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CN110451529A - A kind of method of purification of sodium chloride for injection - Google Patents

A kind of method of purification of sodium chloride for injection Download PDF

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Publication number
CN110451529A
CN110451529A CN201910647691.7A CN201910647691A CN110451529A CN 110451529 A CN110451529 A CN 110451529A CN 201910647691 A CN201910647691 A CN 201910647691A CN 110451529 A CN110451529 A CN 110451529A
Authority
CN
China
Prior art keywords
sodium chloride
nanofiltration system
nanofiltration
injection
solution
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910647691.7A
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Chinese (zh)
Inventor
莫文辉
西蒙·拉斯克里
周志艳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Qingdao Wosai Sea Water Desalination Technology Co Ltd
Original Assignee
Qingdao Wosai Sea Water Desalination Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by Qingdao Wosai Sea Water Desalination Technology Co Ltd filed Critical Qingdao Wosai Sea Water Desalination Technology Co Ltd
Priority to CN201910647691.7A priority Critical patent/CN110451529A/en
Publication of CN110451529A publication Critical patent/CN110451529A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D3/00Halides of sodium, potassium or alkali metals in general
    • C01D3/14Purification
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The invention discloses a kind of methods of purification of sodium chloride for injection, are related to medical supplies preparation technical field.Crude salt is dissolved in pure water first, then it is filtered using ultrafiltration or micro-filtration, remove larger molecular organics, colloid and the particle in solution, it is handled again using second level nanofiltration system filtrate, two-stage nanofiltration system is used in conjunction, the sulfate radical in solution can be effectively removed, nanofiltration system penetrating fluid is pumped into evaporator, is heated in the process using steam, Steam pressure control is in 0.1-0.15Mpa, in the process, nanofiltration system penetrating fluid is become being saturated from unsaturation, and sodium chloride crystallization is precipitated, sodium chloride further purifies while precipitation, it finally filters, dry, packaging.Entire technique combines ultrafiltration/micro-filtration and nanofiltration system, is handled completely using membrane process craft, and simple process, stable effluent quality are easy to control and realize automation, and the sodium chloride as impurity content that final refining obtains is low, and the index of injection is fully achieved.

Description

A kind of method of purification of sodium chloride for injection
Technical field
The present invention relates to medical supplies preparation technical fields, and in particular to a kind of method of purification of sodium chloride for injection.
Background technique
Sodium chloride injection primary treatment: dehydration caused by a variety of causes, including hypo-osmoticity, isotonicity and hypertonicity are lost Water;Hyperosmolar nonketotic diabetic coma can correct dehydration and isotonic state using isotonic or hypotonic sodium chloride;Low chlorine metabolism Property alkalosis.Sodium chloride injection is a kind of traditional medicine that our times various countries clinically generally use in the medical field Product, patient is in use, directly enter blood circulation system by intramuscular injection, due to miscellaneous containing many nocuousness in crude salt sodium chloride Matter will cause many complication into blood, cause to damage to the body of patient if do not removed, although currently having very much Chemical plant, which has, purifies crude salt.As shown in Figure 1, crude salt is dissolved first, is then added for traditional crude salt purifying technique Barium chloride sedimentation removal sulfate ion, the barium ions that then addition sodium carbonate sedimentation removal introduces, then by supernatant by surpassing Filter or microfiltration membrane system filtering, finally by the salt slurry being recrystallized to give twice filtering, dry, packaging.The shortcomings that this technique: 1. add Enter barium chloride and sodium carbonate needs charging tank, area occupied is larger, complicated for operation;2. need to be added twice reagent barium chloride and Sodium carbonate, barium chloride itself has toxicity, and will increase reagent cost;3. it is made a return journey sulfate radical using the precipitation method, such sulphur The removal rate of acid group is not high, cannot thoroughly remove sulfate radical;4. vapo(u)rizing temperature needs 130 degree using distilling twice, it may be desirable to Very high energy consumption, to increase cost;5. during crystallization, some solubility such as sodium sulphate and part metals cation Similar substance can not be removed there are in crystalline solid.
Summary of the invention
Present invention aims to overcome that disadvantage of the existing technology, seeks the preparation side for designing a kind of medical grade sodium chloride Method and device.
To achieve the above object, the invention adopts the following technical scheme:
A kind of method of purification of sodium chloride for injection, comprising the following steps:
(1) crude salt is dissolved in pure water, obtains the sodium chloride solution of 300g/L, in the solution except containing calcium, magnesium, iron and Outside some heavy metal ion elements, also contain the sodium sulphate of about 2g/L;
(2) sodium chloride solution is filtered using ultrafiltration or micro-filtration, removes larger molecular organics in solution, colloid and micro- Grain;
(3) step (2) water outlet is separated using second level nanofiltration system, two-stage nanofiltration system is used in conjunction, and can effectively go Except the sulfate radical in solution;
(3) nanofiltration system penetrating fluid is pumped into evaporator, is heated in the process using steam, Steam pressure control is in 0.1- 0.15Mpa, in the process, nanofiltration system penetrating fluid are become being saturated from unsaturation, and sodium chloride crystallization is precipitated, while sodium chloride is precipitated Further purification;
(4) step (3) salt slurry is squeezed into lautertuns, is filtered using traditional micro-filtration or ultra-filtration and separation technique, by chlorine Change sodium crystal retention;
(5) salt that filter comes out, which enters in drying bed, is dried, and sufficiently after drying, packs according to medical rank, should Product is the standard that can reach the other injection sodium chloride of pharmaceutical grade, subsequent to prepare the salt of various concentration according to actual needs Water is used for hospital patient.
Further, the rate of recovery of first order nanofiltration can reach 90%, and the penetrating fluid of the nanofiltration of the first order is as the second level The water inlet of nanofiltration, the rate of recovery of second level nanofiltration can reach 95%, and overall recovery reaches 85.5%.
Further, in step (2) and (4), filter membrane used is polysulfones, polyether sulfone or polyvinylidene fluoride, feeds hydraulic pressure Power < 10bar, the particulate that membrane aperture is 0.001-0.1 μm, molecular cut off 1000-30000Da.
Compared with the prior art, the invention has the following beneficial effects: (1) entire technique is by ultrafiltration/micro-filtration and nanofiltration system In conjunction with completely using membrane process craft processing, simple process, stable effluent quality are easy to control and realize automation;(2) it reduces The use of chemical agent avoids generating a large amount of solid waste;(3) the sodium chloride as impurity content that final refining obtains is low, complete Reach the index of injection entirely.
Detailed description of the invention
Fig. 1 is the purifying technique flow chart of sodium chloride for injection in traditional handicraft.
Fig. 2 is the purifying technique flow chart of sodium chloride for injection in the embodiment of the present invention 1.
Specific embodiment:
Invention is described further below by specific embodiment and in conjunction with attached drawing.
Embodiment 1
As shown in Figure 1, a kind of sodium chloride for injection purifying technique, specifically includes the following steps:
(1) crude salt is added in pure water, heating stirring dissolves it sufficiently, is dissolved into the sodium chloride solution of 300g/L, should In solution in addition to containing calcium, magnesium, iron and some heavy metal elements, also contain the sodium sulphate of about 2g/L, this solution is subjected to pre- mistake Filter, the pre-filtering use micro-filtration or ultrafiltration system, and filter membrane used is polysulfones, polyether sulfone or polyvinylidene fluoride, feed hydraulic pressure Power < 10bar is higher than 99% to the rate of recovery of its solution, can filter out the particulate that partial size is 0.01-0.1 μm, retention point Son amount is 1000-30000Da, and for removing the suspended matter in solution, solution turbidity < 0.5NT after filtering it can be with Greatly reduce nanofiltration membrane fouling in subsequent technique;
(2) be then filtered by a multistage nanofiltration system, multistage nanofiltration system include first order nanofiltration system and Hydraulic pressure is fed in second level nanofiltration system, the standard cell block that first order nanofiltration system is connected by several series systems, water inlet Power is 25-30bar, and temperature enters standard block room, water and sodium chloride by nanofiltration membrane, generates one in contrast when being room temperature The water inlet lower osmotic flow of impurity, the metal cation and sulfate radical of multivalence are retained by nanofiltration membrane, or because electrostatic repulsion machine Retention of being ostracised is made, nanofiltration membrane surface layer has charge or positive or negative, this depends on solution and mixes the pH value condition made, when this Solution containing metal ion flows through nanofiltration film surface, since solution is per se with certain net charge, film is allowed to go to retain Effects of ion type metal impurities.Nanofiltration membrane, which refers to the retention of metal ion, does not allow these metal ions to pass through, and forms one The retention water flow of the stock higher metal impurities of content, referred to as concentrate.The rate of recovery of the first order nanofiltration system is 90%, 98% can reach to the rejection of sulfate radical, the rejection of other metallic elements reaches 90% or more, i.e., vertical for every 1 The water inlet of square rice can produce 0.1 cubic metre of retention water flow.Second level nanofiltration system is similar with first order nanofiltration system, by several The standard block room of connection forms, but the nanofiltration system unit of the second level is less than first order nanofiltration system unit, and described the Second level nanofiltration system is further processed the osmotic flow that first order nanofiltration system is sent, to further decrease the number of impurity in solution Amount, to improve the purity of salt, the multistage nanofiltration system is by the nanofiltration of commercial criterion size (such as 4 inches or 8 inches) Module composition, nanofiltration membrane are retention and the stable nanofiltration membrane of flux, selectivity and > 1L/m with > 98%2-hr-bar Circulation performance.Multistage nanofiltration system is 80% to 85% to the rate of recovery of water, here sulfuric acid in 80% to 85% penetrating fluid The concentration < 2ppm of root, the only micro metal impurities for being suitable for recycling or reusing generate in concentrate, and solution It is pollution-free for neutrality, it can be directly discharged in the Nature;Or be recycled directly in technological operation and reuse, do not do anyization Processing, such as: it returns in the first order nanofiltration system water inlet circuit after filtering, by the concentration after the retention of multistage nanofiltration system Sodium chloride and a large amount of metal impurities and sulfate radical in liquid containing high concentration can enter the first order and separate again.
(3) the penetrating fluid evaporative crystallization for obtaining multistage nanofiltration system, nanofiltration system penetrating fluid contain the chlorine of very high concentration Change sodium, the sodium chloride of > 300g/L, the sulfate radical of < 2ppm, the content of other metal cations is also very micro, at 100 DEG C of > Turret in be evaporated crystallization, further increase the purity of its sodium chloride;
(4) crystalline solid after crystallization is filtered, the filtering uses micro-filtration or ultrafiltration system, and filter membrane used is poly- Sulfone, polyether sulfone or polyvinylidene fluoride feed water pressure < 10bar, are higher than 99% to the rate of recovery of its solution, can obtain more Pure sodium chloride particle.Then will after filtering obtained granulated salt be sent in 100 DEG C of drying tower be dried to get To more pure sodium chloride product, the sodium chloride after purifying meets sodium chloride in Chinese Pharmacopoeia (injection) standard and (is shown in Table 1)。
Table 1
Obviously, examples detailed above of the invention is just for the sake of clearly illustrating examples of the invention, and being not is pair The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description To make other variations or changes in different ways, there is no necessity and possibility to exhaust all the enbodiments, all at this Any modifications, equivalent replacements, and improvements etc. done within the spirit and principle of invention, should all be included in the claims in the present invention Protection scope within.

Claims (3)

1. a kind of method of purification of sodium chloride for injection, which comprises the following steps:
(1) crude salt is dissolved in pure water, obtains the sodium chloride solution of 300g/L, except containing calcium, magnesium, iron and some in the solution Outside heavy metal ion element, also contain the sodium sulphate of about 2g/L;
(2) sodium chloride solution is filtered using ultrafiltration or micro-filtration, removes larger molecular organics, colloid and the particle in solution;
(3) step (2) water outlet is handled using second level nanofiltration system, two-stage nanofiltration system is used in conjunction, and can effectively remove molten Sulfate radical in liquid;
(3) nanofiltration system penetrating fluid is pumped into evaporator, is heated in the process using steam, Steam pressure control is in 0.1- 0.15Mpa, in the process, nanofiltration system penetrating fluid are become being saturated from unsaturation, and sodium chloride crystallization is precipitated, while sodium chloride is precipitated Further purification;
(4) step (3) salt slurry is squeezed into lautertuns, is filtered using traditional micro-filtration or ultra-filtration and separation technique, by sodium chloride Crystal retention;
(5) salt that filter comes out, which enters in drying bed, is dried, and sufficiently after drying, packs according to medical rank, the product It can reach the standard of the other injection sodium chloride of pharmaceutical grade, the subsequent salt water that can according to actual needs, prepare various concentration supplies Hospital patient uses.
2. the method for purification of sodium chloride for injection according to claim 1, which is characterized in that the rate of recovery of first order nanofiltration It can reach 90%, water inlet of the penetrating fluid of the nanofiltration of the first order as second level nanofiltration, the rate of recovery of second level nanofiltration can reach 95%, overall recovery reaches 85.5%.
3. the method for purification of sodium chloride for injection according to claim 2, which is characterized in that in step (2) and (4), institute It is polysulfones, polyether sulfone or polyvinylidene fluoride with filter membrane, feeds water pressure < 10bar, the particle that membrane aperture is 0.001-0.1 μm Son, molecular cut off 1000-30000Da.
CN201910647691.7A 2019-07-17 2019-07-17 A kind of method of purification of sodium chloride for injection Pending CN110451529A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111362471A (en) * 2020-04-17 2020-07-03 莱特莱德(北京)环境技术股份有限公司 Device for removing sodium sulfate in coal chemical industry byproduct sodium chloride saturated solution
CN112374674A (en) * 2020-09-18 2021-02-19 安徽普朗膜技术有限公司 Industrial waste salt treatment system and process

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070189945A1 (en) * 2006-01-12 2007-08-16 Thorsten Kopp Method for the treatment of salt brine
CN101659424A (en) * 2009-09-04 2010-03-03 广东光华化学厂有限公司 Method for recovering reagent grade sodium chloride from lime milk production waste liquid
CN103723875A (en) * 2013-12-31 2014-04-16 朱江 Seawater full recycling process
CN104229834A (en) * 2013-06-08 2014-12-24 上海润浩环保科技有限公司 Process for preparing liquid edible salt based on brine
CN104326590A (en) * 2014-11-28 2015-02-04 王博 Method and device for making salt by using seawater
US20150352498A1 (en) * 2011-08-17 2015-12-10 Ahilan RAMAN Process and system for producing sodium chloride brine
CN105236447A (en) * 2015-09-15 2016-01-13 华陆工程科技有限责任公司 Method for producing food-grade potassium chloride by using multi-stage nano-filtration membrane separation technology
CN105502791A (en) * 2016-01-21 2016-04-20 厦门嘉戎技术股份有限公司 Coal chemical industry wastewater salt extraction method and facility
CN106396164A (en) * 2016-02-15 2017-02-15 青岛沃赛海水淡化科技有限公司 Industrial acidic wastewater treatment process
CN107055579A (en) * 2017-03-31 2017-08-18 中国神华能源股份有限公司 The method that salt is reclaimed from desulfurization wastewater

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070189945A1 (en) * 2006-01-12 2007-08-16 Thorsten Kopp Method for the treatment of salt brine
CN101659424A (en) * 2009-09-04 2010-03-03 广东光华化学厂有限公司 Method for recovering reagent grade sodium chloride from lime milk production waste liquid
US20150352498A1 (en) * 2011-08-17 2015-12-10 Ahilan RAMAN Process and system for producing sodium chloride brine
CN104229834A (en) * 2013-06-08 2014-12-24 上海润浩环保科技有限公司 Process for preparing liquid edible salt based on brine
CN103723875A (en) * 2013-12-31 2014-04-16 朱江 Seawater full recycling process
CN104326590A (en) * 2014-11-28 2015-02-04 王博 Method and device for making salt by using seawater
CN105236447A (en) * 2015-09-15 2016-01-13 华陆工程科技有限责任公司 Method for producing food-grade potassium chloride by using multi-stage nano-filtration membrane separation technology
CN105502791A (en) * 2016-01-21 2016-04-20 厦门嘉戎技术股份有限公司 Coal chemical industry wastewater salt extraction method and facility
CN106396164A (en) * 2016-02-15 2017-02-15 青岛沃赛海水淡化科技有限公司 Industrial acidic wastewater treatment process
CN107055579A (en) * 2017-03-31 2017-08-18 中国神华能源股份有限公司 The method that salt is reclaimed from desulfurization wastewater

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111362471A (en) * 2020-04-17 2020-07-03 莱特莱德(北京)环境技术股份有限公司 Device for removing sodium sulfate in coal chemical industry byproduct sodium chloride saturated solution
CN112374674A (en) * 2020-09-18 2021-02-19 安徽普朗膜技术有限公司 Industrial waste salt treatment system and process

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