water process starts recirculated water after (5) I effect feed liquid boilings, puts into mixing condenser;
(6) II effect heating rooms not condensing emerge be steam full when, shut not condensing, condensing is not transferred to long ranking by under It sets;
After (7) II effect vaporization chamber feed liquid boilings, steam and water spray systems are put into.It puts into program: opening auxiliary condensation water valve Door supplies water to I grade of steam auxiliary condenser and II grade of steam auxiliary condenser, steam steam is put into after water supply.Throw steam steam When, first steam pressure just should be raised to specified value after half an hour for a small amount of steam preheating steam.While to steam steam supply, open Dynamic water spray pump simultaneously sprays water supply to water.Water spray can disposably supply water to specified value;
(8) III effect heating rooms not the effective hand of condensing touch temperature it is high when close not condensing, fixed gas is transferred to long ranking and is set;
(9) IV effect heating rooms not catch tank touch temperature it is high when, fixed gas is transferred to long ranking by not condenser valve in closing It sets;
(10) DCS system is put into after driving;
(11) primary from salt foot blowdown respectively before to each effect feed liquid crystallization (analysis salt), with exclude each effect precipitate it is miscellaneous Matter.
Beneficial effects of the present invention:
The present invention is using natural bittern as raw material, after level-one film process and second level film process, carries out Dual alkali processing, finally It is concentrated by evaporation the solid sodium chloride for obtaining meeting pharmacopoeial requirements.Former halogen directly cross film, avoid pH adjustment and cooling bring at This pressure, so that compared with the purification that can be achieved with pharmaceutical salts under low operating cost.
Acrylic acid-acrylic ester-sulfonate terpolymer, second is added before carrying out level-one film process and second level film process Hydramine, triethylene tetramine, polyglyceryl fatty acid ester, acetic acid hydroxypropyl methylcellulose succinate are added with what specific proportion mixed Add agent, on the one hand can inhibit the formation of solids, avoid and film is damaged, on the other hand can be concentrated in subsequent evaporation Suitably inhibit crystal is too fast to grow up in step, crystal fast growth is avoided to sweep along impurity.
The mixed liquor of dimethyl ether and acetone can be added before evaporation and concentration as salting-out agents, suitably reduction evaporation conditions, into one Step reduces operating cost.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
The present invention will be further elaborated with reference to the accompanying drawings and examples, it should which explanation, following the description is only It is not to be defined to its content to explain the present invention.
Acrylic acid-acrylic ester of the present invention-sulfonate terpolymer is purchased from the limited public affairs of Guangzhou towing force specialization work Department.
For convenient for comparing, the natural bittern in embodiment is the subsurface brine exploited together.
Embodiment 1:
A kind of pharmaceutical salts process for refining, specific method is: natural bittern carries out after level-one film process and second level film process Dual alkali processing, is finally concentrated by evaporation and obtains purification medicinal salt.
Natural bittern obtains level-one dope and the light liquid of level-one through level-one film process, the former separately uses, and the latter enters second level film process, Second level dope and the light liquid of second level are obtained, the former returns to level-one film process, and the latter enters Dual alkali processing step, then through being concentrated by evaporation Obtain purification medicinal salt." another to use ", which refers to, can be used for the use of other chemical fields, realize waste utilization.
The technological parameter of level-one film process are as follows: the rate of recovery 54%, operating pressure is 1MPa hereinafter, average flux is 92kg/h;The technological parameter of second level film process are as follows: the rate of recovery 75%, operating pressure is 0.95MPa hereinafter, average flux is 110kg/h。
Natural bittern is after level-one film process, and salt content≤10% is the light liquid of level-one, and salt content > 10% is level-one Dope;After second level film process, salt content≤2% is the light liquid of second level, and salt content > 2% is second level dope.
Level-one film process and second level film process are carried out using nanofiltration membrane separation plant.
Dual alkali is realized by the way that sodium carbonate and sodium hydroxide is added, wherein the dosage of sodium carbonate passes through in the light liquid of second level Calcium ion content determines, to form precipitation of calcium carbonate, the dosage of sodium hydroxide is determined by magnesium ion content in the light liquid of second level, with Form magnesium hydrate precipitate.Stir process 40 minutes after addition sodium carbonate and sodium hydroxide, filtering, filtrate is evaporated concentration, Filter residue is that calcium and magnesium mud can export trade.
Concentration is evaporated using MVR evaporator.
The process conditions of evaporation and concentration are as follows: head effect steam pressure: 0.3Mpa;Quality of steam: saturated vapor, the degree of superheat: ≤2℃;Liquid level: liquid level stabilizing is controlled the 80% of evaporation tank volume by DCS;Material liquid pH value in tank: 5;Solid-liquid in tank Than: 30%;Into tank brine turbidity :≤1mg/L;IV effect vaporization chamber vacuum degree: -0.095Mpa.Vapor (steam) temperature >=130 DEG C, salt temperature ≤35℃。
Embodiment 2:
A kind of pharmaceutical salts process for refining, specific method is: natural bittern carries out after level-one film process and second level film process Dual alkali processing, is finally concentrated by evaporation and obtains purification medicinal salt.
Natural bittern obtains level-one dope and the light liquid of level-one through level-one film process, the former separately uses, and the latter enters second level film process, Second level dope and the light liquid of second level are obtained, the former returns to level-one film process, and the latter enters Dual alkali processing step, then through being concentrated by evaporation Obtain purification medicinal salt." another to use ", which refers to, can be used for the use of other chemical fields, realize waste utilization.
The technological parameter of level-one film process are as follows: the rate of recovery 70%, operating pressure is 1MPa hereinafter, average flux is 98kg/h;The technological parameter of second level film process are as follows: the rate of recovery 86%, operating pressure is 0.95MPa hereinafter, average flux is 110kg/h。
Natural bittern is after level-one film process, and salt content≤10% is the light liquid of level-one, and salt content > 10% is level-one Dope;After second level film process, salt content≤2% is the light liquid of second level, and salt content > 2% is second level dope.
Level-one film process and second level film process are carried out using nanofiltration membrane separation plant.
Dual alkali is realized by the way that sodium carbonate and sodium hydroxide is added, wherein the dosage of sodium carbonate passes through in the light liquid of second level Calcium ion content determines, to form precipitation of calcium carbonate, the dosage of sodium hydroxide is determined by magnesium ion content in the light liquid of second level, with Form magnesium hydrate precipitate.Stir process 40 minutes after addition sodium carbonate and sodium hydroxide, filtering, filtrate is evaporated concentration, Filter residue is that calcium and magnesium mud can export trade.
Concentration is evaporated using MVR evaporator.
The process conditions of evaporation and concentration are as follows: head effect steam pressure: 0.3Mpa;Quality of steam: saturated vapor, the degree of superheat: ≤2℃;Liquid level: liquid level stabilizing is controlled the 80% of evaporation tank volume by DCS;Material liquid pH value in tank: 4;Solid-liquid in tank Than: 10%;Into tank brine turbidity :≤1mg/L;IV effect vaporization chamber vacuum degree: -0.095Mpa.Vapor (steam) temperature >=130 DEG C, salt temperature ≤35℃。
Embodiment 3:
A kind of pharmaceutical salts process for refining, specific method is: natural bittern carries out after level-one film process and second level film process Dual alkali processing, is finally concentrated by evaporation and obtains purification medicinal salt.
The additive that 2ppm is added into natural bittern carries out level-one film process and second level film process again, and the additive is By acrylic acid-acrylic ester-sulfonate terpolymer, ethanol amine, triethylene tetramine, polyglyceryl fatty acid ester, acetic acid hydroxypropyl Methylcellulose succinate is obtained by mixing with mass ratio 1:0.3:0.05:3:0.8.Additive the preparation method is as follows: formula ratio Acrylic acid-acrylic ester-sulfonate terpolymer, ethanol amine, triethylene tetramine stir and evenly mix, be added while stirring gather it is sweet Oil and fat acid esters, acetic acid hydroxypropyl methylcellulose succinate, supersonic oscillations are handled 40 minutes.
Natural bittern obtains level-one dope and the light liquid of level-one through level-one film process, the former separately uses, and the latter enters second level film process, Second level dope and the light liquid of second level are obtained, the former returns to level-one film process, and the latter enters Dual alkali processing step, then through being concentrated by evaporation Obtain purification medicinal salt." another to use ", which refers to, can be used for the use of other chemical fields, realize waste utilization.
The technological parameter of level-one film process are as follows: the rate of recovery 54%, operating pressure is 1MPa hereinafter, average flux is 98kg/h;The technological parameter of second level film process are as follows: the rate of recovery 75%, operating pressure is 0.95MPa hereinafter, average flux is 110kg/h。
Natural bittern is after level-one film process, and salt content≤10% is the light liquid of level-one, and salt content > 10% is level-one Dope;After second level film process, salt content≤2% is the light liquid of second level, and salt content > 2% is second level dope.
Level-one film process and second level film process are carried out using nanofiltration membrane separation plant.
Dual alkali is realized by the way that sodium carbonate and sodium hydroxide is added, wherein the dosage of sodium carbonate passes through in the light liquid of second level Calcium ion content determines, to form precipitation of calcium carbonate, the dosage of sodium hydroxide is determined by magnesium ion content in the light liquid of second level, with Form magnesium hydrate precipitate.Stir process 40 minutes after addition sodium carbonate and sodium hydroxide, filtering, filtrate is evaporated concentration, Filter residue is that calcium and magnesium mud can export trade.
Concentration is evaporated using MVR evaporator.
It is evaporated concentration again after the salting-out agents of 8ppm are added in gained filtrate after to Dual alkali processing;The salting-out agents are The mixed liquor of dimethyl ether and acetone, the two volume ratio are 1:2;The process conditions of evaporation and concentration are as follows: head effect steam pressure: 0.18Mpa;Quality of steam: saturated vapor, the degree of superheat :≤2 DEG C;Liquid level: liquid level stabilizing is controlled by DCS and is held in evaporator Long-pending 80%;Material liquid pH value in tank: 4;Solid-to-liquid ratio in tank: 20%;Into tank brine turbidity :≤1mg/L;IV effect vaporization chamber vacuum Degree: -0.05Mpa.
Embodiment 4:
A kind of pharmaceutical salts process for refining, specific method is: natural bittern carries out after level-one film process and second level film process Dual alkali processing, is finally concentrated by evaporation and obtains purification medicinal salt.
The additive that 3ppm is added into natural bittern carries out level-one film process and second level film process again, and the additive is By acrylic acid-acrylic ester-sulfonate terpolymer, ethanol amine, triethylene tetramine, polyglyceryl fatty acid ester, acetic acid hydroxypropyl Methylcellulose succinate is obtained by mixing with mass ratio 1:0.2:0.08:2:1.Additive the preparation method is as follows: formula ratio Acrylic acid-acrylic ester-sulfonate terpolymer, ethanol amine, triethylene tetramine stir and evenly mix, and polyglycereol is added while stirring Aliphatic ester, acetic acid hydroxypropyl methylcellulose succinate, supersonic oscillations are handled 30 minutes.
Natural bittern obtains level-one dope and the light liquid of level-one through level-one film process, the former separately uses, and the latter enters second level film process, Second level dope and the light liquid of second level are obtained, the former returns to level-one film process, and the latter enters Dual alkali processing step, then through being concentrated by evaporation Obtain purification medicinal salt." another to use ", which refers to, can be used for the use of other chemical fields, realize waste utilization.
The technological parameter of level-one film process are as follows: the rate of recovery 70%, operating pressure is 1MPa hereinafter, average flux is 92kg/h;The technological parameter of second level film process are as follows: the rate of recovery 86%, operating pressure is 0.95MPa hereinafter, average flux is 110kg/h。
Natural bittern is after level-one film process, and salt content≤10% is the light liquid of level-one, and salt content > 10% is level-one Dope;After second level film process, salt content≤2% is the light liquid of second level, and salt content > 2% is second level dope.
Level-one film process and second level film process are carried out using nanofiltration membrane separation plant.
Dual alkali is realized by the way that sodium carbonate and sodium hydroxide is added, wherein the dosage of sodium carbonate passes through in the light liquid of second level Calcium ion content determines, to form precipitation of calcium carbonate, the dosage of sodium hydroxide is determined by magnesium ion content in the light liquid of second level, with Form magnesium hydrate precipitate.Stir process 40 minutes after addition sodium carbonate and sodium hydroxide, filtering, filtrate is evaporated concentration, Filter residue is that calcium and magnesium mud can export trade.
Concentration is evaporated using MVR evaporator.
It is evaporated concentration again after the salting-out agents of 5ppm are added in gained filtrate after to Dual alkali processing;The salting-out agents are The mixed liquor of dimethyl ether and acetone, the two volume ratio are 1:3;The process conditions of evaporation and concentration are as follows: head effect steam pressure: 0.2Mpa;Quality of steam: saturated vapor, the degree of superheat :≤2 DEG C;Liquid level: liquid level stabilizing is controlled by DCS and is held in evaporator Long-pending 80%;Material liquid pH value in tank: 5;Solid-to-liquid ratio in tank: 20%;Into tank brine turbidity :≤1mg/L;IV effect vaporization chamber vacuum Degree: -0.05Mpa.
Embodiment 5:
A kind of pharmaceutical salts process for refining, specific method is: natural bittern carries out after level-one film process and second level film process Dual alkali processing, is finally concentrated by evaporation and obtains purification medicinal salt.
The additive that 2.5ppm is added into natural bittern carries out level-one film process and second level film process, the additive again It is by acrylic acid-acrylic ester-sulfonate terpolymer, ethanol amine, triethylene tetramine, polyglyceryl fatty acid ester, acetic acid hydroxyl Third methylcellulose succinate is obtained by mixing with mass ratio 1:0.25:0.06:2.5:0.9.Additive the preparation method is as follows: matching The acrylic acid-acrylic ester just measured-sulfonate terpolymer, ethanol amine, triethylene tetramine stir and evenly mix, and are added while stirring Polyglyceryl fatty acid ester, acetic acid hydroxypropyl methylcellulose succinate, supersonic oscillations are handled 35 minutes.
Natural bittern obtains level-one dope and the light liquid of level-one through level-one film process, the former separately uses, and the latter enters second level film process, Second level dope and the light liquid of second level are obtained, the former returns to level-one film process, and the latter enters Dual alkali processing step, then through being concentrated by evaporation Obtain purification medicinal salt." another to use ", which refers to, can be used for the use of other chemical fields, realize waste utilization.
The technological parameter of level-one film process are as follows: the rate of recovery 60%, operating pressure is 1MPa hereinafter, average flux is 96kg/h;The technological parameter of second level film process are as follows: the rate of recovery 80%, operating pressure is 0.95MPa hereinafter, average flux is 110kg/h。
Natural bittern is after level-one film process, and salt content≤10% is the light liquid of level-one, and salt content > 10% is level-one Dope;After second level film process, salt content≤2% is the light liquid of second level, and salt content > 2% is second level dope.
Level-one film process and second level film process are carried out using nanofiltration membrane separation plant.
Dual alkali is realized by the way that sodium carbonate and sodium hydroxide is added, wherein the dosage of sodium carbonate passes through in the light liquid of second level Calcium ion content determines, to form precipitation of calcium carbonate, the dosage of sodium hydroxide is determined by magnesium ion content in the light liquid of second level, with Form magnesium hydrate precipitate.Stir process 40 minutes after addition sodium carbonate and sodium hydroxide, filtering, filtrate is evaporated concentration, Filter residue is that calcium and magnesium mud can export trade.
Concentration is evaporated using MVR evaporator.
It is evaporated concentration again after the salting-out agents of 6ppm are added in gained filtrate after to Dual alkali processing;The salting-out agents are The mixed liquor of dimethyl ether and acetone, the two volume ratio are 1:2;The process conditions of evaporation and concentration are as follows: head effect steam pressure: 0.18Mpa;Quality of steam: saturated vapor, the degree of superheat :≤2 DEG C;Liquid level: liquid level stabilizing is controlled by DCS and is held in evaporator Long-pending 80%;Material liquid pH value in tank: 4;Solid-to-liquid ratio in tank: 20%;Into tank brine turbidity :≤1mg/L;IV effect vaporization chamber vacuum Degree: -0.03Mpa.
Test example
According to " Chinese Pharmacopoeia version (two) in 2015 ", tests to Examples 1 to 5 products therefrom, the results are shown in Table 1.
1. testing result of table
As shown in Table 1, sodium chloride obtained by Examples 1 to 5 meets States Pharmacopoeia specifications.
Above-mentioned, although the foregoing specific embodiments of the present invention is described with reference to the accompanying drawings, not protects model to the present invention The limitation enclosed, based on the technical solutions of the present invention, those skilled in the art are not needed to make the creative labor and can be done Various modifications or changes out are still within protection scope of the present invention.

Claims (10)

1. a kind of pharmaceutical salts process for refining, which is characterized in that specific method is: natural bittern through level-one film process and secondary membrane at After reason, Dual alkali processing is carried out, is finally concentrated by evaporation and obtains purification medicinal salt.
2. a kind of pharmaceutical salts process for refining according to claim 1, which is characterized in that into natural bittern be added 2~ The additive of 3ppm carries out level-one film process and second level film process again, and the additive is by acrylic acid-acrylic ester-sulfonate Terpolymer, ethanol amine, triethylene tetramine, polyglyceryl fatty acid ester, acetic acid hydroxypropyl methylcellulose succinate are with mass ratio 1:0.2~0.3:0.05~0.08:2~3:0.8~1 is obtained by mixing.
3. a kind of pharmaceutical salts process for refining according to claim 1, which is characterized in that natural bittern is obtained through level-one film process Level-one dope and the light liquid of level-one, the former separately uses, and the latter enters second level film process, obtains second level dope and the light liquid of second level, the former returns Level-one film process, the latter enter Dual alkali processing step, then obtain purification medicinal salt through being concentrated by evaporation.
4. a kind of pharmaceutical salts process for refining according to claim 3, which is characterized in that the technological parameter of level-one film process Are as follows: the rate of recovery is 54~70%, and operating pressure is 1MPa hereinafter, average flux is 92~98kg/h;The technique of second level film process Parameter are as follows: the rate of recovery is 75~86%, and operating pressure is 0.95MPa hereinafter, average flux is 110kg/h.
5. a kind of pharmaceutical salts process for refining according to claim 3, which is characterized in that the natural bittern through level-one film at After reason, salt content≤10% is the light liquid of level-one, and salt content > 10% is level-one dope;After second level film process, salt content≤ 2% is the light liquid of second level, and salt content > 2% is second level dope;Wherein, salt content refer to calcic, magnesium, sulfate radical these three two The total mass concentration of valence ion.
6. a kind of pharmaceutical salts process for refining according to claim 3, which is characterized in that carried out using nanofiltration membrane separation plant Level-one film process and second level film process, the molecular cut off of nanofiltration membrane are 700~800Da.
7. a kind of pharmaceutical salts process for refining according to claim 3, which is characterized in that the Dual alkali is by the way that carbon is added Sour sodium and sodium hydroxide are realized, wherein the dosage of sodium carbonate is determined by calcium ion content in the light liquid of second level, to form calcium carbonate The dosage of precipitating, sodium hydroxide is determined by magnesium ion content in the light liquid of second level, to form magnesium hydrate precipitate.
8. a kind of pharmaceutical salts process for refining according to claim 1, which is characterized in that be evaporated using MVR evaporator Concentration.
9. a kind of pharmaceutical salts process for refining according to claim 8, which is characterized in that the process conditions of evaporation and concentration are such as Under: head effect steam pressure: 0.18~0.3Mpa;Quality of steam: saturated vapor, the degree of superheat :≤2 DEG C;Liquid level: pass through DCS Liquid level stabilizing is controlled the 80% of evaporation tank volume;Material liquid pH value in tank: 4~5;Solid-to-liquid ratio in tank: 10~30%;Into tank brine Turbidity :≤1mg/L;IV effect vaporization chamber vacuum degree: >=-0.095Mpa.
10. a kind of pharmaceutical salts process for refining according to claim 8, which is characterized in that gained filter after to Dual alkali processing It is evaporated concentration again after the salting-out agents of 5~8ppm are added in liquid;The salting-out agents are the mixed liquor of dimethyl ether and acetone, the two Volume ratio is 1:2~3;The process conditions of evaporation and concentration are as follows: head effect steam pressure: 0.18~0.2Mpa;Quality of steam: saturation is steamed Vapour, the degree of superheat :≤2 DEG C;Liquid level: liquid level stabilizing is controlled the 80% of evaporation tank volume by DCS;Material liquid pH value in tank: 4 ~5;Solid-to-liquid ratio in tank: 10~30%;Into tank brine turbidity :≤1mg/L;IV effect vaporization chamber vacuum degree: >=-0.05Mpa.
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