CN102697801A - Manufacturing process of flavouring-containing medicinal mirabilite - Google Patents
Manufacturing process of flavouring-containing medicinal mirabilite Download PDFInfo
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- CN102697801A CN102697801A CN2012101588473A CN201210158847A CN102697801A CN 102697801 A CN102697801 A CN 102697801A CN 2012101588473 A CN2012101588473 A CN 2012101588473A CN 201210158847 A CN201210158847 A CN 201210158847A CN 102697801 A CN102697801 A CN 102697801A
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Abstract
The invention discloses a manufacturing process of flavouring-containing medicinal mirabilite. Raw mirabilite water with concentration of 20 degrees of Be' conveyed under well is filtered by a three-level pipe filter to remove impurities and is then refined and purified by a six-level ion exchanger to obtain refined mirabilite water with impurity content of 2-3ppm; the refined mirabilite water is input into a continuous crystallization process system to subject to continuous solid-liquid separation by a two-level centrifugal machine to obtain crystalline mirabilite containing 0.3-0.5%wt of free water; then, 0.175-1.3%wt of flavouring agent (calculated based on dry basis mirabilite) is added into the obtained crystalline mirabilite; the flavouring agent is edible alcohol solution with concentration of 70-80%wt; after blending, the flavouring agent is uniformly attached to the surface of the crystalline mirabilite; by the action of volatilization of the edible alcohol, the mirabilite crystals containing 0.1-0.2wt% of free water are formed, wherein the recovery system of the edible alcohol performs the condensation recovery at the temperature of 0-1 DEG C of cold water; and finally, the medicinal mirabilite conforming to the Chinese pharmacopoeia is obtained.
Description
Affiliated technical field:
The invention belongs to the fine chemical process field.
Background technology:
Sal glauberi is exactly a Natrii Sulfas, Natrii Sulfas (Na
2SO
410H
2O), English name: hydrous Thenardite.Contain water of crystallization 55.9%wt, sodium sulfate 44.1%wt.Minal contains Na
2O 19.3%wt, SO
324.8%wt.Monoclinic system usually in pelletized form, bulk, also has the cot of being shape or by membranaceous.Water white transparency, impurity is dyed ash, grayish green, yellowish, milky white, black etc. with it.Glassy lustre.Streak white.Hardness 1.5～2.0.Proportion 1.48.Little bitter saline taste is arranged.In the time of 100 ℃, lose water of crystallization.Dehydration and change the white powder thenardite into gradually in dry air, the existing buff of flame during burning.Water-soluble and glycerol and be insoluble to ethanol.And anhydrous sodium sulfate also claims not have liquid glauber salt, thenardite, Matrii Sulfas Exsiccatus; White particulate crystallization or powder, soluble in water, hygroscopicity is arranged, odorless, nontoxic, medicinal glauber salt mainly is to apply to field of medicaments with crystalline form.
The character of medicinal glauber salt:
Product character: medicinal glauber salt (Na
2SO
410H
2O) be prism-shaped, rectangle or irregular bulk and granular.Water white transparency or off-white color are translucent.Matter is crisp, frangible.Section is hyaloid gloss.Odorless, salty in the mouth.
Product function with cure mainly:
1, product function and curing mainly: purging heat to relax the bowels, moistening for dryness and softening hard mass, the detumescence of relieving inflammation or internal heat.Be used for the excess-heat constipation, constipation due to dry stool, stagnant stomachache, external treatment mastalgia, swelling and pain of hemorrhoid.
2. external hot compress, antiinflammatory go to swell.
3. quality index: medicinal glauber salt (smart nitre) national standard:
In Chinese patent CN101041444A, introduced the method for separating Natrii Sulfas (sodium sulfate) with the saline solution freezing and crystallizing, it processes finished product through overregulating pH value, pre-cooling, crystallization control temperature at 0-10 ℃, separation, recrystallize.The technological process that this method adopts is actually processes the Natrii Sulfas that contains water of crystallization with glass gall earlier, and then removes the free water in the Natrii Sulfas, obtains containing the Natrii Sulfas technological process of production of water of crystallization at last; Adopt this process manufacturing to contain its energy consumption height of Natrii Sulfas of water of crystallization, Natrii Sulfas purity is not high yet, is unfavorable for large-scale production simultaneously.
In Chinese patent numbers 97116654.4, introduce the production method that a kind of freezing and crystallizing production contains the Natrii Sulfas of water of crystallization; Its through dehalogenation, concentrate, technological processes such as beach solarization, collection, remove impurity, this method mainly adopts the method for cooling concentration, dry in the sun, and 18 ℃ of temperature controls in hot day; Winter-spring season is controlled at 10 ℃; Its objective is that such one-step method crystallization manufacturing contains the Natrii Sulfas of water of crystallization, still, the Natrii Sulfas purity that produces like this is not high; And unfavorable factor such as the place of need gathering is big, the probability that wants to produce per year few hundred thousand tonnes of simultaneously is very little.
In Chinese patent numbers 2008100446515, introduced a kind of manufacturing approach of special mirabilite with high purity; It has adopted the method for physics and chemistry to handle the glass gall that contains various impurity; With the method for refining purification glass gall among the present invention bigger difference is arranged; In order to improve the efficient of processing, the present invention does not need the glass gall depositing reservoir, directly removes by filter mechanical admixture.Adopt flocculating agent and precipitant rapidly deposition of the metallic compounds such as calcium magnesium in the glass gall and clarification to be removed simultaneously.
Because medicinal glauber salt mainly is to be used to treat constipation patient; Or before the digestive tract corrective surgery, or before the colonoscopy for the patient cleans the medicine of intestinal, and the mouthfeel characteristics of Natrii Sulfas have stronger salty and bitter flavor; Feel after making the patient oral that saline taste is too dense; The precedent that in medicinal glauber salt, adds flavoring agent is not also arranged simultaneously at present both at home and abroad, the objective of the invention is to alleviate the sensation of patient for this reason, thereby reach the purpose of treatment the salty and bitter flavor of Natrii Sulfas.
Summary of the invention:
The objective of the invention is to study a kind of manufacturing process that contains the flavoring agent medicinal glauber salt, make its shortcoming that can overcome existing medicinal glauber salt production technology, conduct heat, mass-transfer efficiency is high, energy consumption is low, helps the production of scale; Overcome in the Natrii Sulfas technological process of production shortcomings such as storage facilities is too much, the technological process of production is shortened.
The manufacturing process that contains the flavoring agent medicinal glauber salt; Filter is removed mechanical admixture through the triode road, six grades of refining purification process of ion exchanges obtain the smart glass gall that impurity metal ion content is 2～3ppm/L with 20 ° of former glass galls of Be ' of delivered downhole under the regulation and control of the monitoring of DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer; Import continuous crystallisation by cooling process system; After the first-stage centrifugal machine carries out continuous solid-liquid separation; Add flavoring agent, use therein flavoring agent is sucralose, fructose, sucrose, glucose, maltose, lactose; Its flavoring agent concentration is the edible alcohol solution of 70-80%wt, and its edible ethanol concentration is 95%v/v; Through the mix stirring and evenly mixing, edible ethanol is fully removed from the volatilization of crystal sodium sulfate surface, and edible ethanol is recycled the pharmaceutical grade Natrii Sulfas that just obtains containing flavoring agent so again, its concrete manufacturing process is following:
1 under the regulation and control of the monitoring of DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer under mine the technological process pipeline of the former glass gall of output through the triode road filter remove mechanical admixture; Wherein remove the above mechanical admixture of 0.5mm, remove the above mechanical admixture of 0.01mm, remove the above mechanical admixture of 0.1um through triode road filter through secondary piping filter through elementary piping filter;
2 under the regulation and control of the monitoring of DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer with 1) glass gall after handling; Handle heavy metal ion such as calcium, magnesium, chloride ion and the ferrum removed in the glass gall, arsenic, lead, cadmium, antimony through six grades of ion exchangers; Making its arsenic, lead, cadmium, the total content of antimony metal ion in glass gall is 2～3ppm/L, thereby obtains purified Natrii Sulfas water; Wherein ion exchanger is to be directly installed on the pipeline of technological process; Have six grades of ion exchangers, i.e. one-level cation exchanger → secondary cation exchanger → one-level anion exchanger → secondary anion exchanger → three grade cation exchanger → level Four cation exchanger;
3 under the regulation and control of the monitoring of DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer with 2) smart glass gall behind the refining purification pumps into the continuous crystallization system; The cold water of smart therein glass gall and 0～1 ℃ carries out heat exchange, forms supersaturated solution---the magma that contains the 21-22%wt sodium sulfate crystal; Magma is from the bottom input of crystallizer; In crystallizer, grow up to 0.3～0.4mm through crystal under the regulation and control of control in-line viscometer; Thereby form the magma of 42～43%wt; Then magma is imported the stiff device, the saturated solution clear liquid of contains sodium sulfate Returning heat-exchanger is again further participated in the circulation cooling, has so just realized the continuous crystallisation technology of medical Natrii Sulfas;
4 under the regulation and control of the monitoring of DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer with 3) obtain the magma input stiff device of 42～43%wt; Continue to make the Natrii Sulfas crystal concentration in the magma mixed liquor to increase therein to 60～61%wt; Its clear liquid returns mine to be continued to use from the top of stiff device, and the crystalline mixed liquor input of the high concentration Natrii Sulfas first-stage centrifugal machine that forms at the stiff device dewaters;
5 under the regulation and control of the monitoring of DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer with 4) the high concentration Natrii Sulfas crystal mixed liquor input first-stage centrifugal machine continuous dehydration technological process that obtains; After the magma mixed liquor of high concentration dewaters through the first-stage centrifugal machine; Formation contains the Natrii Sulfas crystal of Free water 0.3～0.5%wt; Add flavoring agent then,, edible ethanol is fully removed from the volatilization of crystal sodium sulfate surface again through mix stirring and evenly mixing 30min; So just obtain the pharmaceutical grade Natrii Sulfas that contains Free water 0.1～0.2%wt and contain 0.175-1.3%wt flavoring agent (in butt sodium sulfate), simultaneously with the edible ethanol recycling that evaporates;
The manufacturing process that contains the flavoring agent medicinal glauber salt of the present invention has following characteristics:
1, it is few to stick to the Natrii Sulfas crystal of inwall, crystallizer inwall of heat exchanger, has reduced clearance time.Heat transfer efficiency is high, reaches to control nitre liquid degree of supersaturation well, and the crystal size of generation is big and evenly, crystallization is produced high efficiency continuously and improved production efficiency.
2, adopt the regulation and control of AK fluid balance effusion meter and in-line viscometer, the volume flow of the former glass gall of regulating and controlling, refining glass gall.
3, the sodium sulfate concentration of former glass gall is controlled in the regulation and control of the monitoring of employing DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer.
4, adopt crystallizer within the very short time, to grow up to 0.5-1.2mm by the time crystal.
5, adopt crystal stiff device within the very short time, to make magma concentration bring up to 50-80%wt,
6, adopt serialization centrifuge dehydration technology, improve the production capacity of medicinal glauber salt.
7, flavoring agent not only adopts empty calory or sweeting agent low in calories to cover the sensation of patient to the salty and bitter flavor of Natrii Sulfas, at utmost improves the Natrii Sulfas mouthfeel.Especially the Natrii Sulfas that contains sucralose is suitable for diabetics, obesity patient, cardiovascular disease patient use.
8, containing the flavoring agent medicinal glauber salt and be applicable to the treatment constipation patient, is the good medicine of curative effect of intestinal tract cleaning before operation on digestive tract and the colonoscopy simultaneously.
9, flavoring agent concentration is the edible alcohol solution of 70-80%wt, and its edible ethanol concentration is 95%v/v, and wherein the recovery system of edible ethanol adopts 0～1 ℃ cold water to carry out condensing and recycling.Wherein why higher the concentration of the concentration of flavoring agent is, its objective is the use amount that reduces edible ethanol, reduces the cost recovery of edible ethanol simultaneously.
The present invention adopts the purpose of piping filter, removes former glass gall Sedimentation tank on the one hand, has also shortened technological process on the other hand, has reduced production and operation cost.
The present invention adopts the purpose of ion exchanger; Make on the one hand that the various metal ion contents except that sodium ion drop to minimum in the refining sodium sulphate water; Be not add the additive that heavy metal ion such as removing calcium, magnesium plasma and ferrum, arsenic, lead, cadmium, antimony is used on the other hand; Cut operating costs, the 50%wt of technological process before technological process simultaneously shortens to, and reduce nearly 10 covers of various ultra-large type storage tanks.
Adopt crystallizer, enhance productivity on the one hand, reduce energy resource consumption on the other hand.Because in the continuous crystallisation system, must make unexpectedly temperature remain on 8-10 ℃ with mixed liquor, only in this way just can make the crystalline concentration of Natrii Sulfas remain on stable status, help the crystallization of Natrii Sulfas saturated solution.
The present invention breaks the mode of production of medicinal glauber salt in the past fully; Employing contains the manufacturing process flow of flavoring agent Natrii Sulfas; Through the monitoring of employing DCS Automatic monitoring systems and the technological processes such as regulator control system, filter pipeline system, ion exchange system, continuous crystallisation system and continuous centrifugal dewatering system of AK fluid balance effusion meter and in-line viscometer; Not only improve the production capacity of medicinal glauber salt but also shortened the technological process of production of medicinal glauber salt; Also improve the product purity of medicinal glauber salt simultaneously, reduce production and operation cost.
Because medicinal glauber salt mainly is to be used to treat constipation patient; Or before the digestive tract corrective surgery; Or before the colonoscopy for the patient cleans the medicine of intestinal, and the mouthfeel characteristics of Natrii Sulfas have stronger salty and bitter flavor, feel that saline taste is too dense after making the patient oral; The objective of the invention is to alleviate the sensation of patient for this reason, thereby reach the purpose of treatment the salty and bitter flavor of Natrii Sulfas.
The manufacturing process that contains the flavoring agent medicinal glauber salt of the present invention; Be that filter is removed mechanical admixture through the triode road, six grades of refining purification process of ion exchangers obtain the smart glass gall that impurity content is 2～3ppm/L with 20 ° of former glass galls of Be ' concentration of delivered downhole under the regulation and control of the monitoring of DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer; Input contains the flavoring agent process system; Equipment such as heat exchanger, crystallizer and stiff device are arranged in containing the flavoring agent system; Refining glass gall carries out heat exchange with 0～1 ℃ cold water in heat exchanger, form supersaturated solution---the magma that contains 20～22%wt sodium sulfate crystal; Magma is from the bottom input of crystallizer; Crystal is grown up in crystallizer to 0.5～1.2mm; Thereby form the magma of 42～43%wt; Then magma is imported the stiff device, the saturated solution clear liquid of contains sodium sulfate Returning heat-exchanger is again further participated in the circulation cooling, has so just realized the continuous crystallization production technology of medical Natrii Sulfas; Then the magma of 42～43%wt is imported the stiff device; Continue to make Natrii Sulfas crystal concentration in the magma mixed liquor to increase therein to return mine from the top of stiff device to its clear liquid of 60～61%wt and continue to use, the crystalline mixed liquor input of the high concentration Natrii Sulfas first-stage centrifugal machine dehydration in that the stiff device forms forms the crystal Natrii Sulfas that contains Free water 0.3～0.5%wt; Add flavoring agent then; The flavoring agent that uses is the edible alcohol solution of 70-80%wt as one or more concentration of sucralose, fructose, sucrose, glucose, maltose, lactose, and its edible ethanol concentration is 95%v/v, and wherein the recovery system of edible ethanol adopts 0～1 ℃ cold water to carry out condensing and recycling.
Again through mix stirring and evenly mixing 30min; Edible ethanol is fully removed from the volatilization of crystal sodium sulfate surface; So just obtain the pharmaceutical grade Natrii Sulfas that contains Free water 0.1～0.2%wt and contain 0.175-1.3%wt flavoring agent (in butt sodium sulfate), simultaneously with the edible ethanol recycling that evaporates, flavoring agent concentration is the edible alcohol solution of 70-80%wt; Its edible ethanol concentration is 95%v/v, and wherein the recovery system of edible ethanol adopts 0～1 ℃ cold water to carry out condensing and recycling; The medicinal glauber salt that will contain flavoring agent at last, input automatic packaging system packs, puts in storage.
The DCS system is the english abbreviation of project scattered control system, is a kind of " mixed function type " control system of controlling the field, can realize real-time tasks such as data acquisition, process control, sequential control.Why being called " mixed function type " control system, is because system is when carrying out functional design, removes to have kept powerful analog quantity processing and the circuit controls function of conventional DCS system, also has quick logic control function and higher system real time performance concurrently.
Description of drawings:
Accompanying drawing 1 is process flow diagram of the present invention.
The specific embodiment
Do further to detail in the face of technology of the present invention down.
Embodiment 1:
Be that filter is removed mechanical admixture through the triode road, six grades of refining purification process of ion exchangers obtain the smart glass gall that impurity content is 2ppm with 20 ° of former glass galls of Be ' concentration of delivered downhole under the regulation and control of the monitoring of DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer; Input contains the flavoring agent process system; Equipment such as heat exchanger, crystallizer and stiff device are arranged in containing the flavoring agent system; Refining glass gall carries out heat exchange with 0 ℃ cold water in heat exchanger, form supersaturated solution---the magma that contains the 22%wt sodium sulfate crystal; Magma is from the bottom input of crystallizer, and crystal is grown up to 1.2mm in crystallizer, thereby forms the magma of 43%wt; Then magma is imported the stiff device; The saturated solution clear liquid of contains sodium sulfate Returning heat-exchanger is again further participated in the circulation cooling, has so just realized the continuous crystallization production technology of medical Natrii Sulfas, then the magma of 43%wt is imported the stiff device; Continue to make Natrii Sulfas crystal concentration in the magma mixed liquor to increase therein to return mine from the top of stiff device and continue to use to its clear liquid of 61%wt; The crystalline mixed liquor input of high concentration Natrii Sulfas first-stage centrifugal machine dehydration in that the stiff device forms forms the crystal Natrii Sulfas that contains Free water 0.5%wt, and the concentration that adds flavoring agent (flavoring agent is a sucralose) then is the edible alcohol solution of 70%wt; Again through mix stirring and evenly mixing 30min; Edible ethanol is fully removed from the surface volatilization of crystal sodium sulfate, so just obtain the pharmaceutical grade Natrii Sulfas that contains Free water 0.2%wt and contain 1.3%wt flavoring agent (in butt sodium sulfate), simultaneously with the edible ethanol recycling that evaporates; The medicinal glauber salt that will contain flavoring agent at last, input automatic packaging system packs, checks, puts in storage, sells.Wherein flavoring agent concentration is the edible alcohol solution of 70%wt, and its edible ethanol concentration is 95%v/v, and wherein the recovery system of edible ethanol adopts 0 ℃ cold water to carry out condensing and recycling.Obtaining medicinal glauber salt detects various data and sees table 1.
Embodiment 2:
Be that filter is removed mechanical admixture through the triode road, six grades of refining purification process of ion exchangers obtain the smart glass gall that impurity content is 3ppm with 20 ° of former glass galls of Be ' concentration of delivered downhole under the regulation and control of the monitoring of DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer; Input contains the flavoring agent process system; Equipment such as heat exchanger, crystallizer and stiff device are arranged in containing the flavoring agent system; Refining glass gall carries out heat exchange with 1 ℃ cold water in heat exchanger, form supersaturated solution---the magma that contains 20～22%wt sodium sulfate crystal; Magma is from the bottom input of crystallizer; Crystal is grown up in crystallizer to 0.5mm; Thereby form the magma of 42～43%wt, then magma is imported the stiff device, the saturated solution clear liquid of contains sodium sulfate Returning heat-exchanger is again further participated in the circulation cooling; So just realized the continuous crystallization production technology of medical Natrii Sulfas; Then with the magma of 42%wt input stiff device, continue to make Natrii Sulfas crystal concentration in the magma mixed liquor to increase therein to return mine from the top of stiff device and continue to use, the crystalline mixed liquor input of the high concentration Natrii Sulfas first-stage centrifugal machine dehydration that forms at the stiff device to its clear liquid of 60%wt; Formation contains the crystal Natrii Sulfas of Free water 0.3%wt; The concentration that adds flavoring agent (flavoring agent is the equal equivalent of sucralose, fructose, sucrose, glucose, maltose, lactose) mixture then is the edible alcohol solution of 80%wt, again through mix stirring and evenly mixing 30min, edible ethanol is fully removed from the volatilization of crystal sodium sulfate surface; So just obtain the pharmaceutical grade Natrii Sulfas that contains Free water 0.1%wt and contain 0.175%wt flavoring agent (in butt sodium sulfate); With the edible ethanol recycling that evaporates, will contain the medicinal glauber salt of flavoring agent at last simultaneously, input automatic packaging system packs, checks, puts in storage, sells.Wherein flavoring agent concentration is the edible alcohol solution of 80%wt, and its edible ethanol concentration is 95%v/v, and wherein the recovery system of edible ethanol is adopted 1 ℃ cold water and carried out condensing and recycling.Obtain medicinal glauber salt detection data and see table 1.
Embodiment 3:
Be that filter is removed mechanical admixture through the triode road, six grades of refining purification process of ion exchangers obtain the smart glass gall that impurity content is 2.6ppm with 20 ° of former glass galls of Be ' concentration of delivered downhole under the regulation and control of the monitoring of DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer; Input contains the flavoring agent process system; Equipment such as heat exchanger, crystallizer and stiff device are arranged in containing the flavoring agent system; Refining glass gall carries out heat exchange with 0.2 ℃ cold water in heat exchanger, form supersaturated solution---the magma that contains the 20.5%wt sodium sulfate crystal; Magma is from the bottom input of crystallizer; Crystal is grown up in crystallizer to 0.7mm; Thereby form the magma of 42.2%wt, then magma is imported the stiff device, the saturated solution clear liquid of contains sodium sulfate Returning heat-exchanger is again further participated in the circulation cooling; So just realized the continuous crystallization production technology of medical Natrii Sulfas; Then with the magma of 42.2%wt input stiff device, continue to make Natrii Sulfas crystal concentration in the magma mixed liquor to increase therein to return mine from the top of stiff device and continue to use, the crystalline mixed liquor input of the high concentration Natrii Sulfas first-stage centrifugal machine dehydration that forms at the stiff device to its clear liquid of 60.3%wt; Formation contains the crystal Natrii Sulfas of Free water 0.4%wt; The concentration that adds flavoring agent (flavoring agent is the equal equivalent mixture of sucralose, fructose, sucrose, glucose) then is the edible alcohol solution of 70-80%wt, again through mix stirring and evenly mixing 30min, edible ethanol is fully removed from the volatilization of crystal sodium sulfate surface; So just obtain the pharmaceutical grade Natrii Sulfas that contains Free water 0.12%wt and contain 0.25%wt flavoring agent (in butt sodium sulfate); With the edible ethanol recycling that evaporates, will contain the medicinal glauber salt of flavoring agent at last simultaneously, input automatic packaging system packs, checks, puts in storage, sells.Wherein flavoring agent concentration is the edible alcohol solution of 72%wt, and its edible ethanol concentration is 95%v/v, and wherein the recovery system of edible ethanol adopts 0.3 ℃ cold water to carry out condensing and recycling.Obtain medicinal glauber salt detection data and see table 1.
Embodiment 4:
Be that filter is removed mechanical admixture through the triode road, six grades of refining purification process of ion exchangers obtain the smart glass gall that impurity content is 2.5ppm with 20 ° of former glass galls of Be ' concentration of delivered downhole under the regulation and control of the monitoring of DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer; Input contains the flavoring agent process system; Equipment such as heat exchanger, crystallizer and stiff device are arranged in containing the flavoring agent system; Refining glass gall carries out heat exchange with 0.4 ℃ cold water in heat exchanger, form supersaturated solution---the magma that contains the 20.8%wt sodium sulfate crystal; Magma is from the bottom input of crystallizer, and crystal is grown up to 0.9mm in crystallizer, thereby forms the magma of 42.6%wt; Then magma is imported the stiff device; The saturated solution clear liquid of contains sodium sulfate Returning heat-exchanger is again further participated in the circulation cooling, has so just realized the continuous crystallization production technology of medical Natrii Sulfas, then the magma of 42.6%wt is imported the stiff device; Continue to make Natrii Sulfas crystal concentration in the magma mixed liquor to increase therein to return mine from the top of stiff device and continue to use to its clear liquid of 60.5%wt; The crystalline mixed liquor input of high concentration Natrii Sulfas first-stage centrifugal machine dehydration in that the stiff device forms forms the crystal Natrii Sulfas that contains Free water 0.34%wt, adds the edible alcohol solution (composition is with embodiment 2) of flavoring agent then; Again through mix stirring and evenly mixing 30min; Edible ethanol is fully removed from the surface volatilization of crystal sodium sulfate, so just obtain the pharmaceutical grade Natrii Sulfas that contains Free water 0.13%wt and contain 0.4%wt flavoring agent (in butt sodium sulfate), simultaneously with the edible ethanol recycling that evaporates; The medicinal glauber salt that will contain flavoring agent at last, input automatic packaging system packs, checks, puts in storage, sells.Wherein flavoring agent concentration is the edible alcohol solution of 74%wt, and its edible ethanol concentration is 95%v/v, and wherein the recovery system of edible ethanol adopts 0.5 ℃ cold water to carry out condensing and recycling.Obtain medicinal glauber salt detection data and see table 1.
Embodiment 5:
Be that filter is removed mechanical admixture through the triode road, six grades of refining purification process of ion exchangers obtain the smart glass gall that impurity content is 2.3ppm with 20 ° of former glass galls of Be ' concentration of delivered downhole under the regulation and control of the monitoring of DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer; Input contains the flavoring agent process system; Equipment such as heat exchanger, crystallizer and stiff device are arranged in containing crystal system; Refining glass gall carries out heat exchange with 0.8 ℃ cold water in heat exchanger, form supersaturated solution---the magma that contains the 20.8%wt sodium sulfate crystal; Magma is from the bottom input of crystallizer, and crystal is grown up to 1.0mm in crystallizer, thereby forms the magma of 42.5%wt; Then magma is imported the stiff device; The saturated solution clear liquid of contains sodium sulfate Returning heat-exchanger is again further participated in the circulation cooling, has so just realized the continuous crystallization production technology of medical Natrii Sulfas, then the magma of 42.5%wt is imported the stiff device; Continue to make Natrii Sulfas crystal concentration in the magma mixed liquor to increase therein to return mine from the top of stiff device and continue to use to its clear liquid of 60.5%wt; The crystalline mixed liquor input of high concentration Natrii Sulfas first-stage centrifugal machine dehydration in that the stiff device forms forms the crystal Natrii Sulfas that contains Free water 0.45%wt, adds the edible alcohol solution (composition is with embodiment 1) of flavoring agent then; Again through mix stirring and evenly mixing 30min; Edible ethanol is fully removed from the surface volatilization of crystal sodium sulfate, so just obtain the pharmaceutical grade Natrii Sulfas that contains Free water 0.18%wt and contain 0.8%wt flavoring agent (in butt sodium sulfate), simultaneously with the edible ethanol recycling that evaporates; The medicinal glauber salt that will contain flavoring agent at last, input automatic packaging system packs, checks, puts in storage, sells.Wherein flavoring agent concentration is the edible alcohol solution of 76%wt, and its edible ethanol concentration is 95%v/v, and wherein the recovery system of edible ethanol adopts 0.7 ℃ cold water to carry out condensing and recycling.Obtain medicinal glauber salt detection data and see table 1.
Embodiment 6:
Be that filter is removed mechanical admixture through the triode road, six grades of refining purification process of ion exchangers obtain the smart glass gall that impurity content is 2.2ppm with 20 ° of former glass galls of Be ' concentration of delivered downhole under the regulation and control of the monitoring of DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer; Input contains the flavoring agent process system; Equipment such as heat exchanger, crystallizer and stiff device are arranged in containing the flavoring agent system; Refining glass gall carries out heat exchange with 0.6 ℃ cold water in heat exchanger, form supersaturated solution---the magma that contains the 21.8%wt sodium sulfate crystal; Magma is from the bottom input of crystallizer, and crystal is grown up to 0.9mm in crystallizer, thereby forms the magma of 42.8%wt; Then magma is imported the stiff device; The saturated solution clear liquid of contains sodium sulfate Returning heat-exchanger is again further participated in the circulation cooling, has so just realized the continuous crystallization production technology of medical Natrii Sulfas, then the magma of 42.8%wt is imported the stiff device; Continue to make Natrii Sulfas crystal concentration in the magma mixed liquor to increase therein to return mine from the top of stiff device and continue to use to its clear liquid of 60.9%wt; The crystalline mixed liquor input of high concentration Natrii Sulfas first-stage centrifugal machine dehydration in that the stiff device forms forms the crystal Natrii Sulfas that contains Free water 0.41%wt, adds the edible alcohol solution (composition is with embodiment 2) of flavoring agent then; Again through mix stirring and evenly mixing 30min; Edible ethanol is fully removed from the surface volatilization of crystal sodium sulfate, so just obtain the pharmaceutical grade Natrii Sulfas that contains Free water 0.17%wt and contain 1.2%wt flavoring agent (in butt sodium sulfate), simultaneously with the edible ethanol recycling that evaporates; The medicinal glauber salt that will contain flavoring agent at last, input automatic packaging system packs, checks, puts in storage, sells.Wherein flavoring agent concentration is the edible alcohol solution of 78%wt, and its edible ethanol concentration is 95%v/v, and wherein the recovery system of edible ethanol adopts 0.9 ℃ cold water to carry out condensing and recycling.Obtain medicinal glauber salt detection data and see table 1.
Table 1
Claims (4)
1. the manufacturing process that contains the flavoring agent medicinal glauber salt; Filter is removed mechanical admixture through the triode road, six grades of refining purification process of ion exchanges obtain the smart glass gall that impurity metal ion content is 2～3ppm with 20 ° of former glass galls of Be ' of delivered downhole under the regulation and control of the monitoring of DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer; Import continuous crystallisation by cooling process system, after the first-stage centrifugal machine carries out continuous solid-liquid separation, add flavoring agent; Again through the mix stirring and evenly mixing; Edible ethanol is fully removed from the volatilization of crystal sodium sulfate surface, obtain containing the pharmaceutical grade Natrii Sulfas of flavoring agent, its concrete manufacturing process is following:
1), under the regulation and control of the monitoring of DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer under mine the technological process pipeline of the former glass gall of output through the triode road filter remove mechanical admixture;
2), under the regulation and control of the monitoring of DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer with 1) glass gall after handling; Handle heavy metal ion such as calcium, magnesium, chlorine plasma and the ferrum removed in the glass gall, arsenic, lead, cadmium, antimony through six grades of ion exchangers; Making the total contents of metal ion in glass gall such as its arsenic, lead, cadmium, antimony is 2～3ppm, thereby obtains purified Natrii Sulfas water;
3), under the regulation and control of the monitoring of DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer with 2) smart glass gall behind the refining purification pumps into the continuous crystallization system; The cold water of smart therein glass gall and 0～1 ℃ carries out heat exchange, forms supersaturated solution---the magma that contains the 21-22%wt sodium sulfate crystal; Magma is from the bottom input of crystallizer; In crystallizer, grow up to 0.3～0.4mm through crystal under the regulation and control of control in-line viscometer; Thereby form the magma of 42～43%wt; Then magma is imported the stiff device, the saturated solution clear liquid of contains sodium sulfate Returning heat-exchanger is again further participated in the circulation cooling, has so just realized the continuous crystallisation technology of medical Natrii Sulfas;
4), under the regulation and control of the monitoring of DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer with 3) obtain the magma input stiff device of 42～43%wt; Continue to make the Natrii Sulfas crystal concentration in the magma mixed liquor to increase therein to 60～61%wt; Its clear liquid returns mine to be continued to use from the top of stiff device, and the crystalline mixed liquor input of the high concentration Natrii Sulfas first-stage centrifugal machine that forms at the stiff device dewaters;
5), under the regulation and control of the monitoring of DCS Automatic monitoring systems and AK fluid balance effusion meter and in-line viscometer with 4) the high concentration Natrii Sulfas crystal mixed liquor input first-stage centrifugal machine continuous dehydration technological process that obtains; After the magma mixed liquor of high concentration dewaters through the first-stage centrifugal machine; Formation contains the Natrii Sulfas crystal of Free water 0.3～0.5%wt; Add flavoring agent then,, edible ethanol is fully removed from the volatilization of crystal sodium sulfate surface again through mix stirring and evenly mixing 30min; So just obtain the pharmaceutical grade Natrii Sulfas that contains Free water 0.1～0.2%wt and contain the 0.175-1.3%wt flavoring agent, simultaneously with the edible ethanol recycling that evaporates.
2. according to the said manufacturing process that contains the flavoring agent medicinal glauber salt of claim 1; It is characterized in that; The filter pipeline system that adopts is a triode road filter; Remove the above mechanical admixture of 0.5mm through elementary piping filter, remove the above mechanical admixture of 0.01mm, remove the above mechanical admixture of 0.1um through triode road filter through secondary piping filter.
3. according to the said manufacturing process that contains the flavoring agent medicinal glauber salt of claim 1; It is characterized in that; The said ion exchanger that is used for is the pipeline that is directly installed on technological process; Have six grades of ion exchangers, i.e. one-level cation exchanger → secondary cation exchanger → one-level anion exchanger → secondary anion exchanger → three grade cation exchanger → level Four cation exchanger.
4. according to the said manufacturing process that contains the flavoring agent medicinal glauber salt of claim 1; It is characterized in that employed flavoring agent is that one or more concentration of sucralose, fructose, sucrose, glucose, maltose, lactose is the edible alcohol solution of 70-80%wt; Its edible ethanol concentration is 95%v/v, and wherein the recovery system of edible ethanol adopts 0～1 ℃ cold water to carry out condensing and recycling.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109574307A (en) * | 2018-12-16 | 2019-04-05 | 金科环境股份有限公司 | Remove the device of whole hardness in reverse osmosis concentrated water |
| CN109592816A (en) * | 2018-12-16 | 2019-04-09 | 金科环境股份有限公司 | Eliminate the device and method of reverse osmosis concentrated water permanent hardness and temporary hardness |
| CN109592815A (en) * | 2018-12-16 | 2019-04-09 | 金科环境股份有限公司 | The processing system of reverse osmosis concentrated water with high permanent hardness |
| CN109592814A (en) * | 2018-12-16 | 2019-04-09 | 金科环境股份有限公司 | The processing unit and method of strong brine containing high-concentration sulfuric acid calcium |
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| CN101830487A (en) * | 2010-05-20 | 2010-09-15 | 四川省川眉芒硝有限责任公司 | Process for manufacturing sodium sulfate for continuously crystallized medicament |
| CN101830486A (en) * | 2010-05-20 | 2010-09-15 | 四川川眉特种芒硝有限公司 | Preparation process of ultrafine particle thenardite |
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| CN101830486A (en) * | 2010-05-20 | 2010-09-15 | 四川川眉特种芒硝有限公司 | Preparation process of ultrafine particle thenardite |
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Cited By (4)
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| CN109574307A (en) * | 2018-12-16 | 2019-04-05 | 金科环境股份有限公司 | Remove the device of whole hardness in reverse osmosis concentrated water |
| CN109592816A (en) * | 2018-12-16 | 2019-04-09 | 金科环境股份有限公司 | Eliminate the device and method of reverse osmosis concentrated water permanent hardness and temporary hardness |
| CN109592815A (en) * | 2018-12-16 | 2019-04-09 | 金科环境股份有限公司 | The processing system of reverse osmosis concentrated water with high permanent hardness |
| CN109592814A (en) * | 2018-12-16 | 2019-04-09 | 金科环境股份有限公司 | The processing unit and method of strong brine containing high-concentration sulfuric acid calcium |
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